#------------------------------------------------------------------------------ #$Date: 2026-05-29 00:31:41 +0100 (Fri, 29 May 2026) $ #$Revision: 306115 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/73/1577310.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1577310 loop_ _publ_author_name 'Fidelius, Jannis' 'Taube, Clemens' 'Schwedtmann, Kai' 'Hennersdorf, Felix' 'Gomila, Rosa Maria' 'Frontera, Antonio' 'Wolf, Robert' 'Weigand, Jan J.' _publ_section_title ; Imidazoliumyl-Substituted Di-and Iso-Tetraphosphanes and Their Metal-Mediated Fragmentation Reactions ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC02577C _journal_year 2026 _chemical_formula_moiety 'C28 H51 N4 P, 2(C F3 O3 S), C2 H3 N' _chemical_formula_sum 'C32 H54 F6 N5 O6 P S2' _chemical_formula_weight 813.89 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2019-01-21 _audit_creation_method ; Olex2 1.2 (compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103) ; _audit_update_record ; 2026-01-21 deposited with the CCDC. 2026-05-28 downloaded from the CCDC. ; _cell_angle_alpha 88.986(5) _cell_angle_beta 73.486(5) _cell_angle_gamma 62.793(5) _cell_formula_units_Z 2 _cell_length_a 11.1951(5) _cell_length_b 11.9364(7) _cell_length_c 17.3601(11) _cell_measurement_reflns_used 6075 _cell_measurement_temperature 100.01(10) _cell_measurement_theta_max 76.0920 _cell_measurement_theta_min 2.6740 _cell_volume 1960.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2850 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -63.00 32.00 0.50 4.00 -- -38.50 57.00 -30.00 190 2 \w 24.00 73.00 0.50 4.00 -- 42.50-125.00-150.00 98 3 \w 54.00 133.00 0.50 16.00 -- 111.00 -61.00-120.00 158 4 \w 93.00 121.00 0.50 16.00 -- 111.00-125.00-120.00 56 5 \w 56.00 92.00 0.50 16.00 -- 111.00-125.00-120.00 72 6 \w 42.00 98.00 0.50 16.00 -- 111.00-125.00 -60.00 112 7 \w 89.00 120.00 0.50 16.00 -- 111.00-125.00 30.00 62 8 \w 78.00 120.00 0.50 16.00 -- 111.00-125.00 120.00 84 9 \w 59.00 108.00 0.50 16.00 -- 111.00 -94.00 120.00 98 10 \w 83.00 154.00 0.50 16.00 -- 111.00 -15.00 90.00 142 11 \w 126.00 167.00 0.50 16.00 -- 111.00 61.00 60.00 82 12 \w 134.00 177.00 0.50 16.00 -- 111.00 125.00 -30.00 86 13 \w 98.00 125.00 0.50 16.00 -- 111.00 125.00-180.00 54 14 \w 84.00 177.00 0.50 16.00 -- 111.00 61.00-180.00 186 15 \w 88.00 116.00 0.50 16.00 -- 111.00 -30.00-120.00 56 16 \w 41.00 92.00 0.50 4.00 -- 42.50-125.00 30.00 102 17 \w 40.00 114.00 0.50 16.00 -- 111.00-125.00 60.00 148 18 \w 41.00 142.00 0.50 16.00 -- 111.00 -77.00 30.00 202 19 \w 83.00 161.00 0.50 16.00 -- 111.00 61.00 90.00 156 20 \w 95.00 123.00 0.50 16.00 -- 111.00 61.00 60.00 56 21 \w 85.00 169.00 0.50 16.00 -- 111.00 61.00 120.00 168 22 \w 86.00 161.00 0.50 16.00 -- 111.00 61.00 150.00 150 23 \w 39.00 87.00 0.50 16.00 -- 111.00 -30.00-120.00 96 24 \w 39.00 121.00 0.50 16.00 -- 111.00-123.00 -86.58 164 25 \w -109.00 -12.00 0.50 4.00 -- -38.50 -57.00 60.00 194 26 \w -107.00 -15.00 0.50 4.00 -- -38.50 -57.00-180.00 184 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0711412000 _diffrn_orient_matrix_UB_12 -0.1163242000 _diffrn_orient_matrix_UB_13 0.0418884000 _diffrn_orient_matrix_UB_21 0.0212379000 _diffrn_orient_matrix_UB_22 -0.0885664000 _diffrn_orient_matrix_UB_23 -0.0717332000 _diffrn_orient_matrix_UB_31 0.1448605000 _diffrn_orient_matrix_UB_32 -0.0074843000 _diffrn_orient_matrix_UB_33 -0.0426396000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_unetI/netI 0.0511 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 19200 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.124 _diffrn_reflns_theta_min 2.678 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 2.286 _exptl_absorpt_correction_T_max 0.954 _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.378 _exptl_crystal_description needle _exptl_crystal_F_000 860 _exptl_crystal_size_max 0.266 _exptl_crystal_size_mid 0.045 _exptl_crystal_size_min 0.024 _refine_diff_density_max 1.067 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.080 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 757 _refine_ls_number_reflns 7718 _refine_ls_number_restraints 1374 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.0843 _refine_ls_R_factor_gt 0.0703 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1282P)^2^+0.9548P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1909 _refine_ls_wR_factor_ref 0.2070 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6205 _reflns_number_total 7718 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc02577c2.cif _cod_data_source_block jjw1021 _cod_database_code 1577310 _chemical_oxdiff_formula C32H54F6N5O6PS2 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _reflns_odcompleteness_completeness 99.95 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 71.98 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances H18-H23A -2 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints C23A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C23B \\sim C24B \\sim C25B \\sim C26B \\sim C27B \\sim C28B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 S2C \\sim F4C \\sim F5C \\sim F6C \\sim O4C \\sim O5C \\sim O6C \\sim C30C \\sim S2B \\sim F4B \\sim F5B \\sim F6B \\sim O4B \\sim O5B \\sim O6B \\sim C30B \\sim S2A \\sim F4A \\sim F5A \\sim F6A \\sim O4A \\sim O5A \\sim O6A \\sim C30A: within 2.5A with sigma of 0.01 and sigma for terminal atoms of 0.02 S1B \\sim F1B \\sim F2B \\sim F3B \\sim O1B \\sim O2B \\sim O3B \\sim C29B \\sim S1A \\sim F1A \\sim F2A \\sim F3A \\sim O1A \\sim O2A \\sim O3A \\sim C29A: within 2A with sigma of 0.03 and sigma for terminal atoms of 0.06 4. Same fragment restrains {C23B, C24B, C25B, C26B, C27B, C28B} sigma for 1-2: 0.02, 1-3: 0.02 as {C23A, C24A, C25A, C26A, C27A, C28A} {S1B, F1B, F2B, F3B, O1B, O2B, O3B, C29B} sigma for 1-2: 0.02, 1-3: 0.02 as {S1A, F1A, F2A, F3A, O1A, O2A, O3A, C29A} {S2B, F6B, F5B, F4B, O4B, O5B, O6B, C30B} sigma for 1-2: 0.02, 1-3: 0.02 {S2C, F5C, F4C, F6C, O4C, O5C, O6C, C30C} sigma for 1-2: 0.02, 1-3: 0.02 as {S2A, F4A, F5A, F6A, O4A, O5A, O6A, C30A} 5. Others 1*[Sof(S2A)+Sof(F4A)+Sof(F5A)+Sof(F6A)+Sof(O4A)+Sof(O5A)+Sof(O6A)+Sof(C30A)]+ 1*[Sof(S2B)+Sof(F6B)+Sof(F5B)+Sof(F4B)+Sof(O4B)+Sof(O5B)+Sof(O6B)+Sof(C30B)]+1* [Sof(S2C)+Sof(F5C)+Sof(F4C)+Sof(F6C)+Sof(O4C)+Sof(O5C)+Sof(O6C)+Sof(C30C)]=1 with esd of 0 Sof(S1B)=Sof(F1B)=Sof(F2B)=Sof(F3B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(C29B)=1- FVAR(1) Sof(S1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(C29A)= FVAR(1) Sof(S2A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C30A)= FVAR(2) Sof(S2B)=Sof(F6B)=Sof(F5B)=Sof(F4B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(C30B)= FVAR(3) Sof(S2C)=Sof(F5C)=Sof(F4C)=Sof(F6C)=Sof(O4C)=Sof(O5C)=Sof(O6C)=Sof(C30C)= FVAR(4) Sof(C23B)=Sof(H23B)=Sof(C24B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25C)= Sof(H25D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=Sof(C27B)=Sof(H27C)=Sof(H27D)= Sof(C28B)=Sof(H28C)=Sof(H28D)=1-FVAR(5) Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)= Sof(H25B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(C27A)=Sof(H27A)=Sof(H27B)= Sof(C28A)=Sof(H28A)=Sof(H28B)=FVAR(5) 6.a Ternary CH refined with riding coordinates: C4(H4), C7(H7), C15(H15), C18(H18), C23A(H23A), C23B(H23B) 6.b Secondary CH2 refined with riding coordinates: C24A(H24A,H24B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,H27B), C28A(H28A, H28B), C24B(H24C,H24D), C25B(H25C,H25D), C26B(H26C,H26D), C27B(H27C,H27D), C28B(H28C,H28D) 6.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B, H22C), C32(H32A,H32B,H32C) ; _shelx_res_file ; jjw1021.res created by SHELXL-2014/7 TITL jjw1021_a.res in P-1 REM Old TITL jjw1021 in P-1 #2 REM SHELXT solution in P-1 REM R1 0.238, Rweak 0.023, Alpha 0.070, Orientation as input REM Formula found by SHELXT: C41 N11 O S CELL 1.54184 11.195135 11.936404 17.360095 88.9857 73.4858 62.793 ZERR 2 0.000492 0.000681 0.001059 0.0048 0.0046 0.0051 LATT 1 SFAC C H F N O P S UNIT 64 108 12 10 12 2 4 DFIX -2 H18 H23A SIMU 0.01 0.02 2 C23A > C28B SIMU 0.01 0.02 2.5 S2C F4C F5C F6C > S2B F4B F5B F6B O4B > C30B S2A > C30A SIMU 0.03 0.06 2 S1B > C29A SUMP 1 0 1 3 1 4 1 5 L.S. 10 PLAN 20 BOND $H LIST 6 MORE -1 CONF fmap 2 TEMP 100 acta REM REM REM WGHT 0.128200 0.954800 FVAR 4.74239 0.64843 0.65263 0.19266 0.15471 0.34859 P1 6 0.669563 0.346425 0.773148 11.00000 0.03663 0.03973 = 0.02885 -0.00017 -0.00266 -0.02504 N1 4 0.977296 0.210499 0.714279 11.00000 0.03659 0.03424 = 0.03009 0.00330 -0.00682 -0.02240 N2 4 0.880321 0.144982 0.819916 11.00000 0.05223 0.03958 = 0.03044 0.00611 -0.01050 -0.03138 N3 4 0.692741 0.549828 0.827988 11.00000 0.03926 0.03488 = 0.03152 0.00247 -0.00650 -0.02247 N4 4 0.667380 0.578276 0.708246 11.00000 0.03345 0.03777 = 0.03441 0.00510 -0.00478 -0.01684 C1 1 0.851585 0.233177 0.768201 11.00000 0.04412 0.03526 = 0.02863 0.00150 -0.00570 -0.02661 C2 1 1.024145 0.065274 0.797895 11.00000 0.05540 0.04308 = 0.03805 0.00884 -0.01980 -0.03030 C3 1 1.085472 0.107539 0.732366 11.00000 0.04457 0.04034 = 0.03809 0.00551 -0.01587 -0.02523 C4 1 0.770369 0.136215 0.889086 11.00000 0.06712 0.04772 = 0.02987 0.00722 -0.00541 -0.03850 AFIX 13 H4 2 0.678777 0.206766 0.890231 11.00000 -1.20000 AFIX 0 C5 1 0.763616 0.013053 0.876105 11.00000 0.10052 0.06977 = 0.05096 -0.00141 0.00676 -0.06665 AFIX 137 H5A 2 0.762482 0.000702 0.821876 11.00000 -1.50000 H5B 2 0.679315 0.018426 0.914063 11.00000 -1.50000 H5C 2 0.844812 -0.057250 0.884233 11.00000 -1.50000 AFIX 0 C6 1 0.793627 0.154326 0.969879 11.00000 0.08085 0.04917 = 0.03171 0.00698 -0.01019 -0.03189 AFIX 137 H6A 2 0.878276 0.082452 0.973046 11.00000 -1.50000 H6B 2 0.714508 0.161728 1.013856 11.00000 -1.50000 H6C 2 0.802659 0.230135 0.973314 11.00000 -1.50000 AFIX 0 C7 1 0.992324 0.285944 0.646513 11.00000 0.03483 0.03972 = 0.03055 0.00625 -0.00451 -0.02187 AFIX 13 H7 2 0.896992 0.340318 0.643479 11.00000 -1.20000 AFIX 0 C8 1 1.077842 0.201724 0.565304 11.00000 0.04799 0.05279 = 0.03180 0.00349 -0.00566 -0.02092 AFIX 137 H8A 2 1.176406 0.160805 0.560783 11.00000 -1.50000 H8B 2 1.062574 0.252755 0.522198 11.00000 -1.50000 H8C 2 1.048476 0.138503 0.561718 11.00000 -1.50000 AFIX 0 C9 1 1.047582 0.374446 0.665129 11.00000 0.05078 0.05158 = 0.05138 0.01176 -0.01053 -0.03635 AFIX 137 H9A 2 0.983857 0.430356 0.714300 11.00000 -1.50000 H9B 2 1.054426 0.423674 0.621327 11.00000 -1.50000 H9C 2 1.139241 0.325010 0.671476 11.00000 -1.50000 AFIX 0 C10 1 1.098339 -0.047666 0.836490 11.00000 0.07177 0.06354 = 0.06609 0.03228 -0.03731 -0.03990 AFIX 137 H10A 2 1.077719 -0.021990 0.892836 11.00000 -1.50000 H10B 2 1.198378 -0.085024 0.810156 11.00000 -1.50000 H10C 2 1.066761 -0.108806 0.831363 11.00000 -1.50000 AFIX 0 C11 1 1.238963 0.056574 0.688211 11.00000 0.04142 0.04747 = 0.05480 0.00814 -0.01815 -0.02246 AFIX 137 H11A 2 1.261746 0.009949 0.637083 11.00000 -1.50000 H11B 2 1.293368 0.001227 0.719976 11.00000 -1.50000 H11C 2 1.260623 0.125724 0.679140 11.00000 -1.50000 AFIX 0 C12 1 0.681341 0.496790 0.763894 11.00000 0.03206 0.03606 = 0.02969 0.00324 -0.00503 -0.01995 C13 1 0.688443 0.665523 0.812122 11.00000 0.04319 0.03581 = 0.04554 0.00466 -0.00706 -0.02309 C14 1 0.670607 0.683616 0.738474 11.00000 0.04246 0.03568 = 0.04688 0.00630 -0.00385 -0.01936 C15 1 0.704002 0.493864 0.904749 11.00000 0.05297 0.03970 = 0.03105 0.00455 -0.01042 -0.02989 AFIX 13 H15 2 0.684806 0.421807 0.903037 11.00000 -1.20000 AFIX 0 C16 1 0.590339 0.588347 0.978503 11.00000 0.05957 0.05569 = 0.03351 -0.00185 -0.00549 -0.03474 AFIX 137 H16A 2 0.614670 0.653036 0.988184 11.00000 -1.50000 H16B 2 0.584208 0.544488 1.025179 11.00000 -1.50000 H16C 2 0.500853 0.626774 0.968401 11.00000 -1.50000 AFIX 0 C17 1 0.852479 0.440875 0.909105 11.00000 0.05617 0.05162 = 0.04357 0.00734 -0.01853 -0.02901 AFIX 137 H17A 2 0.917513 0.380560 0.861934 11.00000 -1.50000 H17B 2 0.858994 0.399551 0.956815 11.00000 -1.50000 H17C 2 0.875386 0.508803 0.911338 11.00000 -1.50000 AFIX 0 C18 1 0.644189 0.561905 0.629384 11.00000 0.04340 0.05632 = 0.03254 0.00947 -0.00966 -0.02193 AFIX 13 H18 2 0.652838 0.476816 0.623221 11.00000 -1.20000 AFIX 0 C19 1 0.493948 0.656625 0.632009 11.00000 0.04594 0.07581 = 0.05082 0.01831 -0.01748 -0.02091 AFIX 137 H19A 2 0.429476 0.663392 0.684024 11.00000 -1.50000 H19B 2 0.469498 0.627788 0.590434 11.00000 -1.50000 H19C 2 0.488355 0.738284 0.623222 11.00000 -1.50000 AFIX 0 C20 1 0.757073 0.566531 0.557469 11.00000 0.05425 0.08660 = 0.03277 0.01403 -0.00360 -0.02611 AFIX 137 H20A 2 0.745005 0.651509 0.557841 11.00000 -1.50000 H20B 2 0.748359 0.541295 0.507995 11.00000 -1.50000 H20C 2 0.848954 0.509703 0.561277 11.00000 -1.50000 AFIX 0 C21 1 0.703600 0.750182 0.866500 11.00000 0.07834 0.04464 = 0.05836 0.00653 -0.01852 -0.03930 AFIX 137 H21A 2 0.611917 0.810191 0.901259 11.00000 -1.50000 H21B 2 0.748304 0.794912 0.834381 11.00000 -1.50000 H21C 2 0.760339 0.699956 0.898876 11.00000 -1.50000 AFIX 0 C22 1 0.656913 0.796949 0.695498 11.00000 0.06282 0.04572 = 0.05908 0.02015 -0.01338 -0.02509 AFIX 137 H22A 2 0.743374 0.775033 0.652838 11.00000 -1.50000 H22B 2 0.637871 0.865314 0.733264 11.00000 -1.50000 H22C 2 0.580730 0.823036 0.672887 11.00000 -1.50000 AFIX 0 SAME 0.02 0.02 C23B > C28B PART 1 C23A 1 0.647419 0.290600 0.682874 61.00000 0.04030 0.05350 = 0.03487 -0.00666 -0.00095 -0.03046 AFIX 13 H23A 2 0.712814 0.302208 0.636337 61.00000 -1.20000 AFIX 0 C24A 1 0.497173 0.375779 0.676141 61.00000 0.03709 0.05928 = 0.03993 0.00170 -0.00332 -0.03584 AFIX 23 H24A 2 0.427175 0.377814 0.725061 61.00000 -1.20000 H24B 2 0.482841 0.461888 0.671880 61.00000 -1.20000 AFIX 0 C25A 1 0.475512 0.327609 0.602573 61.00000 0.04344 0.05788 = 0.04497 0.00519 -0.01690 -0.03348 AFIX 23 H25A 2 0.376448 0.373989 0.606155 61.00000 -1.20000 H25B 2 0.529298 0.344589 0.553601 61.00000 -1.20000 AFIX 0 C26A 1 0.520834 0.186615 0.596751 61.00000 0.05217 0.05501 = 0.05053 0.00288 -0.01801 -0.03476 AFIX 23 H26A 2 0.458882 0.170916 0.642187 61.00000 -1.20000 H26B 2 0.511504 0.159768 0.547332 61.00000 -1.20000 AFIX 0 C27A 1 0.671945 0.109036 0.596853 61.00000 0.05578 0.05608 = 0.04129 -0.00612 -0.01660 -0.02856 AFIX 23 H27A 2 0.734752 0.120340 0.549579 61.00000 -1.20000 H27B 2 0.696652 0.019677 0.593801 61.00000 -1.20000 AFIX 0 C28A 1 0.691754 0.149985 0.674618 61.00000 0.04022 0.05881 = 0.04054 -0.00462 -0.01008 -0.02713 AFIX 23 H28A 2 0.635445 0.131514 0.721657 61.00000 -1.20000 H28B 2 0.790117 0.101985 0.672267 61.00000 -1.20000 AFIX 0 PART 0 PART 2 C23B 1 0.658489 0.283244 0.678937 -61.00000 0.03587 0.05542 = 0.03256 -0.00698 -0.00373 -0.02729 AFIX 13 H23B 2 0.712626 0.301112 0.629711 -61.00000 -1.20000 AFIX 0 C24B 1 0.498139 0.344108 0.687184 -61.00000 0.03873 0.04838 = 0.04059 0.00172 -0.00643 -0.03195 AFIX 23 H24C 2 0.447203 0.329944 0.738481 -61.00000 -1.20000 H24D 2 0.460162 0.435055 0.686215 -61.00000 -1.20000 AFIX 0 C25B 1 0.478494 0.284328 0.616708 -61.00000 0.04331 0.05679 = 0.04989 0.00551 -0.01470 -0.03269 AFIX 23 H25C 2 0.378665 0.322063 0.622300 -61.00000 -1.20000 H25D 2 0.525591 0.302510 0.565729 -61.00000 -1.20000 AFIX 0 C26B 1 0.538697 0.140803 0.615573 -61.00000 0.05591 0.05414 = 0.05460 0.00087 -0.01739 -0.03870 AFIX 23 H26C 2 0.484071 0.122848 0.663695 -61.00000 -1.20000 H26D 2 0.530560 0.105359 0.568635 -61.00000 -1.20000 AFIX 0 C27B 1 0.692393 0.078067 0.612672 -61.00000 0.05018 0.04807 = 0.03744 0.00137 -0.01291 -0.03104 AFIX 23 H27C 2 0.748726 0.086426 0.561169 -61.00000 -1.20000 H27D 2 0.724952 -0.011841 0.616183 -61.00000 -1.20000 AFIX 0 C28B 1 0.714758 0.137735 0.682643 -61.00000 0.04451 0.05326 = 0.03434 -0.00513 -0.00603 -0.03477 AFIX 23 H28C 2 0.814490 0.097604 0.677643 -61.00000 -1.20000 H28D 2 0.664731 0.123874 0.734367 -61.00000 -1.20000 AFIX 0 PART 0 PART 3 S2C 7 0.339247 0.187437 0.840171 51.00000 0.05277 0.06426 = 0.04463 -0.00169 -0.00952 -0.02400 F5C 3 0.145053 0.292186 0.979236 51.00000 0.06081 0.07695 = 0.05842 -0.00230 -0.00245 -0.02312 F4C 3 0.132482 0.151011 0.933253 51.00000 0.03978 0.06895 = 0.05666 0.00873 -0.01648 -0.03052 F6C 3 0.309268 0.105276 0.979592 51.00000 0.06327 0.08754 = 0.06574 0.00725 -0.01196 -0.01063 O4C 5 0.431097 0.056703 0.810424 51.00000 0.05554 0.07786 = 0.05681 -0.01178 -0.00985 -0.03647 O5C 5 0.402414 0.259326 0.856740 51.00000 0.05188 0.06365 = 0.04738 0.01889 -0.00957 -0.03902 O6C 5 0.220566 0.247350 0.805367 51.00000 0.05833 0.07909 = 0.04993 0.00356 -0.01564 -0.01999 C30C 1 0.232719 0.180665 0.938900 51.00000 0.05277 0.07460 = 0.05041 0.00956 -0.01645 -0.02803 PART 0 PART 2 S2B 7 0.277254 0.251492 0.878781 41.00000 0.05650 0.08000 = 0.05879 0.00940 -0.01458 -0.03258 F6B 3 0.174561 0.102606 0.933896 41.00000 0.05318 0.07328 = 0.07331 0.01877 -0.00804 -0.03557 F5B 3 0.357058 0.000252 0.859378 41.00000 0.04451 0.07816 = 0.06254 -0.00421 -0.00265 -0.03996 F4B 3 0.365246 0.071776 0.965220 41.00000 0.03678 0.09324 = 0.04792 0.02888 -0.01274 -0.01151 O4B 5 0.185138 0.351602 0.944925 41.00000 0.07011 0.07229 = 0.05531 0.00073 -0.01488 -0.02834 O5B 5 0.227755 0.272415 0.811596 41.00000 0.04844 0.06059 = 0.03935 0.00804 -0.01723 -0.03332 O6B 5 0.429581 0.218894 0.868702 41.00000 0.04873 0.06957 = 0.03301 -0.00126 0.00519 -0.04952 C30B 1 0.288707 0.110437 0.914950 41.00000 0.02961 0.05325 = 0.03681 0.01514 -0.01119 -0.03739 S1B 7 0.860581 0.339256 0.401660 -21.00000 0.04261 0.05104 = 0.03924 -0.00012 -0.00361 -0.02260 F1B 3 1.022419 0.142673 0.290684 -21.00000 0.07682 0.10164 = 0.07090 -0.05498 0.01515 -0.02496 F2B 3 0.820566 0.158044 0.358661 -21.00000 0.08025 0.10584 = 0.14033 -0.05465 -0.01627 -0.05713 F3B 3 0.990070 0.092245 0.407201 -21.00000 0.11435 0.06715 = 0.14239 -0.00747 -0.02312 -0.00979 O1B 5 0.800170 0.415679 0.344408 -21.00000 0.06048 0.05850 = 0.09649 0.01681 -0.03913 -0.03273 O2B 5 0.986729 0.346773 0.400360 -21.00000 0.05273 0.03451 = 0.07742 0.00810 -0.02259 -0.02981 O3B 5 0.764519 0.354048 0.479638 -21.00000 0.08525 0.07878 = 0.05229 -0.01628 0.01458 -0.05637 C29B 1 0.919296 0.179813 0.366425 -21.00000 0.04872 0.05519 = 0.08048 0.00481 -0.02855 -0.02591 SAME 0.02 0.02 S1B > C29B PART 0 PART 1 S1A 7 0.946399 0.302019 0.346633 21.00000 0.05100 0.05408 = 0.03577 0.00589 -0.00829 -0.02847 F1A 3 0.809459 0.166961 0.372297 21.00000 0.05670 0.06507 = 0.07981 0.00689 -0.02794 -0.03674 F2A 3 0.782176 0.278057 0.478405 21.00000 0.07816 0.06741 = 0.04460 0.00119 0.00593 -0.03937 F3A 3 0.973529 0.106789 0.425952 21.00000 0.06051 0.04191 = 0.09281 0.02686 -0.03885 -0.03153 O1A 5 0.820350 0.403342 0.336392 21.00000 0.09232 0.07267 = 0.05959 0.03184 -0.03509 -0.01885 O2A 5 1.039299 0.219468 0.274908 21.00000 0.07955 0.09711 = 0.04671 -0.01527 0.01199 -0.05259 O3A 5 1.012780 0.331861 0.396467 21.00000 0.05746 0.06789 = 0.04905 0.01415 -0.01600 -0.03903 C29A 1 0.872581 0.210775 0.410615 21.00000 0.03400 0.03260 = 0.02794 -0.00448 -0.00672 -0.01788 SAME 0.02 0.02 S2B > C30B SAME 0.02 0.02 S2C > C30C S2A 7 0.192584 0.226561 0.913107 31.00000 0.03960 0.04828 = 0.04634 0.00017 -0.01341 -0.02161 F4A 3 0.463683 0.131565 0.846510 31.00000 0.05351 0.15769 = 0.09010 0.06472 -0.00454 -0.03589 F5A 3 0.397617 0.003591 0.846497 31.00000 0.07611 0.10286 = 0.08483 -0.03439 -0.02591 0.01052 F6A 3 0.409265 0.066293 0.957485 31.00000 0.04243 0.08197 = 0.04034 0.02047 -0.01038 -0.02606 O4A 5 0.181504 0.326277 0.963139 31.00000 0.08773 0.04931 = 0.05881 0.00613 -0.02987 -0.03934 O5A 5 0.111776 0.167481 0.959951 31.00000 0.04741 0.06528 = 0.08801 0.00362 -0.00002 -0.02784 O6A 5 0.183148 0.256057 0.833612 31.00000 0.05593 0.07451 = 0.04446 -0.00635 -0.02177 -0.01233 C30A 1 0.373255 0.105055 0.891579 31.00000 0.04443 0.07648 = 0.03129 0.00713 -0.00960 -0.01357 PART 0 N5 4 0.348234 0.624212 0.850343 11.00000 0.05320 0.06579 = 0.04569 0.00019 -0.01046 -0.02141 C31 1 0.253366 0.609638 0.855253 11.00000 0.04996 0.05078 = 0.03464 0.00512 -0.00865 -0.01664 C32 1 0.133618 0.588045 0.861219 11.00000 0.07830 0.09753 = 0.06021 0.02188 -0.02428 -0.05575 AFIX 137 H32A 2 0.048719 0.658232 0.895004 11.00000 -1.50000 H32B 2 0.147278 0.511177 0.884454 11.00000 -1.50000 H32C 2 0.125723 0.580456 0.808143 11.00000 -1.50000 AFIX 0 HKLF 4 REM jjw1021_a.res in P-1 REM R1 = 0.0703 for 6205 Fo > 4sig(Fo) and 0.0843 for all 7718 data REM 757 parameters refined using 1374 restraints END WGHT 0.1282 0.9549 REM Highest difference peak 1.067, deepest hole -0.581, 1-sigma level 0.080 Q1 1 0.8981 0.2384 0.3892 11.00000 0.05 0.75 Q2 1 0.3723 0.0669 0.8896 11.00000 0.05 0.48 Q3 1 0.6340 0.4234 0.7881 11.00000 0.05 0.47 Q4 1 0.7058 0.3394 0.8261 11.00000 0.05 0.39 Q5 1 0.8633 0.2764 0.4861 11.00000 0.05 0.39 Q6 1 0.4613 0.0236 0.8279 11.00000 0.05 0.38 Q7 1 0.3840 0.1326 0.8897 11.00000 0.05 0.37 Q8 1 0.2143 0.0602 0.8976 11.00000 0.05 0.37 Q9 1 0.2559 0.2953 0.9437 11.00000 0.05 0.36 Q10 1 0.6583 0.3403 0.7236 11.00000 0.05 0.34 Q11 1 1.1064 0.2436 0.3747 11.00000 0.05 0.34 Q12 1 0.1208 0.2251 0.9476 11.00000 0.05 0.34 Q13 1 0.3438 0.1561 0.9793 11.00000 0.05 0.33 Q14 1 0.1361 0.3184 0.9316 11.00000 0.05 0.31 Q15 1 1.0421 0.2903 0.2778 11.00000 0.05 0.31 Q16 1 1.0409 0.2997 0.3418 11.00000 0.05 0.31 Q17 1 0.9542 0.3871 0.3512 11.00000 0.05 0.31 Q18 1 0.4923 0.0658 0.8273 11.00000 0.05 0.30 Q19 1 0.9468 0.2380 0.2654 11.00000 0.05 0.30 Q20 1 0.7555 0.3502 0.3820 11.00000 0.05 0.30 ; _shelx_res_checksum 25284 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.498 _oxdiff_exptl_absorpt_empirical_full_min 0.674 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.66956(7) 0.34643(7) 0.77315(4) 0.03390(19) Uani 1 1 d . . . . . N1 N 0.9773(2) 0.2105(2) 0.71428(13) 0.0321(5) Uani 1 1 d . . . . . N2 N 0.8803(3) 0.1450(2) 0.81992(14) 0.0373(5) Uani 1 1 d . . . . . N3 N 0.6927(2) 0.5498(2) 0.82799(14) 0.0342(5) Uani 1 1 d . . . . . N4 N 0.6674(2) 0.5783(2) 0.70825(14) 0.0366(5) Uani 1 1 d . . . . . C1 C 0.8516(3) 0.2332(3) 0.76820(16) 0.0341(5) Uani 1 1 d . . . . . C2 C 1.0241(3) 0.0653(3) 0.79789(18) 0.0414(6) Uani 1 1 d . . . . . C3 C 1.0855(3) 0.1075(3) 0.73237(18) 0.0382(6) Uani 1 1 d . . . . . C4 C 0.7704(4) 0.1362(3) 0.88909(18) 0.0459(7) Uani 1 1 d . . . . . H4 H 0.6788 0.2068 0.8902 0.055 Uiso 1 1 calc R . . . . C5 C 0.7636(5) 0.0131(4) 0.8761(2) 0.0699(12) Uani 1 1 d . . . . . H5A H 0.7625 0.0007 0.8219 0.105 Uiso 1 1 calc GR . . . . H5B H 0.6793 0.0184 0.9141 0.105 Uiso 1 1 calc GR . . . . H5C H 0.8448 -0.0573 0.8842 0.105 Uiso 1 1 calc GR . . . . C6 C 0.7936(4) 0.1543(3) 0.9699(2) 0.0551(8) Uani 1 1 d . . . . . H6A H 0.8783 0.0825 0.9730 0.083 Uiso 1 1 calc GR . . . . H6B H 0.7145 0.1617 1.0139 0.083 Uiso 1 1 calc GR . . . . H6C H 0.8027 0.2301 0.9733 0.083 Uiso 1 1 calc GR . . . . C7 C 0.9923(3) 0.2859(3) 0.64651(16) 0.0346(5) Uani 1 1 d . . . . . H7 H 0.8970 0.3403 0.6435 0.042 Uiso 1 1 calc R . . . . C8 C 1.0778(3) 0.2017(3) 0.56530(18) 0.0469(7) Uani 1 1 d . . . . . H8A H 1.1764 0.1608 0.5608 0.070 Uiso 1 1 calc GR . . . . H8B H 1.0626 0.2528 0.5222 0.070 Uiso 1 1 calc GR . . . . H8C H 1.0485 0.1385 0.5617 0.070 Uiso 1 1 calc GR . . . . C9 C 1.0476(3) 0.3744(3) 0.6651(2) 0.0476(7) Uani 1 1 d . . . . . H9A H 0.9839 0.4304 0.7143 0.071 Uiso 1 1 calc GR . . . . H9B H 1.0544 0.4237 0.6213 0.071 Uiso 1 1 calc GR . . . . H9C H 1.1392 0.3250 0.6715 0.071 Uiso 1 1 calc GR . . . . C10 C 1.0983(4) -0.0477(4) 0.8365(3) 0.0605(9) Uani 1 1 d . . . . . H10A H 1.0777 -0.0220 0.8928 0.091 Uiso 1 1 calc GR . . . . H10B H 1.1984 -0.0850 0.8102 0.091 Uiso 1 1 calc GR . . . . H10C H 1.0668 -0.1088 0.8314 0.091 Uiso 1 1 calc GR . . . . C11 C 1.2390(3) 0.0566(3) 0.6882(2) 0.0465(7) Uani 1 1 d . . . . . H11A H 1.2617 0.0099 0.6371 0.070 Uiso 1 1 calc GR . . . . H11B H 1.2934 0.0012 0.7200 0.070 Uiso 1 1 calc GR . . . . H11C H 1.2606 0.1257 0.6791 0.070 Uiso 1 1 calc GR . . . . C12 C 0.6813(3) 0.4968(3) 0.76389(16) 0.0321(5) Uani 1 1 d . . . . . C13 C 0.6884(3) 0.6655(3) 0.81212(19) 0.0413(6) Uani 1 1 d . . . . . C14 C 0.6706(3) 0.6836(3) 0.7385(2) 0.0437(7) Uani 1 1 d . . . . . C15 C 0.7040(3) 0.4939(3) 0.90475(17) 0.0386(6) Uani 1 1 d . . . . . H15 H 0.6848 0.4218 0.9030 0.046 Uiso 1 1 calc R . . . . C16 C 0.5903(4) 0.5883(3) 0.97850(19) 0.0485(7) Uani 1 1 d . . . . . H16A H 0.6147 0.6530 0.9882 0.073 Uiso 1 1 calc GR . . . . H16B H 0.5842 0.5445 1.0252 0.073 Uiso 1 1 calc GR . . . . H16C H 0.5009 0.6268 0.9684 0.073 Uiso 1 1 calc GR . . . . C17 C 0.8525(4) 0.4409(3) 0.9091(2) 0.0483(7) Uani 1 1 d . . . . . H17A H 0.9175 0.3806 0.8619 0.072 Uiso 1 1 calc GR . . . . H17B H 0.8590 0.3996 0.9568 0.072 Uiso 1 1 calc GR . . . . H17C H 0.8754 0.5088 0.9113 0.072 Uiso 1 1 calc GR . . . . C18 C 0.6442(3) 0.5619(3) 0.62938(18) 0.0453(7) Uani 1 1 d . . . . . H18 H 0.6528 0.4768 0.6232 0.054 Uiso 1 1 calc DR . . . . C19 C 0.4939(4) 0.6566(4) 0.6320(2) 0.0603(9) Uani 1 1 d . . . . . H19A H 0.4295 0.6634 0.6840 0.090 Uiso 1 1 calc GR . . . . H19B H 0.4695 0.6278 0.5904 0.090 Uiso 1 1 calc GR . . . . H19C H 0.4884 0.7383 0.6232 0.090 Uiso 1 1 calc GR . . . . C20 C 0.7571(4) 0.5665(5) 0.5575(2) 0.0632(10) Uani 1 1 d . . . . . H20A H 0.7450 0.6515 0.5578 0.095 Uiso 1 1 calc GR . . . . H20B H 0.7484 0.5413 0.5080 0.095 Uiso 1 1 calc GR . . . . H20C H 0.8490 0.5097 0.5613 0.095 Uiso 1 1 calc GR . . . . C21 C 0.7036(4) 0.7502(3) 0.8665(2) 0.0569(8) Uani 1 1 d . . . . . H21A H 0.6119 0.8102 0.9013 0.085 Uiso 1 1 calc GR . . . . H21B H 0.7483 0.7949 0.8344 0.085 Uiso 1 1 calc GR . . . . H21C H 0.7603 0.7000 0.8989 0.085 Uiso 1 1 calc GR . . . . C22 C 0.6569(4) 0.7969(3) 0.6955(2) 0.0576(9) Uani 1 1 d . . . . . H22A H 0.7434 0.7750 0.6528 0.086 Uiso 1 1 calc GR . . . . H22B H 0.6379 0.8653 0.7333 0.086 Uiso 1 1 calc GR . . . . H22C H 0.5807 0.8230 0.6729 0.086 Uiso 1 1 calc GR . . . . C23A C 0.647(2) 0.2906(14) 0.6829(18) 0.042(3) Uani 0.349(19) 1 d D U P A 1 H23A H 0.7128 0.3022 0.6363 0.050 Uiso 0.349(19) 1 calc DR . P A 1 C24A C 0.4972(16) 0.3758(15) 0.6761(9) 0.042(2) Uani 0.349(19) 1 d D U P A 1 H24A H 0.4272 0.3778 0.7251 0.050 Uiso 0.349(19) 1 calc R . P A 1 H24B H 0.4828 0.4619 0.6719 0.050 Uiso 0.349(19) 1 calc R . P A 1 C25A C 0.4755(13) 0.3276(16) 0.6026(8) 0.044(2) Uani 0.349(19) 1 d D U P A 1 H25A H 0.3764 0.3740 0.6062 0.053 Uiso 0.349(19) 1 calc R . P A 1 H25B H 0.5293 0.3446 0.5536 0.053 Uiso 0.349(19) 1 calc R . P A 1 C26A C 0.5208(13) 0.1866(17) 0.5968(9) 0.048(2) Uani 0.349(19) 1 d D U P A 1 H26A H 0.4589 0.1709 0.6422 0.058 Uiso 0.349(19) 1 calc R . P A 1 H26B H 0.5115 0.1598 0.5473 0.058 Uiso 0.349(19) 1 calc R . P A 1 C27A C 0.6719(16) 0.1090(16) 0.5969(10) 0.050(3) Uani 0.349(19) 1 d D U P A 1 H27A H 0.7348 0.1203 0.5496 0.060 Uiso 0.349(19) 1 calc R . P A 1 H27B H 0.6967 0.0197 0.5938 0.060 Uiso 0.349(19) 1 calc R . P A 1 C28A C 0.692(2) 0.1500(16) 0.6746(14) 0.045(3) Uani 0.349(19) 1 d D U P A 1 H28A H 0.6354 0.1315 0.7217 0.054 Uiso 0.349(19) 1 calc R . P A 1 H28B H 0.7901 0.1020 0.6723 0.054 Uiso 0.349(19) 1 calc R . P A 1 C23B C 0.6585(12) 0.2832(8) 0.6789(9) 0.0404(18) Uani 0.651(19) 1 d D U P A 2 H23B H 0.7126 0.3011 0.6297 0.048 Uiso 0.651(19) 1 calc R . P A 2 C24B C 0.4981(9) 0.3441(8) 0.6872(5) 0.0392(15) Uani 0.651(19) 1 d D U P A 2 H24C H 0.4472 0.3299 0.7385 0.047 Uiso 0.651(19) 1 calc R . P A 2 H24D H 0.4602 0.4351 0.6862 0.047 Uiso 0.651(19) 1 calc R . P A 2 C25B C 0.4785(7) 0.2843(10) 0.6167(5) 0.0462(15) Uani 0.651(19) 1 d D U P A 2 H25C H 0.3787 0.3221 0.6223 0.055 Uiso 0.651(19) 1 calc R . P A 2 H25D H 0.5256 0.3025 0.5657 0.055 Uiso 0.651(19) 1 calc R . P A 2 C26B C 0.5387(8) 0.1408(9) 0.6156(5) 0.0495(17) Uani 0.651(19) 1 d D U P A 2 H26C H 0.4841 0.1228 0.6637 0.059 Uiso 0.651(19) 1 calc R . P A 2 H26D H 0.5306 0.1054 0.5686 0.059 Uiso 0.651(19) 1 calc R . P A 2 C27B C 0.6924(8) 0.0781(8) 0.6127(5) 0.0421(15) Uani 0.651(19) 1 d D U P A 2 H27C H 0.7487 0.0864 0.5612 0.051 Uiso 0.651(19) 1 calc R . P A 2 H27D H 0.7250 -0.0118 0.6162 0.051 Uiso 0.651(19) 1 calc R . P A 2 C28B C 0.7148(11) 0.1377(8) 0.6826(6) 0.0406(14) Uani 0.651(19) 1 d D U P A 2 H28C H 0.8145 0.0976 0.6776 0.049 Uiso 0.651(19) 1 calc R . P A 2 H28D H 0.6647 0.1239 0.7344 0.049 Uiso 0.651(19) 1 calc R . P A 2 S2C S 0.3392(6) 0.1874(6) 0.8402(3) 0.0566(13) Uani 0.155(2) 1 d D U P B 3 F5C F 0.1451(15) 0.2922(15) 0.9792(9) 0.073(4) Uani 0.155(2) 1 d D U P B 3 F4C F 0.132(2) 0.151(2) 0.9333(11) 0.053(3) Uani 0.155(2) 1 d D U P B 3 F6C F 0.3093(18) 0.1053(18) 0.9796(9) 0.084(4) Uani 0.155(2) 1 d D U P B 3 O4C O 0.4311(16) 0.0567(13) 0.8104(11) 0.063(3) Uani 0.155(2) 1 d D U P B 3 O5C O 0.4024(18) 0.2593(16) 0.8567(11) 0.051(3) Uani 0.155(2) 1 d D U P B 3 O6C O 0.221(2) 0.247(2) 0.8054(14) 0.068(6) Uani 0.155(2) 1 d D U P B 3 C30C C 0.2327(15) 0.1807(17) 0.9389(8) 0.060(3) Uani 0.155(2) 1 d D U P B 3 S2B S 0.2773(6) 0.2515(6) 0.8788(4) 0.0657(13) Uani 0.193(2) 1 d D U P C 2 F6B F 0.1746(12) 0.1026(14) 0.9339(10) 0.067(3) Uani 0.193(2) 1 d D U P C 2 F5B F 0.3571(14) 0.0003(12) 0.8594(10) 0.060(3) Uani 0.193(2) 1 d D U P C 2 F4B F 0.3652(17) 0.0718(17) 0.9652(10) 0.068(4) Uani 0.193(2) 1 d D U P C 2 O4B O 0.185(2) 0.3516(15) 0.9449(10) 0.069(4) Uani 0.193(2) 1 d D U P C 2 O5B O 0.2278(18) 0.2724(17) 0.8116(10) 0.046(3) Uani 0.193(2) 1 d D U P C 2 O6B O 0.4296(13) 0.2189(15) 0.8687(8) 0.046(3) Uani 0.193(2) 1 d D U P C 2 C30B C 0.2887(12) 0.1104(11) 0.9149(7) 0.0325(17) Uani 0.193(2) 1 d D U P C 2 S1B S 0.8606(2) 0.3393(2) 0.40166(14) 0.0461(7) Uani 0.352(3) 1 d D U P D 2 F1B F 1.0224(9) 0.1427(10) 0.2907(5) 0.098(3) Uani 0.352(3) 1 d D U P D 2 F2B F 0.821(2) 0.1580(19) 0.3587(15) 0.107(8) Uani 0.352(3) 1 d D U P D 2 F3B F 0.9901(19) 0.0922(13) 0.4072(11) 0.125(8) Uani 0.352(3) 1 d D U P D 2 O1B O 0.8002(19) 0.4157(14) 0.3444(12) 0.067(5) Uani 0.352(3) 1 d D U P D 2 O2B O 0.987(2) 0.347(2) 0.4004(16) 0.051(4) Uani 0.352(3) 1 d D U P D 2 O3B O 0.7645(10) 0.3540(11) 0.4796(5) 0.073(3) Uani 0.352(3) 1 d D U P D 2 C29B C 0.9193(11) 0.1798(9) 0.3664(8) 0.059(3) Uani 0.352(3) 1 d D U P D 2 S1A S 0.94640(13) 0.30202(13) 0.34663(7) 0.0467(4) Uani 0.648(3) 1 d D U P D 1 F1A F 0.8095(9) 0.1670(8) 0.3723(7) 0.0623(17) Uani 0.648(3) 1 d D U P D 1 F2A F 0.7822(4) 0.2781(5) 0.4784(2) 0.0671(10) Uani 0.648(3) 1 d D U P D 1 F3A F 0.9735(6) 0.1068(5) 0.4260(5) 0.0588(12) Uani 0.648(3) 1 d D U P D 1 O1A O 0.8204(13) 0.4033(9) 0.3364(6) 0.081(4) Uani 0.648(3) 1 d D U P D 1 O2A O 1.0393(6) 0.2195(6) 0.2749(3) 0.0771(14) Uani 0.648(3) 1 d D U P D 1 O3A O 1.0128(14) 0.3319(13) 0.3965(8) 0.054(2) Uani 0.648(3) 1 d D U P D 1 C29A C 0.8726(4) 0.2108(4) 0.4106(3) 0.0312(9) Uani 0.648(3) 1 d D U P D 1 S2A S 0.19258(12) 0.22656(12) 0.91311(8) 0.0443(3) Uani 0.653(2) 1 d D U P E 1 F4A F 0.4637(4) 0.1316(7) 0.8465(3) 0.1110(19) Uani 0.653(2) 1 d D U P E 1 F5A F 0.3976(6) 0.0036(6) 0.8465(4) 0.109(3) Uani 0.653(2) 1 d D U P E 1 F6A F 0.4093(4) 0.0663(5) 0.9575(3) 0.0570(10) Uani 0.653(2) 1 d D U P E 1 O4A O 0.1815(7) 0.3263(5) 0.9631(3) 0.0607(14) Uani 0.653(2) 1 d D U P E 1 O5A O 0.1118(6) 0.1675(7) 0.9600(4) 0.0712(17) Uani 0.653(2) 1 d D U P E 1 O6A O 0.1831(6) 0.2561(6) 0.8336(3) 0.0642(15) Uani 0.653(2) 1 d D U P E 1 C30A C 0.3733(5) 0.1051(6) 0.8916(3) 0.0574(13) Uani 0.653(2) 1 d D U P E 1 N5 N 0.3482(3) 0.6242(3) 0.85034(19) 0.0587(7) Uani 1 1 d . . . . . C31 C 0.2534(4) 0.6096(3) 0.85525(19) 0.0491(7) Uani 1 1 d . . . . . C32 C 0.1336(5) 0.5880(5) 0.8612(3) 0.0724(11) Uani 1 1 d . . . . . H32A H 0.0487 0.6582 0.8950 0.109 Uiso 1 1 calc GR . . . . H32B H 0.1473 0.5112 0.8845 0.109 Uiso 1 1 calc GR . . . . H32C H 0.1257 0.5805 0.8081 0.109 Uiso 1 1 calc GR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.0366(3) 0.0397(4) 0.0288(3) -0.0002(3) -0.0027(2) -0.0250(3) N1 0.0366(11) 0.0342(11) 0.0301(11) 0.0033(8) -0.0068(8) -0.0224(9) N2 0.0522(13) 0.0396(12) 0.0304(11) 0.0061(9) -0.0105(10) -0.0314(11) N3 0.0393(11) 0.0349(11) 0.0315(11) 0.0025(9) -0.0065(9) -0.0225(9) N4 0.0335(11) 0.0378(12) 0.0344(12) 0.0051(9) -0.0048(9) -0.0168(9) C1 0.0441(13) 0.0353(13) 0.0286(12) 0.0015(10) -0.0057(10) -0.0266(11) C2 0.0554(16) 0.0431(15) 0.0380(14) 0.0088(12) -0.0198(13) -0.0303(13) C3 0.0446(14) 0.0403(14) 0.0381(14) 0.0055(11) -0.0159(12) -0.0252(12) C4 0.0671(19) 0.0477(17) 0.0299(14) 0.0072(12) -0.0054(13) -0.0385(15) C5 0.101(3) 0.070(2) 0.051(2) -0.0014(18) 0.007(2) -0.067(2) C6 0.081(2) 0.0492(18) 0.0317(15) 0.0070(13) -0.0102(15) -0.0319(17) C7 0.0348(12) 0.0397(13) 0.0306(13) 0.0062(10) -0.0045(10) -0.0219(11) C8 0.0480(16) 0.0528(17) 0.0318(14) 0.0035(12) -0.0057(12) -0.0209(14) C9 0.0508(16) 0.0516(17) 0.0514(18) 0.0118(14) -0.0105(14) -0.0364(15) C10 0.072(2) 0.064(2) 0.066(2) 0.0323(19) -0.0373(19) -0.0399(19) C11 0.0414(15) 0.0475(16) 0.0548(18) 0.0081(14) -0.0181(13) -0.0225(13) C12 0.0321(11) 0.0361(13) 0.0297(12) 0.0032(10) -0.0050(9) -0.0199(10) C13 0.0432(14) 0.0358(14) 0.0455(16) 0.0047(12) -0.0071(12) -0.0231(12) C14 0.0425(14) 0.0357(14) 0.0469(16) 0.0063(12) -0.0039(12) -0.0194(12) C15 0.0530(16) 0.0397(14) 0.0311(13) 0.0046(11) -0.0104(11) -0.0299(13) C16 0.0596(18) 0.0557(18) 0.0335(14) -0.0018(13) -0.0055(13) -0.0347(16) C17 0.0562(17) 0.0516(17) 0.0436(16) 0.0073(13) -0.0185(14) -0.0290(15) C18 0.0434(15) 0.0563(18) 0.0325(14) 0.0095(12) -0.0097(12) -0.0219(14) C19 0.0459(17) 0.076(2) 0.0508(19) 0.0183(18) -0.0175(15) -0.0209(17) C20 0.0542(19) 0.087(3) 0.0328(16) 0.0140(17) -0.0036(14) -0.0261(19) C21 0.078(2) 0.0446(17) 0.058(2) 0.0065(15) -0.0185(18) -0.0393(17) C22 0.063(2) 0.0457(18) 0.059(2) 0.0202(16) -0.0134(16) -0.0251(16) C23A 0.040(4) 0.054(4) 0.035(4) -0.007(4) -0.001(4) -0.030(4) C24A 0.037(3) 0.059(5) 0.040(4) 0.002(4) -0.003(3) -0.036(4) C25A 0.043(3) 0.058(5) 0.045(4) 0.005(4) -0.017(3) -0.033(4) C26A 0.052(4) 0.055(5) 0.051(4) 0.003(4) -0.018(3) -0.035(4) C27A 0.056(4) 0.056(5) 0.041(4) -0.006(4) -0.017(3) -0.029(4) C28A 0.040(4) 0.059(4) 0.041(4) -0.005(3) -0.010(3) -0.027(3) C23B 0.036(3) 0.055(3) 0.033(3) -0.007(2) -0.004(2) -0.027(2) C24B 0.039(2) 0.048(3) 0.041(3) 0.002(2) -0.0064(19) -0.032(2) C25B 0.043(2) 0.057(4) 0.050(3) 0.006(3) -0.0147(19) -0.033(3) C26B 0.056(3) 0.054(4) 0.055(3) 0.001(3) -0.017(2) -0.039(3) C27B 0.050(3) 0.048(3) 0.037(3) 0.001(2) -0.013(2) -0.031(2) C28B 0.045(3) 0.053(3) 0.034(3) -0.005(2) -0.006(2) -0.035(2) S2C 0.053(2) 0.064(3) 0.045(2) -0.002(2) -0.010(2) -0.024(2) F5C 0.061(5) 0.077(6) 0.058(5) -0.002(5) -0.002(5) -0.023(5) F4C 0.040(5) 0.069(5) 0.057(5) 0.009(5) -0.016(4) -0.031(4) F6C 0.063(5) 0.088(5) 0.066(5) 0.007(5) -0.012(5) -0.011(5) O4C 0.056(5) 0.078(6) 0.057(6) -0.012(5) -0.010(5) -0.036(5) O5C 0.052(5) 0.064(6) 0.047(6) 0.019(5) -0.010(4) -0.039(5) O6C 0.058(7) 0.079(7) 0.050(7) 0.004(7) -0.016(6) -0.020(7) C30C 0.053(3) 0.075(4) 0.050(4) 0.010(3) -0.016(3) -0.028(3) S2B 0.057(2) 0.080(3) 0.059(2) 0.009(2) -0.0146(19) -0.033(2) F6B 0.053(5) 0.073(5) 0.073(5) 0.019(5) -0.008(4) -0.036(4) F5B 0.045(4) 0.078(5) 0.063(5) -0.004(4) -0.003(4) -0.040(4) F4B 0.037(6) 0.093(6) 0.048(5) 0.029(5) -0.013(5) -0.012(5) O4B 0.070(5) 0.072(6) 0.055(6) 0.001(5) -0.015(5) -0.028(5) O5B 0.048(5) 0.061(6) 0.039(5) 0.008(5) -0.017(4) -0.033(4) O6B 0.049(5) 0.070(5) 0.033(5) -0.001(5) 0.005(4) -0.050(4) C30B 0.030(3) 0.053(3) 0.037(3) 0.015(3) -0.011(3) -0.037(3) S1B 0.0426(12) 0.0510(13) 0.0392(13) -0.0001(9) -0.0036(10) -0.0226(9) F1B 0.077(5) 0.102(7) 0.071(5) -0.055(5) 0.015(4) -0.025(5) F2B 0.080(9) 0.106(10) 0.140(15) -0.055(8) -0.016(8) -0.057(8) F3B 0.114(10) 0.067(8) 0.142(14) -0.007(8) -0.023(9) -0.010(7) O1B 0.060(6) 0.059(8) 0.096(12) 0.017(7) -0.039(6) -0.033(6) O2B 0.053(7) 0.035(5) 0.077(10) 0.008(5) -0.023(6) -0.030(5) O3B 0.085(6) 0.079(6) 0.052(5) -0.016(5) 0.015(4) -0.056(5) C29B 0.049(5) 0.055(6) 0.080(8) 0.005(6) -0.029(5) -0.026(5) S1A 0.0510(7) 0.0541(7) 0.0358(7) 0.0059(5) -0.0083(6) -0.0285(6) F1A 0.057(3) 0.065(3) 0.080(3) 0.007(3) -0.028(3) -0.037(3) F2A 0.078(2) 0.067(2) 0.0446(18) 0.0012(18) 0.0059(16) -0.039(2) F3A 0.061(2) 0.042(2) 0.093(3) 0.027(2) -0.039(2) -0.032(2) O1A 0.092(6) 0.073(5) 0.060(4) 0.032(4) -0.035(4) -0.019(4) O2A 0.080(3) 0.097(4) 0.047(2) -0.015(2) 0.012(2) -0.053(3) O3A 0.057(4) 0.068(6) 0.049(4) 0.014(3) -0.016(3) -0.039(4) C29A 0.034(2) 0.033(2) 0.028(2) -0.0045(17) -0.0067(16) -0.0179(17) S2A 0.0396(6) 0.0483(6) 0.0463(6) 0.0002(5) -0.0134(5) -0.0216(5) F4A 0.054(2) 0.158(4) 0.090(3) 0.065(3) -0.005(2) -0.036(2) F5A 0.076(4) 0.103(3) 0.085(4) -0.034(3) -0.026(3) 0.011(3) F6A 0.042(2) 0.082(2) 0.0403(18) 0.0205(16) -0.0104(16) -0.0261(19) O4A 0.088(3) 0.049(2) 0.059(3) 0.006(2) -0.030(2) -0.039(2) O5A 0.047(3) 0.065(3) 0.088(4) 0.004(3) 0.000(2) -0.028(2) O6A 0.056(3) 0.075(3) 0.044(3) -0.006(2) -0.022(2) -0.012(2) C30A 0.044(2) 0.076(3) 0.031(2) 0.007(2) -0.0096(17) -0.014(2) N5 0.0532(17) 0.0658(19) 0.0457(16) 0.0002(14) -0.0105(13) -0.0214(14) C31 0.0500(17) 0.0508(18) 0.0346(15) 0.0051(13) -0.0087(13) -0.0166(14) C32 0.078(3) 0.098(3) 0.060(2) 0.022(2) -0.024(2) -0.056(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0121 0 0 1 0.0121 -7 -3 -4 0.1278 7 3 4 0.1278 2 7 -4 0.0161 -3 -7 4 0.0285 1 6 6 0.0145 -1 -6 -6 0.0145 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 P1 C12 100.94(11) . . ? C1 P1 C23B 100.4(3) . . ? C12 P1 C23B 113.0(4) . . ? C23A P1 C1 103.7(6) . . ? C23A P1 C12 112.7(7) . . ? C1 N1 C3 109.4(2) . . ? C1 N1 C7 124.0(2) . . ? C3 N1 C7 126.6(2) . . ? C1 N2 C2 109.6(2) . . ? C1 N2 C4 124.2(3) . . ? C2 N2 C4 126.1(3) . . ? C12 N3 C13 109.5(2) . . ? C12 N3 C15 125.2(2) . . ? C13 N3 C15 125.3(2) . . ? C12 N4 C14 108.4(2) . . ? C12 N4 C18 125.9(3) . . ? C14 N4 C18 125.6(3) . . ? N1 C1 P1 131.1(2) . . ? N2 C1 P1 121.8(2) . . ? N2 C1 N1 106.8(2) . . ? N2 C2 C10 126.6(3) . . ? C3 C2 N2 107.0(3) . . ? C3 C2 C10 126.4(3) . . ? N1 C3 C11 125.2(3) . . ? C2 C3 N1 107.0(3) . . ? C2 C3 C11 127.8(3) . . ? N2 C4 H4 107.2 . . ? N2 C4 C5 111.2(3) . . ? N2 C4 C6 110.6(3) . . ? C5 C4 H4 107.2 . . ? C5 C4 C6 113.1(3) . . ? C6 C4 H4 107.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 H7 106.6 . . ? N1 C7 C8 111.8(2) . . ? N1 C7 C9 110.7(2) . . ? C8 C7 H7 106.6 . . ? C8 C7 C9 113.9(2) . . ? C9 C7 H7 106.6 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2 C10 H10A 109.5 . . ? C2 C10 H10B 109.5 . . ? C2 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C11 H11A 109.5 . . ? C3 C11 H11B 109.5 . . ? C3 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 P1 118.10(19) . . ? N4 C12 P1 134.2(2) . . ? N4 C12 N3 107.3(2) . . ? N3 C13 C21 125.7(3) . . ? C14 C13 N3 106.5(3) . . ? C14 C13 C21 127.8(3) . . ? N4 C14 C22 125.2(3) . . ? C13 C14 N4 108.3(3) . . ? C13 C14 C22 126.5(3) . . ? N3 C15 H15 106.8 . . ? N3 C15 C16 111.1(3) . . ? N3 C15 C17 111.0(2) . . ? C16 C15 H15 106.8 . . ? C17 C15 H15 106.8 . . ? C17 C15 C16 114.1(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 H18 106.9 . . ? N4 C18 C19 110.3(3) . . ? N4 C18 C20 112.0(3) . . ? C19 C18 H18 106.9 . . ? C20 C18 H18 106.9 . . ? C20 C18 C19 113.3(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 H21A 109.5 . . ? C13 C21 H21B 109.5 . . ? C13 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C14 C22 H22A 109.5 . . ? C14 C22 H22B 109.5 . . ? C14 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C23A H23A 105.8 . . ? C24A C23A P1 111.6(14) . . ? C24A C23A H23A 105.8 . . ? C28A C23A P1 113.2(13) . . ? C28A C23A H23A 105.8 . . ? C28A C23A C24A 113.8(11) . . ? C23A C24A H24A 109.2 . . ? C23A C24A H24B 109.2 . . ? H24A C24A H24B 107.9 . . ? C25A C24A C23A 112.1(10) . . ? C25A C24A H24A 109.2 . . ? C25A C24A H24B 109.2 . . ? C24A C25A H25A 109.1 . . ? C24A C25A H25B 109.1 . . ? H25A C25A H25B 107.8 . . ? C26A C25A C24A 112.5(9) . . ? C26A C25A H25A 109.1 . . ? C26A C25A H25B 109.1 . . ? C25A C26A H26A 109.2 . . ? C25A C26A H26B 109.2 . . ? H26A C26A H26B 107.9 . . ? C27A C26A C25A 111.9(9) . . ? C27A C26A H26A 109.2 . . ? C27A C26A H26B 109.2 . . ? C26A C27A H27A 109.5 . . ? C26A C27A H27B 109.5 . . ? C26A C27A C28A 110.9(9) . . ? H27A C27A H27B 108.0 . . ? C28A C27A H27A 109.5 . . ? C28A C27A H27B 109.5 . . ? C23A C28A C27A 110.5(12) . . ? C23A C28A H28A 109.5 . . ? C23A C28A H28B 109.5 . . ? C27A C28A H28A 109.5 . . ? C27A C28A H28B 109.5 . . ? H28A C28A H28B 108.1 . . ? P1 C23B H23B 112.2 . . ? C24B C23B P1 106.4(8) . . ? C24B C23B H23B 112.2 . . ? C28B C23B P1 105.1(7) . . ? C28B C23B H23B 112.2 . . ? C28B C23B C24B 108.2(7) . . ? C23B C24B H24C 109.7 . . ? C23B C24B H24D 109.7 . . ? H24C C24B H24D 108.2 . . ? C25B C24B C23B 109.7(5) . . ? C25B C24B H24C 109.7 . . ? C25B C24B H24D 109.7 . . ? C24B C25B H25C 109.4 . . ? C24B C25B H25D 109.4 . . ? H25C C25B H25D 108.0 . . ? C26B C25B C24B 111.3(5) . . ? C26B C25B H25C 109.4 . . ? C26B C25B H25D 109.4 . . ? C25B C26B H26C 109.3 . . ? C25B C26B H26D 109.3 . . ? H26C C26B H26D 108.0 . . ? C27B C26B C25B 111.5(5) . . ? C27B C26B H26C 109.3 . . ? C27B C26B H26D 109.3 . . ? C26B C27B H27C 109.2 . . ? C26B C27B H27D 109.2 . . ? C26B C27B C28B 112.1(5) . . ? H27C C27B H27D 107.9 . . ? C28B C27B H27C 109.2 . . ? C28B C27B H27D 109.2 . . ? C23B C28B H28C 109.8 . . ? C23B C28B H28D 109.8 . . ? C27B C28B C23B 109.5(6) . . ? C27B C28B H28C 109.8 . . ? C27B C28B H28D 109.8 . . ? H28C C28B H28D 108.2 . . ? O4C S2C O6C 113.9(12) . . ? O4C S2C C30C 102.2(9) . . ? O5C S2C O4C 116.5(10) . . ? O5C S2C O6C 119.2(12) . . ? O5C S2C C30C 104.5(9) . . ? O6C S2C C30C 95.7(9) . . ? F5C C30C S2C 112.5(12) . . ? F5C C30C F4C 95.4(13) . . ? F4C C30C S2C 111.8(12) . . ? F6C C30C S2C 111.9(11) . . ? F6C C30C F5C 112.6(14) . . ? F6C C30C F4C 111.7(15) . . ? O4B S2B O6B 109.1(10) . . ? O4B S2B C30B 106.7(9) . . ? O5B S2B O4B 111.9(10) . . ? O5B S2B O6B 120.3(9) . . ? O5B S2B C30B 111.2(8) . . ? O6B S2B C30B 95.9(7) . . ? F6B C30B S2B 115.3(10) . . ? F6B C30B F5B 90.7(10) . . ? F6B C30B F4B 117.3(12) . . ? F5B C30B S2B 118.3(10) . . ? F4B C30B S2B 112.9(10) . . ? F4B C30B F5B 99.7(11) . . ? O1B S1B O2B 109.2(10) . . ? O1B S1B C29B 107.4(8) . . ? O2B S1B C29B 105.5(9) . . ? O3B S1B O1B 116.0(9) . . ? O3B S1B O2B 116.2(11) . . ? O3B S1B C29B 101.3(6) . . ? F1B C29B S1B 110.8(8) . . ? F2B C29B S1B 113.7(11) . . ? F2B C29B F1B 106.9(13) . . ? F2B C29B F3B 107.7(13) . . ? F3B C29B S1B 116.9(10) . . ? F3B C29B F1B 99.6(10) . . ? O1A S1A C29A 100.5(5) . . ? O2A S1A O1A 113.5(5) . . ? O2A S1A O3A 115.1(7) . . ? O2A S1A C29A 105.5(3) . . ? O3A S1A O1A 117.8(7) . . ? O3A S1A C29A 101.5(5) . . ? F1A C29A S1A 111.3(5) . . ? F2A C29A S1A 111.5(3) . . ? F2A C29A F1A 109.0(6) . . ? F2A C29A F3A 109.0(5) . . ? F3A C29A S1A 111.3(3) . . ? F3A C29A F1A 104.5(5) . . ? O4A S2A O5A 110.3(4) . . ? O4A S2A O6A 114.4(4) . . ? O4A S2A C30A 104.4(4) . . ? O5A S2A C30A 103.6(3) . . ? O6A S2A O5A 119.5(4) . . ? O6A S2A C30A 102.5(3) . . ? F4A C30A S2A 115.3(5) . . ? F4A C30A F5A 100.0(6) . . ? F4A C30A F6A 108.8(5) . . ? F5A C30A S2A 110.8(4) . . ? F6A C30A S2A 113.5(4) . . ? F6A C30A F5A 107.3(6) . . ? N5 C31 C32 178.8(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C1 1.837(3) . ? P1 C12 1.860(3) . ? P1 C23A 1.84(2) . ? P1 C23B 1.872(11) . ? N1 C1 1.357(3) . ? N1 C3 1.385(4) . ? N1 C7 1.487(3) . ? N2 C1 1.356(4) . ? N2 C2 1.381(4) . ? N2 C4 1.497(4) . ? N3 C12 1.355(4) . ? N3 C13 1.385(4) . ? N3 C15 1.492(4) . ? N4 C12 1.348(4) . ? N4 C14 1.390(4) . ? N4 C18 1.496(4) . ? C2 C3 1.368(4) . ? C2 C10 1.489(5) . ? C3 C11 1.491(4) . ? C4 H4 0.9800 . ? C4 C5 1.530(4) . ? C4 C6 1.533(5) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7 0.9800 . ? C7 C8 1.522(4) . ? C7 C9 1.525(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 C14 1.348(5) . ? C13 C21 1.491(5) . ? C14 C22 1.500(4) . ? C15 H15 0.9800 . ? C15 C16 1.531(4) . ? C15 C17 1.509(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18 0.9800 . ? C18 C19 1.526(5) . ? C18 C20 1.524(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23A H23A 0.9800 . ? C23A C24A 1.556(13) . ? C23A C28A 1.513(13) . ? C24A H24A 0.9700 . ? C24A H24B 0.9700 . ? C24A C25A 1.533(12) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C25A C26A 1.515(14) . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C26A C27A 1.513(13) . ? C27A H27A 0.9700 . ? C27A H27B 0.9700 . ? C27A C28A 1.550(14) . ? C28A H28A 0.9700 . ? C28A H28B 0.9700 . ? C23B H23B 0.9800 . ? C23B C24B 1.561(9) . ? C23B C28B 1.561(8) . ? C24B H24C 0.9700 . ? C24B H24D 0.9700 . ? C24B C25B 1.543(7) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C25B C26B 1.526(9) . ? C26B H26C 0.9700 . ? C26B H26D 0.9700 . ? C26B C27B 1.516(8) . ? C27B H27C 0.9700 . ? C27B H27D 0.9700 . ? C27B C28B 1.553(8) . ? C28B H28C 0.9700 . ? C28B H28D 0.9700 . ? S2C O4C 1.421(12) . ? S2C O5C 1.414(14) . ? S2C O6C 1.488(13) . ? S2C C30C 1.813(12) . ? F5C C30C 1.294(16) . ? F4C C30C 1.349(16) . ? F6C C30C 1.288(15) . ? S2B O4B 1.435(12) . ? S2B O5B 1.400(13) . ? S2B O6B 1.522(12) . ? S2B C30B 1.748(10) . ? F6B C30B 1.272(13) . ? F5B C30B 1.397(14) . ? F4B C30B 1.326(13) . ? S1B O1B 1.436(11) . ? S1B O2B 1.449(13) . ? S1B O3B 1.424(8) . ? S1B C29B 1.760(9) . ? F1B C29B 1.396(13) . ? F2B C29B 1.287(13) . ? F3B C29B 1.325(13) . ? S1A O1A 1.435(8) . ? S1A O2A 1.405(5) . ? S1A O3A 1.430(9) . ? S1A C29A 1.833(4) . ? F1A C29A 1.354(8) . ? F2A C29A 1.291(6) . ? F3A C29A 1.329(6) . ? S2A O4A 1.424(5) . ? S2A O5A 1.457(6) . ? S2A O6A 1.439(5) . ? S2A C30A 1.800(5) . ? F4A C30A 1.253(7) . ? F5A C30A 1.328(8) . ? F6A C30A 1.326(6) . ? N5 C31 1.132(5) . ? C31 C32 1.453(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C23A C24A C25A -178.1(12) . . . . ? P1 C23A C28A C27A -179.4(16) . . . . ? P1 C23B C24B C25B -173.1(5) . . . . ? P1 C23B C28B C27B 172.8(7) . . . . ? N2 C2 C3 N1 -1.5(3) . . . . ? N2 C2 C3 C11 177.4(3) . . . . ? N3 C13 C14 N4 -1.4(3) . . . . ? N3 C13 C14 C22 178.8(3) . . . . ? C1 P1 C12 N3 -72.3(2) . . . . ? C1 P1 C12 N4 115.6(3) . . . . ? C1 P1 C23A C24A 180.0(14) . . . . ? C1 P1 C23A C28A 50.0(17) . . . . ? C1 P1 C23B C24B 163.8(6) . . . . ? C1 P1 C23B C28B 49.2(7) . . . . ? C1 N1 C3 C2 1.0(3) . . . . ? C1 N1 C3 C11 -178.0(3) . . . . ? C1 N1 C7 C8 -126.6(3) . . . . ? C1 N1 C7 C9 105.2(3) . . . . ? C1 N2 C2 C3 1.6(3) . . . . ? C1 N2 C2 C10 -176.8(3) . . . . ? C1 N2 C4 C5 114.4(4) . . . . ? C1 N2 C4 C6 -119.1(3) . . . . ? C2 N2 C1 P1 174.34(19) . . . . ? C2 N2 C1 N1 -0.9(3) . . . . ? C2 N2 C4 C5 -64.5(4) . . . . ? C2 N2 C4 C6 62.0(4) . . . . ? C3 N1 C1 P1 -174.7(2) . . . . ? C3 N1 C1 N2 -0.1(3) . . . . ? C3 N1 C7 C8 52.8(3) . . . . ? C3 N1 C7 C9 -75.4(3) . . . . ? C4 N2 C1 P1 -4.7(4) . . . . ? C4 N2 C1 N1 -180.0(2) . . . . ? C4 N2 C2 C3 -179.4(3) . . . . ? C4 N2 C2 C10 2.2(5) . . . . ? C7 N1 C1 P1 4.8(4) . . . . ? C7 N1 C1 N2 179.4(2) . . . . ? C7 N1 C3 C2 -178.5(2) . . . . ? C7 N1 C3 C11 2.5(4) . . . . ? C10 C2 C3 N1 176.8(3) . . . . ? C10 C2 C3 C11 -4.2(5) . . . . ? C12 P1 C1 N1 -51.0(3) . . . . ? C12 P1 C1 N2 135.0(2) . . . . ? C12 P1 C23A C24A -71.7(17) . . . . ? C12 P1 C23A C28A 158.3(14) . . . . ? C12 P1 C23B C24B -89.4(8) . . . . ? C12 P1 C23B C28B 156.0(6) . . . . ? C12 N3 C13 C14 1.6(3) . . . . ? C12 N3 C13 C21 -177.4(3) . . . . ? C12 N3 C15 C16 -125.8(3) . . . . ? C12 N3 C15 C17 106.2(3) . . . . ? C12 N4 C14 C13 0.8(3) . . . . ? C12 N4 C14 C22 -179.4(3) . . . . ? C12 N4 C18 C19 109.1(3) . . . . ? C12 N4 C18 C20 -123.6(3) . . . . ? C13 N3 C12 P1 -175.12(19) . . . . ? C13 N3 C12 N4 -1.1(3) . . . . ? C13 N3 C15 C16 52.4(4) . . . . ? C13 N3 C15 C17 -75.6(3) . . . . ? C14 N4 C12 P1 172.8(2) . . . . ? C14 N4 C12 N3 0.2(3) . . . . ? C14 N4 C18 C19 -67.2(4) . . . . ? C14 N4 C18 C20 60.0(4) . . . . ? C15 N3 C12 P1 3.3(3) . . . . ? C15 N3 C12 N4 177.3(2) . . . . ? C15 N3 C13 C14 -176.8(3) . . . . ? C15 N3 C13 C21 4.2(5) . . . . ? C18 N4 C12 P1 -4.0(4) . . . . ? C18 N4 C12 N3 -176.7(2) . . . . ? C18 N4 C14 C13 177.7(2) . . . . ? C18 N4 C14 C22 -2.5(5) . . . . ? C21 C13 C14 N4 177.5(3) . . . . ? C21 C13 C14 C22 -2.3(5) . . . . ? C23A P1 C1 N1 65.8(9) . . . . ? C23A P1 C1 N2 -108.2(9) . . . . ? C23A P1 C12 N3 177.7(8) . . . . ? C23A P1 C12 N4 5.6(9) . . . . ? C23A C24A C25A C26A 48.8(16) . . . . ? C24A C23A C28A C27A 52(2) . . . . ? C24A C25A C26A C27A -54.8(13) . . . . ? C25A C26A C27A C28A 58.4(16) . . . . ? C26A C27A C28A C23A -56.5(19) . . . . ? C28A C23A C24A C25A -48(2) . . . . ? C23B P1 C1 N1 65.1(5) . . . . ? C23B P1 C1 N2 -108.9(5) . . . . ? C23B P1 C12 N3 -178.7(4) . . . . ? C23B P1 C12 N4 9.2(5) . . . . ? C23B C24B C25B C26B 58.7(8) . . . . ? C24B C23B C28B C27B 59.4(10) . . . . ? C24B C25B C26B C27B -55.2(7) . . . . ? C25B C26B C27B C28B 54.6(8) . . . . ? C26B C27B C28B C23B -57.2(9) . . . . ? C28B C23B C24B C25B -60.6(10) . . . . ? O4C S2C C30C F5C 176.4(14) . . . . ? O4C S2C C30C F4C -77.5(15) . . . . ? O4C S2C C30C F6C 48.5(16) . . . . ? O5C S2C C30C F5C 54.6(15) . . . . ? O5C S2C C30C F4C 160.6(15) . . . . ? O5C S2C C30C F6C -73.3(16) . . . . ? O6C S2C C30C F5C -67.6(17) . . . . ? O6C S2C C30C F4C 38.5(18) . . . . ? O6C S2C C30C F6C 164.6(17) . . . . ? O4B S2B C30B F6B 65.9(16) . . . . ? O4B S2B C30B F5B 171.5(14) . . . . ? O4B S2B C30B F4B -72.7(15) . . . . ? O5B S2B C30B F6B -56.4(15) . . . . ? O5B S2B C30B F5B 49.2(14) . . . . ? O5B S2B C30B F4B 165.0(13) . . . . ? O6B S2B C30B F6B 177.8(12) . . . . ? O6B S2B C30B F5B -76.6(11) . . . . ? O6B S2B C30B F4B 39.2(13) . . . . ? O1B S1B C29B F1B 61.1(11) . . . . ? O1B S1B C29B F2B -59.3(16) . . . . ? O1B S1B C29B F3B 174.2(14) . . . . ? O2B S1B C29B F1B -55.4(13) . . . . ? O2B S1B C29B F2B -175.7(17) . . . . ? O2B S1B C29B F3B 57.8(16) . . . . ? O3B S1B C29B F1B -176.9(8) . . . . ? O3B S1B C29B F2B 62.8(15) . . . . ? O3B S1B C29B F3B -63.7(13) . . . . ? O1A S1A C29A F1A 61.6(7) . . . . ? O1A S1A C29A F2A -60.4(6) . . . . ? O1A S1A C29A F3A 177.7(6) . . . . ? O2A S1A C29A F1A -56.6(6) . . . . ? O2A S1A C29A F2A -178.6(4) . . . . ? O2A S1A C29A F3A 59.5(5) . . . . ? O3A S1A C29A F1A -177.0(8) . . . . ? O3A S1A C29A F2A 61.1(7) . . . . ? O3A S1A C29A F3A -60.9(8) . . . . ? O4A S2A C30A F4A -69.0(6) . . . . ? O4A S2A C30A F5A 178.3(6) . . . . ? O4A S2A C30A F6A 57.5(6) . . . . ? O5A S2A C30A F4A 175.5(6) . . . . ? O5A S2A C30A F5A 62.9(6) . . . . ? O5A S2A C30A F6A -58.0(6) . . . . ? O6A S2A C30A F4A 50.5(7) . . . . ? O6A S2A C30A F5A -62.1(6) . . . . ? O6A S2A C30A F6A 177.0(6) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0001 -0.0005 -0.9998 -0.0418 0.0718 0.0426 0.0001 0.0005 0.9998 0.0418 -0.0718 -0.0426 -7.0006 -3.0049 -3.9961 -0.3159 0.4041 -0.8212 7.0006 3.0049 3.9961 0.3159 -0.4041 0.8212 1.9980 6.9995 -4.0111 -0.8401 -0.2898 0.4081 -2.9982 -6.9998 4.0108 0.7690 0.2686 -0.5529 0.9990 6.0044 5.9882 -0.3766 -0.9401 -0.1556 -0.9990 -6.0044 -5.9882 0.3766 0.9401 0.1556