#------------------------------------------------------------------------------ #$Date: 2026-06-25 00:07:09 +0100 (Thu, 25 Jun 2026) $ #$Revision: 306640 $ #$URL: svn://www.crystallography.net/cod/cif/1/57/74/1577432.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_1577432 loop_ _publ_author_name 'Zhang, Cheng' 'Popov, Roman' 'Leforestier, Baptiste' 'Besnard, C\'eline' 'Mazet, Clement' _publ_section_title ; Pd-catalyzed regio- and enantioselective allylation of cyclic allylboronates ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D6SC04784J _journal_year 2026 _chemical_absolute_configuration ad _chemical_formula_moiety 'C27 H24 N2 O6' _chemical_formula_sum 'C27 H24 N2 O6' _chemical_formula_weight 472.48 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2025-05-28 _audit_creation_method ; Olex2 1.5 (compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224) ; _audit_update_record ; 2026-02-19 deposited with the CCDC. 2026-06-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 94.2746(10) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 6.73693(7) _cell_length_b 21.9971(3) _cell_length_c 7.83072(9) _cell_measurement_reflns_used 20157 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 72.9410 _cell_measurement_theta_min 3.9990 _cell_volume 1157.23(2) _computing_cell_refinement 'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.100a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/2 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 150' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.983 _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 -71.00 -35.00 0.50 13.00 -- -52.78 125.00 -30.00 72 2 \w -63.00 -35.00 0.50 13.00 -- -52.78 125.00 30.00 56 3 \w -92.00 -66.00 0.50 13.00 -- -52.78 -15.00-180.00 52 4 \w -97.00 -43.00 0.50 13.00 -- -52.78 -15.00 120.00 108 5 \w -68.00 -41.00 0.50 13.00 -- -52.78 -15.00 0.00 54 6 \w -79.00 -39.00 0.50 13.00 -- -52.78 125.00 120.00 80 7 \w -74.00 -37.00 0.50 13.00 -- -52.78 125.00-120.00 74 8 \w -71.00 -45.00 0.50 13.00 -- -52.78 125.00-180.00 52 9 \w 42.00 108.00 0.50 13.00 -- 66.63 15.00-180.00 132 10 \w 40.00 66.00 0.50 13.00 -- 66.63 -94.00 90.00 52 11 \w 41.00 72.00 0.50 13.00 -- 66.63 -94.00 -30.00 62 12 \w 45.00 81.00 0.50 13.00 -- 66.63 15.00 60.00 72 13 \w 44.00 70.00 0.50 13.00 -- 66.63 15.00 150.00 52 14 \w 34.00 68.00 0.50 13.00 -- 66.63 -94.00 -90.00 68 15 \w 47.00 73.00 0.50 13.00 -- 66.63 -94.00 30.00 52 16 \w 47.00 105.00 0.50 13.00 -- 66.63 15.00 -30.00 116 17 \w 36.00 81.00 0.50 13.00 -- 66.63-125.00 30.00 90 18 \w 48.00 101.00 0.50 13.00 -- 69.94 15.00 120.00 106 19 \w 59.00 102.00 0.50 13.00 -- 69.94 15.00-120.00 86 20 \w 40.00 65.00 0.50 13.00 -- 69.94-125.00-180.00 50 21 \w 50.00 75.00 0.50 13.00 -- 69.94 -94.00 60.00 50 22 \w 33.00 63.00 0.50 13.00 -- 69.94 -94.00 120.00 60 23 \w 35.00 68.00 0.50 13.00 -- 69.94 -94.00 -60.00 66 24 \w 40.00 70.00 0.50 13.00 -- 69.94 -94.00-150.00 60 25 \w 3.00 28.00 0.50 13.00 -- -4.00 32.00 4.37 50 26 \w 4.00 29.00 0.50 13.00 -- -4.00 33.00 67.02 50 27 \w 11.00 37.00 0.50 13.00 -- 4.00 30.00-100.35 52 28 \w 9.00 34.00 0.50 13.00 -- 4.00 30.00 178.89 50 29 \w 3.00 30.00 0.50 13.00 -- -8.00 33.00 -48.67 54 30 \w 12.00 39.00 0.50 13.00 -- 8.00 29.00-142.93 54 31 \w 1.00 27.00 0.50 13.00 -- -8.00 35.00 126.66 52 32 \w 1.00 26.00 0.50 13.00 -- -8.00 35.00-176.41 50 33 \w 11.00 36.00 0.50 13.00 -- 8.00 29.00 93.10 50 34 \w -5.00 22.00 0.50 13.00 -- -20.00 39.00 80.36 54 35 \w 20.00 46.00 0.50 13.00 -- 20.00 26.00 38.24 52 36 \w -13.00 13.00 0.50 13.00 -- -24.00 47.00 -69.48 52 37 \w 20.00 56.00 0.50 13.00 -- 28.00 24.00 -41.07 72 38 \w -51.00 -26.00 0.50 13.00 -- -32.00 -25.00 -19.56 50 39 \w -51.00 -26.00 0.50 13.00 -- -32.00 -25.00 19.98 50 40 \w 28.00 61.00 0.50 13.00 -- 32.00 23.00 108.37 66 41 \w -26.00 0.00 0.50 13.00 -- -40.00 60.00 -43.80 52 42 \w 24.00 49.00 0.50 13.00 -- 40.00 22.00 -56.41 50 43 \w -62.00 -37.00 0.50 13.00 -- -48.00 -23.00-158.02 50 44 \w 43.00 69.00 0.50 13.00 -- 56.00 22.00 21.91 52 45 \w -70.00 -44.00 0.50 13.00 -- -60.00 -22.00 100.33 52 46 \w -40.00 -14.00 0.50 13.00 -- -60.50 37.00 -32.59 52 47 \w -39.00 -14.00 0.50 13.00 -- -60.50 36.00 -55.24 50 48 \w -38.00 -13.00 0.50 13.00 -- -60.50 36.00 155.50 50 49 \w -71.00 -46.00 0.50 13.00 -- -60.50 -22.00 -92.62 50 50 \w -48.00 -22.00 0.50 13.00 -- -60.50 62.00 153.09 52 51 \w -43.00 -14.00 0.50 13.00 -- -60.50 41.00 -87.93 58 52 \w -45.00 -19.00 0.50 13.00 -- -60.50 51.00-139.28 52 53 \w -44.00 -18.00 0.50 13.00 -- -60.50 50.00-119.29 52 54 \w -49.00 -23.00 0.50 13.00 -- -60.50 60.00 101.19 52 55 \w -48.00 -22.00 0.50 13.00 -- -60.50 63.00 58.35 52 56 \w -45.00 -20.00 0.50 13.00 -- -60.50 64.00 118.52 50 57 \w 38.00 63.00 0.50 13.00 -- 66.63-125.00 90.00 50 58 \w 38.00 64.00 0.50 13.00 -- 66.63-125.00 150.00 52 59 \w 68.00 93.00 0.50 13.00 -- 66.63-125.00 90.00 50 60 \w 68.00 93.00 0.50 13.00 -- 66.63-125.00 150.00 50 61 \w 36.00 62.00 0.50 13.00 -- 66.63-125.00 0.00 52 62 \w 66.00 92.00 0.50 13.00 -- 66.63-125.00 -60.00 52 63 \w 35.00 61.00 0.50 13.00 -- 66.63-125.00 -60.00 52 64 \w 72.00 97.00 0.50 13.00 -- 69.94-125.00 0.00 50 65 \w 38.00 63.00 0.50 13.00 -- 69.94-125.00 0.00 50 66 \w 64.00 97.00 0.50 13.00 -- 69.94-125.00 -90.00 66 67 \w 36.00 62.00 0.50 13.00 -- 69.94-125.00 -90.00 52 68 \w 72.00 97.00 0.50 13.00 -- 69.94-125.00 60.00 50 69 \w 35.00 97.00 0.50 13.00 -- 69.94-125.00-150.00 124 70 \w 35.00 61.00 0.50 13.00 -- 69.94-125.00 60.00 52 71 \w 65.00 111.00 0.50 13.00 -- 72.71 20.00 61.76 92 72 \w 56.00 81.00 0.50 13.00 -- 72.71 21.00 95.34 50 73 \w 54.00 90.00 0.50 13.00 -- 72.71 21.00 -65.29 72 74 \w 90.00 116.00 0.50 13.00 -- 72.71 20.00 124.98 52 75 \w 60.00 86.00 0.50 13.00 -- 72.71 20.00 124.98 52 76 \w 73.00 98.00 0.50 13.00 -- 75.35-119.00 -66.87 50 77 \w 36.00 61.00 0.50 13.00 -- 75.35-119.00 -66.87 50 78 \w 54.00 87.00 0.50 13.00 -- 75.35 20.00 157.70 66 79 \w 96.00 121.00 0.50 13.00 -- 75.35 21.00 -31.40 50 80 \w 57.00 91.00 0.50 13.00 -- 75.35 21.00 -31.40 68 81 \w 75.00 101.00 0.50 13.00 -- 75.35-123.00 49.07 52 82 \w 87.00 113.00 0.50 13.00 -- 75.35 21.00 43.30 52 83 \w 35.00 61.00 0.50 13.00 -- 75.35-123.00 49.07 52 84 \w 60.00 93.00 0.50 13.00 -- 75.35 20.00-156.66 66 85 \w 57.00 83.00 0.50 13.00 -- 75.35 21.00 43.30 52 86 \w 77.00 105.00 0.50 13.00 -- 75.35-131.00 109.88 56 87 \w 41.00 67.00 0.50 13.00 -- 75.35-131.00 109.88 52 88 \w 79.00 113.00 0.50 13.00 -- 75.35 5.00 -56.09 68 89 \w 46.00 72.00 0.50 13.00 -- 75.35 5.00 -56.09 52 90 \w 97.00 122.00 0.50 13.00 -- 75.35 21.00 178.52 50 91 \w 57.00 83.00 0.50 13.00 -- 75.35 21.00 26.89 52 92 \w 59.00 88.00 0.50 13.00 -- 75.35 21.00 178.52 58 93 \w 49.00 74.00 0.50 13.00 -- 75.35 16.00 -49.09 50 94 \w 68.00 93.00 0.50 13.00 -- 75.35-110.00 128.74 50 95 \w 35.00 60.00 0.50 13.00 -- 75.35-110.00 128.74 50 96 \w 77.00 102.00 0.50 13.00 -- 75.35-125.00-131.60 50 97 \w 72.00 115.00 0.50 13.00 -- 75.35 5.00 108.03 86 98 \w 93.00 118.00 0.50 13.00 -- 75.35 16.00 -49.09 50 99 \w 41.00 67.00 0.50 13.00 -- 75.35 5.00 108.03 52 100 \w 35.00 65.00 0.50 13.00 -- 75.35-125.00-131.60 60 101 \w 91.00 116.00 0.50 13.00 -- 75.35 4.00-111.35 50 102 \w 41.00 109.00 0.50 13.00 -- 75.35 7.00 35.74 136 103 \w 40.00 84.00 0.50 13.00 -- 75.35 4.00-111.35 88 104 \w 59.00 89.00 0.50 13.00 -- 75.35 21.00-104.20 60 105 \w 67.00 93.00 0.50 13.00 -- 75.35-109.00 138.15 52 106 \w 57.00 87.00 0.50 13.00 -- 75.35 20.00-135.89 60 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix-Arc 150' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.2026049000 _diffrn_orient_matrix_UB_12 -0.0171335000 _diffrn_orient_matrix_UB_13 -0.0655577000 _diffrn_orient_matrix_UB_21 -0.0988035000 _diffrn_orient_matrix_UB_22 -0.0531377000 _diffrn_orient_matrix_UB_23 -0.1026275000 _diffrn_orient_matrix_UB_31 -0.0418779000 _diffrn_orient_matrix_UB_32 0.0422877000 _diffrn_orient_matrix_UB_33 -0.1552366000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_unetI/netI 0.0113 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.983 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 31684 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.549 _diffrn_reflns_theta_min 4.019 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.797 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.100a (Rigaku Oxford Diffraction, 2023) 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 yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.356 _exptl_crystal_description block _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.115 _exptl_crystal_size_mid 0.084 _exptl_crystal_size_min 0.078 _refine_diff_density_max 0.216 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.026 _refine_ls_abs_structure_details ; Flack x determined using 1920 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.14(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 332 _refine_ls_number_reflns 4518 _refine_ls_number_restraints 4 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0322 _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^)+(0.0524P)^2^+0.1342P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.0879 _reflns_Friedel_coverage 0.911 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.946 _reflns_number_gt 4274 _reflns_number_total 4518 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6sc04784j3.cif _cod_data_source_block cz-10-2 _cod_database_code 1577432 _shelx_shelxl_version_number 2019/2 _chemical_oxdiff_formula 'C27 H24 N2 O6' _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. ; _diffrn_oxdiff_digest_hkl ; 434c6fd3b6d936e7d5bd75792f4cc573e94edc ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2. Rigid body (RIGU) restrains C3, C4 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 3.a Ternary CH refined with riding coordinates: C11(H11) 3.b Secondary CH2 refined with riding coordinates: C9(H9A,H9B), C10(H10A,H10B), C12(H12A,H12B) 3.c Aromatic/amide H refined with riding coordinates: C2(H2), C4(H4), C6(H6), C13(H13), C25(H25), C26(H26), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35) ; _shelx_res_file ; TITL zh_yellow_auto_a.res in P2(1) cz-10-2.res created by SHELXL-2019/2 at 10:07:33 on 28-May-2025 REM Old TITL ZH_yellow_auto in P2(1)/m REM SHELXT solution in P2(1) REM R1 0.127, Rweak 0.039, Alpha 0.001, Orientation as input REM Flack x = 0.366 ( 0.089 ) from Parsons' quotients REM Formula found by SHELXT: C27 C14 CELL 1.54184 6.736932 21.997076 7.830722 90 94.2746 90 ZERR 2 0.000072 0.000256 0.00009 0 0.001 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 54 48 4 12 RIGU C3 C4 L.S. 4 PLAN 5 TEMP -153 CONF BOND $H MORE -1 fmap 2 acta REM REM REM WGHT 0.052400 0.134200 FVAR 4.09423 O8 4 0.562303 0.580078 0.774666 11.00000 0.04152 0.05919 = 0.04106 0.00758 -0.00099 0.01149 O17 4 0.794550 0.622050 0.961081 11.00000 0.05228 0.06695 = 0.05364 -0.00146 -0.00384 0.00622 O19 4 0.921078 0.326096 0.639225 11.00000 0.06027 0.05149 = 0.07929 0.01446 0.00443 0.01039 O20 4 0.650318 0.376315 0.572047 11.00000 0.04604 0.06227 = 0.07567 0.00779 -0.00605 -0.00145 O22 4 1.456522 0.423055 0.983371 11.00000 0.03790 0.08684 = 0.09117 0.02763 0.00107 0.00914 O23 4 1.420449 0.514843 1.080325 11.00000 0.04480 0.09066 = 0.05477 0.01342 -0.00635 -0.00796 N18 3 0.817759 0.371469 0.644259 11.00000 0.04539 0.05115 = 0.06078 0.01747 0.00569 0.00156 N21 3 1.360330 0.469685 1.000515 11.00000 0.03476 0.07490 = 0.05538 0.02785 0.00614 0.00355 C1 1 0.854407 0.524782 0.845147 11.00000 0.03813 0.05717 = 0.03570 0.01419 0.00325 0.00334 C2 1 1.045257 0.522443 0.929058 11.00000 0.03728 0.06228 = 0.03561 0.01383 0.00438 0.00015 AFIX 43 H2 2 1.096604 0.555916 0.995084 11.00000 -1.20000 AFIX 0 C3 1 1.156535 0.470668 0.913755 11.00000 0.03362 0.06620 = 0.04103 0.01910 0.00257 -0.00133 C4 1 1.088187 0.420507 0.823968 11.00000 0.03624 0.06296 = 0.05051 0.02439 0.00964 0.00933 AFIX 43 H4 2 1.167093 0.384892 0.817799 11.00000 -1.20000 AFIX 0 C5 1 0.898312 0.424051 0.742333 11.00000 0.03854 0.05332 = 0.04469 0.01766 0.00415 0.00141 C6 1 0.781512 0.475458 0.750575 11.00000 0.03632 0.05595 = 0.04002 0.01582 0.00273 0.00410 AFIX 43 H6 2 0.652893 0.476896 0.692073 11.00000 -1.20000 AFIX 0 C7 1 0.736796 0.581187 0.868302 11.00000 0.04251 0.05957 = 0.03546 0.00944 0.00339 0.00362 C9 1 0.428496 0.632118 0.792204 11.00000 0.04355 0.06070 = 0.03995 0.00248 0.00424 0.01151 AFIX 23 H9A 2 0.477625 0.657271 0.891346 11.00000 -1.20000 H9B 2 0.293557 0.617362 0.812927 11.00000 -1.20000 AFIX 0 C10 1 0.419293 0.669986 0.631310 11.00000 0.03789 0.04783 = 0.04010 0.00161 0.00371 0.00562 AFIX 23 H10A 2 0.554456 0.685341 0.613978 11.00000 -1.20000 H10B 2 0.332673 0.705609 0.646908 11.00000 -1.20000 AFIX 0 C11 1 0.340302 0.635429 0.469989 11.00000 0.03412 0.04329 = 0.03932 0.00302 0.00295 0.00701 AFIX 13 H11 2 0.432802 0.600730 0.453361 11.00000 -1.20000 AFIX 0 C12 1 0.340311 0.676583 0.310058 11.00000 0.04012 0.04880 = 0.04072 0.00698 0.00423 0.00746 AFIX 23 H12A 2 0.274544 0.654754 0.210763 11.00000 -1.20000 H12B 2 0.261471 0.713600 0.329409 11.00000 -1.20000 AFIX 0 C13 1 0.545337 0.694955 0.268317 11.00000 0.04332 0.05885 = 0.04285 0.01129 0.00872 0.00957 AFIX 43 H13 2 0.628459 0.664157 0.227303 11.00000 -1.20000 AFIX 0 C14 1 0.619462 0.749719 0.283536 11.00000 0.05217 0.06806 = 0.06957 0.01532 0.01259 0.00029 H14A 2 0.761317 0.759130 0.257320 11.00000 0.08080 H14B 2 0.538650 0.782906 0.327766 11.00000 0.07760 C15 1 0.133011 0.609220 0.483582 11.00000 0.03367 0.05281 = 0.03726 0.00694 0.00335 0.00523 C16 1 -0.015798 0.643263 0.535210 11.00000 0.03827 0.06072 = 0.05318 0.00288 0.00654 0.00965 H16A 2 -0.151747 0.625831 0.537616 11.00000 0.05465 H16B 2 0.006163 0.685620 0.567038 11.00000 0.04992 C24 1 0.034904 0.423979 0.310392 11.00000 0.03430 0.05259 = 0.03541 0.01162 0.00050 -0.00417 C25 1 -0.111351 0.468652 0.282924 11.00000 0.03093 0.06003 = 0.03897 0.00888 -0.00197 -0.00238 AFIX 43 H25 2 -0.234597 0.458242 0.223226 11.00000 -1.20000 AFIX 0 C26 1 -0.081606 0.527373 0.340084 11.00000 0.03003 0.05704 = 0.03792 0.00968 0.00069 0.00582 AFIX 43 H26 2 -0.184533 0.556508 0.318587 11.00000 -1.20000 AFIX 0 C27 1 0.097566 0.545187 0.429510 11.00000 0.03310 0.05247 = 0.03514 0.00871 0.00427 0.00335 C28 1 0.240173 0.499923 0.461954 11.00000 0.03182 0.05198 = 0.04210 0.00783 -0.00453 -0.00003 AFIX 43 H28 2 0.362009 0.510005 0.524447 11.00000 -1.20000 AFIX 0 C29 1 0.209892 0.440947 0.406144 11.00000 0.03463 0.04744 = 0.04566 0.00984 -0.00529 0.00213 AFIX 43 H29 2 0.309737 0.411263 0.433213 11.00000 -1.20000 AFIX 0 C30 1 0.010101 0.362241 0.233086 11.00000 0.03959 0.05275 = 0.03639 0.01297 -0.00337 -0.00671 C31 1 -0.177369 0.341178 0.169421 11.00000 0.04001 0.05890 = 0.05843 0.01126 -0.00655 -0.00760 AFIX 43 H31 2 -0.292148 0.365125 0.184327 11.00000 -1.20000 AFIX 0 C32 1 -0.197591 0.285909 0.085041 11.00000 0.05232 0.06832 = 0.05842 0.00816 -0.01357 -0.01875 AFIX 43 H32 2 -0.325588 0.272859 0.040566 11.00000 -1.20000 AFIX 0 C33 1 -0.035079 0.249854 0.065007 11.00000 0.06253 0.06057 = 0.04916 0.00103 -0.00637 -0.01101 AFIX 43 H33 2 -0.049864 0.211935 0.007396 11.00000 -1.20000 AFIX 0 C34 1 0.150537 0.269329 0.129622 11.00000 0.05383 0.05938 = 0.05617 -0.00136 -0.00066 -0.00177 AFIX 43 H34 2 0.263867 0.244411 0.117780 11.00000 -1.20000 AFIX 0 C35 1 0.172252 0.325015 0.211607 11.00000 0.04161 0.05747 = 0.04937 0.00303 -0.00351 -0.00498 AFIX 43 H35 2 0.301159 0.337953 0.254021 11.00000 -1.20000 AFIX 0 HKLF 4 REM zh_yellow_auto_a.res in P2(1) REM wR2 = 0.0879, GooF = S = 1.056, Restrained GooF = 1.056 for all data REM R1 = 0.0322 for 4274 Fo > 4sig(Fo) and 0.0343 for all 4518 data REM 332 parameters refined using 4 restraints END WGHT 0.0524 0.1342 REM Highest difference peak 0.216, deepest hole -0.183, 1-sigma level 0.026 Q1 1 1.4383 0.3923 0.9032 11.00000 0.05 0.22 Q2 1 0.5969 0.3508 0.5011 11.00000 0.05 0.13 Q3 1 1.3309 0.4346 0.9376 11.00000 0.05 0.12 Q4 1 0.8768 0.2979 0.5625 11.00000 0.05 0.12 Q5 1 0.1159 0.4310 0.3604 11.00000 0.05 0.12 ; _shelx_res_checksum 61204 _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 1.287 _oxdiff_exptl_absorpt_empirical_full_min 0.807 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 O8 O 0.5623(2) 0.58008(8) 0.7747(2) 0.0475(4) Uani 1 1 d . . . . . O17 O 0.7946(3) 0.62205(10) 0.9611(2) 0.0580(5) Uani 1 1 d . . . . . O19 O 0.9211(3) 0.32610(9) 0.6392(3) 0.0637(5) Uani 1 1 d . . . . . O20 O 0.6503(3) 0.37632(10) 0.5720(3) 0.0619(5) Uani 1 1 d . . . . . O22 O 1.4565(3) 0.42306(11) 0.9834(3) 0.0722(6) Uani 1 1 d . . . . . O23 O 1.4204(3) 0.51484(11) 1.0803(3) 0.0639(5) Uani 1 1 d . . . . . N18 N 0.8178(3) 0.37147(11) 0.6443(3) 0.0524(5) Uani 1 1 d . . . . . N21 N 1.3603(3) 0.46969(13) 1.0005(3) 0.0549(6) Uani 1 1 d . . . . . C1 C 0.8544(4) 0.52478(12) 0.8451(3) 0.0436(5) Uani 1 1 d . . . . . C2 C 1.0453(3) 0.52244(13) 0.9291(3) 0.0450(5) Uani 1 1 d . . . . . H2 H 1.096604 0.555916 0.995084 0.054 Uiso 1 1 calc R U . . . C3 C 1.1565(3) 0.47067(14) 0.9138(3) 0.0470(6) Uani 1 1 d . . . . . C4 C 1.0882(4) 0.42051(13) 0.8240(3) 0.0496(6) Uani 1 1 d . . . . . H4 H 1.167093 0.384892 0.817799 0.060 Uiso 1 1 calc R U . . . C5 C 0.8983(4) 0.42405(12) 0.7423(3) 0.0455(5) Uani 1 1 d . . . . . C6 C 0.7815(3) 0.47546(12) 0.7506(3) 0.0441(5) Uani 1 1 d . . . . . H6 H 0.652893 0.476896 0.692073 0.053 Uiso 1 1 calc R U . . . C7 C 0.7368(4) 0.58119(13) 0.8683(3) 0.0458(5) Uani 1 1 d . . . . . C9 C 0.4285(4) 0.63212(13) 0.7922(3) 0.0480(6) Uani 1 1 d . . . . . H9A H 0.477625 0.657271 0.891346 0.058 Uiso 1 1 calc R U . . . H9B H 0.293557 0.617362 0.812927 0.058 Uiso 1 1 calc R U . . . C10 C 0.4193(3) 0.66999(11) 0.6313(3) 0.0419(5) Uani 1 1 d . . . . . H10A H 0.554456 0.685341 0.613978 0.050 Uiso 1 1 calc R U . . . H10B H 0.332673 0.705609 0.646908 0.050 Uiso 1 1 calc R U . . . C11 C 0.3403(3) 0.63543(11) 0.4700(3) 0.0389(5) Uani 1 1 d . . . . . H11 H 0.432802 0.600730 0.453361 0.047 Uiso 1 1 calc R U . . . C12 C 0.3403(4) 0.67658(11) 0.3101(3) 0.0432(5) Uani 1 1 d . . . . . H12A H 0.274544 0.654754 0.210763 0.052 Uiso 1 1 calc R U . . . H12B H 0.261471 0.713600 0.329409 0.052 Uiso 1 1 calc R U . . . C13 C 0.5453(4) 0.69496(13) 0.2683(3) 0.0481(6) Uani 1 1 d . . . . . H13 H 0.628459 0.664157 0.227303 0.058 Uiso 1 1 calc R U . . . C14 C 0.6195(5) 0.74972(16) 0.2835(4) 0.0629(7) Uani 1 1 d . . . . . H14A H 0.761(6) 0.7591(18) 0.257(5) 0.081(11) Uiso 1 1 d . . . . . H14B H 0.539(6) 0.7829(17) 0.328(5) 0.078(11) Uiso 1 1 d . . . . . C15 C 0.1330(3) 0.60922(11) 0.4836(3) 0.0412(5) Uani 1 1 d . . . . . C16 C -0.0158(4) 0.64326(14) 0.5352(4) 0.0506(6) Uani 1 1 d . . . . . H16A H -0.152(5) 0.6258(14) 0.538(4) 0.055(8) Uiso 1 1 d . . . . . H16B H 0.006(4) 0.6856(14) 0.567(4) 0.050(8) Uiso 1 1 d . . . . . C24 C 0.0349(3) 0.42398(11) 0.3104(3) 0.0409(5) Uani 1 1 d . . . . . C25 C -0.1114(3) 0.46865(12) 0.2829(3) 0.0435(5) Uani 1 1 d . . . . . H25 H -0.234597 0.458242 0.223226 0.052 Uiso 1 1 calc R U . . . C26 C -0.0816(3) 0.52737(12) 0.3401(3) 0.0418(5) Uani 1 1 d . . . . . H26 H -0.184533 0.556508 0.318587 0.050 Uiso 1 1 calc R U . . . C27 C 0.0976(3) 0.54519(11) 0.4295(3) 0.0401(5) Uani 1 1 d . . . . . C28 C 0.2402(3) 0.49992(12) 0.4620(3) 0.0423(5) Uani 1 1 d . . . . . H28 H 0.362009 0.510005 0.524447 0.051 Uiso 1 1 calc R U . . . C29 C 0.2099(3) 0.44095(11) 0.4061(3) 0.0430(5) Uani 1 1 d . . . . . H29 H 0.309737 0.411263 0.433213 0.052 Uiso 1 1 calc R U . . . C30 C 0.0101(4) 0.36224(12) 0.2331(3) 0.0432(5) Uani 1 1 d . . . . . C31 C -0.1774(4) 0.34118(13) 0.1694(4) 0.0530(6) Uani 1 1 d . . . . . H31 H -0.292148 0.365125 0.184327 0.064 Uiso 1 1 calc R U . . . C32 C -0.1976(5) 0.28591(14) 0.0850(4) 0.0606(7) Uani 1 1 d . . . . . H32 H -0.325588 0.272859 0.040566 0.073 Uiso 1 1 calc R U . . . C33 C -0.0351(4) 0.24985(15) 0.0650(4) 0.0579(7) Uani 1 1 d . . . . . H33 H -0.049864 0.211935 0.007396 0.070 Uiso 1 1 calc R U . . . C34 C 0.1505(4) 0.26933(13) 0.1296(4) 0.0567(7) Uani 1 1 d . . . . . H34 H 0.263867 0.244411 0.117780 0.068 Uiso 1 1 calc R U . . . C35 C 0.1723(4) 0.32502(13) 0.2116(3) 0.0498(6) Uani 1 1 d . . . . . H35 H 0.301159 0.337953 0.254021 0.060 Uiso 1 1 calc R U . . . 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 O8 0.0415(8) 0.0592(10) 0.0411(8) 0.0076(8) -0.0010(7) 0.0115(8) O17 0.0523(10) 0.0669(12) 0.0536(10) -0.0015(10) -0.0038(8) 0.0062(9) O19 0.0603(12) 0.0515(11) 0.0793(14) 0.0145(10) 0.0044(10) 0.0104(9) O20 0.0460(10) 0.0623(11) 0.0757(13) 0.0078(10) -0.0061(9) -0.0014(9) O22 0.0379(10) 0.0868(16) 0.0912(16) 0.0276(13) 0.0011(10) 0.0091(10) O23 0.0448(10) 0.0907(16) 0.0548(11) 0.0134(11) -0.0063(8) -0.0080(10) N18 0.0454(11) 0.0511(12) 0.0608(13) 0.0175(10) 0.0057(10) 0.0016(10) N21 0.0348(10) 0.0749(15) 0.0554(13) 0.0278(12) 0.0061(9) 0.0036(11) C1 0.0381(11) 0.0572(13) 0.0357(11) 0.0142(10) 0.0033(9) 0.0033(10) C2 0.0373(11) 0.0623(15) 0.0356(11) 0.0138(11) 0.0044(9) 0.0002(10) C3 0.0336(11) 0.0662(15) 0.0410(12) 0.0191(11) 0.0026(9) -0.0013(11) C4 0.0362(11) 0.0630(16) 0.0505(13) 0.0244(12) 0.0096(10) 0.0093(11) C5 0.0385(11) 0.0533(14) 0.0447(12) 0.0177(11) 0.0041(9) 0.0014(10) C6 0.0363(11) 0.0560(13) 0.0400(11) 0.0158(11) 0.0027(9) 0.0041(10) C7 0.0425(12) 0.0596(15) 0.0355(11) 0.0094(11) 0.0034(9) 0.0036(11) C9 0.0436(12) 0.0607(15) 0.0399(12) 0.0025(11) 0.0042(9) 0.0115(11) C10 0.0379(11) 0.0478(13) 0.0401(12) 0.0016(10) 0.0037(9) 0.0056(9) C11 0.0341(10) 0.0433(12) 0.0393(11) 0.0030(10) 0.0029(9) 0.0070(9) C12 0.0401(12) 0.0488(13) 0.0407(12) 0.0070(10) 0.0042(9) 0.0075(10) C13 0.0433(12) 0.0589(15) 0.0429(12) 0.0113(11) 0.0087(10) 0.0096(11) C14 0.0522(15) 0.0681(19) 0.0696(19) 0.0153(15) 0.0126(14) 0.0003(14) C15 0.0337(11) 0.0528(13) 0.0373(11) 0.0069(10) 0.0034(8) 0.0052(9) C16 0.0383(12) 0.0607(17) 0.0532(14) 0.0029(12) 0.0065(11) 0.0096(11) C24 0.0343(10) 0.0526(13) 0.0354(11) 0.0116(10) 0.0005(8) -0.0042(9) C25 0.0309(10) 0.0600(14) 0.0390(11) 0.0089(10) -0.0020(9) -0.0024(10) C26 0.0300(10) 0.0570(14) 0.0379(11) 0.0097(10) 0.0007(8) 0.0058(9) C27 0.0331(10) 0.0525(13) 0.0351(11) 0.0087(10) 0.0043(8) 0.0033(9) C28 0.0318(10) 0.0520(13) 0.0421(12) 0.0078(10) -0.0045(9) 0.0000(10) C29 0.0346(11) 0.0474(13) 0.0457(12) 0.0098(10) -0.0053(9) 0.0021(9) C30 0.0396(11) 0.0527(14) 0.0364(11) 0.0130(10) -0.0034(9) -0.0067(10) C31 0.0400(13) 0.0589(15) 0.0584(15) 0.0113(12) -0.0065(11) -0.0076(11) C32 0.0523(15) 0.0683(18) 0.0584(16) 0.0082(14) -0.0136(13) -0.0187(14) C33 0.0625(16) 0.0606(16) 0.0492(14) 0.0010(12) -0.0064(12) -0.0110(14) C34 0.0538(15) 0.0594(17) 0.0562(15) -0.0014(13) -0.0007(12) -0.0018(12) C35 0.0416(13) 0.0575(15) 0.0494(13) 0.0030(11) -0.0035(10) -0.0050(11) 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' 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0459 0 1 -1 0.0545 0 -1 -1 0.0608 0 -1 0 0.0323 0 0 1 0.0479 -1 0 0 0.0425 1 -2 1 0.0395 1 1 0 0.0298 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 C7 O8 C9 117.0(2) . . ? O19 N18 O20 124.3(3) . . ? O19 N18 C5 118.1(2) . . ? O20 N18 C5 117.6(2) . . ? O22 N21 O23 125.2(2) . . ? O22 N21 C3 116.1(3) . . ? O23 N21 C3 118.7(2) . . ? C2 C1 C7 116.8(2) . . ? C6 C1 C2 120.0(2) . . ? C6 C1 C7 123.2(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 C1 118.5(3) . . ? C3 C2 H2 120.7 . . ? C2 C3 N21 117.6(3) . . ? C4 C3 N21 119.1(2) . . ? C4 C3 C2 123.2(2) . . ? C3 C4 H4 121.5 . . ? C3 C4 C5 117.0(2) . . ? C5 C4 H4 121.5 . . ? C4 C5 N18 119.2(2) . . ? C6 C5 N18 118.6(2) . . ? C6 C5 C4 122.2(3) . . ? C1 C6 H6 120.5 . . ? C5 C6 C1 119.1(2) . . ? C5 C6 H6 120.5 . . ? O8 C7 C1 111.8(2) . . ? O17 C7 O8 125.2(2) . . ? O17 C7 C1 123.0(2) . . ? O8 C9 H9A 109.7 . . ? O8 C9 H9B 109.7 . . ? O8 C9 C10 109.85(18) . . ? H9A C9 H9B 108.2 . . ? C10 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C9 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C9 C10 C11 113.8(2) . . ? H10A C10 H10B 107.7 . . ? C11 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? C10 C11 H11 107.7 . . ? C10 C11 C12 110.85(19) . . ? C12 C11 H11 107.7 . . ? C15 C11 C10 113.18(18) . . ? C15 C11 H11 107.7 . . ? C15 C11 C12 109.52(18) . . ? C11 C12 H12A 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C13 C12 C11 112.99(19) . . ? C13 C12 H12A 109.0 . . ? C13 C12 H12B 109.0 . . ? C12 C13 H13 117.2 . . ? C14 C13 C12 125.5(3) . . ? C14 C13 H13 117.2 . . ? C13 C14 H14A 122(2) . . ? C13 C14 H14B 120(2) . . ? H14A C14 H14B 118(3) . . ? C16 C15 C11 121.4(2) . . ? C16 C15 C27 120.6(2) . . ? C27 C15 C11 117.92(19) . . ? C15 C16 H16A 120.1(18) . . ? C15 C16 H16B 120.7(18) . . ? H16A C16 H16B 119(3) . . ? C25 C24 C29 116.8(2) . . ? C25 C24 C30 121.5(2) . . ? C29 C24 C30 121.6(2) . . ? C24 C25 H25 119.1 . . ? C26 C25 C24 121.7(2) . . ? C26 C25 H25 119.1 . . ? C25 C26 H26 119.3 . . ? C25 C26 C27 121.5(2) . . ? C27 C26 H26 119.3 . . ? C26 C27 C15 121.4(2) . . ? C28 C27 C15 122.1(2) . . ? C28 C27 C26 116.5(2) . . ? C27 C28 H28 119.0 . . ? C29 C28 C27 122.0(2) . . ? C29 C28 H28 119.0 . . ? C24 C29 H29 119.4 . . ? C28 C29 C24 121.3(2) . . ? C28 C29 H29 119.4 . . ? C31 C30 C24 121.1(2) . . ? C35 C30 C24 121.5(2) . . ? C35 C30 C31 117.3(2) . . ? C30 C31 H31 119.5 . . ? C32 C31 C30 120.9(3) . . ? C32 C31 H31 119.5 . . ? C31 C32 H32 119.6 . . ? C33 C32 C31 120.8(3) . . ? C33 C32 H32 119.6 . . ? C32 C33 H33 120.4 . . ? C32 C33 C34 119.2(3) . . ? C34 C33 H33 120.4 . . ? C33 C34 H34 119.8 . . ? C33 C34 C35 120.3(3) . . ? C35 C34 H34 119.8 . . ? C30 C35 C34 121.5(2) . . ? C30 C35 H35 119.3 . . ? C34 C35 H35 119.3 . . ? 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 O8 C7 1.339(3) . ? O8 C9 1.470(3) . ? O17 C7 1.202(3) . ? O19 N18 1.219(3) . ? O20 N18 1.228(3) . ? O22 N21 1.226(3) . ? O23 N21 1.226(3) . ? N18 C5 1.470(4) . ? N21 C3 1.486(3) . ? C1 C2 1.401(3) . ? C1 C6 1.383(4) . ? C1 C7 1.490(4) . ? C2 H2 0.9500 . ? C2 C3 1.374(4) . ? C3 C4 1.370(4) . ? C4 H4 0.9500 . ? C4 C5 1.389(3) . ? C5 C6 1.382(4) . ? C6 H6 0.9500 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.508(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.535(3) . ? C11 H11 1.0000 . ? C11 C12 1.545(3) . ? C11 C15 1.522(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 C13 1.498(3) . ? C13 H13 0.9500 . ? C13 C14 1.306(4) . ? C14 H14A 1.01(4) . ? C14 H14B 0.99(4) . ? C15 C16 1.338(3) . ? C15 C27 1.485(4) . ? C16 H16A 0.99(3) . ? C16 H16B 0.97(3) . ? C24 C25 1.397(3) . ? C24 C29 1.400(3) . ? C24 C30 1.491(4) . ? C25 H25 0.9500 . ? C25 C26 1.377(4) . ? C26 H26 0.9500 . ? C26 C27 1.405(3) . ? C27 C28 1.394(3) . ? C28 H28 0.9500 . ? C28 C29 1.379(3) . ? C29 H29 0.9500 . ? C30 C31 1.402(3) . ? C30 C35 1.385(4) . ? C31 H31 0.9500 . ? C31 C32 1.386(4) . ? C32 H32 0.9500 . ? C32 C33 1.370(5) . ? C33 H33 0.9500 . ? C33 C34 1.382(4) . ? C34 H34 0.9500 . ? C34 C35 1.386(4) . ? C35 H35 0.9500 . ? 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 O8 C9 C10 C11 60.6(3) . . . . ? O19 N18 C5 C4 0.5(3) . . . . ? O19 N18 C5 C6 -179.2(2) . . . . ? O20 N18 C5 C4 -179.2(2) . . . . ? O20 N18 C5 C6 1.0(3) . . . . ? O22 N21 C3 C2 -179.4(2) . . . . ? O22 N21 C3 C4 0.9(3) . . . . ? O23 N21 C3 C2 -0.5(3) . . . . ? O23 N21 C3 C4 179.9(2) . . . . ? N18 C5 C6 C1 178.8(2) . . . . ? N21 C3 C4 C5 -178.8(2) . . . . ? C1 C2 C3 N21 178.63(19) . . . . ? C1 C2 C3 C4 -1.7(3) . . . . ? C2 C1 C6 C5 0.8(3) . . . . ? C2 C1 C7 O8 176.24(19) . . . . ? C2 C1 C7 O17 -4.0(3) . . . . ? C2 C3 C4 C5 1.6(3) . . . . ? C3 C4 C5 N18 -180.0(2) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -1.0(3) . . . . ? C6 C1 C2 C3 0.5(3) . . . . ? C6 C1 C7 O8 -5.7(3) . . . . ? C6 C1 C7 O17 174.1(2) . . . . ? C7 O8 C9 C10 109.0(2) . . . . ? C7 C1 C2 C3 178.6(2) . . . . ? C7 C1 C6 C5 -177.2(2) . . . . ? C9 O8 C7 O17 -2.4(3) . . . . ? C9 O8 C7 C1 177.41(19) . . . . ? C9 C10 C11 C12 -178.54(18) . . . . ? C9 C10 C11 C15 58.0(3) . . . . ? C10 C11 C12 C13 65.1(3) . . . . ? C10 C11 C15 C16 49.5(3) . . . . ? C10 C11 C15 C27 -133.4(2) . . . . ? C11 C12 C13 C14 -110.5(3) . . . . ? C11 C15 C27 C26 -140.9(2) . . . . ? C11 C15 C27 C28 38.1(3) . . . . ? C12 C11 C15 C16 -74.7(3) . . . . ? C12 C11 C15 C27 102.3(2) . . . . ? C15 C11 C12 C13 -169.3(2) . . . . ? C15 C27 C28 C29 -177.6(2) . . . . ? C16 C15 C27 C26 36.2(3) . . . . ? C16 C15 C27 C28 -144.9(2) . . . . ? C24 C25 C26 C27 -0.2(3) . . . . ? C24 C30 C31 C32 174.6(2) . . . . ? C24 C30 C35 C34 -175.7(2) . . . . ? C25 C24 C29 C28 -3.6(3) . . . . ? C25 C24 C30 C31 -17.2(3) . . . . ? C25 C24 C30 C35 158.8(2) . . . . ? C25 C26 C27 C15 177.0(2) . . . . ? C25 C26 C27 C28 -2.1(3) . . . . ? C26 C27 C28 C29 1.5(3) . . . . ? C27 C28 C29 C24 1.4(4) . . . . ? C29 C24 C25 C26 3.0(3) . . . . ? C29 C24 C30 C31 166.3(2) . . . . ? C29 C24 C30 C35 -17.8(3) . . . . ? C30 C24 C25 C26 -173.7(2) . . . . ? C30 C24 C29 C28 173.1(2) . . . . ? C30 C31 C32 C33 1.4(4) . . . . ? C31 C30 C35 C34 0.4(4) . . . . ? C31 C32 C33 C34 -0.2(4) . . . . ? C32 C33 C34 C35 -0.9(4) . . . . ? C33 C34 C35 C30 0.8(4) . . . . ? C35 C30 C31 C32 -1.5(4) . . . . ? 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 0.0000 1.0000 -0.0001 -0.0171 -0.0531 0.0423 -0.0000 1.0001 -0.9997 0.0484 0.0495 0.1975 -0.0001 -1.0000 -0.9996 0.0826 0.1557 0.1129 -0.0000 -1.0000 0.0001 0.0171 0.0531 -0.0423 0.0001 -0.0001 0.9997 -0.0655 -0.1026 -0.1552 -0.9997 -0.0013 0.0003 -0.2025 0.0988 0.0418 0.9997 -1.9987 0.9995 0.1713 -0.0951 -0.2815 0.9997 1.0013 -0.0004 0.1854 -0.1519 0.0005