#------------------------------------------------------------------------------ #$Date: 2026-06-28 02:04:10 +0100 (Sun, 28 Jun 2026) $ #$Revision: 306672 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064460.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_7064460 loop_ _publ_author_name 'Vos, Cyler W.' 'Croke, Rylan' 'Lin, Jian-Bin' 'Kozak, Christopher M.' _publ_section_title ; Ring-Opening Polymerization of Lactide and Ring-Opening Copolymerization of Cyclohexene Oxide and Phthalic Anhydride by Multinuclear Complexes of Zinc, Magnesium and Potassium ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ01550F _journal_year 2026 _chemical_formula_moiety 'C48 H66 Mg0.94 N4 O12 Zn2.06' _chemical_formula_sum 'C48 H66 Mg0.94 N4 O12 Zn2.06' _chemical_formula_weight 1048.45 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2026-06-16 _audit_creation_method ; Olex2 1.5-ac6-016 (compiled 2024.01.13 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6897) ; _audit_update_record ; 2026-06-16 deposited with the CCDC. 2026-06-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.071(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.0688(3) _cell_length_b 12.4865(2) _cell_length_c 29.3684(5) _cell_measurement_reflns_used 20589 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 45.1000 _cell_measurement_theta_min 2.5610 _cell_volume 4773.68(16) _computing_cell_refinement 'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 43.119a 64-bit (release 08-04-2024))' _computing_data_reduction 'CrysAlisPro 1.171.43.119a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 1.000 _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 -83.00 -30.00 0.50 35.23 -- -41.61 119.00 121.00 106 2 \w -108.00 -50.00 0.50 35.23 -- -41.61 156.00 -82.00 116 3 \w 52.00 115.00 0.50 35.23 -- 42.86 156.00 -82.00 126 4 \w 9.00 83.00 0.50 35.23 -- 42.86-119.00 36.00 148 5 \w 29.00 107.00 0.50 35.23 -- 42.86-156.00-120.00 156 6 \w -42.00 -16.00 0.50 35.23 -- -41.61 -84.00 57.61 52 7 \w -39.00 -12.00 0.50 35.23 -- -41.61 -92.00 96.69 54 8 \w -31.00 9.00 0.50 35.23 -- 42.86 -19.00 60.00 80 9 \w -29.00 66.00 0.50 35.23 -- 42.86 -77.00 30.00 190 10 \w 27.00 66.00 0.50 35.23 -- 42.86 -77.00 30.00 78 11 \w 21.00 84.00 0.50 35.23 -- 42.86 77.00 90.00 126 12 \w -18.00 8.00 0.50 35.23 -- 42.86 -37.00 -30.00 52 13 \w 29.00 114.00 0.50 35.23 -- 42.86 57.00 150.00 170 14 \w 87.00 113.00 0.50 35.23 -- 42.86 178.00 90.00 52 15 \w -18.00 7.00 0.50 35.23 -- 42.86 -19.00 -90.00 50 16 \w -31.00 7.00 0.50 35.23 -- 42.86 -19.00 30.00 76 17 \w 30.00 97.00 0.50 35.23 -- 42.86 68.00 -2.15 134 18 \w -28.00 8.00 0.50 35.23 -- 42.86 -19.00 120.00 72 19 \w -30.00 7.00 0.50 35.23 -- 42.86 -19.00-150.00 74 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0502208000 _diffrn_orient_matrix_UB_12 -0.0112574000 _diffrn_orient_matrix_UB_13 -0.0060927000 _diffrn_orient_matrix_UB_21 -0.0123835000 _diffrn_orient_matrix_UB_22 -0.0552392000 _diffrn_orient_matrix_UB_23 -0.0017190000 _diffrn_orient_matrix_UB_31 -0.0171379000 _diffrn_orient_matrix_UB_32 0.0069616000 _diffrn_orient_matrix_UB_33 -0.0234045000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_unetI/netI 0.0279 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_number 58548 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.507 _diffrn_reflns_theta_min 2.581 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.112 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.90701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.119a (Rigaku Oxford Diffraction, 2024) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.459 _exptl_crystal_description prism _exptl_crystal_F_000 2204 _exptl_crystal_size_max 0.121 _exptl_crystal_size_mid 0.064 _exptl_crystal_size_min 0.039 _refine_diff_density_max 0.461 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 311 _refine_ls_number_reflns 7302 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0292 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+3.9753P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.0701 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6123 _reflns_number_total 7302 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj01550f2.cif _cod_data_source_block cv-305cold_mo _cod_database_code 7064460 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula C26H36MgN2O8Zn _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. ; _shelx_estimated_absorpt_t_max 0.958 _shelx_estimated_absorpt_t_min 0.877 _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. Shared sites {Zn2, Mg1} 3. Uiso/Uaniso restraints and constraints Uanis(Zn2) = Uanis(Mg1) 4. Others Sof(Mg1)=0.5*(1-FVAR(2)) Sof(Zn2)=0.5*FVAR(2) 5.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C16(H16A,H16B), C19(H19A,H19B), C20(H20A,H20B) 5.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C12(H12), C14(H14) 5.c Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C) ; _shelx_res_file ; TITL cv-305cold_mo_a.res in I2/a cv-305cold_mo.res created by SHELXL-2018/3 at 09:14:33 on 09-Jun-2026 REM Old TITL CV-305 Cold_Mo in I2/a REM SHELXT solution in I2/a: R1 0.074, Rweak 0.004, Alpha 0.023 REM 0.371 for 232 systematic absences, Orientation as input REM Formula found by SHELXT: C48 N6 O10 Mg1 Zn2 CELL 0.71073 13.0688 12.4865 29.3684 90 95.071 90 ZERR 4 0.0003 0.0002 0.0005 0 0.002 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Mg N O Zn UNIT 192 264 3.77 16 48 8.23 EADP Zn2 Mg1 EXYZ Zn2 Mg1 L.S. 15 0 0 PLAN 1 SIZE 0.039 0.064 0.121 TEMP -173(2) CONF BOND LIST 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.032100 3.975300 FVAR 0.18284 0.05865 ZN1 6 0.689238 0.328955 0.609882 11.00000 0.01421 0.01109 = 0.00969 0.00192 -0.00005 -0.00096 PART 3 ZN2 6 0.750000 0.400105 0.500000 20.50000 0.01244 0.01046 = 0.00898 0.00000 0.00164 0.00000 PART 4 MG1 3 0.750000 0.400105 0.500000 -20.50000 0.01244 0.01046 = 0.00898 0.00000 0.00164 0.00000 PART 0 O1 5 0.552543 0.306183 0.628060 11.00000 0.01754 0.02447 = 0.01936 -0.00332 0.00296 -0.00676 O2 5 0.425552 0.146797 0.667869 11.00000 0.04035 0.02708 = 0.04259 0.00073 0.00858 -0.01657 O3 5 0.731895 0.436856 0.566016 11.00000 0.01702 0.00850 = 0.01046 -0.00009 0.00237 0.00087 O4 5 0.637412 0.536594 0.497320 11.00000 0.01474 0.01254 = 0.00918 -0.00069 -0.00065 0.00175 O5 5 0.638673 0.289947 0.493671 11.00000 0.01519 0.01323 = 0.01449 0.00058 0.00080 -0.00157 O6 5 0.670085 0.208276 0.561493 11.00000 0.02617 0.01330 = 0.01412 0.00040 -0.00117 -0.00152 N1 4 0.720322 0.444678 0.667017 11.00000 0.01154 0.01354 = 0.01054 0.00262 0.00081 -0.00053 N2 4 0.805371 0.239634 0.648096 11.00000 0.02060 0.01541 = 0.01316 0.00194 -0.00074 0.00234 C1 1 0.521073 0.318509 0.669246 11.00000 0.01326 0.01871 = 0.01963 0.00478 0.00190 0.00006 C2 1 0.454900 0.243017 0.687918 11.00000 0.01727 0.01907 = 0.02810 0.00829 -0.00050 -0.00163 C3 1 0.413800 0.263162 0.729103 11.00000 0.01525 0.03151 = 0.02792 0.01771 0.00280 -0.00092 AFIX 43 H3 2 0.368178 0.212207 0.740273 11.00000 -1.20000 AFIX 0 C4 1 0.437047 0.355211 0.754549 11.00000 0.01510 0.03544 = 0.01662 0.01160 0.00123 0.00377 C5 1 0.507376 0.425460 0.738704 11.00000 0.01458 0.02787 = 0.01378 0.00467 0.00125 0.00320 AFIX 43 H5 2 0.527537 0.486906 0.756350 11.00000 -1.20000 AFIX 0 C6 1 0.549684 0.407902 0.697041 11.00000 0.01369 0.01888 = 0.01431 0.00502 0.00203 0.00086 C7 1 0.622158 0.489618 0.680628 11.00000 0.01482 0.01576 = 0.01491 0.00041 0.00371 0.00084 AFIX 23 H7A 2 0.587181 0.527831 0.654112 11.00000 -1.20000 H7B 2 0.638002 0.542877 0.705215 11.00000 -1.20000 AFIX 0 C8 1 0.445041 0.119401 0.623018 11.00000 0.03846 0.02370 = 0.06226 -0.01027 0.00944 -0.00959 AFIX 137 H8A 2 0.415175 0.173798 0.601760 11.00000 -1.50000 H8B 2 0.414156 0.049573 0.615120 11.00000 -1.50000 H8C 2 0.519379 0.115734 0.620909 11.00000 -1.50000 AFIX 0 C9 1 0.386224 0.378196 0.797779 11.00000 0.02180 0.05656 = 0.01934 0.01077 0.00666 0.00105 AFIX 137 H9A 2 0.417883 0.441543 0.812851 11.00000 -1.50000 H9B 2 0.395032 0.316525 0.818392 11.00000 -1.50000 H9C 2 0.312802 0.391423 0.790123 11.00000 -1.50000 AFIX 0 C10 1 0.709164 0.541254 0.572436 11.00000 0.01167 0.00996 = 0.01152 0.00005 0.00322 -0.00051 C11 1 0.660499 0.599055 0.535716 11.00000 0.01233 0.01270 = 0.01020 -0.00082 0.00291 -0.00081 C12 1 0.645177 0.708365 0.538299 11.00000 0.01704 0.01320 = 0.01414 0.00065 0.00176 0.00244 AFIX 43 H12 2 0.613425 0.746181 0.512765 11.00000 -1.20000 AFIX 0 C13 1 0.676746 0.763102 0.578797 11.00000 0.01821 0.01135 = 0.01650 -0.00115 0.00331 0.00007 C14 1 0.720726 0.705035 0.615800 11.00000 0.01532 0.01353 = 0.01461 -0.00332 0.00310 -0.00150 AFIX 43 H14 2 0.740500 0.741312 0.643627 11.00000 -1.20000 AFIX 0 C15 1 0.736653 0.594867 0.613209 11.00000 0.01324 0.01209 = 0.01071 0.00042 0.00232 -0.00054 C16 1 0.786751 0.533234 0.653053 11.00000 0.01467 0.01378 = 0.01134 0.00008 0.00068 -0.00290 AFIX 23 H16A 2 0.852694 0.503275 0.644704 11.00000 -1.20000 H16B 2 0.801911 0.582471 0.679202 11.00000 -1.20000 AFIX 0 C17 1 0.570799 0.582066 0.460486 11.00000 0.01472 0.01973 = 0.01219 0.00092 -0.00157 0.00369 AFIX 137 H17A 2 0.605441 0.642571 0.447153 11.00000 -1.50000 H17B 2 0.507176 0.606998 0.472330 11.00000 -1.50000 H17C 2 0.554559 0.527497 0.436969 11.00000 -1.50000 AFIX 0 C18 1 0.665701 0.883074 0.581877 11.00000 0.03328 0.01236 = 0.02243 -0.00186 -0.00073 0.00252 AFIX 137 H18A 2 0.687733 0.916260 0.554125 11.00000 -1.50000 H18B 2 0.708512 0.909648 0.608576 11.00000 -1.50000 H18C 2 0.593681 0.901257 0.584931 11.00000 -1.50000 AFIX 0 C19 1 0.775182 0.381859 0.704224 11.00000 0.01758 0.01726 = 0.01027 0.00183 -0.00198 -0.00060 AFIX 23 H19A 2 0.725227 0.338644 0.719822 11.00000 -1.20000 H19B 2 0.810223 0.431091 0.726978 11.00000 -1.20000 AFIX 0 C20 1 0.853955 0.308175 0.685273 11.00000 0.01650 0.01831 = 0.01536 0.00209 -0.00246 0.00144 AFIX 23 H20A 2 0.908940 0.351754 0.673329 11.00000 -1.20000 H20B 2 0.885689 0.262287 0.710140 11.00000 -1.20000 AFIX 0 C21 1 0.754660 0.146183 0.667380 11.00000 0.03500 0.01574 = 0.02076 0.00578 -0.00486 -0.00166 AFIX 137 H21A 2 0.703264 0.171018 0.687336 11.00000 -1.50000 H21B 2 0.806148 0.102435 0.685111 11.00000 -1.50000 H21C 2 0.720968 0.103183 0.642470 11.00000 -1.50000 AFIX 0 C22 1 0.883572 0.201627 0.618495 11.00000 0.02636 0.03164 = 0.02230 -0.00231 0.00118 0.01279 AFIX 137 H22A 2 0.936602 0.161224 0.636887 11.00000 -1.50000 H22B 2 0.915031 0.263211 0.604453 11.00000 -1.50000 H22C 2 0.850958 0.155232 0.594509 11.00000 -1.50000 AFIX 0 C23 1 0.634074 0.211522 0.520456 11.00000 0.01400 0.01198 = 0.01662 -0.00059 0.00135 -0.00081 C24 1 0.582466 0.110951 0.501336 11.00000 0.03512 0.01630 = 0.02321 0.00118 -0.00752 -0.00905 AFIX 137 H24A 2 0.634830 0.059579 0.493511 11.00000 -1.50000 H24B 2 0.537660 0.128674 0.473839 11.00000 -1.50000 H24C 2 0.541414 0.079331 0.524250 11.00000 -1.50000 AFIX 0 HKLF 4 REM cv-305cold_mo_a.res in I2/a REM wR2 = 0.0701, GooF = S = 1.038, Restrained GooF = 1.038 for all data REM R1 = 0.0292 for 6123 Fo > 4sig(Fo) and 0.0391 for all 7302 data REM 311 parameters refined using 0 restraints END WGHT 0.0321 3.9860 REM Highest difference peak 0.461, deepest hole -0.249, 1-sigma level 0.061 Q1 1 0.6628 0.7267 0.5586 11.00000 0.05 0.46 ; _shelx_res_checksum 12028 _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 1.380 _oxdiff_exptl_absorpt_empirical_full_min 0.821 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' 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 Zn1 Zn 0.68924(2) 0.32896(2) 0.60988(2) 0.01173(4) Uani 1 1 d . . . . . Zn2 Zn 0.750000 0.40011(4) 0.500000 0.01059(19) Uani 0.0586(19) 2 d S T P A 3 Mg1 Mg 0.750000 0.40011(4) 0.500000 0.01059(19) Uani 0.9414(19) 2 d S T P A 4 O1 O 0.55254(8) 0.30618(8) 0.62806(3) 0.0204(2) Uani 1 1 d . . . . . O2 O 0.42555(11) 0.14680(10) 0.66787(5) 0.0364(3) Uani 1 1 d . . . . . O3 O 0.73189(7) 0.43686(7) 0.56602(3) 0.01193(17) Uani 1 1 d . . . . . O4 O 0.63741(7) 0.53659(7) 0.49732(3) 0.01225(17) Uani 1 1 d . . . . . O5 O 0.63867(8) 0.28995(7) 0.49367(3) 0.01433(18) Uani 1 1 d . . . . . O6 O 0.67008(8) 0.20828(8) 0.56149(3) 0.0180(2) Uani 1 1 d . . . . . N1 N 0.72032(8) 0.44468(9) 0.66702(3) 0.0119(2) Uani 1 1 d . . . . . N2 N 0.80537(10) 0.23963(9) 0.64810(4) 0.0165(2) Uani 1 1 d . . . . . C1 C 0.52107(11) 0.31851(11) 0.66925(5) 0.0172(3) Uani 1 1 d . . . . . C2 C 0.45490(12) 0.24302(12) 0.68792(5) 0.0216(3) Uani 1 1 d . . . . . C3 C 0.41380(12) 0.26316(13) 0.72910(5) 0.0248(3) Uani 1 1 d . . . . . H3 H 0.368178 0.212207 0.740273 0.030 Uiso 1 1 calc R U . . . C4 C 0.43705(12) 0.35521(13) 0.75455(5) 0.0224(3) Uani 1 1 d . . . . . C5 C 0.50738(11) 0.42546(12) 0.73870(5) 0.0187(3) Uani 1 1 d . . . . . H5 H 0.527537 0.486906 0.756350 0.022 Uiso 1 1 calc R U . . . C6 C 0.54968(11) 0.40790(11) 0.69704(4) 0.0156(2) Uani 1 1 d . . . . . C7 C 0.62216(11) 0.48962(11) 0.68063(4) 0.0150(2) Uani 1 1 d . . . . . H7A H 0.587181 0.527831 0.654112 0.018 Uiso 1 1 calc R U . . . H7B H 0.638002 0.542877 0.705215 0.018 Uiso 1 1 calc R U . . . C8 C 0.44504(17) 0.11940(15) 0.62302(8) 0.0412(5) Uani 1 1 d . . . . . H8A H 0.415175 0.173798 0.601760 0.062 Uiso 1 1 calc R U . . . H8B H 0.414156 0.049573 0.615120 0.062 Uiso 1 1 calc R U . . . H8C H 0.519379 0.115734 0.620909 0.062 Uiso 1 1 calc R U . . . C9 C 0.38622(14) 0.37820(17) 0.79778(5) 0.0323(4) Uani 1 1 d . . . . . H9A H 0.417883 0.441543 0.812851 0.048 Uiso 1 1 calc R U . . . H9B H 0.395032 0.316525 0.818392 0.048 Uiso 1 1 calc R U . . . H9C H 0.312802 0.391423 0.790123 0.048 Uiso 1 1 calc R U . . . C10 C 0.70916(10) 0.54125(10) 0.57244(4) 0.0109(2) Uani 1 1 d . . . . . C11 C 0.66050(10) 0.59906(10) 0.53572(4) 0.0116(2) Uani 1 1 d . . . . . C12 C 0.64518(11) 0.70837(11) 0.53830(4) 0.0148(2) Uani 1 1 d . . . . . H12 H 0.613425 0.746181 0.512765 0.018 Uiso 1 1 calc R U . . . C13 C 0.67675(11) 0.76310(10) 0.57880(4) 0.0152(2) Uani 1 1 d . . . . . C14 C 0.72073(11) 0.70504(11) 0.61580(4) 0.0144(2) Uani 1 1 d . . . . . H14 H 0.740500 0.741312 0.643627 0.017 Uiso 1 1 calc R U . . . C15 C 0.73665(10) 0.59487(10) 0.61321(4) 0.0119(2) Uani 1 1 d . . . . . C16 C 0.78675(11) 0.53323(10) 0.65305(4) 0.0133(2) Uani 1 1 d . . . . . H16A H 0.852694 0.503275 0.644704 0.016 Uiso 1 1 calc R U . . . H16B H 0.801911 0.582471 0.679202 0.016 Uiso 1 1 calc R U . . . C17 C 0.57080(11) 0.58207(11) 0.46049(4) 0.0157(2) Uani 1 1 d . . . . . H17A H 0.605441 0.642571 0.447153 0.024 Uiso 1 1 calc R U . . . H17B H 0.507176 0.606998 0.472330 0.024 Uiso 1 1 calc R U . . . H17C H 0.554559 0.527497 0.436969 0.024 Uiso 1 1 calc R U . . . C18 C 0.66570(13) 0.88307(11) 0.58188(5) 0.0229(3) Uani 1 1 d . . . . . H18A H 0.687733 0.916260 0.554125 0.034 Uiso 1 1 calc R U . . . H18B H 0.708512 0.909648 0.608576 0.034 Uiso 1 1 calc R U . . . H18C H 0.593681 0.901257 0.584931 0.034 Uiso 1 1 calc R U . . . C19 C 0.77518(11) 0.38186(11) 0.70422(4) 0.0152(2) Uani 1 1 d . . . . . H19A H 0.725227 0.338644 0.719822 0.018 Uiso 1 1 calc R U . . . H19B H 0.810223 0.431091 0.726978 0.018 Uiso 1 1 calc R U . . . C20 C 0.85395(11) 0.30817(11) 0.68527(4) 0.0170(3) Uani 1 1 d . . . . . H20A H 0.908940 0.351754 0.673329 0.020 Uiso 1 1 calc R U . . . H20B H 0.885689 0.262287 0.710140 0.020 Uiso 1 1 calc R U . . . C21 C 0.75466(14) 0.14618(12) 0.66738(5) 0.0243(3) Uani 1 1 d . . . . . H21A H 0.703264 0.171018 0.687336 0.036 Uiso 1 1 calc R U . . . H21B H 0.806148 0.102435 0.685111 0.036 Uiso 1 1 calc R U . . . H21C H 0.720968 0.103183 0.642470 0.036 Uiso 1 1 calc R U . . . C22 C 0.88357(13) 0.20163(14) 0.61850(5) 0.0268(3) Uani 1 1 d . . . . . H22A H 0.936602 0.161224 0.636887 0.040 Uiso 1 1 calc R U . . . H22B H 0.915031 0.263211 0.604453 0.040 Uiso 1 1 calc R U . . . H22C H 0.850958 0.155232 0.594509 0.040 Uiso 1 1 calc R U . . . C23 C 0.63407(11) 0.21152(10) 0.52046(4) 0.0142(2) Uani 1 1 d . . . . . C24 C 0.58247(14) 0.11095(12) 0.50134(5) 0.0255(3) Uani 1 1 d . . . . . H24A H 0.634830 0.059579 0.493511 0.038 Uiso 1 1 calc R U . . . H24B H 0.537660 0.128674 0.473839 0.038 Uiso 1 1 calc R U . . . H24C H 0.541414 0.079331 0.524250 0.038 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 Zn1 0.01421(8) 0.01109(7) 0.00969(7) 0.00192(5) -0.00005(5) -0.00096(6) Zn2 0.0124(3) 0.0105(3) 0.0090(3) 0.000 0.00164(19) 0.000 Mg1 0.0124(3) 0.0105(3) 0.0090(3) 0.000 0.00164(19) 0.000 O1 0.0175(5) 0.0245(5) 0.0194(5) -0.0033(4) 0.0030(4) -0.0068(4) O2 0.0404(8) 0.0271(6) 0.0426(7) 0.0007(5) 0.0086(6) -0.0166(5) O3 0.0170(5) 0.0085(4) 0.0105(4) -0.0001(3) 0.0024(3) 0.0009(3) O4 0.0147(4) 0.0125(4) 0.0092(4) -0.0007(3) -0.0006(3) 0.0017(3) O5 0.0152(5) 0.0132(4) 0.0145(4) 0.0006(3) 0.0008(3) -0.0016(3) O6 0.0262(6) 0.0133(4) 0.0141(4) 0.0004(3) -0.0012(4) -0.0015(4) N1 0.0115(5) 0.0135(5) 0.0105(4) 0.0026(4) 0.0008(4) -0.0005(4) N2 0.0206(6) 0.0154(5) 0.0132(5) 0.0019(4) -0.0007(4) 0.0023(4) C1 0.0133(6) 0.0187(6) 0.0196(6) 0.0048(5) 0.0019(5) 0.0001(5) C2 0.0173(7) 0.0191(7) 0.0281(7) 0.0083(5) -0.0005(6) -0.0016(5) C3 0.0152(7) 0.0315(8) 0.0279(7) 0.0177(6) 0.0028(6) -0.0009(6) C4 0.0151(7) 0.0354(8) 0.0166(6) 0.0116(5) 0.0012(5) 0.0038(6) C5 0.0146(6) 0.0279(7) 0.0138(6) 0.0047(5) 0.0012(5) 0.0032(5) C6 0.0137(6) 0.0189(6) 0.0143(5) 0.0050(5) 0.0020(5) 0.0009(5) C7 0.0148(6) 0.0158(6) 0.0149(5) 0.0004(4) 0.0037(5) 0.0008(5) C8 0.0385(11) 0.0237(9) 0.0623(13) -0.0103(8) 0.0094(9) -0.0096(8) C9 0.0218(8) 0.0566(11) 0.0193(7) 0.0108(7) 0.0067(6) 0.0010(8) C10 0.0117(6) 0.0100(5) 0.0115(5) 0.0000(4) 0.0032(4) -0.0005(4) C11 0.0123(6) 0.0127(5) 0.0102(5) -0.0008(4) 0.0029(4) -0.0008(4) C12 0.0170(6) 0.0132(6) 0.0141(5) 0.0007(4) 0.0018(5) 0.0024(5) C13 0.0182(6) 0.0114(6) 0.0165(6) -0.0012(4) 0.0033(5) 0.0001(5) C14 0.0153(6) 0.0135(6) 0.0146(5) -0.0033(4) 0.0031(5) -0.0015(5) C15 0.0132(6) 0.0121(5) 0.0107(5) 0.0004(4) 0.0023(4) -0.0005(4) C16 0.0147(6) 0.0138(6) 0.0113(5) 0.0001(4) 0.0007(4) -0.0029(5) C17 0.0147(6) 0.0197(6) 0.0122(5) 0.0009(4) -0.0016(5) 0.0037(5) C18 0.0333(9) 0.0124(6) 0.0224(6) -0.0019(5) -0.0007(6) 0.0025(6) C19 0.0176(6) 0.0173(6) 0.0103(5) 0.0018(4) -0.0020(5) -0.0006(5) C20 0.0165(6) 0.0183(6) 0.0154(6) 0.0021(5) -0.0025(5) 0.0014(5) C21 0.0350(9) 0.0157(6) 0.0208(6) 0.0058(5) -0.0049(6) -0.0017(6) C22 0.0264(8) 0.0316(8) 0.0223(7) -0.0023(6) 0.0012(6) 0.0128(7) C23 0.0140(6) 0.0120(5) 0.0166(6) -0.0006(4) 0.0013(5) -0.0008(5) C24 0.0351(9) 0.0163(7) 0.0232(7) 0.0012(5) -0.0075(6) -0.0090(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 1 0 0 0.0648 -1 0 0 0.0453 0 0 1 0.0194 0 0 -1 0.0194 0 -1 1 0.0259 0 1 -1 0.0217 -2 -17 9 0.0194 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 O1 Zn1 O3 126.98(4) . . ? O1 Zn1 O6 91.37(4) . . ? O1 Zn1 N1 89.93(4) . . ? O1 Zn1 N2 114.35(5) . . ? O3 Zn1 O6 94.16(4) . . ? O3 Zn1 N1 90.32(4) . . ? O3 Zn1 N2 118.21(4) . . ? O6 Zn1 N1 173.27(4) . . ? O6 Zn1 N2 91.03(4) . . ? N2 Zn1 N1 82.42(4) . . ? O3 Zn2 O3 153.82(6) 2_656 . ? O3 Zn2 O4 74.36(4) 2_656 2_656 ? O3 Zn2 O4 85.77(4) . 2_656 ? O3 Zn2 O4 85.77(4) 2_656 . ? O3 Zn2 O4 74.36(3) . . ? O4 Zn2 O4 81.42(5) 2_656 . ? O5 Zn2 O3 95.70(4) 2_656 2_656 ? O5 Zn2 O3 95.69(4) . . ? O5 Zn2 O3 102.26(4) 2_656 . ? O5 Zn2 O3 102.27(4) . 2_656 ? O5 Zn2 O4 173.49(4) 2_656 . ? O5 Zn2 O4 173.49(4) . 2_656 ? O5 Zn2 O4 92.85(4) 2_656 2_656 ? O5 Zn2 O4 92.85(4) . . ? O5 Zn2 O5 93.03(6) . 2_656 ? O3 Mg1 O3 153.82(6) 2_656 . ? O3 Mg1 O4 85.77(4) 2_656 . ? O3 Mg1 O4 74.36(3) . . ? O3 Mg1 O4 74.36(4) 2_656 2_656 ? O3 Mg1 O4 85.77(4) . 2_656 ? O3 Mg1 C10 128.29(4) 2_656 . ? O3 Mg1 C10 25.86(3) 2_656 2_656 ? O3 Mg1 C10 128.29(4) . 2_656 ? O3 Mg1 C10 25.86(3) . . ? O4 Mg1 O4 81.42(5) 2_656 . ? O4 Mg1 C10 70.74(4) . 2_656 ? O4 Mg1 C10 52.56(3) 2_656 2_656 ? O4 Mg1 C10 70.74(4) 2_656 . ? O4 Mg1 C10 52.56(3) . . ? O5 Mg1 O3 102.26(4) 2_656 . ? O5 Mg1 O3 95.70(4) 2_656 2_656 ? O5 Mg1 O3 95.69(4) . . ? O5 Mg1 O3 102.27(4) . 2_656 ? O5 Mg1 O4 92.85(4) 2_656 2_656 ? O5 Mg1 O4 92.85(4) . . ? O5 Mg1 O4 173.49(4) 2_656 . ? O5 Mg1 O4 173.49(4) . 2_656 ? O5 Mg1 O5 93.03(6) . 2_656 ? O5 Mg1 C10 108.20(4) 2_656 2_656 ? O5 Mg1 C10 122.62(4) 2_656 . ? O5 Mg1 C10 108.20(4) . . ? O5 Mg1 C10 122.62(4) . 2_656 ? C10 Mg1 C10 103.57(5) . 2_656 ? C1 O1 Zn1 127.37(9) . . ? C2 O2 C8 123.10(14) . . ? Zn1 O3 Zn2 122.16(5) . . ? Zn1 O3 Mg1 122.16(5) . . ? C10 O3 Zn1 119.16(8) . . ? C10 O3 Zn2 113.38(7) . . ? C10 O3 Mg1 113.38(7) . . ? C11 O4 Zn2 107.71(7) . . ? C11 O4 Mg1 107.71(7) . . ? C11 O4 C17 117.59(10) . . ? C17 O4 Zn2 132.36(7) . . ? C17 O4 Mg1 132.36(7) . . ? C23 O5 Zn2 123.43(9) . . ? C23 O5 Mg1 123.43(9) . . ? C23 O6 Zn1 130.36(9) . . ? C7 N1 Zn1 110.09(8) . . ? C16 N1 Zn1 110.33(7) . . ? C16 N1 C7 109.41(10) . . ? C19 N1 Zn1 104.91(8) . . ? C19 N1 C7 112.03(10) . . ? C19 N1 C16 109.99(10) . . ? C20 N2 Zn1 108.98(8) . . ? C21 N2 Zn1 107.06(9) . . ? C21 N2 C20 110.49(11) . . ? C22 N2 Zn1 110.93(8) . . ? C22 N2 C20 110.17(12) . . ? C22 N2 C21 109.18(12) . . ? O1 C1 C2 121.69(13) . . ? O1 C1 C6 122.21(12) . . ? C6 C1 C2 116.09(13) . . ? O2 C2 C1 124.71(14) . . ? O2 C2 C3 114.56(14) . . ? C3 C2 C1 120.73(14) . . ? C2 C3 H3 118.8 . . ? C2 C3 C4 122.34(14) . . ? C4 C3 H3 118.8 . . ? C3 C4 C9 121.15(15) . . ? C5 C4 C3 117.68(14) . . ? C5 C4 C9 121.17(15) . . ? C4 C5 H5 119.3 . . ? C4 C5 C6 121.32(14) . . ? C6 C5 H5 119.3 . . ? C1 C6 C7 119.59(12) . . ? C5 C6 C1 121.48(13) . . ? C5 C6 C7 118.83(12) . . ? N1 C7 C6 114.45(11) . . ? N1 C7 H7A 108.6 . . ? N1 C7 H7B 108.6 . . ? C6 C7 H7A 108.6 . . ? C6 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O3 C10 Mg1 40.76(5) . . ? O3 C10 C11 118.59(10) . . ? O3 C10 C15 122.69(11) . . ? C11 C10 Mg1 81.16(7) . . ? C15 C10 Mg1 152.78(9) . . ? C15 C10 C11 118.64(11) . . ? O4 C11 C10 112.85(11) . . ? O4 C11 C12 125.42(11) . . ? C12 C11 C10 121.59(11) . . ? C11 C12 H12 120.2 . . ? C11 C12 C13 119.65(12) . . ? C13 C12 H12 120.2 . . ? C12 C13 C18 120.83(12) . . ? C14 C13 C12 118.69(12) . . ? C14 C13 C18 120.47(12) . . ? C13 C14 H14 119.1 . . ? C13 C14 C15 121.74(12) . . ? C15 C14 H14 119.1 . . ? C10 C15 C14 119.56(11) . . ? C10 C15 C16 119.07(11) . . ? C14 C15 C16 121.33(11) . . ? N1 C16 C15 111.80(10) . . ? N1 C16 H16A 109.3 . . ? N1 C16 H16B 109.3 . . ? C15 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? O4 C17 H17A 109.5 . . ? O4 C17 H17B 109.5 . . ? O4 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.6 . . ? N1 C19 H19B 109.6 . . ? N1 C19 C20 110.49(10) . . ? H19A C19 H19B 108.1 . . ? C20 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? N2 C20 C19 110.99(11) . . ? N2 C20 H20A 109.4 . . ? N2 C20 H20B 109.4 . . ? C19 C20 H20A 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O5 C23 C24 117.27(12) . . ? O6 C23 O5 126.13(12) . . ? O6 C23 C24 116.58(12) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 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 Zn1 O1 1.9302(11) . ? Zn1 O3 1.9780(9) . ? Zn1 O6 2.0712(10) . ? Zn1 N1 2.2244(11) . ? Zn1 N2 2.1227(11) . ? Zn2 O3 2.0264(9) 2_656 ? Zn2 O3 2.0265(9) . ? Zn2 O4 2.2484(10) . ? Zn2 O4 2.2484(10) 2_656 ? Zn2 O5 1.9989(10) . ? Zn2 O5 1.9989(10) 2_656 ? Mg1 O3 2.0265(9) . ? Mg1 O3 2.0264(9) 2_656 ? Mg1 O4 2.2484(10) . ? Mg1 O4 2.2484(10) 2_656 ? Mg1 O5 1.9989(10) 2_656 ? Mg1 O5 1.9989(10) . ? Mg1 C10 2.8491(12) . ? Mg1 C10 2.8491(12) 2_656 ? O1 C1 1.3206(17) . ? O2 C2 1.377(2) . ? O2 C8 1.406(2) . ? O3 C10 1.3539(14) . ? O4 C11 1.3823(14) . ? O4 C17 1.4436(15) . ? O5 C23 1.2608(16) . ? O6 C23 1.2551(16) . ? N1 C7 1.4870(17) . ? N1 C16 1.4858(16) . ? N1 C19 1.4781(16) . ? N2 C20 1.4850(17) . ? N2 C21 1.4792(19) . ? N2 C22 1.477(2) . ? C1 C2 1.422(2) . ? C1 C6 1.414(2) . ? C2 C3 1.389(2) . ? C3 H3 0.9500 . ? C3 C4 1.390(2) . ? C4 C5 1.381(2) . ? C4 C9 1.511(2) . ? C5 H5 0.9500 . ? C5 C6 1.4038(19) . ? C6 C7 1.5004(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.4025(17) . ? C10 C15 1.3911(16) . ? C11 C12 1.3826(18) . ? C12 H12 0.9500 . ? C12 C13 1.4019(18) . ? C13 C14 1.3880(18) . ? C13 C18 1.5085(19) . ? C14 H14 0.9500 . ? C14 C15 1.3944(18) . ? C15 C16 1.5016(17) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.522(2) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.5100(19) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 Zn1 O1 C1 C2 -137.05(12) . . . . ? Zn1 O1 C1 C6 43.94(18) . . . . ? Zn1 O3 C10 Mg1 -154.87(11) . . . . ? Zn1 O3 C10 C11 -129.08(10) . . . . ? Zn1 O3 C10 C15 54.22(15) . . . . ? Zn1 O6 C23 O5 30.8(2) . . . . ? Zn1 O6 C23 C24 -150.54(11) . . . . ? Zn1 N1 C7 C6 60.58(12) . . . . ? Zn1 N1 C16 C15 61.01(12) . . . . ? Zn1 N1 C19 C20 41.87(12) . . . . ? Zn1 N2 C20 C19 35.84(13) . . . . ? Zn2 O3 C10 C11 25.79(14) . . . . ? Zn2 O3 C10 C15 -150.92(10) . . . . ? Zn2 O4 C11 C10 -26.45(12) . . . . ? Zn2 O4 C11 C12 149.31(12) . . . . ? Zn2 O5 C23 O6 27.1(2) . . . . ? Zn2 O5 C23 C24 -151.50(11) . . . . ? Mg1 O3 C10 C11 25.79(14) . . . . ? Mg1 O3 C10 C15 -150.92(10) . . . . ? Mg1 O4 C11 C10 -26.45(12) . . . . ? Mg1 O4 C11 C12 149.31(12) . . . . ? Mg1 O5 C23 O6 27.1(2) . . . . ? Mg1 O5 C23 C24 -151.50(11) . . . . ? Mg1 C10 C11 O4 19.81(9) . . . . ? Mg1 C10 C11 C12 -156.14(13) . . . . ? Mg1 C10 C15 C14 129.13(17) . . . . ? Mg1 C10 C15 C16 -48.5(2) . . . . ? O1 C1 C2 O2 6.6(2) . . . . ? O1 C1 C2 C3 -172.97(13) . . . . ? O1 C1 C6 C5 173.42(13) . . . . ? O1 C1 C6 C7 -3.0(2) . . . . ? O2 C2 C3 C4 178.49(14) . . . . ? O3 C10 C11 O4 3.11(17) . . . . ? O3 C10 C11 C12 -172.84(12) . . . . ? O3 C10 C15 C14 173.06(12) . . . . ? O3 C10 C15 C16 -4.59(19) . . . . ? O4 C11 C12 C13 -176.84(13) . . . . ? N1 C19 C20 N2 -54.25(14) . . . . ? C1 C2 C3 C4 -1.9(2) . . . . ? C1 C6 C7 N1 -53.84(16) . . . . ? C2 C1 C6 C5 -5.66(19) . . . . ? C2 C1 C6 C7 177.97(12) . . . . ? C2 C3 C4 C5 -3.1(2) . . . . ? C2 C3 C4 C9 176.25(14) . . . . ? C3 C4 C5 C6 3.6(2) . . . . ? C4 C5 C6 C1 0.9(2) . . . . ? C4 C5 C6 C7 177.31(13) . . . . ? C5 C6 C7 N1 129.69(13) . . . . ? C6 C1 C2 O2 -174.30(14) . . . . ? C6 C1 C2 C3 6.1(2) . . . . ? C7 N1 C16 C15 -60.26(13) . . . . ? C7 N1 C19 C20 161.29(11) . . . . ? C8 O2 C2 C1 -10.2(3) . . . . ? C8 O2 C2 C3 169.42(16) . . . . ? C9 C4 C5 C6 -175.79(13) . . . . ? C10 C11 C12 C13 -1.4(2) . . . . ? C10 C15 C16 N1 -59.35(16) . . . . ? C11 C10 C15 C14 -3.64(19) . . . . ? C11 C10 C15 C16 178.70(12) . . . . ? C11 C12 C13 C14 -1.5(2) . . . . ? C11 C12 C13 C18 177.03(14) . . . . ? C12 C13 C14 C15 1.8(2) . . . . ? C13 C14 C15 C10 0.8(2) . . . . ? C13 C14 C15 C16 178.42(13) . . . . ? C14 C15 C16 N1 123.04(13) . . . . ? C15 C10 C11 O4 179.95(11) . . . . ? C15 C10 C11 C12 4.0(2) . . . . ? C16 N1 C7 C6 -178.01(10) . . . . ? C16 N1 C19 C20 -76.78(13) . . . . ? C17 O4 C11 C10 168.79(11) . . . . ? C17 O4 C11 C12 -15.44(19) . . . . ? C18 C13 C14 C15 -176.72(14) . . . . ? C19 N1 C7 C6 -55.75(14) . . . . ? C19 N1 C16 C15 176.27(10) . . . . ? C21 N2 C20 C19 -81.52(14) . . . . ? C22 N2 C20 C19 157.75(12) . . . . ? 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 1.0013 0.0002 -0.0006 0.0503 -0.0124 -0.0171 -1.0013 -0.0002 0.0006 -0.0503 0.0124 0.0171 0.0000 -0.0001 0.9997 -0.0061 -0.0017 -0.0234 -0.0000 0.0001 -0.9997 0.0061 0.0017 0.0234 -0.0003 -1.0010 1.0005 0.0052 0.0536 -0.0304 0.0003 1.0010 -1.0005 -0.0052 -0.0536 0.0304 -2.2183 -17.0751 9.1895 0.0248 0.9549 -0.2959