#------------------------------------------------------------------------------ #$Date: 2021-01-14 07:06:55 +0200 (Thu, 14 Jan 2021) $ #$Revision: 260948 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/00/1560088.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_1560088 loop_ _publ_author_name 'Payne, Jack' 'McKeown, Paul' 'Driscoll, Oliver' 'Kociok-K\"ohn, Gabriele' 'Emanuelsson, Emma Anna Carolina' 'Jones, Matthew' _publ_section_title ; Make or Break: Mg(II)- and Zn(II)-Catalen Complexes for PLA Production and Recycling of Commodity Polyesters ; _journal_name_full 'Polymer Chemistry' _journal_paper_doi 10.1039/D0PY01519A _journal_year 2021 _chemical_formula_sum 'C30 H36 Cl2 Mg N2 O2' _chemical_formula_weight 551.82 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-10-29 deposited with the CCDC. 2020-12-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.319(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.9229(4) _cell_length_b 14.2743(5) _cell_length_c 20.5348(5) _cell_measurement_reflns_used 7524 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 27.8120 _cell_measurement_theta_min 3.2900 _cell_volume 2896.08(17) _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 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; 'WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _computing_structure_refinement ; SHELXL-2014/8 (Sheldrick, 2014) Sheldrick GM (2008) Acta Crystallogr A64:112-122 and C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich ShelXle: a Qt graphical user interface for SHELXL J. Appl. Cryst., 44, (2011) 1281-1284. ; _computing_structure_solution ; SHELXT Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. ; _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 150.0(3) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1468 _diffrn_detector_type EosS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.858 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'New Xcalibur, EosS2' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_unetI/netI 0.0497 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.858 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 20024 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.858 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.637 _diffrn_reflns_theta_min 2.997 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.266 _exptl_crystal_description block _exptl_crystal_F_000 1168 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.618 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.070 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 345 _refine_ls_number_reflns 6390 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0709 _refine_ls_R_factor_gt 0.0524 _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^)+(0.0744P)^2^+1.3747P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1352 _refine_ls_wR_factor_ref 0.1483 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4971 _reflns_number_total 6390 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0py01519a2.cif _cod_data_source_block Mg(2)2 _cod_original_cell_volume 2896.07(17) _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1560088 _shelx_shelxl_version_number 2014/7 _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_min 0.947 _shelx_estimated_absorpt_t_max 0.973 _oxdiff_exptl_absorpt_empirical_full_min 0.878 _oxdiff_exptl_absorpt_empirical_full_max 1.136 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; C:\mj205\XrayData\JACKPA~1\PhD\MAGNES~1\e20mdj14\e20mdj04.res created by SHELXL-2014/7 TITL e20mdj04_a.res in P2(1)/c CELL 0.71073 9.9229 14.2743 20.5348 90.000 95.319 90.000 ZERR 4.0000 0.0004 0.0005 0.0005 0.000 0.003 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H CL MG N O UNIT 120 144 8 4 8 8 MERG 2 FMAP 2 GRID PLAN 6 TEMP -123 SIZE 0.2 0.15 0.1 L.S. 20 ACTA WGHT 0.074400 1.374700 FVAR 3.47576 CL1 3 -0.016979 0.741236 0.316720 11.00000 0.04952 0.02663 = 0.03246 0.00335 0.00441 0.01303 MG1 4 0.039777 0.460743 0.441502 11.00000 0.01789 0.01956 = 0.01731 -0.00230 -0.00241 0.00524 O1 6 0.136875 0.511273 0.524289 11.00000 0.01523 0.01760 = 0.01930 -0.00023 -0.00402 0.00408 N1 5 0.075559 0.331639 0.500705 11.00000 0.01434 0.02054 = 0.02246 -0.00160 -0.00204 0.00042 C1 1 0.227586 0.447816 0.551377 11.00000 0.01256 0.01983 = 0.01505 0.00069 -0.00012 0.00404 CL2 3 0.219247 0.593412 0.114354 11.00000 0.04106 0.05830 = 0.02682 0.00816 0.01158 0.00633 O2 6 0.038801 0.559773 0.377330 11.00000 0.03137 0.02308 = 0.01979 -0.00039 0.00268 0.00700 N2 5 0.125284 0.372089 0.374895 11.00000 0.01737 0.02167 = 0.02307 -0.00373 -0.00247 0.00444 C2 1 0.346409 0.474624 0.590129 11.00000 0.01475 0.02085 = 0.01516 -0.00057 0.00089 0.00215 C3 1 0.431418 0.403030 0.615470 11.00000 0.01519 0.02636 = 0.01700 -0.00135 -0.00245 0.00338 AFIX 43 H3 2 0.511306 0.420185 0.641865 11.00000 -1.20000 AFIX 0 C4 1 0.406760 0.308156 0.604585 11.00000 0.01652 0.02378 = 0.01548 0.00301 0.00022 0.00524 C5 1 0.289539 0.283646 0.566006 11.00000 0.01902 0.01567 = 0.01924 0.00080 0.00010 0.00207 AFIX 43 H5 2 0.269274 0.219525 0.557448 11.00000 -1.20000 AFIX 0 C6 1 0.202014 0.352808 0.539958 11.00000 0.01351 0.02151 = 0.01802 0.00059 -0.00106 0.00124 C7 1 0.379666 0.578095 0.604271 11.00000 0.01633 0.02211 = 0.02166 -0.00278 -0.00292 -0.00074 C8 1 0.388746 0.631617 0.540302 11.00000 0.04569 0.02849 = 0.03204 0.00294 0.00121 -0.01295 AFIX 137 H8A 2 0.461430 0.605042 0.516850 11.00000 -1.50000 H8B 2 0.408065 0.697757 0.549963 11.00000 -1.50000 H8C 2 0.302561 0.626346 0.513104 11.00000 -1.50000 AFIX 0 C9 1 0.271263 0.622524 0.643020 11.00000 0.02502 0.02976 = 0.03674 -0.01207 -0.00089 0.00234 AFIX 137 H9A 2 0.183676 0.620906 0.616728 11.00000 -1.50000 H9B 2 0.295885 0.687657 0.653468 11.00000 -1.50000 H9C 2 0.264943 0.587404 0.683632 11.00000 -1.50000 AFIX 0 C10 1 0.516006 0.589694 0.644862 11.00000 0.02117 0.02780 = 0.04682 -0.00958 -0.00849 0.00031 AFIX 137 H10A 2 0.512273 0.559284 0.687444 11.00000 -1.50000 H10B 2 0.535591 0.656512 0.651344 11.00000 -1.50000 H10C 2 0.587436 0.560711 0.621785 11.00000 -1.50000 AFIX 0 C11 1 0.504947 0.235120 0.636729 11.00000 0.02269 0.02677 = 0.01995 0.00378 -0.00389 0.00794 C12 1 0.516617 0.249037 0.710955 11.00000 0.07843 0.05895 = 0.02750 0.00555 -0.01029 0.03033 AFIX 137 H12A 2 0.427054 0.242383 0.726923 11.00000 -1.50000 H12B 2 0.552236 0.311772 0.721611 11.00000 -1.50000 H12C 2 0.578031 0.201864 0.731849 11.00000 -1.50000 AFIX 0 C13 1 0.458775 0.135210 0.621784 11.00000 0.03707 0.02881 = 0.05519 0.01076 -0.00661 0.00863 AFIX 137 H13A 2 0.525001 0.091299 0.642931 11.00000 -1.50000 H13B 2 0.451031 0.125077 0.574383 11.00000 -1.50000 H13C 2 0.370534 0.124861 0.638404 11.00000 -1.50000 AFIX 0 C14 1 0.645830 0.246983 0.612699 11.00000 0.02724 0.04011 = 0.06183 0.01318 -0.00335 0.01226 AFIX 137 H14A 2 0.709585 0.204210 0.636829 11.00000 -1.50000 H14B 2 0.676447 0.311719 0.620035 11.00000 -1.50000 H14C 2 0.641437 0.232595 0.565886 11.00000 -1.50000 AFIX 0 C15 1 0.076843 0.252378 0.454451 11.00000 0.02324 0.01819 = 0.02868 -0.00255 -0.00730 0.00047 AFIX 23 H15A 2 -0.016524 0.238404 0.435712 11.00000 -1.20000 H15B 2 0.113821 0.195821 0.477603 11.00000 -1.20000 AFIX 0 C16 1 0.163932 0.278341 0.400279 11.00000 0.02417 0.01946 = 0.02693 -0.00533 -0.00451 0.00511 AFIX 23 H16A 2 0.260545 0.278260 0.417392 11.00000 -1.20000 H16B 2 0.151438 0.231678 0.364562 11.00000 -1.20000 AFIX 0 C17 1 0.154272 0.394676 0.317469 11.00000 0.01629 0.02579 = 0.02321 -0.00876 -0.00206 0.00466 AFIX 43 H17 2 0.193143 0.347398 0.292557 11.00000 -1.20000 AFIX 0 C18 1 0.133233 0.485700 0.287008 11.00000 0.01654 0.02724 = 0.02131 -0.00298 -0.00269 0.00270 C19 1 0.175940 0.496434 0.224118 11.00000 0.02223 0.03515 = 0.02453 -0.00483 0.00158 0.00437 AFIX 43 H19 2 0.214660 0.444667 0.203529 11.00000 -1.20000 AFIX 0 C20 1 0.162491 0.580660 0.192028 11.00000 0.02086 0.04532 = 0.01950 0.00252 0.00124 -0.00003 C21 1 0.102902 0.656948 0.220218 11.00000 0.02124 0.03410 = 0.02525 0.00640 -0.00297 -0.00057 AFIX 43 H21 2 0.092052 0.714831 0.197504 11.00000 -1.20000 AFIX 0 C22 1 0.060092 0.646970 0.281481 11.00000 0.02003 0.02696 = 0.02423 -0.00117 -0.00230 0.00261 C23 1 0.075560 0.563084 0.318805 11.00000 0.01588 0.02478 = 0.02125 -0.00203 -0.00306 0.00106 C24 1 0.096112 -0.057853 0.426621 11.00000 0.03945 0.05977 = 0.04730 -0.01270 0.00810 0.00500 AFIX 137 H24A 2 0.120101 -0.124158 0.423221 11.00000 -1.50000 H24B 2 0.008874 -0.046311 0.401468 11.00000 -1.50000 H24C 2 0.089452 -0.041777 0.472609 11.00000 -1.50000 AFIX 0 C25 1 0.203508 0.001577 0.399839 11.00000 0.03199 0.03353 = 0.03648 -0.00809 0.00129 0.01199 C26 1 0.307447 0.040959 0.440860 11.00000 0.04462 0.03492 = 0.03028 -0.00626 -0.00306 0.01076 AFIX 43 H26 2 0.309664 0.031063 0.486695 11.00000 -1.20000 AFIX 0 C27 1 0.407371 0.094021 0.416629 11.00000 0.04264 0.03232 = 0.04384 -0.00621 -0.00692 0.00868 AFIX 43 H27 2 0.477365 0.120215 0.445737 11.00000 -1.20000 AFIX 0 C28 1 0.406230 0.109276 0.350307 11.00000 0.04159 0.02975 = 0.04910 0.00342 0.00606 0.01121 AFIX 43 H28 2 0.475381 0.145535 0.333455 11.00000 -1.20000 AFIX 0 C29 1 0.302986 0.071082 0.308493 11.00000 0.04817 0.04080 = 0.03302 0.00043 0.00282 0.01737 AFIX 43 H29 2 0.300775 0.081597 0.262725 11.00000 -1.20000 AFIX 0 C30 1 0.203442 0.017847 0.333158 11.00000 0.03347 0.04369 = 0.03494 -0.01058 -0.00644 0.01486 AFIX 43 H30 2 0.133470 -0.008198 0.303964 11.00000 -1.20000 AFIX 0 H1 2 0.016420 0.320630 0.529183 11.00000 0.02832 HKLF 4 REM e20mdj04_a.res in P2(1)/c REM R1 = 0.0524 for 4971 Fo > 4sig(Fo) and 0.0709 for all 6390 data REM 345 parameters refined using 0 restraints END WGHT 0.0743 1.3799 REM Highest difference peak 0.618, deepest hole -0.373, 1-sigma level 0.070 Q1 1 0.0161 0.6834 0.2995 11.00000 0.05 0.62 Q2 1 0.3637 0.5258 0.5990 11.00000 0.05 0.47 Q3 1 0.6406 0.2729 0.6708 11.00000 0.05 0.43 Q4 1 -0.0223 0.8082 0.3155 11.00000 0.05 0.41 Q5 1 0.1369 0.5760 0.5229 11.00000 0.05 0.41 Q6 1 0.0568 0.7344 0.2887 11.00000 0.05 0.40 ; _shelx_res_checksum 87456 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' '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 Cl1 Cl -0.01698(7) 0.74124(4) 0.31672(3) 0.03616(18) Uani 1 1 d . . . . . Mg1 Mg 0.03978(7) 0.46074(5) 0.44150(3) 0.01850(18) Uani 1 1 d . . . . . O1 O 0.13688(14) 0.51127(9) 0.52429(7) 0.0177(3) Uani 1 1 d . . . . . N1 N 0.07556(17) 0.33164(12) 0.50071(9) 0.0193(4) Uani 1 1 d . . . . . C1 C 0.22759(19) 0.44782(14) 0.55138(9) 0.0159(4) Uani 1 1 d . . . . . Cl2 Cl 0.21925(7) 0.59341(5) 0.11435(3) 0.04153(19) Uani 1 1 d . . . . . O2 O 0.03880(16) 0.55977(10) 0.37733(7) 0.0247(3) Uani 1 1 d . . . . . N2 N 0.12528(17) 0.37209(12) 0.37489(9) 0.0210(4) Uani 1 1 d . . . . . C2 C 0.3464(2) 0.47462(14) 0.59013(9) 0.0170(4) Uani 1 1 d . . . . . C3 C 0.4314(2) 0.40303(15) 0.61547(10) 0.0198(4) Uani 1 1 d . . . . . H3 H 0.5113 0.4202 0.6419 0.024 Uiso 1 1 calc R U . . . C4 C 0.4068(2) 0.30816(15) 0.60458(9) 0.0187(4) Uani 1 1 d . . . . . C5 C 0.2895(2) 0.28365(14) 0.56601(10) 0.0181(4) Uani 1 1 d . . . . . H5 H 0.2693 0.2195 0.5574 0.022 Uiso 1 1 calc R U . . . C6 C 0.2020(2) 0.35281(14) 0.53996(10) 0.0178(4) Uani 1 1 d . . . . . C7 C 0.3797(2) 0.57809(14) 0.60427(10) 0.0203(4) Uani 1 1 d . . . . . C8 C 0.3887(3) 0.63162(17) 0.54030(12) 0.0356(6) Uani 1 1 d . . . . . H8A H 0.4614 0.6050 0.5168 0.053 Uiso 1 1 calc R U . . . H8B H 0.4081 0.6978 0.5500 0.053 Uiso 1 1 calc R U . . . H8C H 0.3026 0.6263 0.5131 0.053 Uiso 1 1 calc R U . . . C9 C 0.2713(2) 0.62252(17) 0.64302(12) 0.0307(5) Uani 1 1 d . . . . . H9A H 0.1837 0.6209 0.6167 0.046 Uiso 1 1 calc R U . . . H9B H 0.2959 0.6877 0.6535 0.046 Uiso 1 1 calc R U . . . H9C H 0.2649 0.5874 0.6836 0.046 Uiso 1 1 calc R U . . . C10 C 0.5160(2) 0.58969(17) 0.64486(13) 0.0327(6) Uani 1 1 d . . . . . H10A H 0.5123 0.5593 0.6874 0.049 Uiso 1 1 calc R U . . . H10B H 0.5356 0.6565 0.6513 0.049 Uiso 1 1 calc R U . . . H10C H 0.5874 0.5607 0.6218 0.049 Uiso 1 1 calc R U . . . C11 C 0.5049(2) 0.23512(15) 0.63673(10) 0.0235(5) Uani 1 1 d . . . . . C12 C 0.5166(4) 0.2490(2) 0.71095(13) 0.0559(9) Uani 1 1 d . . . . . H12A H 0.4271 0.2424 0.7269 0.084 Uiso 1 1 calc R U . . . H12B H 0.5522 0.3118 0.7216 0.084 Uiso 1 1 calc R U . . . H12C H 0.5780 0.2019 0.7318 0.084 Uiso 1 1 calc R U . . . C13 C 0.4588(3) 0.13521(18) 0.62178(14) 0.0410(6) Uani 1 1 d . . . . . H13A H 0.5250 0.0913 0.6429 0.062 Uiso 1 1 calc R U . . . H13B H 0.4510 0.1251 0.5744 0.062 Uiso 1 1 calc R U . . . H13C H 0.3705 0.1249 0.6384 0.062 Uiso 1 1 calc R U . . . C14 C 0.6458(3) 0.2470(2) 0.61270(15) 0.0435(7) Uani 1 1 d . . . . . H14A H 0.7096 0.2042 0.6368 0.065 Uiso 1 1 calc R U . . . H14B H 0.6764 0.3117 0.6200 0.065 Uiso 1 1 calc R U . . . H14C H 0.6414 0.2326 0.5659 0.065 Uiso 1 1 calc R U . . . C15 C 0.0768(2) 0.25238(14) 0.45445(11) 0.0240(5) Uani 1 1 d . . . . . H15A H -0.0165 0.2384 0.4357 0.029 Uiso 1 1 calc R U . . . H15B H 0.1138 0.1958 0.4776 0.029 Uiso 1 1 calc R U . . . C16 C 0.1639(2) 0.27834(15) 0.40028(11) 0.0239(5) Uani 1 1 d . . . . . H16A H 0.2605 0.2783 0.4174 0.029 Uiso 1 1 calc R U . . . H16B H 0.1514 0.2317 0.3646 0.029 Uiso 1 1 calc R U . . . C17 C 0.1543(2) 0.39468(15) 0.31747(10) 0.0220(5) Uani 1 1 d . . . . . H17 H 0.1931 0.3474 0.2926 0.026 Uiso 1 1 calc R U . . . C18 C 0.1332(2) 0.48570(15) 0.28701(10) 0.0220(4) Uani 1 1 d . . . . . C19 C 0.1759(2) 0.49643(17) 0.22412(11) 0.0273(5) Uani 1 1 d . . . . . H19 H 0.2147 0.4447 0.2035 0.033 Uiso 1 1 calc R U . . . C20 C 0.1625(2) 0.58066(18) 0.19203(11) 0.0286(5) Uani 1 1 d . . . . . C21 C 0.1029(2) 0.65695(17) 0.22022(11) 0.0272(5) Uani 1 1 d . . . . . H21 H 0.0921 0.7148 0.1975 0.033 Uiso 1 1 calc R U . . . C22 C 0.0601(2) 0.64697(16) 0.28148(10) 0.0240(5) Uani 1 1 d . . . . . C23 C 0.0756(2) 0.56308(15) 0.31881(10) 0.0209(4) Uani 1 1 d . . . . . C24 C 0.0961(3) -0.0579(2) 0.42662(15) 0.0486(7) Uani 1 1 d . . . . . H24A H 0.1201 -0.1242 0.4232 0.073 Uiso 1 1 calc R U . . . H24B H 0.0089 -0.0463 0.4015 0.073 Uiso 1 1 calc R U . . . H24C H 0.0895 -0.0418 0.4726 0.073 Uiso 1 1 calc R U . . . C25 C 0.2035(3) 0.00158(18) 0.39984(12) 0.0341(6) Uani 1 1 d . . . . . C26 C 0.3074(3) 0.04096(18) 0.44086(13) 0.0370(6) Uani 1 1 d . . . . . H26 H 0.3097 0.0311 0.4867 0.044 Uiso 1 1 calc R U . . . C27 C 0.4074(3) 0.09402(18) 0.41663(14) 0.0403(6) Uani 1 1 d . . . . . H27 H 0.4774 0.1202 0.4457 0.048 Uiso 1 1 calc R U . . . C28 C 0.4062(3) 0.10928(18) 0.35031(14) 0.0400(6) Uani 1 1 d . . . . . H28 H 0.4754 0.1455 0.3335 0.048 Uiso 1 1 calc R U . . . C29 C 0.3030(3) 0.07108(19) 0.30849(13) 0.0407(6) Uani 1 1 d . . . . . H29 H 0.3008 0.0816 0.2627 0.049 Uiso 1 1 calc R U . . . C30 C 0.2034(3) 0.01785(19) 0.33316(13) 0.0380(6) Uani 1 1 d . . . . . H30 H 0.1335 -0.0082 0.3040 0.046 Uiso 1 1 calc R U . . . H1 H 0.016(3) 0.3206(18) 0.5292(12) 0.028(7) Uiso 1 1 d . . . . . 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 Cl1 0.0495(4) 0.0266(3) 0.0325(3) 0.0033(2) 0.0044(3) 0.0130(3) Mg1 0.0179(4) 0.0196(4) 0.0173(3) -0.0023(3) -0.0024(3) 0.0052(3) O1 0.0152(7) 0.0176(7) 0.0193(7) -0.0002(5) -0.0040(5) 0.0041(5) N1 0.0143(9) 0.0205(9) 0.0225(9) -0.0016(7) -0.0020(7) 0.0004(7) C1 0.0126(9) 0.0198(10) 0.0150(9) 0.0007(7) -0.0001(7) 0.0040(7) Cl2 0.0411(4) 0.0583(4) 0.0268(3) 0.0082(3) 0.0116(3) 0.0063(3) O2 0.0314(9) 0.0231(8) 0.0198(7) -0.0004(6) 0.0027(6) 0.0070(6) N2 0.0174(9) 0.0217(9) 0.0231(9) -0.0037(7) -0.0025(7) 0.0044(7) C2 0.0148(10) 0.0209(10) 0.0152(10) -0.0006(8) 0.0009(8) 0.0021(8) C3 0.0152(10) 0.0264(11) 0.0170(10) -0.0014(8) -0.0025(8) 0.0034(8) C4 0.0165(10) 0.0238(11) 0.0155(9) 0.0030(8) 0.0002(8) 0.0052(8) C5 0.0190(10) 0.0157(10) 0.0192(10) 0.0008(8) 0.0001(8) 0.0021(8) C6 0.0135(10) 0.0215(10) 0.0180(10) 0.0006(8) -0.0011(8) 0.0012(8) C7 0.0163(10) 0.0221(11) 0.0217(10) -0.0028(8) -0.0029(8) -0.0007(8) C8 0.0457(15) 0.0285(13) 0.0320(13) 0.0029(10) 0.0012(11) -0.0130(11) C9 0.0250(12) 0.0298(13) 0.0367(13) -0.0121(10) -0.0009(10) 0.0023(10) C10 0.0212(12) 0.0278(13) 0.0468(15) -0.0096(11) -0.0085(10) 0.0003(9) C11 0.0227(11) 0.0268(11) 0.0200(10) 0.0038(9) -0.0039(8) 0.0079(9) C12 0.078(2) 0.059(2) 0.0275(14) 0.0055(13) -0.0103(14) 0.0303(17) C13 0.0371(15) 0.0288(13) 0.0552(17) 0.0108(12) -0.0066(12) 0.0086(11) C14 0.0272(14) 0.0401(16) 0.0618(19) 0.0132(13) -0.0033(13) 0.0123(11) C15 0.0232(11) 0.0182(10) 0.0287(12) -0.0026(9) -0.0073(9) 0.0005(8) C16 0.0242(11) 0.0195(11) 0.0269(11) -0.0053(9) -0.0045(9) 0.0051(9) C17 0.0163(10) 0.0258(11) 0.0232(11) -0.0088(9) -0.0021(8) 0.0047(8) C18 0.0165(10) 0.0272(11) 0.0213(10) -0.0030(9) -0.0027(8) 0.0027(8) C19 0.0222(11) 0.0351(13) 0.0245(11) -0.0048(10) 0.0016(9) 0.0044(10) C20 0.0209(11) 0.0453(15) 0.0195(11) 0.0025(10) 0.0012(9) 0.0000(10) C21 0.0212(11) 0.0341(13) 0.0252(11) 0.0064(10) -0.0030(9) -0.0006(9) C22 0.0200(11) 0.0270(12) 0.0242(11) -0.0012(9) -0.0023(9) 0.0026(9) C23 0.0159(10) 0.0248(11) 0.0213(10) -0.0020(8) -0.0031(8) 0.0011(8) C24 0.0395(16) 0.0598(19) 0.0473(17) -0.0127(14) 0.0081(13) 0.0050(14) C25 0.0320(13) 0.0335(13) 0.0365(14) -0.0081(11) 0.0013(11) 0.0120(11) C26 0.0446(15) 0.0349(14) 0.0303(13) -0.0063(11) -0.0031(11) 0.0108(12) C27 0.0426(16) 0.0323(14) 0.0438(16) -0.0062(11) -0.0069(12) 0.0087(12) C28 0.0416(15) 0.0297(13) 0.0491(16) 0.0034(12) 0.0061(13) 0.0112(11) C29 0.0482(17) 0.0408(15) 0.0330(14) 0.0004(11) 0.0028(12) 0.0174(13) C30 0.0335(14) 0.0437(15) 0.0349(14) -0.0106(11) -0.0064(11) 0.0149(12) 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' Cl Cl 0.1484 0.1585 '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' 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 O2 Mg1 O1 98.34(7) . 3_566 ? O2 Mg1 O1 106.63(7) . . ? O1 Mg1 O1 89.90(6) 3_566 . ? O2 Mg1 N2 88.48(7) . . ? O1 Mg1 N2 140.72(7) 3_566 . ? O1 Mg1 N2 125.22(7) . . ? O2 Mg1 N1 166.45(7) . . ? O1 Mg1 N1 94.29(7) 3_566 . ? O1 Mg1 N1 78.15(6) . . ? N2 Mg1 N1 78.61(7) . . ? O2 Mg1 C1 124.02(7) . . ? O1 Mg1 C1 105.76(6) 3_566 . ? O1 Mg1 C1 27.03(5) . . ? N2 Mg1 C1 101.92(7) . . ? N1 Mg1 C1 56.09(6) . . ? O2 Mg1 Mg1 107.77(6) . 3_566 ? O1 Mg1 Mg1 45.24(4) 3_566 3_566 ? O1 Mg1 Mg1 44.66(4) . 3_566 ? N2 Mg1 Mg1 162.47(7) . 3_566 ? N1 Mg1 Mg1 84.65(6) . 3_566 ? C1 Mg1 Mg1 63.80(5) . 3_566 ? C1 O1 Mg1 124.15(12) . 3_566 ? C1 O1 Mg1 110.77(12) . . ? Mg1 O1 Mg1 90.10(6) 3_566 . ? C6 N1 C15 117.09(16) . . ? C6 N1 Mg1 102.51(12) . . ? C15 N1 Mg1 107.11(13) . . ? O1 C1 C6 118.40(17) . . ? O1 C1 C2 122.44(18) . . ? C6 C1 C2 119.15(17) . . ? O1 C1 Mg1 42.20(8) . . ? C6 C1 Mg1 80.29(12) . . ? C2 C1 Mg1 153.59(14) . . ? C23 O2 Mg1 132.76(14) . . ? C17 N2 C16 118.75(18) . . ? C17 N2 Mg1 125.94(15) . . ? C16 N2 Mg1 115.12(13) . . ? C3 C2 C1 117.13(18) . . ? C3 C2 C7 121.49(18) . . ? C1 C2 C7 121.38(17) . . ? C4 C3 C2 124.21(19) . . ? C5 C4 C3 117.53(18) . . ? C5 C4 C11 122.60(19) . . ? C3 C4 C11 119.83(18) . . ? C6 C5 C4 120.06(19) . . ? C5 C6 C1 121.91(18) . . ? C5 C6 N1 122.73(18) . . ? C1 C6 N1 115.33(17) . . ? C8 C7 C10 107.11(19) . . ? C8 C7 C9 109.82(19) . . ? C10 C7 C9 107.44(18) . . ? C8 C7 C2 110.29(17) . . ? C10 C7 C2 111.76(17) . . ? C9 C7 C2 110.32(17) . . ? C13 C11 C12 108.4(2) . . ? C13 C11 C4 112.53(19) . . ? C12 C11 C4 109.07(19) . . ? C13 C11 C14 107.8(2) . . ? C12 C11 C14 108.6(2) . . ? C4 C11 C14 110.36(18) . . ? N1 C15 C16 108.89(17) . . ? N2 C16 C15 109.51(17) . . ? N2 C17 C18 125.99(19) . . ? C19 C18 C23 120.2(2) . . ? C19 C18 C17 116.82(19) . . ? C23 C18 C17 122.93(19) . . ? C20 C19 C18 120.9(2) . . ? C19 C20 C21 120.8(2) . . ? C19 C20 Cl2 120.27(18) . . ? C21 C20 Cl2 118.90(18) . . ? C22 C21 C20 118.7(2) . . ? C21 C22 C23 123.7(2) . . ? C21 C22 Cl1 119.14(17) . . ? C23 C22 Cl1 117.20(16) . . ? O2 C23 C22 120.51(19) . . ? O2 C23 C18 123.89(19) . . ? C22 C23 C18 115.61(19) . . ? C30 C25 C26 117.6(3) . . ? C30 C25 C24 121.2(2) . . ? C26 C25 C24 121.2(2) . . ? C27 C26 C25 121.5(2) . . ? C26 C27 C28 120.3(3) . . ? C27 C28 C29 119.2(3) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C25 121.3(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 Cl1 C22 1.738(2) . ? Mg1 O2 1.9320(16) . ? Mg1 O1 1.9884(15) 3_566 ? Mg1 O1 2.0087(15) . ? Mg1 N2 2.0994(18) . ? Mg1 N1 2.2181(19) . ? Mg1 C1 2.796(2) . ? Mg1 Mg1 2.8290(13) 3_566 ? O1 C1 1.359(2) . ? O1 Mg1 1.9885(15) 3_566 ? N1 C6 1.459(3) . ? N1 C15 1.478(3) . ? C1 C6 1.396(3) . ? C1 C2 1.413(3) . ? Cl2 C20 1.750(2) . ? O2 C23 1.289(3) . ? N2 C17 1.281(3) . ? N2 C16 1.474(3) . ? C2 C3 1.395(3) . ? C2 C7 1.535(3) . ? C3 C4 1.391(3) . ? C4 C5 1.390(3) . ? C4 C11 1.534(3) . ? C5 C6 1.389(3) . ? C7 C8 1.529(3) . ? C7 C10 1.531(3) . ? C7 C9 1.533(3) . ? C11 C13 1.520(3) . ? C11 C12 1.531(3) . ? C11 C14 1.534(4) . ? C15 C16 1.517(3) . ? C17 C18 1.449(3) . ? C18 C19 1.404(3) . ? C18 C23 1.429(3) . ? C19 C20 1.372(3) . ? C20 C21 1.391(3) . ? C21 C22 1.372(3) . ? C22 C23 1.422(3) . ? C24 C25 1.505(4) . ? C25 C30 1.389(4) . ? C25 C26 1.389(4) . ? C26 C27 1.377(4) . ? C27 C28 1.378(4) . ? C28 C29 1.386(4) . ? C29 C30 1.379(4) . ?