#------------------------------------------------------------------------------ #$Date: 2020-10-06 10:40:06 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257404 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557286.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_1557286 loop_ _publ_author_name 'Du, Jing' 'Lang, Zhong-Ling' 'Ma, Yuan-Yuan' 'Tan, Hua-Qiao' 'Liu, Bai-Ling' 'Wang, Yong-Hui' 'Kang, Zhen-Hui' 'Li, Yang-Guang' _publ_section_title ; Polyoxometalate-based electron transfer modulation for efficient electrocatalytic carbon dioxide reduction ; _journal_issue 11 _journal_name_full 'Chemical Science' _journal_page_first 3007 _journal_page_last 3015 _journal_paper_doi 10.1039/C9SC05392A _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'O40 P W12, 3(C15 H11 Mn N3 O3), 2(C2 H3 N)' _chemical_formula_sum 'C49 H39 Mn3 N11 O49 P W12' _chemical_formula_weight 3967.78 _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 _atom_sites_solution_primary dual _audit_creation_date 2019-01-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-01-27 deposited with the CCDC. 2020-02-03 downloaded from the CCDC. ; _cell_angle_alpha 79.8800(10) _cell_angle_beta 89.029(2) _cell_angle_gamma 86.775(2) _cell_formula_units_Z 2 _cell_length_a 13.0328(5) _cell_length_b 15.6142(5) _cell_length_c 20.1424(7) _cell_measurement_reflns_used 9805 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 25.08 _cell_measurement_theta_min 2.65 _cell_volume 4028.6(2) _computing_cell_refinement 'SAINT v8.37A (Bruker, 2015)' _computing_data_reduction 'SAINT v8.37A (Bruker, 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_temperature 173.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0757 _diffrn_reflns_av_unetI/netI 0.0611 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 60836 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 2.242 _exptl_absorpt_coefficient_mu 17.627 _exptl_absorpt_correction_T_max 0.091 _exptl_absorpt_correction_T_min 0.076 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour orange _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 3.271 _exptl_crystal_description block _exptl_crystal_F_000 3559 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _refine_diff_density_max 2.904 _refine_diff_density_min -2.792 _refine_diff_density_rms 0.334 _refine_ls_extinction_coef 0.000179(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/1 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1132 _refine_ls_number_reflns 14148 _refine_ls_number_restraints 1972 _refine_ls_restrained_S_all 0.989 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0395 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+73.6504P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.1033 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11346 _reflns_number_total 14148 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc05392a2.cif _cod_data_source_block 1_CCDC1 _cod_depositor_comments ;Adding full bibliography for 1557284--1557286.cif. Adding full bibliography for 1557284--1557286.cif. ; _cod_database_code 1557286 _shelx_shelxl_version_number 2018/1 _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 0.092 _shelx_estimated_absorpt_t_min 0.077 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints O38, P1, O36, O26, O6 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3. Uiso/Uaniso restraints and constraints C29 \\sim C30 \\sim C28 \\sim C27 \\sim C26 \\sim C16 \\sim C17 \\sim C20 \\sim C21 \\sim C25 \\sim C24 \\sim C22 \\sim C23 \\sim C43 \\sim C41 \\sim C36 \\sim C40 \\sim C37 \\sim C35 \\sim C31 \\sim C32 \\sim C33 \\sim C11 \\sim C13 \\sim C12 \\sim C14 \\sim C15 \\sim C1 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C10 \\sim C9 \\sim C8 \\sim C7 \\sim C2 \\sim C19 \\sim C18 \\sim C39 \\sim C38 \\sim C44 \\sim C45 \\sim C34 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C42: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 N6 \\sim N4 \\sim N5 \\sim N3 \\sim N2 \\sim N1 \\sim N9 \\sim N10 \\sim N7 \\sim N8 \\sim N11: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 P1 \\sim O34 \\sim O40 \\sim O38 \\sim O22 \\sim O18 \\sim O4 \\sim O29 \\sim O26 \\sim O37 \\sim O2 \\sim O13 \\sim O21 \\sim O8 \\sim O19 \\sim O16 \\sim O6 \\sim O35 \\sim O10 \\sim O17 \\sim O20 \\sim O12 \\sim O28 \\sim O36 \\sim O23 \\sim O14 \\sim O27 \\sim O15 \\sim O31 \\sim O11 \\sim O5 \\sim O39 \\sim O9 \\sim O1 \\sim O7 \\sim O30 \\sim O33 \\sim O25 \\sim O24 \\sim O3 \\sim O32 \\sim O49 \\sim O46 \\sim O45 \\sim O44 \\sim O41 \\sim O42 \\sim O43 \\sim O47 \\sim O48: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.03 Uanis(N11) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O48) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.02 Uanis(P1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O33) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4.a Aromatic/amide H refined with riding coordinates: C16(H16), C17(H17), C25(H25), C24(H24), C22(H22), C23(H23), C40(H40), C37(H37), C31(H31), C32(H32), C33(H33), C1(H1), C3(H3), C4(H4), C10(H10), C9(H9), C8(H8), C7(H7), C2(H2), C19(H19), C18(H18), C39(H39), C38(H38), C34(H34) 4.b Idealised Me refined as rotating group: C30(H30A,H30B,H30C), C15(H15A,H15B,H15C), C45(H45A,H45B,H45C), C47(H47A,H47B, H47C), C49(H49A,H49B,H49C) ; _shelx_res_file ; TITL 1 P -1 R 1.res 1.res created by SHELXL-2018/1 at 15:34:30 on 27-Jan-2019 CELL 0.71073 13.0328 15.6142 20.1424 79.88 89.029 86.775 ZERR 2 0.0005 0.0005 0.0007 0.001 0.002 0.002 LATT 1 SFAC C 2.310 20.844 1.02 10.208 1.589 0.569 0.865 51.651 0.216 0.003 0.002 = 11.5 0.68 12.01 SFAC H SFAC Mn 11.282 5.341 7.357 0.343 3.019 17.867 2.244 83.754 1.09 0.337 = 0.728 3020 1.4 54.94 SFAC N 12.213 0.006 3.132 9.893 2.013 28.997 1.166 0.583 -11.529 0.006 = 0.003 19.6 0.68 14.01 SFAC O 3.049 13.277 2.287 5.701 1.546 0.324 0.867 32.909 0.251 0.011 0.006 = 32.5 0.68 16 SFAC P 6.434 1.907 4.179 27.157 1.78 0.526 1.491 68.165 1.115 0.102 0.094 = 410 1.05 30.97 SFAC W 29.082 1.72 15.43 9.226 14.433 0.322 5.12 57.056 9.887 -0.849 6.872 = 28600 1.37 183.84 UNIT 98 78 6 22 98 2 24 EQIV $1 -1+X,+Y,+Z EQIV $2 -1+X,-1+Y,+Z EQIV $3 +X,-1+Y,+Z EQIV $4 2-X,1-Y,1-Z EQIV $5 1-X,1-Y,2-Z EQIV $6 1-X,1-Y,1-Z DELU 0.001 0.001 O38 P1 O36 O26 O6 SIMU 0.01 0.03 3.8 $C SIMU 0.01 0.03 3.8 $N SIMU 0.01 0.03 3.8 P1 $O ISOR 0.01 0.02 N11 C48 C49 ISOR 0.1 0.02 O48 ISOR 0.001 0.002 P1 ISOR 0.005 0.01 O33 L.S. 20 PLAN 20 SIZE 0.26 0.28 0.3 TEMP -100 HTAB C30 O48 HTAB C30 O5_$1 HTAB C16 O13_$2 HTAB C40 O32 HTAB C37 O10_$3 HTAB C37 O1_$4 HTAB C15 O22 HTAB C15 O25 HTAB C1 O34_$5 HTAB C2 O24_$5 HTAB C19 O34_$1 HTAB C45 O23_$6 HTAB C47 O9_$4 HTAB C49 O44_$5 HTAB C49 O14 htab bond $H fmap 2 acta OMIT -3 50 OMIT 6 -9 11 OMIT 1 10 18 REM REM REM WGHT 0.031100 73.650398 EXTI 0.000179 FVAR 0.02585 W5 7 0.749338 0.795793 0.825865 11.00000 0.01481 0.01635 = 0.00959 -0.00395 0.00288 -0.00011 W7 7 0.606553 0.675314 0.718508 11.00000 0.00978 0.01983 = 0.01656 -0.00182 -0.00098 -0.00489 W3 7 1.009433 0.816011 0.801803 11.00000 0.01328 0.01516 = 0.00924 -0.00208 -0.00309 -0.00438 PART 1 W11 7 0.829103 0.806616 0.522946 11.00000 0.01803 0.01997 = 0.00661 0.00068 -0.00260 -0.00107 PART 0 W9 7 0.776796 0.497977 0.755390 11.00000 0.01617 0.01146 = 0.01330 -0.00164 0.00070 -0.00429 W4 7 0.958723 0.915405 0.625324 11.00000 0.01544 0.01267 = 0.00920 -0.00008 -0.00051 -0.00453 W1 7 1.055387 0.525925 0.730346 11.00000 0.01776 0.01510 = 0.01529 -0.00043 0.00032 0.00558 W10 7 1.009966 0.614940 0.564869 11.00000 0.02382 0.01581 = 0.00974 -0.00331 0.00477 0.00155 W2 7 1.143250 0.726168 0.664485 11.00000 0.00990 0.01586 = 0.01259 -0.00015 0.00106 -0.00079 W6 7 0.699309 0.891264 0.648128 11.00000 0.01348 0.01467 = 0.01373 -0.00142 -0.00311 0.00336 W12 7 0.916472 0.617185 0.865342 11.00000 0.01342 0.01742 = 0.00633 0.00143 -0.00107 -0.00114 W8 7 0.731404 0.590909 0.590218 11.00000 0.01976 0.01726 = 0.01044 -0.00372 -0.00181 -0.00773 P1 6 0.873785 0.705690 0.693148 11.00000 0.00087 0.00219 = 0.00068 -0.00074 0.00037 -0.00065 O34 5 0.753190 0.395764 0.794703 11.00000 0.04111 0.01834 = 0.01845 -0.00119 0.00236 -0.00712 O40 5 0.718555 0.874551 0.557370 11.00000 0.02123 0.01966 = 0.01454 -0.00300 -0.00408 -0.00167 O38 5 0.850873 0.791455 0.644348 11.00000 0.01584 0.00843 = 0.01019 0.00312 -0.00336 0.00096 O22 5 0.646613 0.559119 0.762611 11.00000 0.01744 0.02129 = 0.01322 -0.00210 -0.00075 -0.00412 O18 5 0.603604 0.970526 0.638504 11.00000 0.01995 0.02226 = 0.02279 0.00262 -0.00931 0.00733 O4 5 0.943249 0.725251 0.529831 11.00000 0.01879 0.01940 = 0.01279 0.00059 0.00197 0.00109 O29 5 1.103595 0.759182 0.749503 11.00000 0.01416 0.01889 = 0.01001 0.00003 -0.00347 0.00074 O26 5 0.883134 0.725024 0.764491 11.00000 0.01342 0.01624 = 0.00438 -0.00592 -0.00173 -0.00103 O37 5 0.823112 0.551166 0.827519 11.00000 0.01378 0.02015 = 0.01576 -0.00183 0.00105 -0.00173 O2 5 0.874979 0.574240 0.576284 11.00000 0.01509 0.01922 = 0.01597 -0.00084 0.00221 -0.00230 O13 5 0.972821 0.892054 0.720231 11.00000 0.01818 0.01507 = 0.00987 -0.00056 0.00014 0.00326 O21 5 0.478512 0.677040 0.733957 11.00000 0.01599 0.03270 = 0.02688 -0.00701 0.00385 -0.00144 O8 5 1.066920 0.827940 0.624148 11.00000 0.01473 0.01518 = 0.01133 0.00068 -0.00002 0.00021 O19 5 0.662140 0.719157 0.790768 11.00000 0.01840 0.02072 = 0.01591 -0.00227 -0.00047 -0.00541 O16 5 0.674768 0.841520 0.880281 11.00000 0.02397 0.03567 = 0.01400 -0.01420 0.00782 -0.00089 O6 5 0.976182 0.662442 0.672645 11.00000 0.00840 0.01575 = 0.01126 -0.00234 0.00402 0.00465 O35 5 0.747226 0.706299 0.546283 11.00000 0.01807 0.01670 = 0.01631 0.00158 -0.00049 -0.00222 O10 5 1.021010 1.008525 0.603708 11.00000 0.02235 0.02228 = 0.02007 0.00395 -0.00046 -0.00470 O17 5 0.726966 0.871761 0.742874 11.00000 0.01845 0.01743 = 0.00982 -0.00398 -0.00250 -0.00181 O20 5 0.628642 0.787040 0.666933 11.00000 0.01907 0.02063 = 0.01394 -0.00358 -0.00327 -0.00496 O12 5 1.085269 0.876936 0.839615 11.00000 0.02211 0.03198 = 0.02247 -0.00980 -0.00550 -0.00814 O28 5 1.018743 0.570369 0.809533 11.00000 0.01595 0.01930 = 0.01619 0.00100 -0.00032 0.00034 O36 5 0.787416 0.644426 0.690673 11.00000 0.01112 0.01461 = 0.01457 -0.00433 -0.00087 -0.00954 O23 5 0.612548 0.630084 0.635371 11.00000 0.01463 0.02505 = 0.01770 -0.00212 -0.00147 -0.00667 O14 5 0.875602 0.847723 0.835576 11.00000 0.01766 0.02031 = 0.01753 -0.00149 -0.00021 -0.00257 O27 5 1.004522 0.711972 0.866984 11.00000 0.01560 0.02088 = 0.01242 0.00434 -0.00194 -0.00123 O15 5 0.819591 0.959753 0.636022 11.00000 0.02131 0.02047 = 0.01198 -0.00279 -0.00244 0.00052 O31 5 0.918321 0.488135 0.732833 11.00000 0.01487 0.02050 = 0.01558 -0.00201 -0.00143 -0.00019 O11 5 0.918594 0.895263 0.538835 11.00000 0.01968 0.01918 = 0.01553 -0.00191 -0.00212 -0.00371 O5 5 1.057270 0.524168 0.635133 11.00000 0.02504 0.01996 = 0.01629 -0.00432 0.00246 0.00122 O39 5 0.814873 0.835206 0.438433 11.00000 0.02561 0.02658 = 0.01510 -0.00232 -0.00372 -0.00789 O9 5 1.160169 0.608870 0.712999 11.00000 0.01721 0.02136 = 0.01661 0.00389 -0.00303 0.00382 O1 5 1.053605 0.579840 0.494976 11.00000 0.03366 0.02742 = 0.02593 -0.01724 0.01430 -0.00443 O7 5 1.268143 0.755424 0.655626 11.00000 0.01375 0.03500 = 0.02393 0.00338 0.00277 -0.00425 O30 5 1.127075 0.433520 0.758803 11.00000 0.02348 0.01685 = 0.02641 0.00575 0.00788 0.00403 O33 5 0.678864 0.544850 0.530021 11.00000 0.04190 0.02640 = 0.01811 -0.01233 -0.00802 -0.01198 O25 5 0.806199 0.693596 0.884580 11.00000 0.01938 0.02167 = 0.01640 -0.00221 -0.00121 -0.00345 O24 5 0.937921 0.554893 0.941945 11.00000 0.02344 0.02164 = 0.01735 0.00138 -0.00078 -0.00603 O3 5 1.127187 0.677799 0.585751 11.00000 0.02160 0.02060 = 0.01899 -0.00255 0.00185 0.00123 O32 5 0.742678 0.495734 0.664564 11.00000 0.01882 0.01949 = 0.01529 -0.00076 0.00120 -0.00608 O49 5 0.607650 0.104761 0.725499 11.00000 0.04411 0.04490 = 0.03229 -0.00625 0.00679 -0.01496 O46 5 0.420442 0.147151 0.801423 11.00000 0.02034 0.07304 = 0.07477 -0.03694 -0.00146 0.00137 O45 5 0.230767 0.009606 0.699537 11.00000 0.06006 0.04557 = 0.04255 -0.02434 -0.01124 0.02005 O44 5 0.217115 -0.008495 0.907299 11.00000 0.05015 0.03226 = 0.02514 -0.00087 -0.00556 -0.00505 O41 5 0.612088 0.907535 1.027271 11.00000 0.06364 0.06317 = 0.04110 0.00328 -0.01605 -0.04216 O42 5 0.300416 0.929390 1.060105 11.00000 0.07153 0.04374 = 0.04838 -0.01035 0.02370 0.00651 O43 5 0.470887 0.711944 1.150663 11.00000 0.11302 0.06510 = 0.01991 0.00876 -0.02320 -0.02162 O47 5 0.529744 0.373250 0.686900 11.00000 0.08111 0.07010 = 0.06885 -0.02821 0.01611 0.03054 N6 4 0.189075 0.238312 0.714195 11.00000 0.02348 0.02253 = 0.02195 -0.00832 -0.00082 0.00144 N4 4 0.039807 0.136968 0.789611 11.00000 0.02346 0.01613 = 0.01664 -0.00761 -0.00003 0.00483 N5 4 0.154558 0.228553 0.850375 11.00000 0.02593 0.01594 = 0.01683 -0.00406 -0.00743 0.00078 N3 4 0.526969 0.703915 0.976262 11.00000 0.00872 0.02859 = 0.02710 0.00132 0.00269 -0.00227 N2 4 0.412808 0.843557 0.908684 11.00000 0.00766 0.01380 = 0.02257 -0.00634 0.00718 0.00116 N1 4 0.324270 0.723306 0.991960 11.00000 0.00832 0.02387 = 0.03173 -0.00209 0.00444 0.00083 N9 4 0.589120 0.329869 0.519797 11.00000 0.03772 0.03441 = 0.03124 -0.00318 0.00445 0.00109 N10 4 0.607425 0.516921 0.096367 11.00000 0.07491 0.08783 = 0.04433 0.00877 0.01058 0.01383 N7 4 0.636337 0.156005 0.539311 11.00000 0.01964 0.02509 = 0.01663 -0.00484 0.00889 -0.00964 N8 4 0.742578 0.247820 0.605703 11.00000 0.01910 0.01692 = 0.01953 -0.00385 0.00611 -0.00377 N11 4 1.083035 0.837388 1.008612 11.00000 0.12422 0.09769 = 0.08591 0.00670 0.00793 -0.03083 MN1 3 0.439636 0.798533 1.009443 11.00000 0.02588 0.02093 = 0.01672 -0.00061 0.00089 -0.00559 MN2 3 0.195643 0.136968 0.791685 11.00000 0.02021 0.02121 = 0.01461 -0.00595 -0.00010 0.00024 MN3 3 0.588657 0.239044 0.603204 11.00000 0.01724 0.03859 = 0.02600 -0.00848 0.00116 0.00609 C29 1 0.191424 0.293477 0.669279 11.00000 0.02630 0.02875 = 0.02184 -0.01505 -0.00102 0.00428 C30 1 0.197607 0.362322 0.611014 11.00000 0.06509 0.02419 = 0.02379 0.00094 0.00511 0.00102 AFIX 137 H30A 2 0.251569 0.346210 0.580310 11.00000 -1.50000 H30B 2 0.213915 0.416545 0.625728 11.00000 -1.50000 H30C 2 0.131516 0.370740 0.587625 11.00000 -1.50000 AFIX 0 C28 1 0.332444 0.144219 0.796462 11.00000 0.02562 0.02969 = 0.02972 -0.00996 -0.00218 0.00189 C27 1 0.217241 0.059477 0.734234 11.00000 0.02343 0.02977 = 0.02616 -0.01097 -0.00571 0.00589 C26 1 0.205668 0.046416 0.862968 11.00000 0.02443 0.02581 = 0.02540 -0.01336 -0.00335 -0.00343 C16 1 -0.016105 0.082289 0.762268 11.00000 0.02858 0.02760 = 0.02560 -0.01067 -0.00337 -0.00224 AFIX 43 H16 2 0.019546 0.040669 0.739924 11.00000 -1.20000 AFIX 0 C17 1 -0.121549 0.082975 0.764688 11.00000 0.02836 0.03434 = 0.02614 -0.00879 -0.00688 -0.00582 AFIX 43 H17 2 -0.157428 0.042668 0.744837 11.00000 -1.20000 AFIX 0 C20 1 -0.012875 0.195791 0.820070 11.00000 0.02735 0.02628 = 0.02482 -0.01093 -0.00120 -0.00442 C21 1 0.053741 0.249864 0.853235 11.00000 0.02889 0.02618 = 0.02595 -0.01182 0.00133 -0.00472 C25 1 0.219587 0.271490 0.882317 11.00000 0.03024 0.02755 = 0.02560 -0.01011 -0.00335 -0.00740 AFIX 43 H25 2 0.291230 0.256896 0.880664 11.00000 -1.20000 AFIX 0 C24 1 0.184889 0.336501 0.917610 11.00000 0.03958 0.03288 = 0.02879 -0.00840 -0.00457 -0.01365 AFIX 43 H24 2 0.232419 0.365615 0.939794 11.00000 -1.20000 AFIX 0 C22 1 0.014529 0.315897 0.886898 11.00000 0.03293 0.02888 = 0.02795 -0.00955 0.00169 -0.00423 AFIX 43 H22 2 -0.057076 0.331152 0.886773 11.00000 -1.20000 AFIX 0 C23 1 0.081762 0.358411 0.920253 11.00000 0.03671 0.02417 = 0.02793 -0.00919 -0.00005 -0.00756 AFIX 43 H23 2 0.056973 0.402214 0.944690 11.00000 -1.20000 AFIX 0 C43 1 0.599062 0.155608 0.677234 11.00000 0.02319 0.03443 = 0.02468 -0.00817 -0.00003 -0.00633 C41 1 0.553396 0.321390 0.654052 11.00000 0.03256 0.04514 = 0.03293 -0.00356 0.00039 0.01138 C36 1 0.799746 0.192184 0.573895 11.00000 0.02561 0.02542 = 0.02080 -0.00025 0.00233 -0.00537 C40 1 0.792695 0.297610 0.641860 11.00000 0.02806 0.02985 = 0.02549 -0.00272 0.00497 -0.00197 AFIX 43 H40 2 0.754257 0.336659 0.665218 11.00000 -1.20000 AFIX 0 C37 1 0.905234 0.186488 0.575779 11.00000 0.02560 0.02764 = 0.02150 0.00290 0.00386 -0.00283 AFIX 43 H37 2 0.943803 0.149695 0.550545 11.00000 -1.20000 AFIX 0 C35 1 0.739012 0.144496 0.533097 11.00000 0.02563 0.02533 = 0.02075 -0.00064 0.00370 -0.00615 C31 1 0.575862 0.118370 0.500388 11.00000 0.03008 0.03287 = 0.02487 0.00077 -0.00235 -0.00856 AFIX 43 H31 2 0.503519 0.128757 0.503147 11.00000 -1.20000 AFIX 0 C32 1 0.614567 0.065161 0.456494 11.00000 0.03913 0.02882 = 0.02014 0.00047 -0.00748 -0.01206 AFIX 43 H32 2 0.569927 0.040158 0.429297 11.00000 -1.20000 AFIX 0 C33 1 0.718053 0.049719 0.453403 11.00000 0.04083 0.02883 = 0.02334 0.00172 0.00038 -0.00645 AFIX 43 H33 2 0.746672 0.011872 0.424997 11.00000 -1.20000 AFIX 0 C11 1 0.548303 0.866062 1.017860 11.00000 0.03105 0.02846 = 0.02661 0.00237 -0.00138 -0.00486 C13 1 0.457695 0.746160 1.095818 11.00000 0.02928 0.02931 = 0.03266 0.00011 -0.00338 -0.00565 C12 1 0.353573 0.880695 1.038792 11.00000 0.02942 0.02808 = 0.02872 0.00264 0.00369 -0.00212 C14 1 0.568249 0.647248 0.956457 11.00000 0.02220 0.02655 = 0.03022 0.00511 0.00014 -0.00160 C15 1 0.616196 0.570841 0.934868 11.00000 0.03297 0.03487 = 0.03416 0.00168 0.01358 -0.00687 AFIX 137 H15A 2 0.598155 0.570763 0.887845 11.00000 -1.50000 H15B 2 0.591931 0.518354 0.963456 11.00000 -1.50000 H15C 2 0.690988 0.571639 0.938677 11.00000 -1.50000 AFIX 0 C1 1 0.279336 0.666788 1.039339 11.00000 0.02369 0.02574 = 0.03819 0.00249 0.00541 -0.00304 AFIX 43 H1 2 0.295543 0.664592 1.085434 11.00000 -1.20000 AFIX 0 C3 1 0.186452 0.612181 0.957445 11.00000 0.02200 0.02663 = 0.04309 0.00000 -0.00257 -0.00341 AFIX 43 H3 2 0.140702 0.572060 0.945721 11.00000 -1.20000 AFIX 0 C4 1 0.230063 0.672026 0.908030 11.00000 0.02412 0.02667 = 0.04163 0.00527 -0.00545 0.00044 AFIX 43 H4 2 0.212581 0.675162 0.862037 11.00000 -1.20000 AFIX 0 C5 1 0.300200 0.727962 0.926336 11.00000 0.02253 0.02460 = 0.03178 0.00056 0.00065 -0.00078 C6 1 0.352234 0.794693 0.880040 11.00000 0.02114 0.02482 = 0.03003 0.00116 -0.00018 0.00175 C10 1 0.462129 0.907740 0.869316 11.00000 0.02160 0.02397 = 0.02837 0.00245 0.00302 0.00085 AFIX 43 H10 2 0.502543 0.944279 0.890058 11.00000 -1.20000 AFIX 0 C9 1 0.455721 0.921918 0.800094 11.00000 0.02299 0.03016 = 0.02768 0.00458 0.00433 0.00584 AFIX 43 H9 2 0.492333 0.966775 0.773486 11.00000 -1.20000 AFIX 0 C8 1 0.396402 0.870972 0.770325 11.00000 0.02460 0.03348 = 0.02890 0.00046 0.00282 0.00640 AFIX 43 H8 2 0.391786 0.879522 0.722574 11.00000 -1.20000 AFIX 0 C7 1 0.342218 0.805971 0.810173 11.00000 0.02032 0.02834 = 0.03112 -0.00214 -0.00181 0.00245 AFIX 43 H7 2 0.299566 0.770291 0.790196 11.00000 -1.20000 AFIX 0 C2 1 0.209209 0.611229 1.021935 11.00000 0.02152 0.02673 = 0.04442 0.00554 0.00489 -0.00641 AFIX 43 H2 2 0.176911 0.571965 1.056313 11.00000 -1.20000 AFIX 0 C19 1 -0.119887 0.201421 0.824803 11.00000 0.03037 0.03409 = 0.02895 -0.00714 0.00216 -0.00250 AFIX 43 H19 2 -0.154837 0.243775 0.846761 11.00000 -1.20000 AFIX 0 C18 1 -0.173398 0.142684 0.796159 11.00000 0.02928 0.03536 = 0.02616 -0.00863 -0.00352 -0.00304 AFIX 43 H18 2 -0.246324 0.144247 0.798566 11.00000 -1.20000 AFIX 0 C39 1 0.899361 0.292646 0.645435 11.00000 0.02870 0.03305 = 0.02150 -0.00159 0.00008 -0.01320 AFIX 43 H39 2 0.933319 0.329939 0.669381 11.00000 -1.20000 AFIX 0 C38 1 0.953857 0.235578 0.615267 11.00000 0.02562 0.03618 = 0.02365 -0.00026 0.00099 -0.00691 AFIX 43 H38 2 1.026245 0.228611 0.620903 11.00000 -1.20000 AFIX 0 C44 1 0.597905 0.375103 0.470853 11.00000 0.03617 0.04554 = 0.03535 -0.00510 -0.00893 0.00987 C45 1 0.609593 0.435532 0.406876 11.00000 0.05202 0.05754 = 0.04109 0.00793 -0.01416 -0.01283 AFIX 137 H45A 2 0.579233 0.411575 0.370369 11.00000 -1.50000 H45B 2 0.682768 0.443500 0.397378 11.00000 -1.50000 H45C 2 0.574576 0.491850 0.410186 11.00000 -1.50000 AFIX 0 C34 1 0.780523 0.088734 0.491203 11.00000 0.03034 0.02659 = 0.02210 -0.00072 0.00361 -0.00479 AFIX 43 H34 2 0.852872 0.077969 0.489082 11.00000 -1.20000 AFIX 0 C46 1 0.614552 0.514645 0.152110 11.00000 0.03668 0.05459 = 0.04142 0.00364 0.00930 -0.01254 C47 1 0.621924 0.514095 0.223567 11.00000 0.03938 0.05376 = 0.04924 0.00126 0.00350 -0.00651 AFIX 137 H47A 2 0.641132 0.571407 0.231078 11.00000 -1.50000 H47B 2 0.674273 0.469647 0.242976 11.00000 -1.50000 H47C 2 0.555374 0.500860 0.245190 11.00000 -1.50000 AFIX 0 C48 1 1.008376 0.873934 0.993459 11.00000 0.07159 0.07880 = 0.05526 -0.01503 0.01103 -0.02038 C49 1 0.913806 0.920873 0.966093 11.00000 0.11292 0.12083 = 0.07915 -0.06482 0.01122 -0.01524 AFIX 137 H49A 2 0.930601 0.976244 0.938023 11.00000 -1.50000 H49B 2 0.868529 0.932304 1.003252 11.00000 -1.50000 H49C 2 0.878926 0.885518 0.938670 11.00000 -1.50000 AFIX 0 C42 1 0.455171 0.222259 0.601063 11.00000 0.03063 0.05448 = 0.03438 -0.00485 -0.00557 0.00377 O48 5 0.372710 0.202390 0.605561 11.00000 0.02586 0.20061 = 0.10357 -0.04044 -0.00741 -0.02546 HKLF 4 REM 1 P -1 R 1.res REM R1 = 0.0395 for 11346 Fo > 4sig(Fo) and 0.0572 for all 14148 data REM 1132 parameters refined using 1972 restraints END WGHT 0.0311 73.6416 REM Instructions for potential hydrogen bonds HTAB C30 O48 HTAB C30 O5_$1 HTAB C16 O13_$2 HTAB C40 O32 HTAB C37 O10_$3 HTAB C37 O11_$4 HTAB C15 O22 HTAB C15 O25 HTAB C1 O34_$5 HTAB C2 O24_$5 HTAB C19 O34_$1 HTAB C45 O23_$6 HTAB C47 O9_$4 HTAB C49 O44_$5 HTAB C49 O14 REM Highest difference peak 2.904, deepest hole -2.792, 1-sigma level 0.334 Q1 1 0.8149 0.7565 0.5240 11.00000 0.05 2.90 Q2 1 1.0039 0.4990 0.7488 11.00000 0.05 2.19 Q3 1 0.6522 0.5850 0.8915 11.00000 0.05 2.05 Q4 1 0.6902 0.8382 0.6475 11.00000 0.05 2.01 Q5 1 0.8206 0.8204 0.4781 11.00000 0.05 1.96 Q6 1 0.9664 0.8601 0.6261 11.00000 0.05 1.94 Q7 1 0.7944 0.4739 0.7991 11.00000 0.05 1.90 Q8 1 0.9639 0.5815 0.5675 11.00000 0.05 1.76 Q9 1 0.7003 0.9011 0.6014 11.00000 0.05 1.74 Q10 1 0.7788 0.5535 0.7495 11.00000 0.05 1.73 Q11 1 0.9067 0.5664 0.8666 11.00000 0.05 1.73 Q12 1 0.9015 0.1729 0.5032 11.00000 0.05 1.71 Q13 1 0.6993 0.8802 0.6963 11.00000 0.05 1.71 Q14 1 0.4420 0.2236 0.4583 11.00000 0.05 1.69 Q15 1 0.7598 0.5647 0.6380 11.00000 0.05 1.67 Q16 1 0.7321 0.7349 0.8318 11.00000 0.05 1.61 Q17 1 0.4960 0.5212 0.2216 11.00000 0.05 1.61 Q18 1 0.6052 0.7346 0.7137 11.00000 0.05 1.60 Q19 1 0.7952 0.5535 0.6394 11.00000 0.05 1.60 Q20 1 0.5997 0.7338 0.6628 11.00000 0.05 1.58 ; _shelx_res_checksum 77626 _olex2_submission_special_instructions 'No special instructions were received' 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_disorder_assembly _atom_site_disorder_group W5 W 0.74934(4) 0.79579(3) 0.82587(2) 0.01344(11) Uani 1 1 d . . . . W7 W 0.60655(4) 0.67531(3) 0.71851(2) 0.01539(12) Uani 1 1 d . . . . W3 W 1.00943(4) 0.81601(3) 0.80180(2) 0.01240(11) Uani 1 1 d . . . . W11 W 0.82910(4) 0.80662(3) 0.52295(2) 0.01520(12) Uani 1 1 d . . A 1 W9 W 0.77680(4) 0.49798(3) 0.75539(2) 0.01358(11) Uani 1 1 d . . . . W4 W 0.95872(4) 0.91541(3) 0.62532(2) 0.01251(11) Uani 1 1 d . . . . W1 W 1.05539(4) 0.52592(3) 0.73035(3) 0.01657(12) Uani 1 1 d . . . . W10 W 1.00997(4) 0.61494(3) 0.56487(2) 0.01648(12) Uani 1 1 d . . . . W2 W 1.14325(4) 0.72617(3) 0.66449(2) 0.01307(11) Uani 1 1 d . . . . W6 W 0.69931(4) 0.89126(3) 0.64813(2) 0.01421(11) Uani 1 1 d . . . . W12 W 0.91647(4) 0.61718(3) 0.86534(2) 0.01279(11) Uani 1 1 d . . . . W8 W 0.73140(4) 0.59091(3) 0.59022(2) 0.01539(12) Uani 1 1 d . . . . P1 P 0.87378(19) 0.70569(15) 0.69315(13) 0.0012(5) Uani 1 1 d . U . . O34 O 0.7532(7) 0.3958(5) 0.7947(4) 0.026(2) Uani 1 1 d . U . . O40 O 0.7186(6) 0.8746(5) 0.5574(4) 0.0184(14) Uani 1 1 d . U . . O38 O 0.8509(6) 0.7915(4) 0.6443(4) 0.0121(10) Uani 1 1 d . U . . O22 O 0.6466(6) 0.5591(5) 0.7626(4) 0.0173(14) Uani 1 1 d . U . . O18 O 0.6036(6) 0.9705(5) 0.6385(4) 0.0227(19) Uani 1 1 d . U . . O4 O 0.9432(6) 0.7253(5) 0.5298(4) 0.0175(13) Uani 1 1 d . U . . O29 O 1.1036(6) 0.7592(5) 0.7495(4) 0.0147(13) Uani 1 1 d . U . . O26 O 0.8831(6) 0.7250(5) 0.7645(4) 0.0108(10) Uani 1 1 d . U . . O37 O 0.8231(6) 0.5512(5) 0.8275(4) 0.0167(13) Uani 1 1 d . U . . O2 O 0.8750(6) 0.5742(5) 0.5763(4) 0.0170(13) Uani 1 1 d . U . . O13 O 0.9728(6) 0.8921(5) 0.7202(4) 0.0147(13) Uani 1 1 d . U . . O21 O 0.4785(6) 0.6770(6) 0.7340(5) 0.025(2) Uani 1 1 d . U . . O8 O 1.0669(6) 0.8279(5) 0.6241(4) 0.0141(13) Uani 1 1 d . U . . O19 O 0.6621(6) 0.7192(5) 0.7908(4) 0.0183(13) Uani 1 1 d . U . . O16 O 0.6748(7) 0.8415(6) 0.8803(4) 0.0235(19) Uani 1 1 d . U . . O6 O 0.9762(6) 0.6624(5) 0.6726(4) 0.0121(10) Uani 1 1 d . U . . O35 O 0.7472(6) 0.7063(5) 0.5463(4) 0.0175(13) Uani 1 1 d . U . . O10 O 1.0210(7) 1.0085(5) 0.6037(4) 0.0224(19) Uani 1 1 d . U . . O17 O 0.7270(6) 0.8718(5) 0.7429(4) 0.0150(13) Uani 1 1 d . U . . O20 O 0.6286(6) 0.7870(5) 0.6669(4) 0.0176(13) Uani 1 1 d . U . . O12 O 1.0853(7) 0.8769(6) 0.8396(4) 0.025(2) Uani 1 1 d . U . . O28 O 1.0187(6) 0.5704(5) 0.8095(4) 0.0177(13) Uani 1 1 d . U . . O36 O 0.7874(6) 0.6444(5) 0.6907(4) 0.0129(10) Uani 1 1 d . U . . O23 O 0.6125(6) 0.6301(5) 0.6354(4) 0.0191(14) Uani 1 1 d . U . . O14 O 0.8756(6) 0.8477(5) 0.8356(4) 0.0187(14) Uani 1 1 d . U . . O27 O 1.0045(6) 0.7120(5) 0.8670(4) 0.0171(14) Uani 1 1 d . U . . O15 O 0.8196(6) 0.9598(5) 0.6360(4) 0.0180(14) Uani 1 1 d . U . . O31 O 0.9183(6) 0.4881(5) 0.7328(4) 0.0171(13) Uani 1 1 d . U . . O11 O 0.9186(6) 0.8953(5) 0.5388(4) 0.0181(14) Uani 1 1 d . U . . O5 O 1.0573(7) 0.5242(5) 0.6351(4) 0.0204(15) Uani 1 1 d . U . . O39 O 0.8149(7) 0.8352(5) 0.4384(4) 0.0223(19) Uani 1 1 d . U . . O9 O 1.1602(6) 0.6089(5) 0.7130(4) 0.0194(15) Uani 1 1 d . U . . O1 O 1.0536(7) 0.5798(6) 0.4950(5) 0.028(2) Uani 1 1 d . U . . O7 O 1.2681(6) 0.7554(6) 0.6556(4) 0.025(2) Uani 1 1 d . U . . O30 O 1.1271(7) 0.4335(5) 0.7588(4) 0.024(2) Uani 1 1 d . U . . O33 O 0.6789(7) 0.5448(6) 0.5300(4) 0.027(2) Uani 1 1 d . U . . O25 O 0.8062(6) 0.6936(5) 0.8846(4) 0.0192(14) Uani 1 1 d . U . . O24 O 0.9379(7) 0.5549(5) 0.9419(4) 0.0212(19) Uani 1 1 d . U . . O3 O 1.1272(6) 0.6778(5) 0.5858(4) 0.0206(15) Uani 1 1 d . U . . O32 O 0.7427(6) 0.4957(5) 0.6646(4) 0.0180(14) Uani 1 1 d . U . . O49 O 0.6076(8) 0.1048(7) 0.7255(5) 0.040(3) Uani 1 1 d . U . . O46 O 0.4204(8) 0.1472(8) 0.8014(7) 0.053(3) Uani 1 1 d . U . . O45 O 0.2308(9) 0.0096(7) 0.6995(6) 0.048(3) Uani 1 1 d . U . . O44 O 0.2171(8) -0.0085(6) 0.9073(5) 0.036(2) Uani 1 1 d . U . . O41 O 0.6121(10) 0.9075(8) 1.0273(6) 0.056(3) Uani 1 1 d . U . . O42 O 0.3004(10) 0.9294(7) 1.0601(6) 0.055(3) Uani 1 1 d . U . . O43 O 0.4709(12) 0.7119(8) 1.1507(6) 0.067(4) Uani 1 1 d . U . . O47 O 0.5297(11) 0.3732(9) 0.6869(7) 0.073(4) Uani 1 1 d . U . . N6 N 0.1891(8) 0.2383(7) 0.7142(6) 0.022(2) Uani 1 1 d . U . . N4 N 0.0398(8) 0.1370(6) 0.7896(5) 0.018(2) Uani 1 1 d . U . . N5 N 0.1546(8) 0.2286(6) 0.8504(5) 0.019(2) Uani 1 1 d . U . . N3 N 0.5270(8) 0.7039(7) 0.9763(5) 0.022(2) Uani 1 1 d . U . . N2 N 0.4128(7) 0.8436(6) 0.9087(5) 0.0144(19) Uani 1 1 d . U . . N1 N 0.3243(7) 0.7233(7) 0.9920(6) 0.022(2) Uani 1 1 d . U . . N9 N 0.5891(10) 0.3299(8) 0.5198(6) 0.035(2) Uani 1 1 d . U . . N10 N 0.6074(14) 0.5169(12) 0.0964(9) 0.072(5) Uani 1 1 d . U . . N7 N 0.6363(8) 0.1560(6) 0.5393(5) 0.020(2) Uani 1 1 d . U . . N8 N 0.7426(8) 0.2478(6) 0.6057(5) 0.018(2) Uani 1 1 d . U . . N11 N 1.083(2) 0.8374(15) 1.0086(11) 0.105(7) Uani 1 1 d . U . . Mn1 Mn 0.43964(15) 0.79853(12) 1.00944(10) 0.0214(4) Uani 1 1 d . . . . Mn2 Mn 0.19564(14) 0.13697(12) 0.79168(9) 0.0184(4) Uani 1 1 d . . . . Mn3 Mn 0.58866(15) 0.23904(14) 0.60320(11) 0.0272(5) Uani 1 1 d . . . . C29 C 0.1914(10) 0.2935(9) 0.6693(7) 0.025(2) Uani 1 1 d . U . . C30 C 0.1976(13) 0.3623(9) 0.6110(7) 0.039(4) Uani 1 1 d . U . . H30A H 0.251569 0.346210 0.580310 0.058 Uiso 1 1 calc GR . . . H30B H 0.213915 0.416545 0.625728 0.058 Uiso 1 1 calc GR . . . H30C H 0.131516 0.370740 0.587625 0.058 Uiso 1 1 calc GR . . . C28 C 0.3324(11) 0.1442(9) 0.7965(7) 0.028(2) Uani 1 1 d . U . . C27 C 0.2172(10) 0.0595(9) 0.7342(7) 0.026(2) Uani 1 1 d . U . . C26 C 0.2057(10) 0.0464(8) 0.8630(7) 0.024(2) Uani 1 1 d . U . . C16 C -0.0161(10) 0.0823(8) 0.7623(7) 0.0265(19) Uani 1 1 d . U . . H16 H 0.019546 0.040669 0.739924 0.032 Uiso 1 1 calc R . . . C17 C -0.1215(11) 0.0830(9) 0.7647(7) 0.029(2) Uani 1 1 d . U . . H17 H -0.157428 0.042668 0.744837 0.035 Uiso 1 1 calc R . . . C20 C -0.0129(10) 0.1958(8) 0.8201(7) 0.0252(18) Uani 1 1 d . U . . C21 C 0.0537(11) 0.2499(8) 0.8532(7) 0.0260(18) Uani 1 1 d . U . . C25 C 0.2196(11) 0.2715(8) 0.8823(7) 0.0269(19) Uani 1 1 d . U . . H25 H 0.291230 0.256896 0.880664 0.032 Uiso 1 1 calc R . . . C24 C 0.1849(12) 0.3365(9) 0.9176(7) 0.033(2) Uani 1 1 d . U . . H24 H 0.232419 0.365615 0.939794 0.039 Uiso 1 1 calc R . . . C22 C 0.0145(11) 0.3159(8) 0.8869(7) 0.029(2) Uani 1 1 d . U . . H22 H -0.057076 0.331152 0.886773 0.035 Uiso 1 1 calc R . . . C23 C 0.0818(11) 0.3584(8) 0.9203(7) 0.029(2) Uani 1 1 d . U . . H23 H 0.056973 0.402214 0.944690 0.035 Uiso 1 1 calc R . . . C43 C 0.5991(10) 0.1556(9) 0.6772(7) 0.027(2) Uani 1 1 d . U . . C41 C 0.5534(12) 0.3214(10) 0.6541(8) 0.038(3) Uani 1 1 d . U . . C36 C 0.7997(10) 0.1922(8) 0.5739(7) 0.0243(18) Uani 1 1 d . U . . C40 C 0.7927(11) 0.2976(9) 0.6419(7) 0.028(2) Uani 1 1 d . U . . H40 H 0.754257 0.336659 0.665218 0.034 Uiso 1 1 calc R . . . C37 C 0.9052(10) 0.1865(8) 0.5758(7) 0.026(2) Uani 1 1 d . U . . H37 H 0.943803 0.149695 0.550545 0.031 Uiso 1 1 calc R . . . C35 C 0.7390(10) 0.1445(8) 0.5331(7) 0.0242(18) Uani 1 1 d . U . . C31 C 0.5759(11) 0.1184(9) 0.5004(7) 0.030(2) Uani 1 1 d . U . . H31 H 0.503519 0.128757 0.503147 0.036 Uiso 1 1 calc R . . . C32 C 0.6146(11) 0.0652(9) 0.4565(7) 0.029(2) Uani 1 1 d . U . . H32 H 0.569927 0.040158 0.429297 0.035 Uiso 1 1 calc R . . . C33 C 0.7181(12) 0.0497(9) 0.4534(7) 0.032(2) Uani 1 1 d . U . . H33 H 0.746672 0.011872 0.424997 0.038 Uiso 1 1 calc R . . . C11 C 0.5483(11) 0.8661(9) 1.0179(7) 0.029(2) Uani 1 1 d . U . . C13 C 0.4577(11) 0.7462(9) 1.0958(8) 0.031(2) Uani 1 1 d . U . . C12 C 0.3536(11) 0.8807(9) 1.0388(7) 0.030(2) Uani 1 1 d . U . . C14 C 0.5682(10) 0.6472(9) 0.9565(7) 0.028(2) Uani 1 1 d . U . . C15 C 0.6162(11) 0.5708(9) 0.9349(8) 0.035(3) Uani 1 1 d . U . . H15A H 0.598155 0.570763 0.887845 0.052 Uiso 1 1 calc GR . . . H15B H 0.591931 0.518354 0.963456 0.052 Uiso 1 1 calc GR . . . H15C H 0.690988 0.571639 0.938677 0.052 Uiso 1 1 calc GR . . . C1 C 0.2793(10) 0.6668(8) 1.0393(8) 0.030(2) Uani 1 1 d . U . . H1 H 0.295543 0.664592 1.085434 0.036 Uiso 1 1 calc R . . . C3 C 0.1865(10) 0.6122(9) 0.9574(8) 0.031(2) Uani 1 1 d . U . . H3 H 0.140702 0.572060 0.945721 0.037 Uiso 1 1 calc R . . . C4 C 0.2301(10) 0.6720(8) 0.9080(8) 0.032(2) Uani 1 1 d . U . . H4 H 0.212581 0.675162 0.862037 0.039 Uiso 1 1 calc R . . . C5 C 0.3002(10) 0.7280(8) 0.9263(7) 0.0270(18) Uani 1 1 d . U . . C6 C 0.3522(10) 0.7947(8) 0.8800(7) 0.0262(18) Uani 1 1 d . U . . C10 C 0.4621(10) 0.9077(8) 0.8693(7) 0.0256(19) Uani 1 1 d . U . . H10 H 0.502543 0.944279 0.890058 0.031 Uiso 1 1 calc R . . . C9 C 0.4557(10) 0.9219(9) 0.8001(7) 0.028(2) Uani 1 1 d . U . . H9 H 0.492333 0.966775 0.773486 0.034 Uiso 1 1 calc R . . . C8 C 0.3964(10) 0.8710(9) 0.7703(7) 0.030(2) Uani 1 1 d . U . . H8 H 0.391786 0.879522 0.722574 0.036 Uiso 1 1 calc R . . . C7 C 0.3422(10) 0.8060(8) 0.8102(7) 0.027(2) Uani 1 1 d . U . . H7 H 0.299566 0.770291 0.790196 0.033 Uiso 1 1 calc R . . . C2 C 0.2092(10) 0.6112(9) 1.0219(8) 0.032(2) Uani 1 1 d . U . . H2 H 0.176911 0.571965 1.056313 0.039 Uiso 1 1 calc R . . . C19 C -0.1199(11) 0.2014(9) 0.8248(7) 0.031(2) Uani 1 1 d . U . . H19 H -0.154837 0.243775 0.846761 0.037 Uiso 1 1 calc R . . . C18 C -0.1734(11) 0.1427(9) 0.7962(7) 0.030(2) Uani 1 1 d . U . . H18 H -0.246324 0.144247 0.798566 0.036 Uiso 1 1 calc R . . . C39 C 0.8994(10) 0.2926(9) 0.6454(7) 0.028(2) Uani 1 1 d . U . . H39 H 0.933319 0.329939 0.669381 0.033 Uiso 1 1 calc R . . . C38 C 0.9539(11) 0.2356(9) 0.6153(7) 0.029(2) Uani 1 1 d . U . . H38 H 1.026245 0.228611 0.620903 0.035 Uiso 1 1 calc R . . . C44 C 0.5979(12) 0.3751(10) 0.4709(8) 0.040(3) Uani 1 1 d . U . . C45 C 0.6096(14) 0.4355(11) 0.4069(9) 0.052(4) Uani 1 1 d . U . . H45A H 0.579233 0.411575 0.370369 0.078 Uiso 1 1 calc GR . . . H45B H 0.682768 0.443500 0.397378 0.078 Uiso 1 1 calc GR . . . H45C H 0.574576 0.491850 0.410186 0.078 Uiso 1 1 calc GR . . . C34 C 0.7805(11) 0.0887(8) 0.4912(7) 0.027(2) Uani 1 1 d . U . . H34 H 0.852872 0.077969 0.489082 0.032 Uiso 1 1 calc R . . . C46 C 0.6146(13) 0.5146(11) 0.1521(9) 0.045(4) Uani 1 1 d . U . . C47 C 0.6219(13) 0.5141(11) 0.2236(9) 0.049(4) Uani 1 1 d . U . . H47A H 0.641132 0.571407 0.231078 0.073 Uiso 1 1 calc GR . . . H47B H 0.674273 0.469647 0.242976 0.073 Uiso 1 1 calc GR . . . H47C H 0.555374 0.500860 0.245190 0.073 Uiso 1 1 calc GR . . . C48 C 1.008(2) 0.8739(16) 0.9935(11) 0.068(6) Uani 1 1 d . U . . C49 C 0.914(2) 0.9209(17) 0.9661(13) 0.098(7) Uani 1 1 d . U . . H49A H 0.930601 0.976244 0.938023 0.148 Uiso 1 1 calc GR . . . H49B H 0.868529 0.932304 1.003252 0.148 Uiso 1 1 calc GR . . . H49C H 0.878926 0.885518 0.938670 0.148 Uiso 1 1 calc GR . . . C42 C 0.4552(12) 0.2223(11) 0.6011(8) 0.040(3) Uani 1 1 d . U . . O48 O 0.3727(10) 0.2024(14) 0.6056(9) 0.108(6) Uani 1 1 d . 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 W5 0.0148(3) 0.0163(2) 0.0096(2) -0.00395(19) 0.00288(19) -0.00011(19) W7 0.0098(2) 0.0198(2) 0.0166(3) -0.0018(2) -0.00098(19) -0.00489(19) W3 0.0133(2) 0.0152(2) 0.0092(2) -0.00208(18) -0.00309(18) -0.00438(18) W11 0.0180(3) 0.0200(2) 0.0066(2) 0.00068(19) -0.00260(19) -0.0011(2) W9 0.0162(3) 0.0115(2) 0.0133(3) -0.00164(19) 0.00070(19) -0.00429(18) W4 0.0154(2) 0.0127(2) 0.0092(2) -0.00008(18) -0.00051(18) -0.00453(18) W1 0.0178(3) 0.0151(2) 0.0153(3) -0.0004(2) 0.0003(2) 0.00558(19) W10 0.0238(3) 0.0158(2) 0.0097(2) -0.00331(19) 0.0048(2) 0.0016(2) W2 0.0099(2) 0.0159(2) 0.0126(2) -0.00015(19) 0.00106(18) -0.00079(18) W6 0.0135(3) 0.0147(2) 0.0137(3) -0.00142(19) -0.00311(19) 0.00336(19) W12 0.0134(2) 0.0174(2) 0.0063(2) 0.00143(18) -0.00107(18) -0.00114(19) W8 0.0198(3) 0.0173(2) 0.0104(2) -0.00372(19) -0.0018(2) -0.0077(2) P1 0.0009(8) 0.0022(7) 0.0007(8) -0.0007(6) 0.0004(7) -0.0007(6) O34 0.041(5) 0.018(4) 0.018(5) -0.001(4) 0.002(4) -0.007(4) O40 0.021(3) 0.020(3) 0.015(3) -0.003(3) -0.004(3) -0.002(3) O38 0.016(2) 0.0084(16) 0.0102(19) 0.0031(15) -0.003(2) 0.0010(15) O22 0.017(3) 0.021(3) 0.013(3) -0.002(3) -0.001(3) -0.004(3) O18 0.020(5) 0.022(4) 0.023(5) 0.003(4) -0.009(4) 0.007(4) O4 0.019(3) 0.019(3) 0.013(3) 0.001(2) 0.002(2) 0.001(2) O29 0.014(3) 0.019(3) 0.010(3) 0.000(2) -0.003(2) 0.001(2) O26 0.013(2) 0.016(2) 0.0044(13) -0.0059(14) -0.0017(17) -0.001(2) O37 0.014(3) 0.020(3) 0.016(3) -0.002(2) 0.001(2) -0.002(2) O2 0.015(3) 0.019(3) 0.016(3) -0.001(2) 0.002(2) -0.002(2) O13 0.018(3) 0.015(2) 0.010(3) -0.001(2) 0.000(2) 0.003(2) O21 0.016(4) 0.033(5) 0.027(5) -0.007(4) 0.004(4) -0.001(4) O8 0.015(3) 0.015(2) 0.011(3) 0.001(2) 0.000(2) 0.000(2) O19 0.018(3) 0.021(3) 0.016(3) -0.002(2) 0.000(2) -0.005(2) O16 0.024(5) 0.036(5) 0.014(4) -0.014(4) 0.008(4) -0.001(4) O6 0.0084(15) 0.016(2) 0.011(2) -0.0023(19) 0.0040(19) 0.0047(15) O35 0.018(3) 0.017(3) 0.016(3) 0.002(2) 0.000(2) -0.002(2) O10 0.022(5) 0.022(4) 0.020(5) 0.004(4) 0.000(4) -0.005(4) O17 0.018(3) 0.017(3) 0.010(3) -0.004(2) -0.003(2) -0.002(2) O20 0.019(3) 0.021(3) 0.014(3) -0.004(2) -0.003(2) -0.005(2) O12 0.022(5) 0.032(5) 0.022(5) -0.010(4) -0.005(4) -0.008(4) O28 0.016(3) 0.019(3) 0.016(3) 0.001(2) 0.000(2) 0.000(2) O36 0.0111(18) 0.015(2) 0.015(2) -0.0043(18) -0.001(2) -0.0095(16) O23 0.015(3) 0.025(3) 0.018(3) -0.002(3) -0.001(3) -0.007(3) O14 0.018(3) 0.020(3) 0.018(3) -0.001(3) 0.000(3) -0.003(3) O27 0.016(3) 0.021(3) 0.012(3) 0.004(3) -0.002(3) -0.001(3) O15 0.021(3) 0.020(3) 0.012(3) -0.003(3) -0.002(3) 0.001(3) O31 0.015(3) 0.021(3) 0.016(3) -0.002(2) -0.001(2) 0.000(2) O11 0.020(3) 0.019(3) 0.016(3) -0.002(3) -0.002(3) -0.004(3) O5 0.025(3) 0.020(3) 0.016(3) -0.004(3) 0.002(3) 0.001(3) O39 0.026(5) 0.027(4) 0.015(4) -0.002(4) -0.004(4) -0.008(4) O9 0.017(3) 0.021(3) 0.017(3) 0.004(3) -0.003(3) 0.004(3) O1 0.034(5) 0.027(4) 0.026(5) -0.017(4) 0.014(4) -0.004(4) O7 0.014(4) 0.035(5) 0.024(5) 0.003(4) 0.003(4) -0.004(4) O30 0.023(5) 0.017(4) 0.026(5) 0.006(4) 0.008(4) 0.004(4) O33 0.042(5) 0.026(4) 0.018(4) -0.012(4) -0.008(4) -0.012(4) O25 0.019(3) 0.022(3) 0.016(3) -0.002(3) -0.001(3) -0.003(3) O24 0.023(5) 0.022(4) 0.017(4) 0.001(4) -0.001(4) -0.006(4) O3 0.022(3) 0.021(3) 0.019(3) -0.003(3) 0.002(3) 0.001(3) O32 0.019(3) 0.019(3) 0.015(3) -0.001(3) 0.001(3) -0.006(3) O49 0.044(7) 0.045(6) 0.032(6) -0.006(5) 0.007(5) -0.015(5) O46 0.020(6) 0.073(8) 0.075(9) -0.037(7) -0.001(5) 0.001(5) O45 0.060(8) 0.046(6) 0.043(7) -0.024(6) -0.011(6) 0.020(6) O44 0.050(7) 0.032(5) 0.025(6) -0.001(5) -0.006(5) -0.005(5) O41 0.064(8) 0.063(7) 0.041(7) 0.003(6) -0.016(6) -0.042(7) O42 0.072(9) 0.044(6) 0.048(8) -0.010(6) 0.024(7) 0.007(6) O43 0.113(12) 0.065(8) 0.020(6) 0.009(6) -0.023(7) -0.022(8) O47 0.081(9) 0.070(8) 0.069(9) -0.028(7) 0.016(7) 0.031(7) N6 0.023(5) 0.023(4) 0.022(5) -0.008(4) -0.001(4) 0.001(4) N4 0.023(5) 0.016(4) 0.017(5) -0.008(4) 0.000(4) 0.005(4) N5 0.026(5) 0.016(4) 0.017(5) -0.004(4) -0.007(4) 0.001(4) N3 0.009(4) 0.029(5) 0.027(5) 0.001(4) 0.003(4) -0.002(4) N2 0.008(4) 0.014(4) 0.023(5) -0.006(4) 0.007(4) 0.001(3) N1 0.008(4) 0.024(4) 0.032(5) -0.002(4) 0.004(4) 0.001(4) N9 0.038(6) 0.034(5) 0.031(5) -0.003(5) 0.004(5) 0.001(5) N10 0.075(13) 0.088(13) 0.044(11) 0.009(9) 0.011(9) 0.014(10) N7 0.020(5) 0.025(4) 0.017(5) -0.005(4) 0.009(4) -0.010(4) N8 0.019(5) 0.017(4) 0.020(5) -0.004(4) 0.006(4) -0.004(4) N11 0.124(15) 0.098(13) 0.086(13) 0.007(11) 0.008(12) -0.031(12) Mn1 0.0259(11) 0.0209(9) 0.0167(10) -0.0006(8) 0.0009(8) -0.0056(8) Mn2 0.0202(10) 0.0212(9) 0.0146(10) -0.0059(8) -0.0001(8) 0.0002(8) Mn3 0.0172(11) 0.0386(12) 0.0260(12) -0.0085(10) 0.0012(9) 0.0061(9) C29 0.026(5) 0.029(5) 0.022(5) -0.015(5) -0.001(5) 0.004(5) C30 0.065(11) 0.024(7) 0.024(8) 0.001(6) 0.005(7) 0.001(7) C28 0.026(5) 0.030(4) 0.030(5) -0.010(4) -0.002(4) 0.002(4) C27 0.023(5) 0.030(4) 0.026(5) -0.011(4) -0.006(4) 0.006(4) C26 0.024(4) 0.026(4) 0.025(4) -0.013(4) -0.003(4) -0.003(4) C16 0.029(4) 0.028(4) 0.026(4) -0.011(3) -0.003(4) -0.002(4) C17 0.028(5) 0.034(4) 0.026(5) -0.009(4) -0.007(4) -0.006(4) C20 0.027(4) 0.026(3) 0.025(4) -0.011(3) -0.001(3) -0.004(3) C21 0.029(4) 0.026(3) 0.026(4) -0.012(3) 0.001(3) -0.005(3) C25 0.030(4) 0.028(4) 0.026(4) -0.010(3) -0.003(4) -0.007(4) C24 0.040(5) 0.033(4) 0.029(5) -0.008(4) -0.005(4) -0.014(4) C22 0.033(4) 0.029(4) 0.028(4) -0.010(4) 0.002(4) -0.004(4) C23 0.037(4) 0.024(4) 0.028(4) -0.009(4) 0.000(4) -0.008(4) C43 0.023(4) 0.034(4) 0.025(4) -0.008(4) 0.000(4) -0.006(4) C41 0.033(5) 0.045(5) 0.033(5) -0.004(5) 0.000(4) 0.011(5) C36 0.026(4) 0.025(3) 0.021(4) 0.000(3) 0.002(3) -0.005(3) C40 0.028(4) 0.030(4) 0.025(4) -0.003(4) 0.005(4) -0.002(4) C37 0.026(4) 0.028(4) 0.021(4) 0.003(4) 0.004(4) -0.003(4) C35 0.026(4) 0.025(3) 0.021(4) -0.001(3) 0.004(3) -0.006(3) C31 0.030(4) 0.033(4) 0.025(4) 0.001(4) -0.002(4) -0.009(4) C32 0.039(5) 0.029(4) 0.020(5) 0.000(4) -0.007(4) -0.012(4) C33 0.041(5) 0.029(4) 0.023(4) 0.002(4) 0.000(4) -0.006(4) C11 0.031(5) 0.028(5) 0.027(5) 0.002(4) -0.001(5) -0.005(5) C13 0.029(5) 0.029(4) 0.033(5) 0.000(4) -0.003(4) -0.006(4) C12 0.029(4) 0.028(4) 0.029(4) 0.003(4) 0.004(4) -0.002(4) C14 0.022(5) 0.027(5) 0.030(5) 0.005(4) 0.000(4) -0.002(4) C15 0.033(8) 0.035(7) 0.034(8) 0.002(7) 0.014(7) -0.007(6) C1 0.024(4) 0.026(4) 0.038(4) 0.002(4) 0.005(4) -0.003(3) C3 0.022(4) 0.027(4) 0.043(5) 0.000(4) -0.003(4) -0.003(4) C4 0.024(4) 0.027(4) 0.042(4) 0.005(4) -0.005(4) 0.000(4) C5 0.023(3) 0.025(3) 0.032(4) 0.001(3) 0.001(3) -0.001(3) C6 0.021(3) 0.025(3) 0.030(4) 0.001(3) 0.000(3) 0.002(3) C10 0.022(4) 0.024(4) 0.028(4) 0.002(4) 0.003(4) 0.001(3) C9 0.023(5) 0.030(4) 0.028(5) 0.005(4) 0.004(4) 0.006(4) C8 0.025(4) 0.033(4) 0.029(4) 0.000(4) 0.003(4) 0.006(4) C7 0.020(4) 0.028(4) 0.031(4) -0.002(4) -0.002(4) 0.002(4) C2 0.022(5) 0.027(4) 0.044(5) 0.006(4) 0.005(4) -0.006(4) C19 0.030(4) 0.034(4) 0.029(4) -0.007(4) 0.002(4) -0.002(4) C18 0.029(4) 0.035(4) 0.026(4) -0.009(4) -0.004(4) -0.003(4) C39 0.029(5) 0.033(4) 0.021(5) -0.002(4) 0.000(4) -0.013(4) C38 0.026(4) 0.036(4) 0.024(4) 0.000(4) 0.001(4) -0.007(4) C44 0.036(6) 0.046(6) 0.035(6) -0.005(6) -0.009(5) 0.010(5) C45 0.052(10) 0.058(10) 0.041(9) 0.008(8) -0.014(8) -0.013(8) C34 0.030(4) 0.027(4) 0.022(4) -0.001(4) 0.004(4) -0.005(4) C46 0.037(9) 0.055(10) 0.041(10) 0.004(8) 0.009(8) -0.013(8) C47 0.039(9) 0.054(9) 0.049(10) 0.001(8) 0.004(8) -0.007(8) C48 0.072(9) 0.079(9) 0.055(9) -0.015(7) 0.011(8) -0.020(8) C49 0.113(14) 0.121(14) 0.079(13) -0.065(11) 0.011(11) -0.015(12) C42 0.031(5) 0.054(5) 0.034(5) -0.005(5) -0.006(4) 0.004(5) O48 0.026(7) 0.201(15) 0.104(12) -0.040(11) -0.007(7) -0.025(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Mn Mn 0.3370 0.7280 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8720 '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 O19 W5 O26 83.1(3) O19 W5 O25 86.9(3) O16 W5 O26 168.6(4) O16 W5 O19 105.0(4) O16 W5 O17 103.5(4) O16 W5 O14 100.4(4) O16 W5 O25 100.9(4) O17 W5 O26 85.0(3) O17 W5 O19 85.6(3) O17 W5 O14 89.9(3) O17 W5 O25 155.6(3) O14 W5 O26 71.6(3) O14 W5 O19 154.6(3) O14 W5 O25 87.0(3) O25 W5 O26 71.1(3) O22 W7 O36 71.6(3) O22 W7 O23 86.7(3) O21 W7 O22 100.4(4) O21 W7 O19 104.4(4) O21 W7 O20 104.4(4) O21 W7 O36 168.7(3) O21 W7 O23 100.7(4) O19 W7 O22 89.3(3) O19 W7 O20 85.4(3) O19 W7 O36 83.9(3) O19 W7 O23 154.9(3) O20 W7 O22 155.2(3) O20 W7 O36 83.7(3) O20 W7 O23 87.9(3) O23 W7 O36 71.4(3) O29 W3 O26 84.9(3) O29 W3 O13 86.7(3) O29 W3 O14 155.8(3) O29 W3 O27 90.1(3) O13 W3 O26 83.0(3) O13 W3 O14 86.6(3) O13 W3 O27 155.0(3) O12 W3 O29 102.9(4) O12 W3 O26 170.5(3) O12 W3 O13 102.6(4) O12 W3 O14 101.2(4) O12 W3 O27 102.2(4) O14 W3 O26 71.2(3) O27 W3 O26 72.1(3) O27 W3 O14 86.3(3) O40 W11 O38 72.1(3) O4 W11 O40 155.2(3) O4 W11 O38 83.4(3) O4 W11 O35 85.6(3) O4 W11 O11 89.6(3) O35 W11 O40 87.9(3) O35 W11 O38 84.2(3) O35 W11 O11 156.5(3) O11 W11 O40 86.9(3) O11 W11 O38 72.4(3) O39 W11 O40 102.5(4) O39 W11 O38 170.4(3) O39 W11 O4 102.3(4) O39 W11 O35 103.8(4) O39 W11 O11 99.7(4) O34 W9 O22 102.1(4) O34 W9 O37 102.8(4) O34 W9 O36 171.8(4) O34 W9 O31 102.8(4) O34 W9 O32 102.6(4) O22 W9 O37 87.5(3) O22 W9 O36 72.2(3) O37 W9 O36 83.2(3) O31 W9 O22 155.0(3) O31 W9 O37 84.6(3) O31 W9 O36 83.2(3) O31 W9 O32 89.8(3) O32 W9 O22 87.2(3) O32 W9 O37 154.5(3) O32 W9 O36 71.5(3) O13 W4 O38 84.1(3) O13 W4 O8 85.9(3) O13 W4 O15 89.5(3) O13 W4 O11 156.7(3) O8 W4 O38 83.4(3) O8 W4 O15 156.0(3) O8 W4 O11 88.0(3) O10 W4 O38 171.7(3) O10 W4 O13 102.2(4) O10 W4 O8 102.3(4) O10 W4 O15 101.6(4) O10 W4 O11 101.1(4) O15 W4 O38 72.7(3) O11 W4 O38 72.9(3) O11 W4 O15 87.0(3) O28 W1 O6 84.3(3) O28 W1 O31 85.8(3) O28 W1 O5 155.6(3) O28 W1 O9 88.9(3) O31 W1 O6 83.5(3) O31 W1 O5 87.9(3) O31 W1 O9 155.5(3) O5 W1 O6 71.6(3) O9 W1 O6 72.1(3) O9 W1 O5 87.1(4) O30 W1 O6 169.3(3) O30 W1 O28 104.0(4) O30 W1 O31 103.7(4) O30 W1 O5 100.4(4) O30 W1 O9 100.8(4) O4 W10 O6 82.8(3) O4 W10 O3 87.7(3) O2 W10 O4 85.3(3) O2 W10 O6 84.2(3) O2 W10 O5 89.9(4) O2 W10 O3 155.7(3) O5 W10 O4 154.2(3) O5 W10 O6 71.6(3) O5 W10 O3 86.3(4) O1 W10 O4 102.8(4) O1 W10 O2 103.8(4) O1 W10 O6 170.5(4) O1 W10 O5 103.0(4) O1 W10 O3 100.4(4) O3 W10 O6 71.8(3) O29 W2 O6 83.8(3) O8 W2 O29 86.1(3) O8 W2 O6 83.4(3) O8 W2 O9 154.9(3) O8 W2 O3 89.8(3) O9 W2 O29 86.7(3) O9 W2 O6 71.9(3) O7 W2 O29 102.4(4) O7 W2 O8 103.6(4) O7 W2 O6 170.8(3) O7 W2 O9 101.4(4) O7 W2 O3 101.1(4) O3 W2 O29 156.5(3) O3 W2 O6 72.8(3) O3 W2 O9 87.3(4) O40 W6 O38 72.1(3) O40 W6 O17 155.7(3) O40 W6 O15 87.4(3) O18 W6 O40 100.7(4) O18 W6 O38 170.0(3) O18 W6 O17 103.6(4) O18 W6 O20 103.6(4) O18 W6 O15 101.2(4) O17 W6 O38 83.6(3) O17 W6 O15 87.1(3) O20 W6 O40 89.6(3) O20 W6 O38 83.6(3) O20 W6 O17 85.6(3) O20 W6 O15 155.1(3) O15 W6 O38 71.9(3) O37 W12 O26 84.5(3) O37 W12 O28 85.8(3) O37 W12 O27 156.2(3) O37 W12 O25 89.9(3) O28 W12 O26 83.8(3) O28 W12 O27 87.6(3) O27 W12 O26 72.1(3) O25 W12 O26 72.1(3) O25 W12 O28 155.7(3) O25 W12 O27 86.8(3) O24 W12 O26 171.3(3) O24 W12 O37 101.7(4) O24 W12 O28 102.6(4) O24 W12 O27 102.1(4) O24 W12 O25 101.6(4) O2 W8 O36 82.8(3) O2 W8 O23 154.2(3) O2 W8 O32 87.9(3) O35 W8 O2 85.6(3) O35 W8 O36 84.3(3) O35 W8 O23 89.2(3) O35 W8 O32 154.8(3) O23 W8 O36 71.6(3) O23 W8 O32 86.1(3) O33 W8 O2 103.8(4) O33 W8 O35 102.9(4) O33 W8 O36 170.4(4) O33 W8 O23 102.0(4) O33 W8 O32 102.3(4) O32 W8 O36 70.7(3) O38 P1 O6 109.4(4) O26 P1 O38 109.0(4) O26 P1 O6 109.2(4) O36 P1 O38 109.8(4) O36 P1 O26 110.0(4) O36 P1 O6 109.4(4) W6 O40 W11 126.7(4) W11 O38 W6 89.0(2) W4 O38 W11 89.2(2) W4 O38 W6 89.5(2) P1 O38 W11 125.7(4) P1 O38 W4 125.8(4) P1 O38 W6 125.9(4) W9 O22 W7 126.9(4) W11 O4 W10 152.1(5) W3 O29 W2 150.0(5) W3 O26 W5 89.4(2) W12 O26 W5 89.4(2) W12 O26 W3 89.3(2) P1 O26 W5 125.7(4) P1 O26 W3 125.9(4) P1 O26 W12 125.6(4) W12 O37 W9 152.1(4) W8 O2 W10 152.4(4) W4 O13 W3 151.3(4) W2 O8 W4 151.8(4) W7 O19 W5 151.7(5) W1 O6 W10 89.5(2) W1 O6 W2 89.6(2) W2 O6 W10 89.3(2) P1 O6 W1 125.5(4) P1 O6 W10 125.2(4) P1 O6 W2 126.2(4) W8 O35 W11 150.8(5) W5 O17 W6 150.8(4) W6 O20 W7 152.2(5) W1 O28 W12 150.3(5) W7 O36 W8 89.1(2) W9 O36 W7 89.2(2) W9 O36 W8 89.2(2) P1 O36 W7 125.1(4) P1 O36 W9 126.5(4) P1 O36 W8 126.0(4) W8 O23 W7 127.9(4) W5 O14 W3 127.6(4) W3 O27 W12 126.6(4) W4 O15 W6 125.8(4) W9 O31 W1 152.5(4) W4 O11 W11 125.5(4) W10 O5 W1 127.2(4) W1 O9 W2 126.2(4) W12 O25 W5 127.3(4) W2 O3 W10 126.1(4) W9 O32 W8 128.5(4) C29 N6 Mn2 175.6(11) C16 N4 Mn2 126.5(8) C20 N4 Mn2 116.9(8) C20 N4 C16 116.6(11) C21 N5 Mn2 115.6(8) C21 N5 C25 118.3(11) C25 N5 Mn2 126.0(9) C14 N3 Mn1 173.8(11) C6 N2 Mn1 114.2(8) C6 N2 C10 119.2(12) C10 N2 Mn1 125.7(9) C1 N1 Mn1 124.4(10) C1 N1 C5 120.1(12) C5 N1 Mn1 115.2(8) C44 N9 Mn3 172.4(13) C35 N7 Mn3 114.9(8) C35 N7 C31 118.5(11) C31 N7 Mn3 126.4(9) C36 N8 Mn3 116.2(8) C36 N8 C40 117.7(11) C40 N8 Mn3 125.7(8) N3 Mn1 N2 84.4(4) N3 Mn1 N1 82.3(4) N1 Mn1 N2 78.9(4) C11 Mn1 N3 94.5(5) C11 Mn1 N2 97.1(5) C11 Mn1 N1 175.0(5) C13 Mn1 N3 91.3(6) C13 Mn1 N2 172.8(5) C13 Mn1 N1 94.8(5) C13 Mn1 C11 89.0(6) C13 Mn1 C12 88.9(6) C12 Mn1 N3 176.5(5) C12 Mn1 N2 95.0(5) C12 Mn1 N1 94.2(5) C12 Mn1 C11 89.0(6) N6 Mn2 N4 88.6(4) N6 Mn2 N5 85.0(4) N4 Mn2 N5 78.6(4) C28 Mn2 N6 90.3(6) C28 Mn2 N4 175.6(5) C28 Mn2 N5 97.1(5) C28 Mn2 C27 89.0(6) C28 Mn2 C26 87.9(6) C27 Mn2 N6 91.5(5) C27 Mn2 N4 95.2(5) C27 Mn2 N5 173.0(5) C27 Mn2 C26 89.3(6) C26 Mn2 N6 178.0(5) C26 Mn2 N4 93.1(5) C26 Mn2 N5 94.3(5) N9 Mn3 N7 84.1(4) N9 Mn3 N8 87.2(5) N8 Mn3 N7 79.2(4) C43 Mn3 N9 175.4(6) C43 Mn3 N7 93.6(5) C43 Mn3 N8 88.5(5) C43 Mn3 C41 91.3(6) C41 Mn3 N9 90.7(6) C41 Mn3 N7 174.0(6) C41 Mn3 N8 97.6(6) C42 Mn3 N9 95.4(6) C42 Mn3 N7 97.3(6) C42 Mn3 N8 175.4(6) C42 Mn3 C43 88.9(7) C42 Mn3 C41 86.2(7) N6 C29 C30 177.9(14) C29 C30 H30A 109.5 C29 C30 H30B 109.5 C29 C30 H30C 109.5 H30A C30 H30B 109.5 H30A C30 H30C 109.5 H30B C30 H30C 109.5 O46 C28 Mn2 177.9(14) O45 C27 Mn2 178.5(13) O44 C26 Mn2 176.4(12) N4 C16 H16 118.0 N4 C16 C17 124.0(12) C17 C16 H16 118.0 C16 C17 H17 120.8 C18 C17 C16 118.5(13) C18 C17 H17 120.8 N4 C20 C21 113.6(12) N4 C20 C19 123.4(12) C19 C20 C21 122.8(12) N5 C21 C20 114.7(11) N5 C21 C22 122.3(12) C22 C21 C20 122.9(13) N5 C25 H25 119.0 N5 C25 C24 121.9(13) C24 C25 H25 119.0 C25 C24 H24 120.2 C23 C24 C25 119.7(13) C23 C24 H24 120.2 C21 C22 H22 120.6 C23 C22 C21 118.8(14) C23 C22 H22 120.6 C24 C23 C22 119.0(13) C24 C23 H23 120.5 C22 C23 H23 120.5 O49 C43 Mn3 177.3(12) O47 C41 Mn3 179.0(16) N8 C36 C37 122.5(12) N8 C36 C35 113.7(12) C37 C36 C35 123.7(12) N8 C40 H40 119.4 N8 C40 C39 121.2(12) C39 C40 H40 119.4 C36 C37 H37 120.8 C36 C37 C38 118.4(13) C38 C37 H37 120.8 N7 C35 C36 115.3(11) N7 C35 C34 120.0(12) C34 C35 C36 124.7(12) N7 C31 H31 118.6 N7 C31 C32 122.9(13) C32 C31 H31 118.6 C31 C32 H32 120.9 C33 C32 C31 118.2(13) C33 C32 H32 120.9 C32 C33 H33 120.2 C32 C33 C34 119.7(14) C34 C33 H33 120.2 O41 C11 Mn1 175.3(13) O43 C13 Mn1 178.7(15) O42 C12 Mn1 176.6(13) N3 C14 C15 175.7(14) C14 C15 H15A 109.5 C14 C15 H15B 109.5 C14 C15 H15C 109.5 H15A C15 H15B 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 N1 C1 H1 119.7 N1 C1 C2 120.5(14) C2 C1 H1 119.7 C4 C3 H3 120.4 C2 C3 H3 120.4 C2 C3 C4 119.3(14) C3 C4 H4 120.4 C3 C4 C5 119.3(14) C5 C4 H4 120.4 N1 C5 C4 120.0(12) N1 C5 C6 114.4(12) C4 C5 C6 125.6(13) N2 C6 C5 115.7(12) N2 C6 C7 121.4(12) C7 C6 C5 122.9(13) N2 C10 H10 119.0 N2 C10 C9 122.1(13) C9 C10 H10 119.0 C10 C9 H9 120.4 C8 C9 C10 119.1(13) C8 C9 H9 120.4 C9 C8 H8 120.1 C9 C8 C7 119.7(14) C7 C8 H8 120.1 C6 C7 C8 118.4(13) C6 C7 H7 120.8 C8 C7 H7 120.8 C1 C2 H2 119.6 C3 C2 C1 120.8(13) C3 C2 H2 119.6 C20 C19 H19 121.3 C18 C19 C20 117.4(13) C18 C19 H19 121.3 C17 C18 C19 120.1(14) C17 C18 H18 119.9 C19 C18 H18 119.9 C40 C39 H39 120.0 C38 C39 C40 119.9(13) C38 C39 H39 120.0 C37 C38 H38 120.0 C39 C38 C37 120.1(14) C39 C38 H38 120.0 N9 C44 C45 179.3(18) C44 C45 H45A 109.5 C44 C45 H45B 109.5 C44 C45 H45C 109.5 H45A C45 H45B 109.5 H45A C45 H45C 109.5 H45B C45 H45C 109.5 C35 C34 H34 119.8 C33 C34 C35 120.5(14) C33 C34 H34 119.8 N10 C46 C47 178(2) C46 C47 H47A 109.5 C46 C47 H47B 109.5 C46 C47 H47C 109.5 H47A C47 H47B 109.5 H47A C47 H47C 109.5 H47B C47 H47C 109.5 N11 C48 C49 174(3) C48 C49 H49A 109.5 C48 C49 H49B 109.5 C48 C49 H49C 109.5 H49A C49 H49B 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 O48 C42 Mn3 171.3(18) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance W5 O26 2.445(7) W5 O19 1.924(8) W5 O16 1.678(8) W5 O17 1.889(8) W5 O14 1.903(8) W5 O25 1.931(8) W7 O22 1.923(8) W7 O21 1.692(8) W7 O19 1.885(8) W7 O20 1.901(8) W7 O36 2.455(8) W7 O23 1.927(8) W3 O29 1.888(8) W3 O26 2.444(7) W3 O13 1.901(8) W3 O12 1.688(8) W3 O14 1.932(8) W3 O27 1.904(8) W11 O40 1.932(8) W11 O38 2.435(8) W11 O4 1.892(8) W11 O35 1.930(8) W11 O11 1.931(8) W11 O39 1.693(8) W9 O34 1.695(8) W9 O22 1.916(8) W9 O37 1.917(8) W9 O36 2.435(7) W9 O31 1.896(8) W9 O32 1.897(8) W4 O38 2.428(7) W4 O13 1.892(8) W4 O8 1.910(8) W4 O10 1.691(8) W4 O15 1.927(8) W4 O11 1.910(8) W1 O6 2.425(7) W1 O28 1.892(8) W1 O31 1.910(8) W1 O5 1.923(8) W1 O9 1.920(8) W1 O30 1.691(8) W10 O4 1.909(8) W10 O2 1.901(8) W10 O6 2.440(7) W10 O5 1.902(8) W10 O1 1.678(8) W10 O3 1.952(8) W2 O29 1.928(8) W2 O8 1.890(8) W2 O6 2.436(7) W2 O9 1.921(8) W2 O7 1.713(8) W2 O3 1.892(8) W6 O40 1.902(8) W6 O38 2.455(7) W6 O18 1.696(8) W6 O17 1.916(8) W6 O20 1.892(8) W6 O15 1.935(8) W12 O26 2.428(8) W12 O37 1.890(8) W12 O28 1.924(8) W12 O27 1.928(8) W12 O25 1.895(8) W12 O24 1.692(8) W8 O2 1.898(8) W8 O35 1.883(8) W8 O36 2.457(7) W8 O23 1.908(8) W8 O33 1.687(8) W8 O32 1.917(8) P1 O38 1.533(7) P1 O26 1.528(7) P1 O6 1.544(7) P1 O36 1.525(7) O49 C43 1.145(17) O46 C28 1.157(16) O45 C27 1.139(15) O44 C26 1.130(16) O41 C11 1.120(16) O42 C12 1.135(16) O43 C13 1.151(17) O47 C41 1.158(18) N6 Mn2 2.017(11) N6 C29 1.136(17) N4 Mn2 2.032(10) N4 C16 1.346(16) N4 C20 1.343(15) N5 Mn2 2.053(10) N5 C21 1.340(17) N5 C25 1.347(16) N3 Mn1 2.014(11) N3 C14 1.138(16) N2 Mn1 2.057(10) N2 C6 1.333(16) N2 C10 1.350(15) N1 Mn1 2.031(10) N1 C1 1.333(16) N1 C5 1.352(17) N9 Mn3 1.999(13) N9 C44 1.116(19) N10 C46 1.12(2) N7 Mn3 2.047(10) N7 C35 1.347(16) N7 C31 1.348(17) N8 Mn3 2.020(10) N8 C36 1.352(16) N8 C40 1.354(17) N11 C48 1.12(3) Mn1 C11 1.840(14) Mn1 C13 1.801(15) Mn1 C12 1.826(14) Mn2 C28 1.798(14) Mn2 C27 1.823(13) Mn2 C26 1.830(15) Mn3 C43 1.801(15) Mn3 C41 1.815(15) Mn3 C42 1.776(16) C29 C30 1.450(19) C30 H30A 0.9800 C30 H30B 0.9800 C30 H30C 0.9800 C16 H16 0.9500 C16 C17 1.374(19) C17 H17 0.9500 C17 C18 1.360(19) C20 C21 1.488(17) C20 C19 1.395(19) C21 C22 1.400(18) C25 H25 0.9500 C25 C24 1.390(18) C24 H24 0.9500 C24 C23 1.37(2) C22 H22 0.9500 C22 C23 1.379(19) C23 H23 0.9500 C36 C37 1.373(18) C36 C35 1.470(18) C40 H40 0.9500 C40 C39 1.390(19) C37 H37 0.9500 C37 C38 1.381(19) C35 C34 1.397(18) C31 H31 0.9500 C31 C32 1.386(19) C32 H32 0.9500 C32 C33 1.36(2) C33 H33 0.9500 C33 C34 1.361(19) C14 C15 1.446(19) C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C1 H1 0.9500 C1 C2 1.385(19) C3 H3 0.9500 C3 C4 1.379(19) C3 C2 1.33(2) C4 H4 0.9500 C4 C5 1.396(19) C5 C6 1.460(18) C6 C7 1.395(19) C10 H10 0.9500 C10 C9 1.376(19) C9 H9 0.9500 C9 C8 1.36(2) C8 H8 0.9500 C8 C7 1.396(19) C7 H7 0.9500 C2 H2 0.9500 C19 H19 0.9500 C19 C18 1.390(19) C18 H18 0.9500 C39 H39 0.9500 C39 C38 1.331(19) C38 H38 0.9500 C44 C45 1.47(2) C45 H45A 0.9800 C45 H45B 0.9800 C45 H45C 0.9800 C34 H34 0.9500 C46 C47 1.44(2) C47 H47A 0.9800 C47 H47B 0.9800 C47 H47C 0.9800 C48 C49 1.46(3) C49 H49A 0.9800 C49 H49B 0.9800 C49 H49C 0.9800 C42 O48 1.133(19) loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C30 H30A O48 0.98 2.65 3.30(2) 124.2 . yes C30 H30B O5 0.98 2.60 3.138(17) 115.0 1_455 yes C16 H16 O13 0.95 2.53 3.240(15) 131.6 1_445 yes C40 H40 O32 0.95 2.48 3.235(15) 136.6 . yes C37 H37 O10 0.95 2.44 3.053(16) 121.8 1_545 yes C15 H15A O22 0.98 2.62 3.521(17) 152.1 . yes C15 H15C O25 0.98 2.57 3.256(16) 127.0 . yes C1 H1 O34 0.95 2.52 3.341(17) 145.1 2_667 yes C2 H2 O24 0.95 2.54 3.284(15) 134.9 2_667 yes C19 H19 O34 0.95 2.65 3.337(17) 129.7 1_455 yes C45 H45A O23 0.98 2.63 3.298(19) 125.8 2_666 yes C47 H47B O9 0.98 2.52 3.47(2) 164.0 2_766 yes C49 H49B O44 0.98 2.54 3.48(2) 160.8 2_667 yes C49 H49C O14 0.98 2.26 3.10(2) 143.7 . yes