#------------------------------------------------------------------------------ #$Date: 2021-12-07 04:50:57 +0200 (Tue, 07 Dec 2021) $ #$Revision: 271153 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243745.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_7243745 loop_ _publ_author_name 'Ying, Jun' 'Jin, Liang' 'Yu, Hai-Yan' 'Tian, Ai-Xiang' 'Wang, Xiu-Li' _publ_section_title ; A series of polyoxometalate-based hybrid complexes constructed by a tripodal ligand containing mixed N/O donors ; _journal_issue 44 _journal_name_full CrystEngComm _journal_page_first 7846 _journal_page_last 7854 _journal_paper_doi 10.1039/D1CE01195B _journal_volume 23 _journal_year 2021 _chemical_formula_moiety 'C26 H26 Co2 Mo8 N8 O34, 0.5(H4 O2)' _chemical_formula_sum 'C26 H28 Co2 Mo8 N8 O35' _chemical_formula_weight 1897.94 _chemical_name_systematic 'Compound 3' _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 mixed _audit_block_doi 10.5517/ccdc.csd.cc26pfr3 _audit_creation_date 2020-11-23 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972) ; _audit_update_record ; 2020-11-25 deposited with the CCDC. 2021-10-15 downloaded from the CCDC. ; _cell_angle_alpha 83.416(3) _cell_angle_beta 68.138(2) _cell_angle_gamma 73.915(2) _cell_formula_units_Z 1 _cell_length_a 9.5767(13) _cell_length_b 11.1881(15) _cell_length_c 12.2524(17) _cell_measurement_reflns_used 3689 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 28.35 _cell_measurement_theta_min 2.37 _cell_volume 1170.6(3) _computing_cell_refinement 'SAINT V8.18C (?, 2016)' _computing_data_reduction 'SAINT V8.18C (?, 2016)' _computing_molecular_graphics 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3-alpha (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_unetI/netI 0.0465 _diffrn_reflns_Laue_measured_fraction_full 0.989 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 8594 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.428 _diffrn_reflns_theta_min 1.895 _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_voltage 40.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.873 _exptl_absorpt_correction_T_max 0.650 _exptl_absorpt_correction_T_min 0.585 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0685 before and 0.0319 after correction. The Ratio of minimum to maximum transmission is 0.8414. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 2.692 _exptl_crystal_description block _exptl_crystal_F_000 910 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.703 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.213 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 368 _refine_ls_number_reflns 5718 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0363 _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^)+(0.0462P)^2^+5.1348P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0978 _refine_ls_wR_factor_ref 0.1035 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4865 _reflns_number_total 5894 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01195b2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7243745--7243750.cif.' _cod_database_code 7243745 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances Co1-H3A \\sim Co1-H3B with sigma of 0.02 3. Uiso/Uaniso restraints and constraints O1W: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A Uanis(O1W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4. Rigid body (RIGU) restrains O1W with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.01 5. Others Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5) 6.a Free rotating group: O3(H3A,H3B), O1W(H1WA,H1WB) 6.b Rotating group: O4(H4A,H4B) 6.c Aromatic/amide H refined with riding coordinates: C7(H7), C10(H10), C9(H9), C5(H5), C11(H11), C3(H3), C1(H1), C12(H12), C2(H2) ; _shelx_res_file ; TITL 2_a.res in P-1 2.res created by SHELXL-2018/3 at 10:33:20 on 23-Nov-2020 REM Old TITL 2 in P-1 REM SHELXT solution in P-1: R1 0.069, Rweak 0.005, Alpha 0.052 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C15 N6 O16 Co Mo4 CELL 0.71073 9.5767 11.1881 12.2524 83.416 68.138 73.915 ZERR 1 0.0013 0.0015 0.0017 0.003 0.002 0.002 LATT 1 SFAC C H Co Mo N O UNIT 26 28 2 8 8 35 ISOR 0.005 0.01 O1W RIGU 0.005 0.01 O1W SIMU 0.005 0.01 2 O1W SADI Co1 H3a Co1 H3b L.S. 5 0 0 PLAN 5 TEMP 23 CONF list 4 MORE -1 BOND $H fmap 2 53 acta OMIT 0 -2 3 OMIT 1 -2 6 OMIT 1 -2 5 OMIT 1 -4 8 OMIT 0 -5 7 OMIT 0 -3 3 OMIT 0 -6 10 OMIT 0 -2 2 OMIT 1 -3 6 OMIT 0 -7 10 OMIT 6 10 13 OMIT 0 -4 7 OMIT 1 -3 9 OMIT 0 -4 6 OMIT 6 9 14 REM REM REM WGHT 0.046200 5.134800 FVAR 0.28003 MO4 4 0.766698 0.519542 0.678913 11.00000 0.01202 0.00937 = 0.00864 0.00182 -0.00474 -0.00379 MO2 4 0.507969 0.589423 1.102604 11.00000 0.01348 0.00969 = 0.01007 0.00264 -0.00672 -0.00448 MO3 4 0.447433 0.727118 0.799545 11.00000 0.01496 0.01026 = 0.01303 0.00426 -0.00586 -0.00268 MO1 4 0.186526 0.662087 1.043792 11.00000 0.01245 0.01271 = 0.01148 0.00324 -0.00628 -0.00223 CO1 3 0.804360 0.521723 0.373400 11.00000 0.01776 0.01219 = 0.01307 0.00111 -0.00802 -0.00555 O13 6 0.446079 0.621935 0.967459 11.00000 0.01622 0.01386 = 0.00953 0.00586 -0.00678 -0.00417 O15 6 0.264312 0.578454 1.164164 11.00000 0.01644 0.01274 = 0.01347 0.00434 -0.00710 -0.00363 O7 6 0.676436 0.669388 0.757320 11.00000 0.01433 0.01161 = 0.01316 -0.00145 -0.00368 -0.00380 O10 6 0.242178 0.698225 0.876548 11.00000 0.01857 0.01597 = 0.01501 0.00675 -0.00890 -0.00540 O14 6 0.709198 0.543546 1.033434 11.00000 0.01796 0.01429 = 0.01808 0.00299 -0.00883 -0.00485 O6 6 0.960708 0.506389 0.648506 11.00000 0.01620 0.02071 = 0.01832 0.00132 -0.00689 -0.00590 O17 6 0.480680 0.485287 1.239957 11.00000 0.01670 0.01595 = 0.01123 0.00157 -0.00712 -0.00677 O12 6 0.012036 0.627607 1.072205 11.00000 0.01697 0.02678 = 0.02385 0.00547 -0.00954 -0.00754 O2 6 0.799717 0.337590 0.626684 11.00000 0.03075 0.01223 = 0.01526 0.00210 -0.01246 -0.00827 O5 6 0.740466 0.565933 0.546571 11.00000 0.02186 0.01459 = 0.01250 0.00088 -0.00621 -0.00398 AFIX 6 O3 6 0.878983 0.450983 0.208620 11.00000 0.03180 0.02415 = 0.01480 0.00244 -0.01121 -0.01535 H3A 2 0.913394 0.492502 0.146389 11.00000 -1.50000 H3B 2 0.832401 0.406274 0.190430 11.00000 -1.50000 AFIX 0 O9 6 0.427241 0.865501 0.855418 11.00000 0.02726 0.01447 = 0.03053 -0.00103 -0.00662 -0.00340 O4 6 0.571356 0.555394 0.395083 11.00000 0.02585 0.03987 = 0.02432 -0.00386 -0.01386 -0.01269 AFIX 7 H4A 2 0.577646 0.506444 0.343443 11.00000 -1.50000 H4B 2 0.477375 0.592334 0.388174 11.00000 -1.50000 AFIX 0 O1 6 0.814169 0.334749 0.439003 11.00000 0.04468 0.01439 = 0.01659 0.00544 -0.01248 -0.01277 O16 6 0.475986 0.732761 1.154001 11.00000 0.02894 0.01484 = 0.02274 -0.00357 -0.01101 -0.00596 O11 6 0.137575 0.809428 1.091216 11.00000 0.03182 0.01797 = 0.02615 -0.00034 -0.01287 -0.00286 O8 6 0.442798 0.761755 0.661798 11.00000 0.02597 0.02828 = 0.01901 0.00764 -0.01086 -0.00445 N2 5 0.767385 -0.109762 0.414845 11.00000 0.02886 0.00930 = 0.02401 -0.00018 -0.01377 -0.00616 N4 5 0.788479 -0.080876 0.798094 11.00000 0.02838 0.01360 = 0.01871 0.00688 -0.01211 -0.00474 N1 5 0.784931 -0.285118 0.338552 11.00000 0.02606 0.01373 = 0.01448 0.00245 -0.00734 -0.00967 N3 5 0.833673 -0.215966 0.929860 11.00000 0.05093 0.03432 = 0.03861 0.01855 -0.02821 -0.01380 C8 1 0.790597 -0.025144 0.687305 11.00000 0.02192 0.01440 = 0.01748 0.00410 -0.00943 -0.00371 C00S 1 0.803874 0.286537 0.537325 11.00000 0.01923 0.01079 = 0.01433 0.00364 -0.00553 -0.00725 C7 1 0.801597 0.097531 0.664028 11.00000 0.01898 0.01527 = 0.01513 0.00114 -0.00707 -0.00661 AFIX 43 H7 2 0.811274 0.142108 0.719256 11.00000 -1.20000 AFIX 0 C6 1 0.797893 0.152118 0.557243 11.00000 0.01901 0.01012 = 0.01739 0.00246 -0.00644 -0.00591 C10 1 0.863146 -0.198064 0.816005 11.00000 0.03964 0.01469 = 0.03376 0.00873 -0.01937 -0.00803 AFIX 43 H10 2 0.925113 -0.256598 0.757894 11.00000 -1.20000 AFIX 0 C9 1 0.776797 -0.091631 0.604555 11.00000 0.02543 0.01005 = 0.02527 0.00279 -0.01117 -0.00493 AFIX 43 H9 2 0.766605 -0.172685 0.620934 11.00000 -1.20000 AFIX 0 C5 1 0.787785 0.086357 0.472871 11.00000 0.02627 0.01359 = 0.01760 0.00524 -0.00990 -0.00990 AFIX 43 H5 2 0.787301 0.123435 0.401042 11.00000 -1.20000 AFIX 0 C4 1 0.778378 -0.035809 0.497110 11.00000 0.02294 0.01189 = 0.01894 0.00107 -0.01047 -0.00521 C11 1 0.710711 -0.024321 0.906481 11.00000 0.04089 0.02738 = 0.01928 -0.00050 -0.00922 -0.01010 AFIX 43 H11 2 0.650036 0.057084 0.920476 11.00000 -1.20000 AFIX 0 C3 1 0.837677 -0.233056 0.400115 11.00000 0.02460 0.01143 = 0.02839 0.00024 -0.01300 -0.00438 AFIX 43 H3 2 0.914136 -0.275443 0.430163 11.00000 -1.20000 AFIX 0 C1 1 0.673713 -0.190242 0.310420 11.00000 0.04632 0.02019 = 0.02700 0.00588 -0.02541 -0.01108 AFIX 43 H1 2 0.616293 -0.199558 0.266658 11.00000 -1.20000 AFIX 0 C12 1 0.738742 -0.107633 0.986524 11.00000 0.04894 0.04600 = 0.02035 0.00841 -0.01041 -0.01715 AFIX 43 H12 2 0.700776 -0.095075 1.067199 11.00000 -1.20000 AFIX 0 C2 1 0.662531 -0.082281 0.356953 11.00000 0.04012 0.01655 = 0.03379 0.00213 -0.02609 -0.00273 AFIX 43 H2 2 0.597211 -0.004900 0.351128 11.00000 -1.20000 AFIX 6 PART 1 O1W 6 0.921488 0.044026 0.176782 10.50000 0.05280 0.05188 = 0.07281 0.00878 -0.01487 -0.01212 H1WA 2 0.942920 -0.029534 0.152790 10.50000 -1.50000 H1WB 2 0.913611 0.090347 0.118242 10.50000 -1.50000 AFIX 0 HKLF 4 REM 2_a.res in P-1 REM wR2 = 0.1035, GooF = S = 1.086, Restrained GooF = 1.086 for all data REM R1 = 0.0363 for 4865 Fo > 4sig(Fo) and 0.0461 for all 5718 data REM 368 parameters refined using 7 restraints END WGHT 0.0462 5.1347 REM Highest difference peak 1.703, deepest hole -1.468, 1-sigma level 0.213 Q1 1 0.6627 0.5483 0.7141 11.00000 0.05 1.70 Q2 1 0.8609 0.4851 0.6435 11.00000 0.05 1.70 Q3 1 0.2757 0.6233 0.9999 11.00000 0.05 1.69 Q4 1 0.6141 0.5556 1.0604 11.00000 0.05 1.66 Q5 1 0.8164 0.5583 0.7023 11.00000 0.05 1.60 ; _shelx_res_checksum 70205 _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_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo4 Mo 0.76670(5) 0.51954(4) 0.67891(4) 0.00963(10) Uani 1 1 d . . . . . Mo2 Mo 0.50797(5) 0.58942(4) 1.10260(4) 0.01024(10) Uani 1 1 d . . . . . Mo3 Mo 0.44743(5) 0.72712(4) 0.79954(4) 0.01298(11) Uani 1 1 d . . . . . Mo1 Mo 0.18653(5) 0.66209(4) 1.04379(4) 0.01212(11) Uani 1 1 d . . . . . Co1 Co 0.80436(8) 0.52172(6) 0.37340(6) 0.01332(15) Uani 1 1 d D . . . . O13 O 0.4461(4) 0.6219(3) 0.9675(3) 0.0130(7) Uani 1 1 d . . . . . O15 O 0.2643(4) 0.5785(3) 1.1642(3) 0.0141(7) Uani 1 1 d . . . . . O7 O 0.6764(4) 0.6694(3) 0.7573(3) 0.0132(7) Uani 1 1 d . . . . . O10 O 0.2422(4) 0.6982(3) 0.8765(3) 0.0160(7) Uani 1 1 d . . . . . O14 O 0.7092(4) 0.5435(3) 1.0334(3) 0.0162(7) Uani 1 1 d . . . . . O6 O 0.9607(4) 0.5064(4) 0.6485(3) 0.0181(8) Uani 1 1 d . . . . . O17 O 0.4807(4) 0.4853(3) 1.2400(3) 0.0136(7) Uani 1 1 d . . . . . O12 O 0.0120(4) 0.6276(4) 1.0722(4) 0.0219(8) Uani 1 1 d . . . . . O2 O 0.7997(5) 0.3376(3) 0.6267(3) 0.0177(8) Uani 1 1 d . . . . . O5 O 0.7405(4) 0.5659(3) 0.5466(3) 0.0165(7) Uani 1 1 d . . . . . O3 O 0.8790(5) 0.4510(4) 0.2086(3) 0.0212(8) Uani 1 1 d G . . . . H3A H 0.913394 0.492502 0.146389 0.032 Uiso 1 1 d DG U . . . H3B H 0.832401 0.406274 0.190430 0.032 Uiso 1 1 d DG U . . . O9 O 0.4272(5) 0.8655(4) 0.8554(4) 0.0255(9) Uani 1 1 d . . . . . O4 O 0.5714(5) 0.5554(4) 0.3951(4) 0.0273(9) Uani 1 1 d . . . . . H4A H 0.577646 0.506444 0.343443 0.041 Uiso 1 1 d R U . . . H4B H 0.477375 0.592334 0.388174 0.041 Uiso 1 1 d R U . . . O1 O 0.8142(5) 0.3347(4) 0.4390(4) 0.0241(9) Uani 1 1 d . . . . . O16 O 0.4760(5) 0.7328(4) 1.1540(4) 0.0213(8) Uani 1 1 d . . . . . O11 O 0.1376(5) 0.8094(4) 1.0912(4) 0.0253(9) Uani 1 1 d . . . . . O8 O 0.4428(5) 0.7618(4) 0.6618(4) 0.0248(9) Uani 1 1 d . . . . . N2 N 0.7674(6) -0.1098(4) 0.4148(4) 0.0191(10) Uani 1 1 d . . . . . N4 N 0.7885(6) -0.0809(4) 0.7981(4) 0.0199(10) Uani 1 1 d . . . . . N1 N 0.7849(6) -0.2851(4) 0.3386(4) 0.0173(9) Uani 1 1 d . . . . . N3 N 0.8337(8) -0.2160(6) 0.9299(6) 0.0386(14) Uani 1 1 d . . . . . C8 C 0.7906(6) -0.0251(5) 0.6873(5) 0.0178(11) Uani 1 1 d . . . . . C00S C 0.8039(6) 0.2865(5) 0.5373(5) 0.0145(10) Uani 1 1 d . . . . . C7 C 0.8016(6) 0.0975(5) 0.6640(5) 0.0158(10) Uani 1 1 d . . . . . H7 H 0.811274 0.142108 0.719256 0.019 Uiso 1 1 calc R U . . . C6 C 0.7979(6) 0.1521(5) 0.5572(5) 0.0153(10) Uani 1 1 d . . . . . C10 C 0.8631(8) -0.1981(5) 0.8160(6) 0.0280(14) Uani 1 1 d . . . . . H10 H 0.925113 -0.256598 0.757894 0.034 Uiso 1 1 calc R U . . . C9 C 0.7768(7) -0.0916(5) 0.6046(5) 0.0198(11) Uani 1 1 d . . . . . H9 H 0.766605 -0.172685 0.620934 0.024 Uiso 1 1 calc R U . . . C5 C 0.7878(6) 0.0864(5) 0.4729(5) 0.0180(11) Uani 1 1 d . . . . . H5 H 0.787301 0.123435 0.401042 0.022 Uiso 1 1 calc R U . . . C4 C 0.7784(6) -0.0358(5) 0.4971(5) 0.0170(10) Uani 1 1 d . . . . . C11 C 0.7107(8) -0.0243(6) 0.9065(5) 0.0293(14) Uani 1 1 d . . . . . H11 H 0.650036 0.057084 0.920476 0.035 Uiso 1 1 calc R U . . . C3 C 0.8377(7) -0.2331(5) 0.4001(5) 0.0205(11) Uani 1 1 d . . . . . H3 H 0.914136 -0.275443 0.430163 0.025 Uiso 1 1 calc R U . . . C1 C 0.6737(8) -0.1902(6) 0.3104(6) 0.0275(13) Uani 1 1 d . . . . . H1 H 0.616293 -0.199558 0.266658 0.033 Uiso 1 1 calc R U . . . C12 C 0.7387(9) -0.1076(7) 0.9865(6) 0.0387(17) Uani 1 1 d . . . . . H12 H 0.700776 -0.095075 1.067199 0.046 Uiso 1 1 calc R U . . . C2 C 0.6625(8) -0.0823(6) 0.3570(6) 0.0275(13) Uani 1 1 d . . . . . H2 H 0.597211 -0.004900 0.351128 0.033 Uiso 1 1 calc R U . . . O1W O 0.9215(16) 0.0440(12) 0.1768(13) 0.062(3) Uani 0.5 1 d G U P A 1 H1WA H 0.942920 -0.029534 0.152790 0.094 Uiso 0.5 1 d G U P A 1 H1WB H 0.913611 0.090347 0.118242 0.094 Uiso 0.5 1 d G U P A 1 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 Mo4 0.0120(2) 0.00937(19) 0.00864(19) 0.00182(15) -0.00474(15) -0.00379(15) Mo2 0.0135(2) 0.00969(19) 0.01007(19) 0.00264(15) -0.00672(15) -0.00448(15) Mo3 0.0150(2) 0.0103(2) 0.0130(2) 0.00426(16) -0.00586(16) -0.00268(15) Mo1 0.0124(2) 0.0127(2) 0.0115(2) 0.00324(16) -0.00628(16) -0.00223(15) Co1 0.0178(3) 0.0122(3) 0.0131(3) 0.0011(3) -0.0080(3) -0.0056(3) O13 0.0162(18) 0.0139(16) 0.0095(16) 0.0059(13) -0.0068(13) -0.0042(14) O15 0.0164(18) 0.0127(17) 0.0135(17) 0.0043(14) -0.0071(14) -0.0036(14) O7 0.0143(17) 0.0116(16) 0.0132(17) -0.0015(14) -0.0037(14) -0.0038(13) O10 0.0186(19) 0.0160(17) 0.0150(18) 0.0067(15) -0.0089(15) -0.0054(14) O14 0.0180(19) 0.0143(17) 0.0181(18) 0.0030(15) -0.0088(15) -0.0048(14) O6 0.0162(18) 0.0207(19) 0.0183(19) 0.0013(16) -0.0069(15) -0.0059(15) O17 0.0167(18) 0.0160(17) 0.0112(16) 0.0016(14) -0.0071(14) -0.0068(14) O12 0.0170(19) 0.027(2) 0.024(2) 0.0055(17) -0.0095(16) -0.0075(16) O2 0.031(2) 0.0122(17) 0.0153(18) 0.0021(15) -0.0125(16) -0.0083(15) O5 0.0219(19) 0.0146(17) 0.0125(17) 0.0009(14) -0.0062(15) -0.0040(15) O3 0.032(2) 0.024(2) 0.0148(18) 0.0024(16) -0.0112(17) -0.0154(17) O9 0.027(2) 0.0145(19) 0.031(2) -0.0010(17) -0.0066(18) -0.0034(16) O4 0.026(2) 0.040(3) 0.024(2) -0.0039(19) -0.0139(18) -0.0127(19) O1 0.045(3) 0.0144(18) 0.0166(19) 0.0054(16) -0.0125(18) -0.0128(18) O16 0.029(2) 0.0148(18) 0.023(2) -0.0036(16) -0.0110(17) -0.0060(16) O11 0.032(2) 0.0180(19) 0.026(2) -0.0003(17) -0.0129(18) -0.0029(17) O8 0.026(2) 0.028(2) 0.019(2) 0.0076(17) -0.0109(17) -0.0045(17) N2 0.029(3) 0.009(2) 0.024(2) -0.0002(18) -0.014(2) -0.0062(18) N4 0.028(3) 0.014(2) 0.019(2) 0.0069(18) -0.012(2) -0.0047(19) N1 0.026(2) 0.014(2) 0.014(2) 0.0025(17) -0.0073(18) -0.0097(18) N3 0.051(4) 0.034(3) 0.039(3) 0.019(3) -0.028(3) -0.014(3) C8 0.022(3) 0.014(2) 0.017(3) 0.004(2) -0.009(2) -0.004(2) C00S 0.019(3) 0.011(2) 0.014(2) 0.0036(19) -0.006(2) -0.0073(19) C7 0.019(3) 0.015(2) 0.015(2) 0.001(2) -0.007(2) -0.007(2) C6 0.019(3) 0.010(2) 0.017(3) 0.0025(19) -0.006(2) -0.0059(19) C10 0.040(4) 0.015(3) 0.034(3) 0.009(2) -0.019(3) -0.008(2) C9 0.025(3) 0.010(2) 0.025(3) 0.003(2) -0.011(2) -0.005(2) C5 0.026(3) 0.014(2) 0.018(3) 0.005(2) -0.010(2) -0.010(2) C4 0.023(3) 0.012(2) 0.019(3) 0.001(2) -0.010(2) -0.005(2) C11 0.041(4) 0.027(3) 0.019(3) 0.000(2) -0.009(3) -0.010(3) C3 0.025(3) 0.011(2) 0.028(3) 0.000(2) -0.013(2) -0.004(2) C1 0.046(4) 0.020(3) 0.027(3) 0.006(2) -0.025(3) -0.011(3) C12 0.049(4) 0.046(4) 0.020(3) 0.008(3) -0.010(3) -0.017(3) C2 0.040(4) 0.017(3) 0.034(3) 0.002(2) -0.026(3) -0.003(2) O1W 0.053(6) 0.052(6) 0.073(7) 0.009(6) -0.015(6) -0.012(5) 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 '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 O15 Mo4 O17 71.44(14) 2_667 2_667 ? O15 Mo4 O2 77.95(14) 2_667 . ? O7 Mo4 O15 91.29(15) . 2_667 ? O7 Mo4 O17 78.15(14) . 2_667 ? O7 Mo4 O2 161.16(16) . . ? O6 Mo4 O15 94.42(17) . 2_667 ? O6 Mo4 O7 101.15(17) . . ? O6 Mo4 O17 165.76(16) . 2_667 ? O6 Mo4 O2 95.13(17) . . ? O6 Mo4 O5 104.45(18) . . ? O2 Mo4 O17 83.73(14) . 2_667 ? O5 Mo4 O15 155.82(17) . 2_667 ? O5 Mo4 O7 99.58(17) . . ? O5 Mo4 O17 89.63(16) . 2_667 ? O5 Mo4 O2 85.32(16) . . ? O13 Mo2 O13 77.08(15) . 2_667 ? O13 Mo2 O15 73.53(14) . . ? O15 Mo2 O13 81.50(12) . 2_667 ? O14 Mo2 O13 76.73(15) . 2_667 ? O14 Mo2 O13 100.08(17) . . ? O14 Mo2 O15 158.19(15) . . ? O14 Mo2 O17 100.61(17) . . ? O17 Mo2 O13 139.88(16) . . ? O17 Mo2 O13 74.77(13) . 2_667 ? O17 Mo2 O15 74.51(14) . . ? O16 Mo2 O13 178.58(16) . 2_667 ? O16 Mo2 O13 104.20(18) . . ? O16 Mo2 O15 98.26(17) . . ? O16 Mo2 O14 103.54(19) . . ? O16 Mo2 O17 103.81(18) . . ? O13 Mo3 O17 72.15(13) . 2_667 ? O7 Mo3 O13 82.86(14) . . ? O7 Mo3 O17 72.74(13) . 2_667 ? O10 Mo3 O13 72.99(14) . . ? O10 Mo3 O7 150.08(15) . . ? O10 Mo3 O17 83.06(14) . 2_667 ? O9 Mo3 O13 93.49(18) . . ? O9 Mo3 O7 95.95(18) . . ? O9 Mo3 O10 102.77(18) . . ? O9 Mo3 O17 162.43(18) . 2_667 ? O9 Mo3 O8 105.0(2) . . ? O8 Mo3 O13 161.21(18) . . ? O8 Mo3 O7 98.49(18) . . ? O8 Mo3 O10 98.95(18) . . ? O8 Mo3 O17 90.26(17) . 2_667 ? O13 Mo1 O14 70.72(13) . 2_667 ? O15 Mo1 O13 72.66(14) . . ? O15 Mo1 O10 144.48(16) . . ? O15 Mo1 O14 80.44(14) . 2_667 ? O10 Mo1 O13 73.23(14) . . ? O10 Mo1 O14 79.31(14) . 2_667 ? O12 Mo1 O13 153.34(17) . . ? O12 Mo1 O15 106.48(18) . . ? O12 Mo1 O10 99.55(18) . . ? O12 Mo1 O14 82.78(16) . 2_667 ? O11 Mo1 O13 101.60(18) . . ? O11 Mo1 O15 97.97(18) . . ? O11 Mo1 O10 98.24(19) . . ? O11 Mo1 O14 172.31(18) . 2_667 ? O11 Mo1 O12 104.9(2) . . ? O6 Co1 O1 89.48(16) 2_766 . ? O6 Co1 N1 90.14(17) 2_766 1_565 ? O5 Co1 O6 89.91(15) . 2_766 ? O5 Co1 O4 89.61(16) . . ? O5 Co1 O1 84.68(15) . . ? O5 Co1 N1 85.58(16) . 1_565 ? O3 Co1 O6 87.64(16) . 2_766 ? O3 Co1 O5 171.47(16) . . ? O3 Co1 O4 93.08(17) . . ? O3 Co1 O1 87.13(16) . . ? O3 Co1 N1 102.59(17) . 1_565 ? O4 Co1 O6 178.23(17) . 2_766 ? O4 Co1 O1 92.17(18) . . ? O4 Co1 N1 88.13(18) . 1_565 ? N1 Co1 O1 170.25(17) 1_565 . ? Mo2 O13 Mo2 102.92(14) . 2_667 ? Mo2 O13 Mo3 150.77(19) . . ? Mo2 O13 Mo1 104.04(15) . . ? Mo3 O13 Mo2 98.01(13) . 2_667 ? Mo1 O13 Mo2 96.49(13) . 2_667 ? Mo1 O13 Mo3 93.51(13) . . ? Mo4 O15 Mo2 104.27(15) 2_667 . ? Mo1 O15 Mo4 150.6(2) . 2_667 ? Mo1 O15 Mo2 105.07(16) . . ? Mo4 O7 Mo3 114.45(18) . . ? Mo3 O10 Mo1 114.72(19) . . ? Mo2 O14 Mo1 115.98(18) . 2_667 ? Mo4 O6 Co1 174.1(2) . 2_766 ? Mo4 O17 Mo3 90.22(13) 2_667 2_667 ? Mo2 O17 Mo4 109.30(17) . 2_667 ? Mo2 O17 Mo3 113.89(16) . 2_667 ? C00S O2 Mo4 136.9(3) . . ? Mo4 O5 Co1 145.9(2) . . ? Co1 O3 H3A 122.6 . . ? Co1 O3 H3B 122.6 . . ? H3A O3 H3B 104.5 . . ? Co1 O4 H4A 100.5 . . ? Co1 O4 H4B 160.4 . . ? H4A O4 H4B 82.5 . . ? C00S O1 Co1 132.7(4) . . ? C3 N2 C4 123.6(5) . . ? C3 N2 C2 106.6(5) . . ? C2 N2 C4 128.4(5) . . ? C10 N4 C8 126.0(5) . . ? C10 N4 C11 107.7(5) . . ? C11 N4 C8 126.3(5) . . ? C3 N1 Co1 114.2(4) . 1_545 ? C3 N1 C1 105.9(5) . . ? C1 N1 Co1 132.6(4) . 1_545 ? C10 N3 C12 108.3(6) . . ? C7 C8 N4 119.7(5) . . ? C9 C8 N4 119.9(5) . . ? C9 C8 C7 120.4(5) . . ? O2 C00S C6 114.0(5) . . ? O1 C00S O2 127.2(5) . . ? O1 C00S C6 118.8(5) . . ? C8 C7 H7 120.5 . . ? C6 C7 C8 119.0(5) . . ? C6 C7 H7 120.5 . . ? C7 C6 C00S 117.4(5) . . ? C5 C6 C00S 121.3(5) . . ? C5 C6 C7 121.3(5) . . ? N4 C10 H10 125.7 . . ? N3 C10 N4 108.5(6) . . ? N3 C10 H10 125.7 . . ? C8 C9 H9 120.4 . . ? C4 C9 C8 119.3(5) . . ? C4 C9 H9 120.4 . . ? C6 C5 H5 120.6 . . ? C6 C5 C4 118.8(5) . . ? C4 C5 H5 120.6 . . ? C9 C4 N2 116.6(5) . . ? C5 C4 N2 122.3(5) . . ? C5 C4 C9 121.1(5) . . ? N4 C11 H11 126.4 . . ? C12 C11 N4 107.2(6) . . ? C12 C11 H11 126.4 . . ? N2 C3 H3 124.1 . . ? N1 C3 N2 111.8(5) . . ? N1 C3 H3 124.1 . . ? N1 C1 H1 125.4 . . ? C2 C1 N1 109.2(5) . . ? C2 C1 H1 125.4 . . ? N3 C12 H12 125.9 . . ? C11 C12 N3 108.2(6) . . ? C11 C12 H12 125.9 . . ? N2 C2 H2 126.7 . . ? C1 C2 N2 106.5(5) . . ? C1 C2 H2 126.7 . . ? H1WA O1W H1WB 104.5 . . ? 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 Mo4 O15 2.064(4) 2_667 ? Mo4 O7 1.852(3) . ? Mo4 O6 1.720(4) . ? Mo4 O17 2.215(4) 2_667 ? Mo4 O2 2.108(4) . ? Mo4 O5 1.732(4) . ? Mo2 O13 2.476(4) 2_667 ? Mo2 O13 1.923(4) . ? Mo2 O15 2.204(4) . ? Mo2 O14 1.741(4) . ? Mo2 O17 1.910(4) . ? Mo2 O16 1.696(4) . ? Mo3 O13 2.247(3) . ? Mo3 O7 1.985(4) . ? Mo3 O10 1.939(4) . ? Mo3 O17 2.338(4) 2_667 ? Mo3 O9 1.698(4) . ? Mo3 O8 1.702(4) . ? Mo1 O13 2.236(4) . ? Mo1 O15 1.929(4) . ? Mo1 O10 1.940(4) . ? Mo1 O14 2.389(4) 2_667 ? Mo1 O12 1.719(4) . ? Mo1 O11 1.692(4) . ? Co1 O6 2.100(4) 2_766 ? Co1 O5 2.056(4) . ? Co1 O3 2.047(4) . ? Co1 O4 2.075(4) . ? Co1 O1 2.143(4) . ? Co1 N1 2.124(4) 1_565 ? O2 C00S 1.275(6) . ? O3 H3A 0.8498 . ? O3 H3B 0.8498 . ? O4 H4A 0.8583 . ? O4 H4B 0.9114 . ? O1 C00S 1.243(7) . ? N2 C4 1.425(7) . ? N2 C3 1.357(7) . ? N2 C2 1.384(8) . ? N4 C8 1.423(7) . ? N4 C10 1.345(7) . ? N4 C11 1.383(8) . ? N1 C3 1.308(7) . ? N1 C1 1.394(8) . ? N3 C10 1.319(9) . ? N3 C12 1.375(10) . ? C8 C7 1.394(7) . ? C8 C9 1.388(8) . ? C00S C6 1.509(7) . ? C7 H7 0.9300 . ? C7 C6 1.388(7) . ? C6 C5 1.381(8) . ? C10 H10 0.9300 . ? C9 H9 0.9300 . ? C9 C4 1.388(8) . ? C5 H5 0.9300 . ? C5 C4 1.386(7) . ? C11 H11 0.9300 . ? C11 C12 1.323(10) . ? C3 H3 0.9300 . ? C1 H1 0.9300 . ? C1 C2 1.355(8) . ? C12 H12 0.9300 . ? C2 H2 0.9300 . ? O1W H1WA 0.8502 . ? O1W H1WB 0.8498 . ? 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 Mo4 O2 C00S O1 13.5(9) . . . . ? Mo4 O2 C00S C6 -167.5(4) . . . . ? Co1 O1 C00S O2 -7.9(9) . . . . ? Co1 O1 C00S C6 173.2(4) . . . . ? Co1 N1 C3 N2 -153.7(4) 1_545 . . . ? Co1 N1 C1 C2 147.0(5) 1_545 . . . ? O13 Mo2 O14 Mo1 -76.4(2) . . . 2_667 ? O13 Mo2 O14 Mo1 -2.33(16) 2_667 . . 2_667 ? O15 Mo4 O7 Mo3 -89.40(19) 2_667 . . . ? O15 Mo4 O5 Co1 -80.0(6) 2_667 . . . ? O15 Mo2 O14 Mo1 -5.7(5) . . . 2_667 ? O7 Mo4 O5 Co1 164.4(4) . . . . ? O6 Mo4 O7 Mo3 175.84(19) . . . . ? O6 Mo4 O5 Co1 60.2(4) . . . . ? O17 Mo4 O7 Mo3 -18.67(17) 2_667 . . . ? O17 Mo4 O5 Co1 -117.6(4) 2_667 . . . ? O17 Mo2 O14 Mo1 69.1(2) . . . 2_667 ? O2 Mo4 O7 Mo3 -34.9(6) . . . . ? O2 Mo4 O5 Co1 -33.9(4) . . . . ? O2 C00S C6 C7 -5.1(7) . . . . ? O2 C00S C6 C5 174.3(5) . . . . ? O5 Mo4 O7 Mo3 68.9(2) . . . . ? O1 C00S C6 C7 173.9(5) . . . . ? O1 C00S C6 C5 -6.6(8) . . . . ? O16 Mo2 O14 Mo1 176.2(2) . . . 2_667 ? N4 C8 C7 C6 -177.7(5) . . . . ? N4 C8 C9 C4 179.7(5) . . . . ? N4 C11 C12 N3 0.2(8) . . . . ? N1 C1 C2 N2 -0.1(7) . . . . ? C8 N4 C10 N3 180.0(6) . . . . ? C8 N4 C11 C12 -179.9(6) . . . . ? C8 C7 C6 C00S 177.7(5) . . . . ? C8 C7 C6 C5 -1.8(8) . . . . ? C8 C9 C4 N2 178.6(5) . . . . ? C8 C9 C4 C5 -2.4(9) . . . . ? C00S C6 C5 C4 -178.3(5) . . . . ? C7 C8 C9 C4 1.8(8) . . . . ? C7 C6 C5 C4 1.2(8) . . . . ? C6 C5 C4 N2 179.9(5) . . . . ? C6 C5 C4 C9 0.9(8) . . . . ? C10 N4 C8 C7 -139.1(6) . . . . ? C10 N4 C8 C9 42.9(9) . . . . ? C10 N4 C11 C12 -0.4(8) . . . . ? C10 N3 C12 C11 0.1(9) . . . . ? C9 C8 C7 C6 0.3(8) . . . . ? C4 N2 C3 N1 166.7(5) . . . . ? C4 N2 C2 C1 -166.0(6) . . . . ? C11 N4 C8 C7 40.2(9) . . . . ? C11 N4 C8 C9 -137.7(6) . . . . ? C11 N4 C10 N3 0.5(7) . . . . ? C3 N2 C4 C9 -38.0(8) . . . . ? C3 N2 C4 C5 143.0(6) . . . . ? C3 N2 C2 C1 0.3(7) . . . . ? C3 N1 C1 C2 -0.1(7) . . . . ? C1 N1 C3 N2 0.3(7) . . . . ? C12 N3 C10 N4 -0.4(8) . . . . ? C2 N2 C4 C9 126.2(7) . . . . ? C2 N2 C4 C5 -52.8(9) . . . . ? C2 N2 C3 N1 -0.4(7) . . . . ?