#------------------------------------------------------------------------------ #$Date: 2021-10-17 01:39:36 +0300 (Sun, 17 Oct 2021) $ #$Revision: 269981 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/37/7243747.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_7243747 loop_ _publ_author_name 'Ying, Jun' 'Jin, Liang' 'Yu, Haiyan' 'Tian, Aixiang' 'Wang, Xiuli' _publ_section_title ; A series of polyoxometalate-based hybrid complexes constructed by a tripodal ligand containing mixed N/O donors ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE01195B _journal_year 2021 _chemical_formula_moiety 'C26 H28 Cu2 Mo8 N8 O34, 0.5(H4 O2)' _chemical_formula_sum 'C26 H30 Cu2 Mo8 N8 O35' _chemical_formula_weight 1909.18 _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.cc26rr0r _audit_creation_date 2020-12-05 _audit_creation_method ; Olex2 1.3-alpha (compiled 2019.10.31 svn.r3677 for OlexSys, GUI svn.r5972) ; _audit_update_record ; 2020-12-07 deposited with the CCDC. 2021-10-15 downloaded from the CCDC. ; _cell_angle_alpha 83.427(4) _cell_angle_beta 68.122(4) _cell_angle_gamma 73.812(4) _cell_formula_units_Z 1 _cell_length_a 9.593(2) _cell_length_b 11.205(2) _cell_length_c 12.283(3) _cell_measurement_reflns_used 2494 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 26.80 _cell_measurement_theta_min 2.37 _cell_volume 1176.5(4) _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 1.000 _diffrn_measured_fraction_theta_max 0.992 _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 0.0341 _diffrn_reflns_av_unetI/netI 0.0646 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7578 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.879 _diffrn_reflns_theta_min 1.787 _diffrn_source_current 30.0 _diffrn_source_power 1.2 _diffrn_source_voltage 40.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.057 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.5437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0715 before and 0.0379 after correction. The Ratio of minimum to maximum transmission is 0.7293. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.694 _exptl_crystal_description block _exptl_crystal_F_000 916 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _refine_diff_density_max 1.535 _refine_diff_density_min -2.178 _refine_diff_density_rms 0.225 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 366 _refine_ls_number_reflns 5033 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.997 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0429 _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^)+(0.0611P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1008 _refine_ls_wR_factor_ref 0.1107 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3929 _reflns_number_total 5076 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01195b2.cif _cod_data_source_block 2_CCDC2 _cod_original_cell_volume 1176.6(4) _cod_database_code 7243747 _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, All O(H,H,H) groups 2. Others Fixed Sof: O1W(0.5) H1WA(0.5) H1WB(0.5) 3.a Free rotating group: O1W(H1,H1WA,H1WB) 3.b Rotating group: O3(H3A,H3B), O17(H17A,H17B) 3.c Aromatic/amide H refined with riding coordinates: C9(H9), C13(H13), C11(H11), C2(H2), C5(H5), C4(H4), C7(H7), C3(H3), C6(H6) ; _shelx_res_file ; TITL 2_a.res in P-1 2.res created by SHELXL-2018/3 at 14:50:05 on 05-Dec-2020 REM Old TITL 2 in P-1 REM SHELXT solution in P-1: R1 0.102, Rweak 0.004, Alpha 0.053 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C15 N8 O12 Zn3 Mo2 CELL 0.71073 9.5929 11.2052 12.2831 83.427 68.122 73.812 ZERR 1 0.0021 0.0023 0.0027 0.004 0.004 0.004 LATT 1 SFAC C H Cu Mo N O UNIT 26 30 2 8 8 35 L.S. 4 0 0 PLAN 5 TEMP 23 CONF list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.061100 FVAR 0.35143 MO1 4 0.766207 0.019466 0.678693 11.00000 0.01555 0.01668 = 0.00858 0.00110 -0.00663 -0.00644 MO4 4 0.508124 0.089803 1.102245 11.00000 0.01649 0.01569 = 0.00914 0.00206 -0.00842 -0.00637 MO2 4 0.446374 0.226884 0.799886 11.00000 0.01797 0.01660 = 0.01243 0.00402 -0.00789 -0.00518 MO3 4 0.186390 0.161659 1.044258 11.00000 0.01533 0.01928 = 0.01049 0.00229 -0.00792 -0.00426 CU05 3 0.801967 0.023826 0.370115 11.00000 0.02047 0.01832 = 0.01183 -0.00063 -0.00964 -0.00788 O14 6 0.266259 0.078864 1.164223 11.00000 0.01822 0.01966 = 0.01202 0.00586 -0.00881 -0.00935 O11 6 0.445001 0.121663 0.967715 11.00000 0.01773 0.01581 = 0.00985 0.00324 -0.00543 -0.00453 O12 6 0.241994 0.197431 0.876850 11.00000 0.01959 0.02436 = 0.01471 0.00400 -0.01225 -0.00711 O7 6 0.675581 0.168681 0.757044 11.00000 0.01146 0.02301 = 0.01328 -0.00093 -0.00388 -0.00817 O15 6 0.481210 -0.015504 1.238715 11.00000 0.01737 0.02080 = 0.01020 0.00309 -0.01043 -0.00674 O4 6 0.736713 0.065284 0.548406 11.00000 0.02804 0.02110 = 0.01054 0.00068 -0.00657 -0.00790 O9 6 0.709048 0.044051 1.032602 11.00000 0.02323 0.02549 = 0.01276 0.00296 -0.01021 -0.00894 O1 6 0.800343 0.836266 0.627376 11.00000 0.03713 0.01758 = 0.01995 -0.00249 -0.01685 -0.00743 O16 6 0.012426 0.126747 1.072831 11.00000 0.01932 0.03553 = 0.02425 0.00578 -0.00952 -0.01175 O5 6 0.960246 0.007831 0.647132 11.00000 0.01295 0.02460 = 0.02465 -0.00207 -0.00438 -0.00808 O2 6 0.814703 0.835036 0.439953 11.00000 0.05125 0.02067 = 0.01476 0.00481 -0.01557 -0.01817 O10 6 0.476508 0.232906 1.152869 11.00000 0.03147 0.01799 = 0.02725 -0.00264 -0.01716 -0.00813 O3 6 0.881617 -0.051236 0.207426 11.00000 0.03888 0.02880 = 0.01235 0.00363 -0.01374 -0.01699 AFIX 7 H3A 2 0.877285 0.006784 0.156095 11.00000 -1.50000 H3B 2 0.819402 -0.091580 0.204463 11.00000 -1.50000 AFIX 0 O13 6 0.137111 0.309283 1.091109 11.00000 0.03100 0.02387 = 0.02767 -0.00166 -0.01246 -0.00550 O8 6 0.425329 0.365001 0.855333 11.00000 0.03302 0.02291 = 0.02730 0.00121 -0.01122 -0.00954 O6 6 0.441659 0.260879 0.662766 11.00000 0.02968 0.03264 = 0.01788 0.00619 -0.01084 -0.00586 O17 6 0.568922 0.053928 0.395469 11.00000 0.03218 0.05320 = 0.02608 -0.00097 -0.01922 -0.02151 AFIX 7 H17A 2 0.559570 0.044113 0.330844 11.00000 -1.50000 H17B 2 0.566915 0.130396 0.398063 11.00000 -1.50000 AFIX 0 N1 5 0.767329 0.389430 0.415031 11.00000 0.02705 0.01555 = 0.02034 -0.00092 -0.01293 -0.00667 N3 5 0.787914 0.418450 0.798524 11.00000 0.02846 0.02042 = 0.01697 0.00459 -0.01131 -0.00837 N2 5 0.783752 0.214510 0.338575 11.00000 0.02692 0.02739 = 0.01234 -0.00194 -0.00592 -0.01198 C1 1 0.804880 0.785555 0.536965 11.00000 0.01370 0.02297 = 0.01175 -0.00484 -0.00550 -0.00585 C12 1 0.791818 0.474849 0.687286 11.00000 0.02553 0.02035 = 0.01952 0.00619 -0.01292 -0.00818 N4 5 0.832206 0.284187 0.930593 11.00000 0.04940 0.04455 = 0.02978 0.01568 -0.02418 -0.01738 C10 1 0.798333 0.652220 0.558962 11.00000 0.01847 0.01195 = 0.01968 0.00231 -0.01084 -0.00219 C9 1 0.788090 0.586221 0.472624 11.00000 0.02237 0.01984 = 0.01650 0.00039 -0.00961 -0.00662 AFIX 43 H9 2 0.787797 0.622978 0.400853 11.00000 -1.20000 AFIX 0 C13 1 0.776637 0.408014 0.605048 11.00000 0.02876 0.01255 = 0.02296 0.00333 -0.01219 -0.00664 AFIX 43 H13 2 0.765540 0.327358 0.621606 11.00000 -1.20000 AFIX 0 C11 1 0.801440 0.597127 0.664602 11.00000 0.01816 0.02487 = 0.01596 -0.00088 -0.00752 -0.00679 AFIX 43 H11 2 0.809926 0.641583 0.720297 11.00000 -1.20000 AFIX 0 C8 1 0.778423 0.464096 0.498477 11.00000 0.02165 0.01652 = 0.02473 -0.00239 -0.01048 -0.00400 C2 1 0.861258 0.302018 0.816576 11.00000 0.03873 0.02141 = 0.03283 0.00440 -0.02431 -0.00559 AFIX 43 H2 2 0.922553 0.243222 0.758697 11.00000 -1.20000 AFIX 0 C5 1 0.835655 0.267552 0.402272 11.00000 0.02690 0.02348 = 0.02498 -0.00161 -0.01281 -0.00964 AFIX 43 H5 2 0.910207 0.225119 0.433984 11.00000 -1.20000 AFIX 0 C4 1 0.710813 0.476426 0.905616 11.00000 0.03826 0.02779 = 0.02036 0.00018 -0.00898 -0.00637 AFIX 43 H4 2 0.650913 0.558076 0.918807 11.00000 -1.20000 AFIX 0 C7 1 0.664532 0.418909 0.355740 11.00000 0.04672 0.02819 = 0.03350 0.00402 -0.02677 -0.01129 AFIX 43 H7 2 0.601213 0.496689 0.348290 11.00000 -1.20000 AFIX 0 C3 1 0.738629 0.392718 0.987068 11.00000 0.05079 0.05094 = 0.01573 0.00916 -0.01386 -0.01846 AFIX 43 H3 2 0.701248 0.405790 1.067453 11.00000 -1.20000 AFIX 0 C6 1 0.675660 0.311230 0.311214 11.00000 0.04436 0.02244 = 0.02230 0.00176 -0.02267 -0.00471 AFIX 43 H6 2 0.618014 0.302755 0.267526 11.00000 -1.20000 AFIX 6 O1W 6 -0.077806 0.543566 1.175202 10.50000 0.06055 0.03541 = 0.08835 0.00302 -0.01778 0.00586 H1 2 0.801252 0.914141 0.649186 11.00000 -1.50000 H1WA 2 -0.076749 0.492959 1.128225 10.50000 -1.50000 H1WB 2 -0.129478 0.613294 1.158419 10.50000 -1.50000 AFIX 0 HKLF 4 REM 2_a.res in P-1 REM wR2 = 0.1107, GooF = S = 0.997, Restrained GooF = 0.997 for all data REM R1 = 0.0429 for 3929 Fo > 4sig(Fo) and 0.0621 for all 5033 data REM 366 parameters refined using 0 restraints END WGHT 0.0611 0.0000 REM Highest difference peak 1.535, deepest hole -2.178, 1-sigma level 0.225 Q1 1 0.8246 0.1021 0.6627 11.00000 0.05 1.54 Q2 1 0.5696 0.1648 1.0893 11.00000 0.05 1.26 Q3 1 0.0812 0.1729 1.0794 11.00000 0.05 1.18 Q4 1 0.4464 0.1633 1.1634 11.00000 0.05 1.15 Q5 1 0.3391 0.2382 0.8399 11.00000 0.05 1.13 ; _shelx_res_checksum 16310 _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 Mo1 Mo 0.76621(6) 0.01947(5) 0.67869(4) 0.01252(14) Uani 1 1 d . . . . . Mo4 Mo 0.50812(6) 0.08980(5) 1.10224(4) 0.01233(14) Uani 1 1 d . . . . . Mo2 Mo 0.44637(6) 0.22688(5) 0.79989(5) 0.01513(14) Uani 1 1 d . . . . . Mo3 Mo 0.18639(6) 0.16166(5) 1.04426(5) 0.01429(14) Uani 1 1 d . . . . . Cu05 Cu 0.80197(9) 0.02383(7) 0.37012(6) 0.01505(18) Uani 1 1 d . . . . . O14 O 0.2663(5) 0.0789(4) 1.1642(4) 0.0152(9) Uani 1 1 d . . . . . O11 O 0.4450(5) 0.1217(4) 0.9677(4) 0.0146(9) Uani 1 1 d . . . . . O12 O 0.2420(5) 0.1974(4) 0.8768(4) 0.0178(10) Uani 1 1 d . . . . . O7 O 0.6756(5) 0.1687(4) 0.7570(4) 0.0152(9) Uani 1 1 d . . . . . O15 O 0.4812(5) -0.0155(4) 1.2387(4) 0.0144(9) Uani 1 1 d . . . . . O4 O 0.7367(5) 0.0653(4) 0.5484(4) 0.0197(10) Uani 1 1 d . . . . . O9 O 0.7090(5) 0.0441(4) 1.0326(4) 0.0191(10) Uani 1 1 d . . . . . O1 O 0.8003(6) 0.8363(4) 0.6274(4) 0.0226(11) Uani 1 1 d . . . . . O16 O 0.0124(5) 0.1267(4) 1.0728(4) 0.0254(11) Uani 1 1 d . . . . . O5 O 0.9602(5) 0.0078(4) 0.6471(4) 0.0206(10) Uani 1 1 d . . . . . O2 O 0.8147(6) 0.8350(4) 0.4400(4) 0.0263(11) Uani 1 1 d . . . . . O10 O 0.4765(6) 0.2329(4) 1.1529(4) 0.0230(11) Uani 1 1 d . . . . . O3 O 0.8816(6) -0.0512(4) 0.2074(4) 0.0238(11) Uani 1 1 d . . . . . H3A H 0.877285 0.006784 0.156095 0.036 Uiso 1 1 d R U . . . H3B H 0.819402 -0.091580 0.204463 0.036 Uiso 1 1 d R U . . . O13 O 0.1371(6) 0.3093(4) 1.0911(4) 0.0271(11) Uani 1 1 d . . . . . O8 O 0.4253(6) 0.3650(4) 0.8553(4) 0.0272(11) Uani 1 1 d . . . . . O6 O 0.4417(6) 0.2609(4) 0.6628(4) 0.0270(11) Uani 1 1 d . . . . . O17 O 0.5689(6) 0.0539(5) 0.3955(4) 0.0322(12) Uani 1 1 d . . . . . H17A H 0.559570 0.044113 0.330844 0.048 Uiso 1 1 d R U . . . H17B H 0.566915 0.130396 0.398063 0.048 Uiso 1 1 d R U . . . N1 N 0.7673(7) 0.3894(5) 0.4150(5) 0.0193(12) Uani 1 1 d . . . . . N3 N 0.7879(7) 0.4185(5) 0.7985(5) 0.0209(12) Uani 1 1 d . . . . . N2 N 0.7838(7) 0.2145(5) 0.3386(5) 0.0213(12) Uani 1 1 d . . . . . C1 C 0.8049(7) 0.7856(6) 0.5370(5) 0.0152(13) Uani 1 1 d . . . . . C12 C 0.7918(8) 0.4748(6) 0.6873(6) 0.0204(14) Uani 1 1 d . . . . . N4 N 0.8322(8) 0.2842(6) 0.9306(6) 0.0385(17) Uani 1 1 d . . . . . C10 C 0.7983(7) 0.6522(6) 0.5590(6) 0.0161(13) Uani 1 1 d . . . . . C9 C 0.7881(8) 0.5862(6) 0.4726(6) 0.0186(14) Uani 1 1 d . . . . . H9 H 0.787797 0.622978 0.400853 0.022 Uiso 1 1 calc R U . . . C13 C 0.7766(8) 0.4080(6) 0.6050(6) 0.0206(14) Uani 1 1 d . . . . . H13 H 0.765540 0.327358 0.621606 0.025 Uiso 1 1 calc R U . . . C11 C 0.8014(7) 0.5971(6) 0.6646(6) 0.0189(14) Uani 1 1 d . . . . . H11 H 0.809926 0.641583 0.720297 0.023 Uiso 1 1 calc R U . . . C8 C 0.7784(8) 0.4641(6) 0.4985(6) 0.0203(14) Uani 1 1 d . . . . . C2 C 0.8613(9) 0.3020(7) 0.8166(7) 0.0284(17) Uani 1 1 d . . . . . H2 H 0.922553 0.243222 0.758697 0.034 Uiso 1 1 calc R U . . . C5 C 0.8357(8) 0.2676(6) 0.4023(6) 0.0233(15) Uani 1 1 d . . . . . H5 H 0.910207 0.225119 0.433984 0.028 Uiso 1 1 calc R U . . . C4 C 0.7108(9) 0.4764(7) 0.9056(6) 0.0297(17) Uani 1 1 d . . . . . H4 H 0.650913 0.558076 0.918807 0.036 Uiso 1 1 calc R U . . . C7 C 0.6645(10) 0.4189(7) 0.3557(7) 0.0324(18) Uani 1 1 d . . . . . H7 H 0.601213 0.496689 0.348290 0.039 Uiso 1 1 calc R U . . . C3 C 0.7386(10) 0.3927(8) 0.9871(7) 0.038(2) Uani 1 1 d . . . . . H3 H 0.701248 0.405790 1.067453 0.046 Uiso 1 1 calc R U . . . C6 C 0.6757(9) 0.3112(6) 0.3112(6) 0.0275(17) Uani 1 1 d . . . . . H6 H 0.618014 0.302755 0.267526 0.033 Uiso 1 1 calc R U . . . O1W O -0.0778(16) 0.5436(12) 1.1752(14) 0.068(4) Uani 0.5 1 d G . P . . H1 H 0.801252 0.914141 0.649186 0.102 Uiso 1 1 d G U . . . H1WA H -0.076749 0.492959 1.128225 0.102 Uiso 0.5 1 d G U P . . H1WB H -0.129478 0.613294 1.158419 0.102 Uiso 0.5 1 d G U P . . 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 Mo1 0.0155(3) 0.0167(3) 0.0086(2) 0.0011(2) -0.0066(2) -0.0064(2) Mo4 0.0165(3) 0.0157(3) 0.0091(2) 0.0021(2) -0.0084(2) -0.0064(2) Mo2 0.0180(3) 0.0166(3) 0.0124(3) 0.0040(2) -0.0079(2) -0.0052(2) Mo3 0.0153(3) 0.0193(3) 0.0105(3) 0.0023(2) -0.0079(2) -0.0043(2) Cu05 0.0205(4) 0.0183(4) 0.0118(4) -0.0006(3) -0.0096(3) -0.0079(3) O14 0.018(2) 0.020(2) 0.012(2) 0.0059(17) -0.0088(18) -0.0093(19) O11 0.018(2) 0.016(2) 0.010(2) 0.0032(17) -0.0054(18) -0.0045(18) O12 0.020(2) 0.024(2) 0.015(2) 0.0040(18) -0.0122(19) -0.007(2) O7 0.011(2) 0.023(2) 0.013(2) -0.0009(18) -0.0039(18) -0.0082(19) O15 0.017(2) 0.021(2) 0.010(2) 0.0031(17) -0.0104(18) -0.0067(19) O4 0.028(3) 0.021(2) 0.011(2) 0.0007(18) -0.007(2) -0.008(2) O9 0.023(3) 0.025(2) 0.013(2) 0.0030(18) -0.010(2) -0.009(2) O1 0.037(3) 0.018(2) 0.020(2) -0.0025(19) -0.017(2) -0.007(2) O16 0.019(3) 0.036(3) 0.024(3) 0.006(2) -0.010(2) -0.012(2) O5 0.013(2) 0.025(3) 0.025(3) -0.002(2) -0.0044(19) -0.008(2) O2 0.051(3) 0.021(2) 0.015(2) 0.0048(19) -0.016(2) -0.018(2) O10 0.031(3) 0.018(2) 0.027(3) -0.003(2) -0.017(2) -0.008(2) O3 0.039(3) 0.029(3) 0.012(2) 0.0036(19) -0.014(2) -0.017(2) O13 0.031(3) 0.024(3) 0.028(3) -0.002(2) -0.012(2) -0.005(2) O8 0.033(3) 0.023(3) 0.027(3) 0.001(2) -0.011(2) -0.010(2) O6 0.030(3) 0.033(3) 0.018(2) 0.006(2) -0.011(2) -0.006(2) O17 0.032(3) 0.053(3) 0.026(3) -0.001(2) -0.019(2) -0.022(3) N1 0.027(3) 0.016(3) 0.020(3) -0.001(2) -0.013(3) -0.007(2) N3 0.028(3) 0.020(3) 0.017(3) 0.005(2) -0.011(3) -0.008(3) N2 0.027(3) 0.027(3) 0.012(3) -0.002(2) -0.006(2) -0.012(3) C1 0.014(3) 0.023(3) 0.012(3) -0.005(3) -0.006(2) -0.006(3) C12 0.026(4) 0.020(3) 0.020(3) 0.006(3) -0.013(3) -0.008(3) N4 0.049(5) 0.045(4) 0.030(4) 0.016(3) -0.024(3) -0.017(4) C10 0.018(3) 0.012(3) 0.020(3) 0.002(2) -0.011(3) -0.002(3) C9 0.022(4) 0.020(3) 0.017(3) 0.000(3) -0.010(3) -0.007(3) C13 0.029(4) 0.013(3) 0.023(4) 0.003(3) -0.012(3) -0.007(3) C11 0.018(3) 0.025(4) 0.016(3) -0.001(3) -0.008(3) -0.007(3) C8 0.022(4) 0.017(3) 0.025(4) -0.002(3) -0.010(3) -0.004(3) C2 0.039(5) 0.021(4) 0.033(4) 0.004(3) -0.024(4) -0.006(3) C5 0.027(4) 0.023(4) 0.025(4) -0.002(3) -0.013(3) -0.010(3) C4 0.038(5) 0.028(4) 0.020(4) 0.000(3) -0.009(3) -0.006(3) C7 0.047(5) 0.028(4) 0.034(4) 0.004(3) -0.027(4) -0.011(4) C3 0.051(5) 0.051(5) 0.016(4) 0.009(3) -0.014(4) -0.018(4) C6 0.044(5) 0.022(4) 0.022(4) 0.002(3) -0.023(4) -0.005(3) O1W 0.061(10) 0.035(7) 0.088(12) 0.003(7) -0.018(9) 0.006(7) 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' Cu Cu 0.3201 1.2651 '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 O14 Mo1 O15 70.73(16) 2_657 2_657 ? O14 Mo1 O1 77.42(17) 2_657 1_545 ? O14 Mo1 H1 77(10) 2_657 1_545 ? O7 Mo1 O14 91.22(18) . 2_657 ? O7 Mo1 O15 77.60(17) . 2_657 ? O7 Mo1 O1 160.97(19) . 1_545 ? O7 Mo1 H1 165(10) . 1_545 ? O15 Mo1 H1 91(10) 2_657 1_545 ? O4 Mo1 O14 154.57(19) . 2_657 ? O4 Mo1 O7 99.5(2) . . ? O4 Mo1 O15 89.02(19) . 2_657 ? O4 Mo1 O1 85.58(19) . 1_545 ? O4 Mo1 H1 89(10) . 1_545 ? O1 Mo1 O15 84.20(17) 1_545 2_657 ? O1 Mo1 H1 7(10) 1_545 1_545 ? O5 Mo1 O14 95.5(2) . 2_657 ? O5 Mo1 O7 100.96(19) . . ? O5 Mo1 O15 166.00(18) . 2_657 ? O5 Mo1 O4 104.9(2) . . ? O5 Mo1 O1 95.3(2) . 1_545 ? O5 Mo1 H1 89(10) . 1_545 ? O14 Mo4 O11 81.67(15) . 2_657 ? O11 Mo4 O14 73.43(17) . . ? O11 Mo4 O11 76.97(17) . 2_657 ? O15 Mo4 O14 74.18(16) . . ? O15 Mo4 O11 74.25(16) . 2_657 ? O15 Mo4 O11 139.11(18) . . ? O9 Mo4 O14 158.22(18) . . ? O9 Mo4 O11 100.13(19) . . ? O9 Mo4 O11 76.58(17) . 2_657 ? O9 Mo4 O15 100.73(19) . . ? O10 Mo4 O14 98.4(2) . . ? O10 Mo4 O11 178.73(18) . 2_657 ? O10 Mo4 O11 104.3(2) . . ? O10 Mo4 O15 104.5(2) . . ? O10 Mo4 O9 103.4(2) . . ? O11 Mo2 O15 71.90(15) . 2_657 ? O12 Mo2 O11 72.76(16) . . ? O12 Mo2 O7 149.82(18) . . ? O12 Mo2 O15 82.93(17) . 2_657 ? O7 Mo2 O11 83.03(16) . . ? O7 Mo2 O15 72.42(16) . 2_657 ? O8 Mo2 O11 93.6(2) . . ? O8 Mo2 O12 102.8(2) . . ? O8 Mo2 O7 96.4(2) . . ? O8 Mo2 O15 162.38(19) . 2_657 ? O8 Mo2 O6 105.0(2) . . ? O6 Mo2 O11 161.0(2) . . ? O6 Mo2 O12 99.0(2) . . ? O6 Mo2 O7 98.3(2) . . ? O6 Mo2 O15 90.34(19) . 2_657 ? O14 Mo3 O11 72.33(17) . . ? O14 Mo3 O12 144.12(19) . . ? O14 Mo3 O9 80.59(16) . 2_657 ? O11 Mo3 O9 70.71(15) . 2_657 ? O12 Mo3 O11 73.10(16) . . ? O12 Mo3 O9 79.29(17) . 2_657 ? O16 Mo3 O14 106.9(2) . . ? O16 Mo3 O11 153.2(2) . . ? O16 Mo3 O12 99.6(2) . . ? O16 Mo3 O9 82.6(2) . 2_657 ? O13 Mo3 O14 97.9(2) . . ? O13 Mo3 O11 101.6(2) . . ? O13 Mo3 O12 98.1(2) . . ? O13 Mo3 O9 172.3(2) . 2_657 ? O13 Mo3 O16 105.0(2) . . ? O4 Cu05 O5 88.59(18) . 2_756 ? O4 Cu05 O2 82.26(17) . 1_545 ? O5 Cu05 O2 87.22(18) 2_756 1_545 ? O3 Cu05 O4 168.70(18) . . ? O3 Cu05 O5 87.42(18) . 2_756 ? O3 Cu05 O2 86.99(18) . 1_545 ? O3 Cu05 O17 95.04(19) . . ? O3 Cu05 N2 104.8(2) . . ? O17 Cu05 O4 88.77(19) . . ? O17 Cu05 O5 177.25(19) . 2_756 ? O17 Cu05 O2 91.7(2) . 1_545 ? O17 Cu05 N2 89.9(2) . . ? N2 Cu05 O4 85.84(19) . . ? N2 Cu05 O5 90.6(2) . 2_756 ? N2 Cu05 O2 167.95(19) . 1_545 ? Mo1 O14 Mo4 104.95(17) 2_657 . ? Mo3 O14 Mo1 149.6(2) . 2_657 ? Mo3 O14 Mo4 105.40(18) . . ? Mo4 O11 Mo4 103.03(17) . 2_657 ? Mo4 O11 Mo2 150.3(2) . . ? Mo4 O11 Mo3 104.20(19) . . ? Mo2 O11 Mo4 98.07(15) . 2_657 ? Mo3 O11 Mo4 96.62(15) . 2_657 ? Mo3 O11 Mo2 93.71(15) . . ? Mo2 O12 Mo3 114.8(2) . . ? Mo1 O7 Mo2 114.8(2) . . ? Mo1 O15 Mo2 90.63(15) 2_657 2_657 ? Mo4 O15 Mo1 109.60(18) . 2_657 ? Mo4 O15 Mo2 114.58(19) . 2_657 ? Mo1 O4 Cu05 146.4(3) . . ? Mo4 O9 Mo3 116.0(2) . 2_657 ? Mo1 O1 H1 8.8 1_565 . ? C1 O1 Mo1 136.0(4) . 1_565 ? C1 O1 H1 138.6 . . ? Mo1 O5 Cu05 171.7(3) . 2_756 ? C1 O2 Cu05 134.9(4) . 1_565 ? Cu05 O3 H3A 109.8 . . ? Cu05 O3 H3B 109.4 . . ? H3A O3 H3B 104.1 . . ? Cu05 O17 H17A 109.6 . . ? Cu05 O17 H17B 83.8 . . ? H17A O17 H17B 106.9 . . ? C5 N1 C8 122.9(6) . . ? C5 N1 C7 107.6(5) . . ? C7 N1 C8 128.1(6) . . ? C2 N3 C12 126.1(6) . . ? C2 N3 C4 108.2(6) . . ? C4 N3 C12 125.7(6) . . ? C5 N2 Cu05 115.2(5) . . ? C5 N2 C6 104.0(6) . . ? C6 N2 Cu05 133.5(5) . . ? O1 C1 C10 112.6(5) . . ? O2 C1 O1 126.8(6) . . ? O2 C1 C10 120.6(5) . . ? C13 C12 N3 119.2(6) . . ? C11 C12 N3 120.1(6) . . ? C11 C12 C13 120.6(6) . . ? C2 N4 C3 108.3(6) . . ? C9 C10 C1 119.9(6) . . ? C11 C10 C1 118.9(5) . . ? C11 C10 C9 121.2(6) . . ? C10 C9 H9 121.2 . . ? C8 C9 C10 117.6(6) . . ? C8 C9 H9 121.2 . . ? C12 C13 H13 120.7 . . ? C8 C13 C12 118.6(6) . . ? C8 C13 H13 120.7 . . ? C12 C11 H11 120.2 . . ? C10 C11 C12 119.6(6) . . ? C10 C11 H11 120.2 . . ? C9 C8 N1 121.3(6) . . ? C13 C8 N1 116.4(6) . . ? C13 C8 C9 122.3(6) . . ? N3 C2 H2 125.7 . . ? N4 C2 N3 108.7(7) . . ? N4 C2 H2 125.7 . . ? N1 C5 H5 124.1 . . ? N2 C5 N1 111.7(6) . . ? N2 C5 H5 124.1 . . ? N3 C4 H4 126.5 . . ? C3 C4 N3 107.0(7) . . ? C3 C4 H4 126.5 . . ? N1 C7 H7 127.4 . . ? C6 C7 N1 105.2(6) . . ? C6 C7 H7 127.4 . . ? N4 C3 H3 126.1 . . ? C4 C3 N4 107.8(7) . . ? C4 C3 H3 126.1 . . ? N2 C6 H6 124.3 . . ? C7 C6 N2 111.4(6) . . ? C7 C6 H6 124.3 . . ? 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 Mo1 O14 2.071(4) 2_657 ? Mo1 O7 1.847(4) . ? Mo1 O15 2.218(4) 2_657 ? Mo1 O4 1.724(4) . ? Mo1 O1 2.118(4) 1_545 ? Mo1 O5 1.724(4) . ? Mo1 H1 1.19(17) 1_545 ? Mo4 O14 2.191(4) . ? Mo4 O11 1.927(4) . ? Mo4 O11 2.478(4) 2_657 ? Mo4 O15 1.914(4) . ? Mo4 O9 1.741(5) . ? Mo4 O10 1.693(4) . ? Mo2 O11 2.252(4) . ? Mo2 O12 1.938(4) . ? Mo2 O7 1.988(4) . ? Mo2 O15 2.326(4) 2_657 ? Mo2 O8 1.692(5) . ? Mo2 O6 1.698(5) . ? Mo3 O14 1.937(4) . ? Mo3 O11 2.231(4) . ? Mo3 O12 1.946(4) . ? Mo3 O9 2.390(4) 2_657 ? Mo3 O16 1.720(5) . ? Mo3 O13 1.694(5) . ? Cu05 O4 2.110(4) . ? Cu05 O5 2.140(4) 2_756 ? Cu05 O2 2.178(4) 1_545 ? Cu05 O3 2.043(4) . ? Cu05 O17 2.072(5) . ? Cu05 N2 2.097(6) . ? O1 C1 1.286(7) . ? O1 H1 0.9449 . ? O2 C1 1.237(7) . ? O3 H3A 0.8559 . ? O3 H3B 0.8557 . ? O17 H17A 0.8537 . ? O17 H17B 0.8557 . ? N1 C8 1.445(8) . ? N1 C5 1.339(8) . ? N1 C7 1.382(9) . ? N3 C12 1.430(8) . ? N3 C2 1.336(9) . ? N3 C4 1.379(9) . ? N2 C5 1.332(8) . ? N2 C6 1.383(8) . ? C1 C10 1.502(8) . ? C12 C13 1.395(9) . ? C12 C11 1.388(9) . ? N4 C2 1.325(9) . ? N4 C3 1.373(11) . ? C10 C9 1.407(8) . ? C10 C11 1.379(8) . ? C9 H9 0.9300 . ? C9 C8 1.390(9) . ? C13 H13 0.9300 . ? C13 C8 1.382(9) . ? C11 H11 0.9300 . ? C2 H2 0.9300 . ? C5 H5 0.9300 . ? C4 H4 0.9300 . ? C4 C3 1.340(10) . ? C7 H7 0.9300 . ? C7 C6 1.342(10) . ? C3 H3 0.9300 . ? C6 H6 0.9300 . ? O1W H1WA 0.8497 . ? O1W H1WB 0.8497 . ? 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 Mo1 O1 C1 O2 13.3(11) 1_565 . . . ? Mo1 O1 C1 C10 -167.3(4) 1_565 . . . ? Cu05 O2 C1 O1 -8.8(11) 1_565 . . . ? Cu05 O2 C1 C10 171.8(4) 1_565 . . . ? Cu05 N2 C5 N1 -154.7(5) . . . . ? Cu05 N2 C6 C7 148.2(6) . . . . ? O14 Mo1 O7 Mo2 -88.9(2) 2_657 . . . ? O14 Mo1 O4 Cu05 -84.3(7) 2_657 . . . ? O14 Mo4 O9 Mo3 -5.8(6) . . . 2_657 ? O11 Mo4 O9 Mo3 -76.3(2) . . . 2_657 ? O11 Mo4 O9 Mo3 -2.43(17) 2_657 . . 2_657 ? O7 Mo1 O4 Cu05 162.0(4) . . . . ? O15 Mo1 O7 Mo2 -18.9(2) 2_657 . . . ? O15 Mo1 O4 Cu05 -120.7(5) 2_657 . . . ? O15 Mo4 O9 Mo3 68.4(2) . . . 2_657 ? O4 Mo1 O7 Mo2 68.0(3) . . . . ? O1 Mo1 O7 Mo2 -36.2(7) 1_545 . . . ? O1 Mo1 O4 Cu05 -36.4(5) 1_545 . . . ? O1 C1 C10 C9 174.3(6) . . . . ? O1 C1 C10 C11 -5.2(9) . . . . ? O5 Mo1 O7 Mo2 175.3(2) . . . . ? O5 Mo1 O4 Cu05 57.9(5) . . . . ? O2 C1 C10 C9 -6.2(10) . . . . ? O2 C1 C10 C11 174.3(6) . . . . ? O10 Mo4 O9 Mo3 176.3(2) . . . 2_657 ? N1 C7 C6 N2 -0.9(9) . . . . ? N3 C12 C13 C8 179.1(6) . . . . ? N3 C12 C11 C10 -177.2(6) . . . . ? N3 C4 C3 N4 0.1(9) . . . . ? C1 C10 C9 C8 -178.4(6) . . . . ? C1 C10 C11 C12 178.5(6) . . . . ? C12 N3 C2 N4 179.0(6) . . . . ? C12 N3 C4 C3 -178.8(6) . . . . ? C12 C13 C8 N1 178.1(6) . . . . ? C12 C13 C8 C9 -2.8(11) . . . . ? C10 C9 C8 N1 179.9(6) . . . . ? C10 C9 C8 C13 0.9(10) . . . . ? C9 C10 C11 C12 -1.0(10) . . . . ? C13 C12 C11 C10 -1.0(10) . . . . ? C11 C12 C13 C8 2.9(10) . . . . ? C11 C10 C9 C8 1.1(10) . . . . ? C8 N1 C5 N2 167.2(6) . . . . ? C8 N1 C7 C6 -166.0(7) . . . . ? C2 N3 C12 C13 43.9(10) . . . . ? C2 N3 C12 C11 -139.8(7) . . . . ? C2 N3 C4 C3 -0.4(9) . . . . ? C2 N4 C3 C4 0.3(9) . . . . ? C5 N1 C8 C9 143.7(7) . . . . ? C5 N1 C8 C13 -37.2(10) . . . . ? C5 N1 C7 C6 0.7(8) . . . . ? C5 N2 C6 C7 0.8(8) . . . . ? C4 N3 C12 C13 -138.0(7) . . . . ? C4 N3 C12 C11 38.3(10) . . . . ? C4 N3 C2 N4 0.6(8) . . . . ? C7 N1 C8 C9 -51.4(10) . . . . ? C7 N1 C8 C13 127.7(8) . . . . ? C7 N1 C5 N2 -0.3(8) . . . . ? C3 N4 C2 N3 -0.5(9) . . . . ? C6 N2 C5 N1 -0.3(8) . . . . ?