#------------------------------------------------------------------------------ #$Date: 2017-11-08 07:00:28 +0200 (Wed, 08 Nov 2017) $ #$Revision: 202941 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/47/7044700.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_7044700 loop_ _publ_author_name 'Jia, Mingjun' 'Song, Xiaojing' 'Yan, Yan' 'Wang, Yanning' 'Hu, Dianwen' 'Xiao, Lina' 'Yu, Jie-hui' 'Zhang, Wenxiang' _publ_section_title ; Hybrid compounds assembled from copper-triazole complex and polyoxometalate acid as advanced catalysts for olefins oxidation with oxygen ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C7DT03198J _journal_year 2017 _chemical_formula_sum 'C6 H12 Cu3 Mo12 N12 O40 P' _chemical_formula_weight 2265.15 _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3 :H' _symmetry_space_group_name_Hall '-R 3' _symmetry_space_group_name_H-M 'R -3 :H' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2017-11-05 deposited with the CCDC. 2017-11-07 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 6 _cell_length_a 17.6135(3) _cell_length_b 17.6135(3) _cell_length_c 23.0663(7) _cell_measurement_reflns_used 8969 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.2864 _cell_measurement_theta_min 2.2138 _cell_volume 6197.3(2) _computing_cell_refinement 'Bruker SMAR' _computing_data_collection 'Bruker SMAR' _computing_data_reduction 'Bruker SMAR' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_detector_area_resol_mean 9.00cm _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_unetI/netI 0.0209 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 15253 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.286 _diffrn_reflns_theta_min 1.600 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 5.186 _exptl_absorpt_correction_T_max 0.595 _exptl_absorpt_correction_T_min 0.515 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 6348 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.629 _refine_diff_density_min -2.315 _refine_diff_density_rms 0.259 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 3410 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.185 _refine_ls_R_factor_all 0.0290 _refine_ls_R_factor_gt 0.0267 _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^)+(0.0340P)^2^+30.9039P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0704 _refine_ls_wR_factor_ref 0.0714 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3193 _reflns_number_total 3410 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt03198j2.cif _cod_data_source_block 2-1 _cod_original_cell_volume 6197.3(3) _cod_database_code 7044700 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_res_file ; 2-1.res created by SHELXL-2014/7 TITL 1 in R-3 CELL 0.71073 17.6135 17.6135 23.0663 90.000 90.000 120.000 ZERR 6.00 0.0003 0.0003 0.0007 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H N O P CU MO UNIT 36 72 72 240 6 18 72 TEMP 23.000 L.S. 4 acta BOND FMAP 2 PLAN -5 WGHT 0.034000 30.903900 FVAR 0.04281 MO1 7 0.565883 0.367960 -0.010733 11.00000 0.02104 0.02397 = 0.01385 -0.00026 -0.00311 0.01394 MO2 7 0.448042 0.292749 0.113880 11.00000 0.01278 0.02088 = 0.02353 0.00290 0.00119 0.00857 MO3 7 0.542201 0.241435 0.240554 11.00000 0.01764 0.02252 = 0.01406 0.00200 0.00350 0.00668 MO4 7 0.495558 0.110612 0.105543 11.00000 0.01579 0.01391 = 0.02123 -0.00064 0.00168 0.00421 CU1 6 0.606621 0.500782 -0.157555 11.00000 0.03990 0.05033 = 0.04234 0.00561 -0.00958 0.02080 P1 5 0.666667 0.333333 0.112175 10.33333 0.01207 0.01207 = 0.01067 0.00000 0.00000 0.00604 O1 4 0.538182 0.384120 -0.077689 11.00000 0.02881 0.03409 = 0.01964 0.00099 -0.00645 0.01734 O2 4 0.571332 0.266785 -0.018662 11.00000 0.02248 0.02169 = 0.01701 -0.00260 -0.00287 0.01172 O3 4 0.459713 0.315413 0.029275 11.00000 0.01681 0.02461 = 0.02063 -0.00156 -0.00428 0.01071 O4 4 0.340505 0.255106 0.122361 11.00000 0.01545 0.02979 = 0.03651 0.00268 0.00245 0.01097 O5 4 0.451657 0.187633 0.094713 11.00000 0.02035 0.01879 = 0.02118 -0.00044 0.00004 0.00999 O6 4 0.493643 0.415855 0.121818 11.00000 0.01690 0.02171 = 0.02341 0.00073 0.00026 0.01182 O7 4 0.483619 0.282969 0.187873 11.00000 0.02106 0.02121 = 0.02013 -0.00020 0.00147 0.01086 O8 4 0.464436 0.190734 0.291546 11.00000 0.02440 0.03433 = 0.01753 0.00196 0.00489 0.00672 O9 4 0.637424 0.235530 0.270530 11.00000 0.02311 0.02136 = 0.01617 0.00412 0.00134 0.01083 O10 4 0.666667 0.333333 0.178964 10.33333 0.01601 0.01601 = 0.01307 0.00000 0.00000 0.00801 O11 4 0.517310 0.155427 0.185684 11.00000 0.02023 0.01917 = 0.01726 0.00036 0.00002 0.00921 O12 4 0.402807 0.013469 0.112950 11.00000 0.02066 0.01816 = 0.03307 0.00105 0.00344 0.00510 O13 4 0.521275 0.111485 0.026896 11.00000 0.02049 0.01974 = 0.01936 -0.00355 -0.00164 0.00831 O14 4 0.638034 0.240754 0.090023 11.00000 0.01486 0.01331 = 0.01561 -0.00027 -0.00027 0.00712 N1 3 0.522178 0.453012 -0.217133 11.00000 0.02852 0.03798 = 0.02743 0.00499 0.00541 0.01998 N2 3 0.461180 0.365512 -0.227464 11.00000 0.03480 0.03653 = 0.03458 0.00051 0.01273 0.02059 N3 3 0.443934 0.442840 -0.293516 11.00000 0.03684 0.05655 = 0.03144 -0.00649 -0.00364 0.02794 N4 3 0.553275 0.585932 -0.264663 11.00000 0.04144 0.04136 = 0.03448 0.00842 -0.00257 0.02147 AFIX 93 H4B 2 0.594606 0.618353 -0.240947 11.00000 -1.20000 H4C 2 0.540105 0.609520 -0.292652 11.00000 -1.20000 AFIX 0 C1 1 0.415735 0.361936 -0.272807 11.00000 0.03209 0.05130 = 0.03347 -0.01125 0.00471 0.02011 AFIX 43 H1B 2 0.370281 0.310733 -0.288595 11.00000 -1.20000 AFIX 0 C2 1 0.509317 0.498504 -0.257993 11.00000 0.03034 0.04556 = 0.02515 0.00267 0.00454 0.02369 HKLF 4 REM 1 in R-3 REM R1 = 0.0267 for 3193 Fo > 4sig(Fo) and 0.0290 for all 3410 data REM 223 parameters refined using 0 restraints END WGHT 0.0340 31.0013 REM Highest difference peak 1.629, deepest hole -2.315, 1-sigma level 0.259 Q1 1 0.3336 0.6985 0.1666 11.00000 0.05 1.63 Q2 1 0.3333 0.6667 0.1667 10.16667 0.05 1.57 Q3 1 0.5370 0.3097 0.1986 11.00000 0.05 0.64 Q4 1 0.6135 0.4563 -0.1674 11.00000 0.05 0.60 Q5 1 0.4207 0.4614 -0.3151 11.00000 0.05 0.57 ; _shelx_res_checksum 51969 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 Mo1 Mo 0.56588(2) 0.36796(2) -0.01073(2) 0.01843(9) Uani 1 1 d . . . Mo2 Mo 0.44804(2) 0.29275(2) 0.11388(2) 0.01899(9) Uani 1 1 d . . . Mo3 Mo 0.54220(2) 0.24143(2) 0.24055(2) 0.01957(9) Uani 1 1 d . . . Mo4 Mo 0.49556(2) 0.11061(2) 0.10554(2) 0.01840(9) Uani 1 1 d . . . Cu1 Cu 0.60662(4) 0.50078(5) -0.15755(3) 0.04497(17) Uani 1 1 d . . . P1 P 0.6667 0.3333 0.11218(6) 0.0116(3) Uani 1 3 d S T P O1 O 0.53818(19) 0.3841(2) -0.07769(12) 0.0268(6) Uani 1 1 d . . . O2 O 0.57133(18) 0.26678(17) -0.01866(11) 0.0201(5) Uani 1 1 d . . . O3 O 0.45971(16) 0.31541(18) 0.02927(11) 0.0205(5) Uani 1 1 d . . . O4 O 0.34051(18) 0.25511(19) 0.12236(13) 0.0274(6) Uani 1 1 d . . . O5 O 0.45166(17) 0.18763(17) 0.09471(11) 0.0200(5) Uani 1 1 d . . . O6 O 0.49364(17) 0.41585(17) 0.12182(11) 0.0197(5) Uani 1 1 d . . . O7 O 0.48362(17) 0.28297(17) 0.18787(11) 0.0207(5) Uani 1 1 d . . . O8 O 0.46444(19) 0.1907(2) 0.29155(12) 0.0290(6) Uani 1 1 d . . . O9 O 0.63742(17) 0.23553(17) 0.27053(11) 0.0203(5) Uani 1 1 d . . . O10 O 0.6667 0.3333 0.17896(17) 0.0150(8) Uani 1 3 d S T P O11 O 0.51731(17) 0.15543(17) 0.18568(11) 0.0192(5) Uani 1 1 d . . . O12 O 0.40281(18) 0.01347(18) 0.11295(13) 0.0260(6) Uani 1 1 d . . . O13 O 0.52127(17) 0.11149(17) 0.02690(11) 0.0206(5) Uani 1 1 d . . . O14 O 0.63803(15) 0.24075(15) 0.09002(10) 0.0146(5) Uani 1 1 d . . . N1 N 0.5222(2) 0.4530(3) -0.21713(16) 0.0298(8) Uani 1 1 d . . . N2 N 0.4612(3) 0.3655(3) -0.22746(17) 0.0341(8) Uani 1 1 d . . . N3 N 0.4439(3) 0.4428(3) -0.29352(17) 0.0396(9) Uani 1 1 d . . . N4 N 0.5533(3) 0.5859(3) -0.26466(17) 0.0388(9) Uani 1 1 d . . . H4B H 0.5946 0.6184 -0.2409 0.047 Uiso 1 1 calc R U . H4C H 0.5401 0.6095 -0.2927 0.047 Uiso 1 1 calc R U . C1 C 0.4157(3) 0.3619(4) -0.2728(2) 0.0393(11) Uani 1 1 d . . . H1B H 0.3703 0.3107 -0.2886 0.047 Uiso 1 1 calc R U . C2 C 0.5093(3) 0.4985(3) -0.25799(19) 0.0316(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.02104(16) 0.02397(17) 0.01385(15) -0.00026(11) -0.00311(11) 0.01394(13) Mo2 0.01278(15) 0.02088(16) 0.02353(17) 0.00290(12) 0.00119(11) 0.00857(12) Mo3 0.01764(15) 0.02252(17) 0.01406(15) 0.00200(11) 0.00350(11) 0.00668(13) Mo4 0.01579(15) 0.01391(15) 0.02123(16) -0.00064(11) 0.00168(11) 0.00421(12) Cu1 0.0399(3) 0.0503(4) 0.0423(4) 0.0056(3) -0.0096(3) 0.0208(3) P1 0.0121(4) 0.0121(4) 0.0107(6) 0.000 0.000 0.0060(2) O1 0.0288(15) 0.0341(16) 0.0196(13) 0.0010(11) -0.0064(11) 0.0173(13) O2 0.0225(13) 0.0217(13) 0.0170(12) -0.0026(10) -0.0029(10) 0.0117(11) O3 0.0168(12) 0.0246(13) 0.0206(13) -0.0016(10) -0.0043(10) 0.0107(11) O4 0.0155(13) 0.0298(15) 0.0365(16) 0.0027(12) 0.0025(11) 0.0110(12) O5 0.0204(13) 0.0188(12) 0.0212(13) -0.0004(10) 0.0000(10) 0.0100(11) O6 0.0169(12) 0.0217(13) 0.0234(13) 0.0007(10) 0.0003(10) 0.0118(11) O7 0.0211(13) 0.0212(13) 0.0201(12) -0.0002(10) 0.0015(10) 0.0109(11) O8 0.0244(14) 0.0343(16) 0.0175(13) 0.0020(12) 0.0049(11) 0.0067(13) O9 0.0231(13) 0.0214(13) 0.0162(12) 0.0041(10) 0.0013(10) 0.0108(11) O10 0.0160(12) 0.0160(12) 0.0131(19) 0.000 0.000 0.0080(6) O11 0.0202(13) 0.0192(12) 0.0173(12) 0.0004(10) 0.0000(10) 0.0092(11) O12 0.0207(13) 0.0182(13) 0.0331(15) 0.0010(11) 0.0034(11) 0.0051(11) O13 0.0205(13) 0.0197(13) 0.0194(12) -0.0035(10) -0.0016(10) 0.0083(11) O14 0.0149(11) 0.0133(11) 0.0156(11) -0.0003(9) -0.0003(9) 0.0071(10) N1 0.0285(18) 0.038(2) 0.0274(17) 0.0050(15) 0.0054(14) 0.0200(17) N2 0.035(2) 0.037(2) 0.035(2) 0.0005(16) 0.0127(16) 0.0206(18) N3 0.037(2) 0.057(3) 0.031(2) -0.0065(19) -0.0036(17) 0.028(2) N4 0.041(2) 0.041(2) 0.034(2) 0.0084(17) -0.0026(17) 0.0215(19) C1 0.032(2) 0.051(3) 0.033(2) -0.011(2) 0.0047(19) 0.020(2) C2 0.030(2) 0.046(3) 0.025(2) 0.0027(18) 0.0045(17) 0.024(2) 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' 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' P P 0.1023 0.0942 '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' 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 O1 Mo1 O2 103.41(13) . . O1 Mo1 O3 103.54(13) . . O2 Mo1 O3 95.36(12) . . O1 Mo1 O13 100.01(13) . 3_665 O2 Mo1 O13 155.30(11) . 3_665 O3 Mo1 O13 86.63(11) . 3_665 O1 Mo1 O2 100.16(13) . 3_665 O2 Mo1 O2 84.83(16) . 3_665 O3 Mo1 O2 155.55(11) . 3_665 O13 Mo1 O2 83.42(11) 3_665 3_665 O1 Mo1 O14 171.76(12) . 3_665 O2 Mo1 O14 84.76(10) . 3_665 O3 Mo1 O14 74.23(10) . 3_665 O13 Mo1 O14 72.06(9) 3_665 3_665 O2 Mo1 O14 81.46(9) 3_665 3_665 O4 Mo2 O7 102.90(13) . . O4 Mo2 O6 100.88(13) . . O7 Mo2 O6 92.72(11) . . O4 Mo2 O5 102.68(13) . . O7 Mo2 O5 86.97(11) . . O6 Mo2 O5 155.90(11) . . O4 Mo2 O3 100.22(13) . . O7 Mo2 O3 156.71(11) . . O6 Mo2 O3 85.60(11) . . O5 Mo2 O3 85.30(11) . . O4 Mo2 O14 171.05(12) . 3_665 O7 Mo2 O14 84.77(10) . 3_665 O6 Mo2 O14 73.85(9) . 3_665 O5 Mo2 O14 82.14(10) . 3_665 O3 Mo2 O14 72.44(9) . 3_665 O8 Mo3 O11 104.28(13) . . O8 Mo3 O9 103.14(13) . . O11 Mo3 O9 93.41(12) . . O8 Mo3 O7 101.00(13) . . O11 Mo3 O7 85.87(11) . . O9 Mo3 O7 155.24(11) . . O8 Mo3 O9 99.35(13) . 3_665 O11 Mo3 O9 155.51(11) . 3_665 O9 Mo3 O9 87.36(16) . 3_665 O7 Mo3 O9 83.38(11) . 3_665 O8 Mo3 O10 170.53(12) . . O11 Mo3 O10 84.89(10) . . O9 Mo3 O10 73.54(10) . . O7 Mo3 O10 81.75(9) . . O9 Mo3 O10 71.84(9) 3_665 . O12 Mo4 O13 102.42(13) . . O12 Mo4 O5 101.91(13) . . O13 Mo4 O5 92.89(11) . . O12 Mo4 O6 101.11(13) . 2_655 O13 Mo4 O6 87.87(11) . 2_655 O5 Mo4 O6 156.23(11) . 2_655 O12 Mo4 O11 101.98(13) . . O13 Mo4 O11 155.47(11) . . O5 Mo4 O11 84.47(11) . . O6 Mo4 O11 85.08(11) 2_655 . O12 Mo4 O14 172.78(11) . . O13 Mo4 O14 73.62(10) . . O5 Mo4 O14 84.46(10) . . O6 Mo4 O14 72.96(9) 2_655 . O11 Mo4 O14 81.86(9) . . N1 Cu1 N2 168.07(16) . 17_554 O14 P1 O14 109.48(10) 2_655 3_665 O14 P1 O14 109.48(10) 2_655 . O14 P1 O14 109.48(10) 3_665 . O14 P1 O10 109.46(10) 2_655 . O14 P1 O10 109.46(10) 3_665 . O14 P1 O10 109.46(10) . . Mo1 O2 Mo1 152.44(15) . 2_655 Mo1 O3 Mo2 124.39(13) . . Mo4 O5 Mo2 151.67(15) . . Mo2 O6 Mo4 124.08(13) . 3_665 Mo2 O7 Mo3 150.61(15) . . Mo3 O9 Mo3 125.32(13) . 2_655 P1 O10 Mo3 125.81(8) . . P1 O10 Mo3 125.81(8) . 2_655 Mo3 O10 Mo3 89.23(11) . 2_655 P1 O10 Mo3 125.81(8) . 3_665 Mo3 O10 Mo3 89.23(11) . 3_665 Mo3 O10 Mo3 89.23(11) 2_655 3_665 Mo3 O11 Mo4 152.66(15) . . Mo4 O13 Mo1 125.08(13) . 2_655 P1 O14 Mo2 125.72(13) . 2_655 P1 O14 Mo1 126.09(14) . 2_655 Mo2 O14 Mo1 88.94(8) 2_655 2_655 P1 O14 Mo4 126.03(13) . . Mo2 O14 Mo4 89.07(8) 2_655 . Mo1 O14 Mo4 89.08(8) 2_655 . C2 N1 N2 106.1(4) . . C2 N1 Cu1 125.6(3) . . N2 N1 Cu1 128.3(3) . . C1 N2 N1 107.9(4) . . C1 N2 Cu1 127.5(4) . 18_544 N1 N2 Cu1 123.9(3) . 18_544 C1 N3 C2 106.5(4) . . N2 C1 N3 110.1(5) . . N1 C2 N4 126.8(4) . . N1 C2 N3 109.4(4) . . N4 C2 N3 123.8(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Mo1 O1 1.686(3) . Mo1 O2 1.841(3) . Mo1 O3 1.864(3) . Mo1 O13 1.977(3) 3_665 Mo1 O2 1.986(3) 3_665 Mo1 O14 2.429(2) 3_665 Mo2 O4 1.676(3) . Mo2 O7 1.856(3) . Mo2 O6 1.908(3) . Mo2 O5 1.935(3) . Mo2 O3 1.982(3) . Mo2 O14 2.427(2) 3_665 Mo3 O8 1.683(3) . Mo3 O11 1.851(3) . Mo3 O9 1.865(3) . Mo3 O7 1.957(3) . Mo3 O9 1.975(3) 3_665 Mo3 O10 2.428(2) . Mo4 O12 1.682(3) . Mo4 O13 1.868(3) . Mo4 O5 1.884(3) . Mo4 O6 1.952(3) 2_655 Mo4 O11 1.971(3) . Mo4 O14 2.435(2) . Cu1 N1 1.886(4) . Cu1 N2 1.892(4) 17_554 P1 O14 1.534(2) 2_655 P1 O14 1.534(2) 3_665 P1 O14 1.534(2) . P1 O10 1.541(4) . O2 Mo1 1.986(3) 2_655 O6 Mo4 1.952(3) 3_665 O9 Mo3 1.975(3) 2_655 O10 Mo3 2.428(2) 2_655 O10 Mo3 2.428(2) 3_665 O13 Mo1 1.977(3) 2_655 O14 Mo2 2.427(2) 2_655 O14 Mo1 2.429(2) 2_655 N1 C2 1.328(6) . N1 N2 1.389(5) . N2 C1 1.299(6) . N2 Cu1 1.892(4) 18_544 N3 C1 1.341(7) . N3 C2 1.353(6) . N4 C2 1.342(6) .