# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H8 Mo5 O21 P2, 2(C10 H11 N3), H2 O' _chemical_formula_sum 'C28 H32 Mo5 N6 O22 P2' _chemical_formula_weight 1346.23 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' 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' Mo Mo -1.6832 0.6857 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4959(7) _cell_length_b 19.4686(12) _cell_length_c 18.3104(11) _cell_angle_alpha 90 _cell_angle_beta 105.4640(10) _cell_angle_gamma 90 _cell_volume 3949.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5860 _cell_measurement_theta_min 2.0580 _cell_measurement_theta_max 32.0508 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_density_meas 2.25(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.264 _exptl_crystal_F_000 2632 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.585 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.186 _exptl_absorpt_coefficient_mu 1.721 _shelx_estimated_absorpt_T_min 0.433 _shelx_estimated_absorpt_T_max 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 0.74 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29843 _diffrn_reflns_av_unetI/netI 0.0103 _diffrn_reflns_av_R_equivalents 0.0123 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.557 _diffrn_reflns_theta_max 25.682 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 7495 _reflns_number_gt 7165 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+8.8933P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7495 _refine_ls_number_parameters 598 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0165 _refine_ls_R_factor_gt 0.0154 _refine_ls_wR_factor_ref 0.0401 _refine_ls_wR_factor_gt 0.0394 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.60957(2) 0.67461(2) 0.34370(2) 0.00997(4) Uani 1 1 d . . . . . Mo2 Mo 0.64208(2) 0.82537(2) 0.43846(2) 0.00893(4) Uani 1 1 d . . . . . Mo3 Mo 0.96519(2) 0.86512(2) 0.48018(2) 0.00901(4) Uani 1 1 d . . . . . Mo4 Mo 1.10245(2) 0.71388(2) 0.47612(2) 0.01001(4) Uani 1 1 d . . . . . Mo5 Mo 0.88814(2) 0.60093(2) 0.38125(2) 0.01049(4) Uani 1 1 d . . . . . P1 P 0.83474(4) 0.70650(3) 0.51705(3) 0.00882(10) Uani 1 1 d . . . . . P2 P 0.84865(4) 0.77302(3) 0.32856(3) 0.00912(10) Uani 1 1 d . . . . . O1 O 0.54275(13) 0.60336(8) 0.36913(9) 0.0168(3) Uani 1 1 d . . . . . O2 O 0.52195(13) 0.69634(8) 0.25593(8) 0.0172(3) Uani 1 1 d . . . . . O3 O 0.55743(12) 0.73885(7) 0.40812(8) 0.0120(3) Uani 1 1 d . . . . . O4 O 0.73120(12) 0.76371(7) 0.35408(8) 0.0099(3) Uani 1 1 d . . . . . O5 O 0.73829(12) 0.63075(7) 0.31114(8) 0.0119(3) Uani 1 1 d . . . . . O6 O 0.78137(12) 0.65473(7) 0.45308(8) 0.0105(3) Uani 1 1 d . . . . . O7 O 0.73765(12) 0.75280(7) 0.53090(8) 0.0107(3) Uani 1 1 d . . . . . O8 O 0.56713(12) 0.85447(7) 0.50233(8) 0.0133(3) Uani 1 1 d . . . . . O9 O 0.57575(13) 0.87331(7) 0.36019(8) 0.0137(3) Uani 1 1 d . . . . . O10 O 0.79251(12) 0.86962(7) 0.46651(8) 0.0108(3) Uani 1 1 d . . . . . O11 O 1.00722(13) 0.87143(8) 0.57679(8) 0.0147(3) Uani 1 1 d . . . . . O12 O 1.00007(13) 0.94363(8) 0.45147(8) 0.0146(3) Uani 1 1 d . . . . . O13 O 0.90586(12) 0.84077(7) 0.35816(8) 0.0109(3) Uani 1 1 d . . . . . O14 O 0.93493(12) 0.74982(7) 0.49697(8) 0.0102(3) Uani 1 1 d . . . . . O15 O 1.10185(12) 0.81218(7) 0.46379(8) 0.0110(3) Uani 1 1 d . . . . . O16 O 1.17570(13) 0.70690(8) 0.56938(8) 0.0153(3) Uani 1 1 d . . . . . O17 O 1.21059(13) 0.69891(8) 0.42857(9) 0.0172(3) Uani 1 1 d . . . . . O18 O 1.02074(12) 0.62625(7) 0.46217(8) 0.0121(3) Uani 1 1 d . . . . . O19 O 0.93637(12) 0.71270(7) 0.35500(8) 0.0114(3) Uani 1 1 d . . . . . O20 O 0.95343(13) 0.57468(8) 0.31174(8) 0.0158(3) Uani 1 1 d . . . . . O21 O 0.84375(13) 0.52470(8) 0.41231(8) 0.0160(3) Uani 1 1 d . . . . . O90 O 0.1354(2) 0.84473(13) 0.78029(12) 0.0440(5) Uani 1 1 d D . . . . H90A H 0.069(2) 0.8638(18) 0.784(2) 0.053 Uiso 1 1 d D U . . . H90B H 0.174(3) 0.8801(15) 0.8103(18) 0.053 Uiso 1 1 d D U . . . N1 N 0.17093(16) 0.65397(10) 0.83799(10) 0.0147(4) Uani 1 1 d D . . . . N2 N 0.29731(16) 0.58754(9) 0.65910(10) 0.0129(3) Uani 1 1 d D . . . . N3 N 0.50990(17) 0.66055(11) 0.52712(11) 0.0196(4) Uani 1 1 d D . . . . N4 N 0.23395(17) 0.89869(10) 0.67951(10) 0.0177(4) Uani 1 1 d D . . . . N5 N 0.35751(16) 0.93131(9) 0.49125(10) 0.0134(4) Uani 1 1 d D . . . . N6 N 0.28538(16) 1.07672(9) 0.32250(10) 0.0144(4) Uani 1 1 d D . . . . C1 C 0.91177(18) 0.66165(11) 0.60232(11) 0.0126(4) Uani 1 1 d . . . . . H1A H 0.9702 0.6291 0.5902 0.015 Uiso 1 1 calc R U . . . H1B H 0.9581 0.6953 0.6393 0.015 Uiso 1 1 calc R U . . . C2 C 0.82881(18) 0.62250(11) 0.63861(11) 0.0133(4) Uani 1 1 d . . . . . C3 C 0.8003(2) 0.55493(12) 0.61434(12) 0.0205(5) Uani 1 1 d . . . . . H3 H 0.8369 0.5353 0.5784 0.025 Uiso 1 1 calc R U . . . C4 C 0.7203(2) 0.51619(12) 0.64149(13) 0.0246(5) Uani 1 1 d . . . . . H4 H 0.7026 0.4702 0.6249 0.030 Uiso 1 1 calc R U . . . C5 C 0.77801(18) 0.65113(11) 0.69348(11) 0.0123(4) Uani 1 1 d . . . . . C6 C 0.69587(19) 0.61125(12) 0.71946(12) 0.0169(4) Uani 1 1 d . . . . . H6 H 0.6597 0.6301 0.7560 0.020 Uiso 1 1 calc R U . . . C7 C 0.6660(2) 0.54523(12) 0.69334(12) 0.0213(5) Uani 1 1 d . . . . . H7 H 0.6083 0.5197 0.7109 0.026 Uiso 1 1 calc R U . . . C8 C 0.80858(19) 0.77710(11) 0.22547(11) 0.0142(4) Uani 1 1 d . . . . . H8A H 0.8768 0.7591 0.2077 0.017 Uiso 1 1 calc R U . . . H8B H 0.7383 0.7468 0.2050 0.017 Uiso 1 1 calc R U . . . C9 C 0.11041(19) 0.60605(11) 0.78948(12) 0.0145(4) Uani 1 1 d . . . . . H9 H 0.0380 0.5871 0.7965 0.017 Uiso 1 1 calc R U . . . C10 C 0.15270(18) 0.58451(11) 0.73012(12) 0.0133(4) Uani 1 1 d . . . . . H10 H 0.1101 0.5503 0.6964 0.016 Uiso 1 1 calc R U . . . C11 C 0.27405(19) 0.68116(11) 0.83008(12) 0.0162(4) Uani 1 1 d . . . . . H11 H 0.3154 0.7144 0.8656 0.019 Uiso 1 1 calc R U . . . C12 C 0.25935(18) 0.61302(11) 0.71902(11) 0.0122(4) Uani 1 1 d . . . . . C13 C 0.32102(19) 0.66196(11) 0.77166(12) 0.0141(4) Uani 1 1 d . . . . . H13 H 0.3943 0.6815 0.7669 0.017 Uiso 1 1 calc R U . . . C14 C 0.37309(18) 0.61452(11) 0.61944(12) 0.0130(4) Uani 1 1 d . . . . . C15 C 0.3876(2) 0.57456(12) 0.55839(12) 0.0185(4) Uani 1 1 d . . . . . H15 H 0.3502 0.5308 0.5486 0.022 Uiso 1 1 calc R U . . . C16 C 0.43322(19) 0.67769(11) 0.63308(12) 0.0149(4) Uani 1 1 d . . . . . H16 H 0.4275 0.7054 0.6747 0.018 Uiso 1 1 calc R U . . . C17 C 0.4559(2) 0.59913(13) 0.51317(13) 0.0222(5) Uani 1 1 d . . . . . H17 H 0.4650 0.5724 0.4716 0.027 Uiso 1 1 calc R U . . . C18 C 0.50060(19) 0.69907(12) 0.58563(12) 0.0170(4) Uani 1 1 d . . . . . H18 H 0.5413 0.7420 0.5946 0.020 Uiso 1 1 calc R U . . . C19 C 0.28432(19) 0.84742(12) 0.65036(12) 0.0173(4) Uani 1 1 d . . . . . H19 H 0.2919 0.8033 0.6734 0.021 Uiso 1 1 calc R U . . . C20 C 0.21965(19) 0.96125(12) 0.64817(12) 0.0163(4) Uani 1 1 d . . . . . H20 H 0.1816 0.9963 0.6696 0.020 Uiso 1 1 calc R U . . . C21 C 0.32503(19) 0.85788(11) 0.58765(12) 0.0153(4) Uani 1 1 d . . . . . H21 H 0.3616 0.8215 0.5673 0.018 Uiso 1 1 calc R U . . . C22 C 0.25921(18) 0.97553(11) 0.58553(11) 0.0131(4) Uani 1 1 d . . . . . H22 H 0.2508 1.0203 0.5641 0.016 Uiso 1 1 calc R U . . . C23 C 0.31226(17) 0.92277(11) 0.55379(11) 0.0123(4) Uani 1 1 d . . . . . C24 C 0.32989(18) 0.98099(10) 0.43639(11) 0.0116(4) Uani 1 1 d . . . . . C25 C 0.22412(18) 1.02037(10) 0.42003(11) 0.0116(4) Uani 1 1 d . . . . . H25 H 0.1661 1.0139 0.4479 0.014 Uiso 1 1 calc R U . . . C26 C 0.41063(18) 0.99002(11) 0.39126(12) 0.0139(4) Uani 1 1 d . . . . . H26 H 0.4819 0.9630 0.4000 0.017 Uiso 1 1 calc R U . . . C27 C 0.20538(18) 1.06824(11) 0.36350(11) 0.0135(4) Uani 1 1 d . . . . . H27 H 0.1348 1.0959 0.3531 0.016 Uiso 1 1 calc R U . . . C28 C 0.38539(19) 1.03791(11) 0.33491(12) 0.0154(4) Uani 1 1 d . . . . . H28 H 0.4392 1.0439 0.3040 0.018 Uiso 1 1 calc R U . . . H2' H 0.255(2) 0.5535(11) 0.6377(14) 0.018(6) Uiso 1 1 d D . . . . H6' H 0.269(2) 1.1029(12) 0.2824(12) 0.023(7) Uiso 1 1 d D . . . . H1' H 0.145(2) 0.6685(14) 0.8754(13) 0.028(7) Uiso 1 1 d D . . . . H5' H 0.418(2) 0.9059(13) 0.4913(16) 0.027(7) Uiso 1 1 d D . . . . H4' H 0.206(2) 0.8900(15) 0.7176(13) 0.031(8) Uiso 1 1 d D . . . . H3' H 0.544(2) 0.6784(14) 0.4952(14) 0.026(7) Uiso 1 1 d 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 0.00964(8) 0.01110(9) 0.00978(8) -0.00202(6) 0.00365(6) -0.00216(6) Mo2 0.00743(8) 0.00936(8) 0.01063(8) -0.00080(6) 0.00351(6) 0.00032(6) Mo3 0.00785(8) 0.00928(8) 0.01038(8) -0.00175(6) 0.00324(6) -0.00085(6) Mo4 0.00837(8) 0.01080(9) 0.01146(8) 0.00015(6) 0.00369(6) 0.00100(6) Mo5 0.01236(8) 0.00898(9) 0.01100(8) -0.00158(6) 0.00462(6) -0.00007(6) P1 0.0096(2) 0.0095(2) 0.0080(2) -0.00005(19) 0.00341(18) -0.00013(19) P2 0.0094(2) 0.0103(2) 0.0086(2) 0.00027(19) 0.00391(18) -0.00046(19) O1 0.0180(8) 0.0151(8) 0.0200(8) -0.0039(6) 0.0100(6) -0.0054(6) O2 0.0142(7) 0.0225(8) 0.0133(7) -0.0018(6) 0.0011(6) -0.0014(6) O3 0.0093(7) 0.0139(7) 0.0136(7) -0.0021(6) 0.0045(5) -0.0014(5) O4 0.0099(6) 0.0102(7) 0.0104(7) -0.0006(5) 0.0042(5) -0.0004(5) O5 0.0133(7) 0.0129(7) 0.0103(7) -0.0031(6) 0.0043(5) -0.0004(6) O6 0.0120(7) 0.0101(7) 0.0103(7) -0.0005(5) 0.0045(5) -0.0007(5) O7 0.0112(7) 0.0115(7) 0.0104(7) -0.0003(5) 0.0048(5) 0.0001(5) O8 0.0113(7) 0.0144(7) 0.0152(7) -0.0019(6) 0.0055(6) 0.0006(6) O9 0.0121(7) 0.0145(7) 0.0149(7) 0.0006(6) 0.0044(6) 0.0028(6) O10 0.0096(7) 0.0098(7) 0.0133(7) -0.0021(5) 0.0038(5) -0.0005(5) O11 0.0128(7) 0.0177(8) 0.0136(7) -0.0037(6) 0.0036(6) -0.0010(6) O12 0.0137(7) 0.0124(7) 0.0182(7) -0.0017(6) 0.0053(6) -0.0021(6) O13 0.0109(7) 0.0111(7) 0.0113(7) 0.0000(5) 0.0039(5) -0.0010(5) O14 0.0095(6) 0.0108(7) 0.0113(7) -0.0005(5) 0.0041(5) 0.0001(5) O15 0.0091(7) 0.0116(7) 0.0128(7) -0.0007(6) 0.0039(5) -0.0003(5) O16 0.0129(7) 0.0155(8) 0.0163(7) 0.0019(6) 0.0015(6) 0.0010(6) O17 0.0157(7) 0.0162(8) 0.0228(8) -0.0007(6) 0.0105(6) 0.0014(6) O18 0.0130(7) 0.0102(7) 0.0134(7) 0.0004(6) 0.0038(6) 0.0021(5) O19 0.0118(7) 0.0117(7) 0.0117(7) 0.0000(6) 0.0049(5) 0.0000(5) O20 0.0171(7) 0.0147(7) 0.0170(7) -0.0028(6) 0.0069(6) 0.0006(6) O21 0.0191(8) 0.0127(7) 0.0167(7) -0.0010(6) 0.0055(6) -0.0010(6) O90 0.0427(12) 0.0583(15) 0.0411(12) 0.0191(10) 0.0291(10) 0.0165(11) N1 0.0177(9) 0.0154(9) 0.0132(9) 0.0006(7) 0.0081(7) 0.0038(7) N2 0.0150(9) 0.0115(9) 0.0140(9) -0.0015(7) 0.0070(7) -0.0016(7) N3 0.0184(9) 0.0255(10) 0.0185(10) 0.0033(8) 0.0112(8) -0.0016(8) N4 0.0165(9) 0.0246(10) 0.0126(9) 0.0050(8) 0.0050(7) 0.0003(8) N5 0.0140(9) 0.0126(9) 0.0143(9) 0.0020(7) 0.0051(7) 0.0046(7) N6 0.0178(9) 0.0148(9) 0.0108(8) 0.0030(7) 0.0040(7) 0.0002(7) C1 0.0134(10) 0.0155(10) 0.0093(9) 0.0010(8) 0.0036(8) 0.0035(8) C2 0.0142(10) 0.0161(11) 0.0082(9) 0.0031(8) 0.0008(8) 0.0024(8) C3 0.0294(12) 0.0180(11) 0.0141(10) -0.0019(9) 0.0058(9) 0.0007(9) C4 0.0359(14) 0.0174(12) 0.0173(11) -0.0012(9) 0.0014(10) -0.0081(10) C5 0.0127(10) 0.0144(10) 0.0084(9) 0.0009(8) 0.0003(7) 0.0006(8) C6 0.0159(10) 0.0236(12) 0.0105(10) 0.0027(9) 0.0024(8) 0.0003(9) C7 0.0215(11) 0.0248(12) 0.0149(11) 0.0045(9) 0.0003(9) -0.0092(10) C8 0.0194(10) 0.0149(10) 0.0094(9) -0.0003(8) 0.0058(8) -0.0009(8) C9 0.0146(10) 0.0129(10) 0.0174(10) 0.0037(8) 0.0068(8) 0.0019(8) C10 0.0148(10) 0.0118(10) 0.0138(10) 0.0011(8) 0.0047(8) 0.0002(8) C11 0.0175(10) 0.0157(11) 0.0142(10) -0.0006(8) 0.0024(8) 0.0007(8) C12 0.0133(10) 0.0115(10) 0.0122(10) 0.0040(8) 0.0040(8) 0.0043(8) C13 0.0128(10) 0.0148(10) 0.0147(10) 0.0015(8) 0.0036(8) 0.0000(8) C14 0.0102(9) 0.0157(10) 0.0135(10) 0.0037(8) 0.0040(8) 0.0029(8) C15 0.0205(11) 0.0182(11) 0.0188(11) -0.0026(9) 0.0087(9) -0.0030(9) C16 0.0148(10) 0.0150(10) 0.0161(10) 0.0002(8) 0.0060(8) 0.0024(8) C17 0.0246(12) 0.0268(13) 0.0190(11) -0.0039(10) 0.0121(9) -0.0034(10) C18 0.0132(10) 0.0161(11) 0.0216(11) 0.0037(9) 0.0045(8) 0.0008(8) C19 0.0147(10) 0.0172(11) 0.0182(11) 0.0068(9) 0.0011(8) 0.0001(8) C20 0.0157(10) 0.0196(11) 0.0129(10) -0.0003(8) 0.0026(8) 0.0019(9) C21 0.0137(10) 0.0133(10) 0.0174(10) 0.0016(8) 0.0017(8) 0.0012(8) C22 0.0132(10) 0.0121(10) 0.0126(10) 0.0010(8) 0.0012(8) -0.0004(8) C23 0.0087(9) 0.0153(10) 0.0113(10) 0.0014(8) 0.0000(7) -0.0020(8) C24 0.0142(10) 0.0100(10) 0.0094(9) -0.0028(8) 0.0012(8) -0.0019(8) C25 0.0116(9) 0.0138(10) 0.0095(9) -0.0023(8) 0.0031(7) -0.0017(8) C26 0.0117(10) 0.0149(10) 0.0154(10) -0.0016(8) 0.0039(8) 0.0021(8) C27 0.0132(10) 0.0141(10) 0.0130(10) -0.0013(8) 0.0033(8) 0.0014(8) C28 0.0165(10) 0.0170(11) 0.0145(10) -0.0018(8) 0.0075(8) -0.0021(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.7067(15) . ? Mo1 O1 1.7094(15) . ? Mo1 O3 1.9214(14) . ? Mo1 O5 1.9352(14) . ? Mo1 O4 2.2041(14) . ? Mo1 O6 2.4397(14) . ? Mo2 O9 1.7099(14) . ? Mo2 O8 1.7229(14) . ? Mo2 O10 1.8770(14) . ? Mo2 O3 1.9504(14) . ? Mo2 O7 2.2531(14) . ? Mo2 O4 2.3921(13) . ? Mo3 O12 1.6989(15) . ? Mo3 O11 1.7093(14) . ? Mo3 O10 1.9354(14) . ? Mo3 O15 1.9677(14) . ? Mo3 O13 2.2066(14) . ? Mo3 O14 2.3046(14) . ? Mo4 O16 1.6961(15) . ? Mo4 O17 1.7221(14) . ? Mo4 O15 1.9269(14) . ? Mo4 O18 1.9313(14) . ? Mo4 O14 2.1763(13) . ? Mo4 O19 2.5113(14) . ? Mo5 O21 1.7149(15) . ? Mo5 O20 1.7186(14) . ? Mo5 O18 1.8862(14) . ? Mo5 O5 1.9426(14) . ? Mo5 O6 2.2792(13) . ? Mo5 O19 2.3273(14) . ? P1 O7 1.5078(14) . ? P1 O6 1.5430(14) . ? P1 O14 1.5488(14) . ? P1 C1 1.802(2) . ? P2 O13 1.5087(15) . ? P2 O19 1.5394(15) . ? P2 O4 1.5526(14) . ? P2 C8 1.821(2) . ? O90 H90A 0.870(18) . ? O90 H90B 0.919(18) . ? N1 C11 1.341(3) . ? N1 C9 1.347(3) . ? N1 H1' 0.863(17) . ? N2 C12 1.377(3) . ? N2 C14 1.378(3) . ? N2 H2' 0.851(17) . ? N3 C18 1.335(3) . ? N3 C17 1.340(3) . ? N3 H3' 0.859(17) . ? N4 C19 1.335(3) . ? N4 C20 1.338(3) . ? N4 H4' 0.859(17) . ? N5 C24 1.369(3) . ? N5 C23 1.388(3) . ? N5 H5' 0.851(17) . ? N6 C28 1.344(3) . ? N6 C27 1.343(3) . ? N6 H6' 0.872(17) . ? C1 C2 1.507(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.399(3) . ? C2 C5 1.405(3) . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C7 1.388(3) . ? C4 H4 0.9500 . ? C5 C6 1.400(3) . ? C5 C8 1.520(3) 4_576 ? C6 C7 1.383(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C5 1.520(3) 4_575 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.370(3) . ? C9 H9 0.9500 . ? C10 C12 1.409(3) . ? C10 H10 0.9500 . ? C11 C13 1.372(3) . ? C11 H11 0.9500 . ? C12 C13 1.405(3) . ? C13 H13 0.9500 . ? C14 C16 1.400(3) . ? C14 C15 1.408(3) . ? C15 C17 1.370(3) . ? C15 H15 0.9500 . ? C16 C18 1.374(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.366(3) . ? C19 H19 0.9500 . ? C20 C22 1.370(3) . ? C20 H20 0.9500 . ? C21 C23 1.398(3) . ? C21 H21 0.9500 . ? C22 C23 1.398(3) . ? C22 H22 0.9500 . ? C24 C25 1.401(3) . ? C24 C26 1.409(3) . ? C25 C27 1.367(3) . ? C25 H25 0.9500 . ? C26 C28 1.363(3) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 105.21(7) . . ? O2 Mo1 O3 102.38(7) . . ? O1 Mo1 O3 97.16(6) . . ? O2 Mo1 O5 97.30(7) . . ? O1 Mo1 O5 99.32(7) . . ? O3 Mo1 O5 149.96(6) . . ? O2 Mo1 O4 95.03(6) . . ? O1 Mo1 O4 159.38(6) . . ? O3 Mo1 O4 74.30(5) . . ? O5 Mo1 O4 81.62(5) . . ? O2 Mo1 O6 163.26(6) . . ? O1 Mo1 O6 88.39(6) . . ? O3 Mo1 O6 85.18(5) . . ? O5 Mo1 O6 70.42(5) . . ? O4 Mo1 O6 72.42(5) . . ? O9 Mo2 O8 101.39(7) . . ? O9 Mo2 O10 98.69(7) . . ? O8 Mo2 O10 104.74(6) . . ? O9 Mo2 O3 98.95(7) . . ? O8 Mo2 O3 100.11(6) . . ? O10 Mo2 O3 145.85(6) . . ? O9 Mo2 O7 172.34(6) . . ? O8 Mo2 O7 85.89(6) . . ? O10 Mo2 O7 81.55(6) . . ? O3 Mo2 O7 77.22(6) . . ? O9 Mo2 O4 84.53(6) . . ? O8 Mo2 O4 168.90(6) . . ? O10 Mo2 O4 83.40(5) . . ? O3 Mo2 O4 69.50(5) . . ? O7 Mo2 O4 87.91(5) . . ? O12 Mo3 O11 103.33(7) . . ? O12 Mo3 O10 103.75(6) . . ? O11 Mo3 O10 97.34(6) . . ? O12 Mo3 O15 99.22(6) . . ? O11 Mo3 O15 100.29(6) . . ? O10 Mo3 O15 146.83(6) . . ? O12 Mo3 O13 85.10(6) . . ? O11 Mo3 O13 171.51(6) . . ? O10 Mo3 O13 81.33(5) . . ? O15 Mo3 O13 77.11(5) . . ? O12 Mo3 O14 166.94(6) . . ? O11 Mo3 O14 86.74(6) . . ? O10 Mo3 O14 82.84(5) . . ? O15 Mo3 O14 70.44(5) . . ? O13 Mo3 O14 84.78(5) . . ? O16 Mo4 O17 105.31(7) . . ? O16 Mo4 O15 100.54(7) . . ? O17 Mo4 O15 95.13(7) . . ? O16 Mo4 O18 98.96(7) . . ? O17 Mo4 O18 100.07(7) . . ? O15 Mo4 O18 151.09(6) . . ? O16 Mo4 O14 94.25(6) . . ? O17 Mo4 O14 159.22(6) . . ? O15 Mo4 O14 74.07(5) . . ? O18 Mo4 O14 83.41(6) . . ? O16 Mo4 O19 160.89(6) . . ? O17 Mo4 O19 91.91(6) . . ? O15 Mo4 O19 85.83(5) . . ? O18 Mo4 O19 69.31(5) . . ? O14 Mo4 O19 69.99(5) . . ? O21 Mo5 O20 102.45(7) . . ? O21 Mo5 O18 102.43(7) . . ? O20 Mo5 O18 103.79(7) . . ? O21 Mo5 O5 100.84(7) . . ? O20 Mo5 O5 94.87(6) . . ? O18 Mo5 O5 146.05(6) . . ? O21 Mo5 O6 87.29(6) . . ? O20 Mo5 O6 166.59(6) . . ? O18 Mo5 O6 82.72(5) . . ? O5 Mo5 O6 74.03(5) . . ? O21 Mo5 O19 170.41(6) . . ? O20 Mo5 O19 87.13(6) . . ? O18 Mo5 O19 74.38(5) . . ? O5 Mo5 O19 78.58(5) . . ? O6 Mo5 O19 83.34(5) . . ? O7 P1 O6 110.84(8) . . ? O7 P1 O14 110.19(8) . . ? O6 P1 O14 110.23(8) . . ? O7 P1 C1 111.02(9) . . ? O6 P1 C1 110.20(9) . . ? O14 P1 C1 104.17(9) . . ? O13 P2 O19 111.57(8) . . ? O13 P2 O4 108.95(8) . . ? O19 P2 O4 111.45(8) . . ? O13 P2 C8 107.44(9) . . ? O19 P2 C8 108.82(9) . . ? O4 P2 C8 108.49(9) . . ? Mo1 O3 Mo2 121.56(7) . . ? P2 O4 Mo1 130.42(8) . . ? P2 O4 Mo2 133.82(8) . . ? Mo1 O4 Mo2 94.56(5) . . ? Mo1 O5 Mo5 122.99(7) . . ? P1 O6 Mo5 124.89(8) . . ? P1 O6 Mo1 126.19(8) . . ? Mo5 O6 Mo1 92.40(5) . . ? P1 O7 Mo2 118.88(8) . . ? Mo2 O10 Mo3 148.54(8) . . ? P2 O13 Mo3 122.61(8) . . ? P1 O14 Mo4 127.99(8) . . ? P1 O14 Mo3 135.25(8) . . ? Mo4 O14 Mo3 96.76(5) . . ? Mo4 O15 Mo3 118.71(7) . . ? Mo5 O18 Mo4 126.69(7) . . ? P2 O19 Mo5 127.30(8) . . ? P2 O19 Mo4 123.42(8) . . ? Mo5 O19 Mo4 89.60(5) . . ? H90A O90 H90B 86(3) . . ? C11 N1 C9 121.22(18) . . ? C11 N1 H1' 117(2) . . ? C9 N1 H1' 122(2) . . ? C12 N2 C14 131.43(19) . . ? C12 N2 H2' 112.6(17) . . ? C14 N2 H2' 114.5(17) . . ? C18 N3 C17 121.46(19) . . ? C18 N3 H3' 117.8(19) . . ? C17 N3 H3' 120.3(19) . . ? C19 N4 C20 121.76(19) . . ? C19 N4 H4' 118(2) . . ? C20 N4 H4' 120(2) . . ? C24 N5 C23 128.69(18) . . ? C24 N5 H5' 116.1(19) . . ? C23 N5 H5' 114.5(19) . . ? C28 N6 C27 121.26(19) . . ? C28 N6 H6' 117.1(18) . . ? C27 N6 H6' 121.0(18) . . ? C2 C1 P1 113.87(14) . . ? C2 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C5 119.6(2) . . ? C3 C2 C1 117.23(19) . . ? C5 C2 C1 123.19(19) . . ? C4 C3 C2 121.4(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C7 119.2(2) . . ? C3 C4 H4 120.4 . . ? C7 C4 H4 120.4 . . ? C6 C5 C2 118.0(2) . . ? C6 C5 C8 119.11(18) . 4_576 ? C2 C5 C8 122.88(18) . 4_576 ? C7 C6 C5 121.7(2) . . ? C7 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C6 C7 C4 120.0(2) . . ? C6 C7 H7 120.0 . . ? C4 C7 H7 120.0 . . ? C5 C8 P2 114.09(14) 4_575 . ? C5 C8 H8A 108.7 4_575 . ? P2 C8 H8A 108.7 . . ? C5 C8 H8B 108.7 4_575 . ? P2 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? N1 C9 C10 120.35(19) . . ? N1 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C12 120.0(2) . . ? C9 C10 H10 120.0 . . ? C12 C10 H10 120.0 . . ? N1 C11 C13 121.3(2) . . ? N1 C11 H11 119.3 . . ? C13 C11 H11 119.3 . . ? N2 C12 C13 125.57(19) . . ? N2 C12 C10 116.48(19) . . ? C13 C12 C10 117.87(19) . . ? C11 C13 C12 119.2(2) . . ? C11 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? N2 C14 C16 126.30(19) . . ? N2 C14 C15 115.66(19) . . ? C16 C14 C15 118.01(19) . . ? C17 C15 C14 119.7(2) . . ? C17 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C18 C16 C14 119.2(2) . . ? C18 C16 H16 120.4 . . ? C14 C16 H16 120.4 . . ? N3 C17 C15 120.5(2) . . ? N3 C17 H17 119.8 . . ? C15 C17 H17 119.8 . . ? N3 C18 C16 121.1(2) . . ? N3 C18 H18 119.4 . . ? C16 C18 H18 119.4 . . ? N4 C19 C21 120.5(2) . . ? N4 C19 H19 119.8 . . ? C21 C19 H19 119.8 . . ? N4 C20 C22 120.9(2) . . ? N4 C20 H20 119.6 . . ? C22 C20 H20 119.6 . . ? C19 C21 C23 119.3(2) . . ? C19 C21 H21 120.4 . . ? C23 C21 H21 120.4 . . ? C20 C22 C23 118.6(2) . . ? C20 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? N5 C23 C21 117.13(19) . . ? N5 C23 C22 123.78(19) . . ? C21 C23 C22 119.06(19) . . ? N5 C24 C25 124.17(19) . . ? N5 C24 C26 117.28(18) . . ? C25 C24 C26 118.46(19) . . ? C27 C25 C24 119.19(19) . . ? C27 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C28 C26 C24 119.26(19) . . ? C28 C26 H26 120.4 . . ? C24 C26 H26 120.4 . . ? N6 C27 C25 120.92(19) . . ? N6 C27 H27 119.5 . . ? C25 C27 H27 119.5 . . ? N6 C28 C26 120.83(19) . . ? N6 C28 H28 119.6 . . ? C26 C28 H28 119.6 . . ? 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 O13 P2 O4 Mo1 -172.75(9) . . . . ? O19 P2 O4 Mo1 -49.20(12) . . . . ? C8 P2 O4 Mo1 70.58(12) . . . . ? O13 P2 O4 Mo2 -8.53(13) . . . . ? O19 P2 O4 Mo2 115.02(11) . . . . ? C8 P2 O4 Mo2 -125.20(11) . . . . ? O7 P1 O6 Mo5 156.88(8) . . . . ? O14 P1 O6 Mo5 34.60(11) . . . . ? C1 P1 O6 Mo5 -79.82(11) . . . . ? O7 P1 O6 Mo1 31.89(11) . . . . ? O14 P1 O6 Mo1 -90.38(10) . . . . ? C1 P1 O6 Mo1 155.19(9) . . . . ? O6 P1 O7 Mo2 -64.83(10) . . . . ? O14 P1 O7 Mo2 57.47(10) . . . . ? C1 P1 O7 Mo2 172.35(9) . . . . ? O9 Mo2 O10 Mo3 -114.87(15) . . . . ? O8 Mo2 O10 Mo3 140.85(15) . . . . ? O3 Mo2 O10 Mo3 5.5(2) . . . . ? O7 Mo2 O10 Mo3 57.40(15) . . . . ? O4 Mo2 O10 Mo3 -31.46(15) . . . . ? O19 P2 O13 Mo3 -63.26(11) . . . . ? O4 P2 O13 Mo3 60.21(11) . . . . ? C8 P2 O13 Mo3 177.54(9) . . . . ? O7 P1 O14 Mo4 176.89(9) . . . . ? O6 P1 O14 Mo4 -60.45(12) . . . . ? C1 P1 O14 Mo4 57.74(12) . . . . ? O7 P1 O14 Mo3 -2.39(14) . . . . ? O6 P1 O14 Mo3 120.27(11) . . . . ? C1 P1 O14 Mo3 -121.53(12) . . . . ? O21 Mo5 O18 Mo4 -169.18(9) . . . . ? O20 Mo5 O18 Mo4 84.48(10) . . . . ? O5 Mo5 O18 Mo4 -36.93(16) . . . . ? O6 Mo5 O18 Mo4 -83.59(9) . . . . ? O19 Mo5 O18 Mo4 1.50(8) . . . . ? O13 P2 O19 Mo5 147.75(9) . . . . ? O4 P2 O19 Mo5 25.71(12) . . . . ? C8 P2 O19 Mo5 -93.88(11) . . . . ? O13 P2 O19 Mo4 28.26(11) . . . . ? O4 P2 O19 Mo4 -93.78(9) . . . . ? C8 P2 O19 Mo4 146.63(9) . . . . ? O7 P1 C1 C2 54.06(17) . . . . ? O6 P1 C1 C2 -69.14(16) . . . . ? O14 P1 C1 C2 172.64(14) . . . . ? P1 C1 C2 C3 88.3(2) . . . . ? P1 C1 C2 C5 -90.3(2) . . . . ? C5 C2 C3 C4 2.0(3) . . . . ? C1 C2 C3 C4 -176.7(2) . . . . ? C2 C3 C4 C7 0.7(4) . . . . ? C3 C2 C5 C6 -2.8(3) . . . . ? C1 C2 C5 C6 175.83(19) . . . . ? C3 C2 C5 C8 177.15(19) . . . 4_576 ? C1 C2 C5 C8 -4.3(3) . . . 4_576 ? C2 C5 C6 C7 0.9(3) . . . . ? C8 C5 C6 C7 -179.0(2) 4_576 . . . ? C5 C6 C7 C4 1.8(3) . . . . ? C3 C4 C7 C6 -2.6(3) . . . . ? O13 P2 C8 C5 -30.04(17) . . . 4_575 ? O19 P2 C8 C5 -150.99(14) . . . 4_575 ? O4 P2 C8 C5 87.59(16) . . . 4_575 ? C11 N1 C9 C10 -0.7(3) . . . . ? N1 C9 C10 C12 -0.7(3) . . . . ? C9 N1 C11 C13 0.9(3) . . . . ? C14 N2 C12 C13 -24.2(3) . . . . ? C14 N2 C12 C10 159.3(2) . . . . ? C9 C10 C12 N2 178.59(19) . . . . ? C9 C10 C12 C13 1.8(3) . . . . ? N1 C11 C13 C12 0.3(3) . . . . ? N2 C12 C13 C11 -178.0(2) . . . . ? C10 C12 C13 C11 -1.6(3) . . . . ? C12 N2 C14 C16 0.9(4) . . . . ? C12 N2 C14 C15 -177.4(2) . . . . ? N2 C14 C15 C17 176.4(2) . . . . ? C16 C14 C15 C17 -2.1(3) . . . . ? N2 C14 C16 C18 -176.4(2) . . . . ? C15 C14 C16 C18 1.8(3) . . . . ? C18 N3 C17 C15 1.0(4) . . . . ? C14 C15 C17 N3 0.7(4) . . . . ? C17 N3 C18 C16 -1.2(3) . . . . ? C14 C16 C18 N3 -0.2(3) . . . . ? C20 N4 C19 C21 1.1(3) . . . . ? C19 N4 C20 C22 -1.6(3) . . . . ? N4 C19 C21 C23 -0.7(3) . . . . ? N4 C20 C22 C23 1.6(3) . . . . ? C24 N5 C23 C21 160.6(2) . . . . ? C24 N5 C23 C22 -21.6(3) . . . . ? C19 C21 C23 N5 178.56(19) . . . . ? C19 C21 C23 C22 0.7(3) . . . . ? C20 C22 C23 N5 -178.85(19) . . . . ? C20 C22 C23 C21 -1.1(3) . . . . ? C23 N5 C24 C25 -20.7(3) . . . . ? C23 N5 C24 C26 162.8(2) . . . . ? N5 C24 C25 C27 -179.45(19) . . . . ? C26 C24 C25 C27 -3.0(3) . . . . ? N5 C24 C26 C28 178.63(19) . . . . ? C25 C24 C26 C28 1.9(3) . . . . ? C28 N6 C27 C25 0.9(3) . . . . ? C24 C25 C27 N6 1.6(3) . . . . ? C27 N6 C28 C26 -2.0(3) . . . . ? C24 C26 C28 N6 0.6(3) . . . . ? _refine_diff_density_max 1.286 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.066 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957889' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H8 Mo5 O21 P2, 2(C10 H11 N3)' _chemical_formula_sum 'C28 H30 Mo5 N6 O21 P2' _chemical_formula_weight 1328.22 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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system trigonal _space_group_IT_number 145 _space_group_name_H-M_alt 'P 32' _space_group_name_Hall 'P 32' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' _cell_length_a 11.1778(7) _cell_length_b 11.1778(7) _cell_length_c 27.6410(17) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2990.9(4) _cell_formula_units_Z 3 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 2202 _cell_measurement_theta_min 2.1494 _cell_measurement_theta_max 29.1792 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_density_meas 2.20(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.212 _exptl_crystal_F_000 1944 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.265 _exptl_crystal_size_mid 0.154 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 1.701 _shelx_estimated_absorpt_T_min 0.661 _shelx_estimated_absorpt_T_max 0.876 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.88 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32751 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.104 _diffrn_reflns_theta_max 27.095 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 8572 _reflns_number_gt 8346 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.946 _reflns_Friedel_fraction_max 0.946 _reflns_Friedel_fraction_full 0.992 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+12.8222P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3950 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.002(9) _chemical_absolute_configuration ? _refine_ls_number_reflns 8572 _refine_ls_number_parameters 560 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 1.15857(7) 0.71566(7) 0.31185(3) 0.01639(15) Uani 1 1 d . . . . . Mo2 Mo 0.94565(8) 0.81303(7) 0.36164(3) 0.01747(16) Uani 1 1 d . . . . . Mo3 Mo 0.67841(7) 0.53954(8) 0.41701(3) 0.01796(16) Uani 1 1 d . . . . . Mo4 Mo 1.06339(7) 0.39100(7) 0.35212(3) 0.01630(15) Uani 1 1 d . . . . . Mo5 Mo 0.70357(7) 0.25655(7) 0.39677(2) 0.01626(15) Uani 1 1 d . . . . . P1 P 0.8103(2) 0.4909(2) 0.30721(7) 0.0146(4) Uani 1 1 d . . . . . P2 P 1.0028(2) 0.5839(2) 0.42716(7) 0.0132(4) Uani 1 1 d . . . . . O1 O 1.3067(7) 0.8529(7) 0.3339(2) 0.0273(15) Uani 1 1 d . . . . . O2 O 1.1982(7) 0.7119(7) 0.2516(2) 0.0262(14) Uani 1 1 d . . . . . O3 O 0.9598(6) 0.5185(6) 0.3086(2) 0.0162(12) Uani 1 1 d . . . . . O4 O 1.1967(6) 0.5754(6) 0.3373(2) 0.0167(11) Uani 1 1 d . . . . . O5 O 1.0399(7) 0.3137(7) 0.2967(2) 0.0218(13) Uani 1 1 d . . . . . O6 O 1.1558(7) 0.3306(7) 0.3818(2) 0.0220(13) Uani 1 1 d . . . . . O7 O 0.8809(6) 0.2773(6) 0.3777(2) 0.0174(12) Uani 1 1 d . . . . . O8 O 1.0770(6) 0.5019(6) 0.4239(2) 0.0156(11) Uani 1 1 d . . . . . O9 O 0.7012(7) 0.2063(7) 0.4553(2) 0.0236(13) Uani 1 1 d . . . . . O10 O 0.5943(6) 0.3470(7) 0.4013(2) 0.0213(13) Uani 1 1 d . . . . . O11 O 0.7122(6) 0.3391(6) 0.3187(2) 0.0184(12) Uani 1 1 d . . . . . O12 O 0.8451(6) 0.4852(6) 0.4219(2) 0.0149(11) Uani 1 1 d . . . . . O13 O 0.5506(7) 0.5660(8) 0.3945(3) 0.0277(15) Uani 1 1 d . . . . . O14 O 1.0561(6) 0.6982(6) 0.3885(2) 0.0155(11) Uani 1 1 d . . . . . O15 O 0.5899(7) 0.1041(7) 0.3696(2) 0.0256(14) Uani 1 1 d . . . . . O16 O 0.8530(7) 0.8724(7) 0.3297(2) 0.0258(14) Uani 1 1 d . . . . . O17 O 0.6559(7) 0.5327(7) 0.4779(2) 0.0295(15) Uani 1 1 d . . . . . O18 O 0.7903(6) 0.5861(6) 0.3427(2) 0.0138(11) Uani 1 1 d . . . . . O19 O 0.8328(6) 0.7290(6) 0.4166(2) 0.0185(12) Uani 1 1 d . . . . . O20 O 1.0728(7) 0.9592(7) 0.3880(2) 0.0250(14) Uani 1 1 d . . . . . O21 O 1.0409(7) 0.7919(6) 0.3064(2) 0.0192(12) Uani 1 1 d . . . . . N1 N -0.1667(11) -0.2235(9) 0.1264(3) 0.039(2) Uani 1 1 d . . . . . H1' H -0.2124 -0.2781 0.1021 0.046 Uiso 1 1 calc R U . . . N2 N 0.0388(8) 0.0141(8) 0.2461(3) 0.0221(16) Uani 1 1 d . . . . . H2' H -0.0182 0.0216 0.2662 0.027 Uiso 1 1 calc R U . . . N3 N 0.4392(8) 0.2125(8) 0.2963(3) 0.0219(16) Uani 1 1 d . . . . . H3' H 0.5245 0.2549 0.3073 0.026 Uiso 1 1 calc R U . . . N4 N 0.3991(9) -0.0816(9) 0.4390(3) 0.0320(19) Uani 1 1 d . . . . . H4' H 0.4137 -0.1244 0.4150 0.038 Uiso 1 1 calc R U . . . N5 N 0.3503(10) 0.1309(10) 0.5521(3) 0.034(2) Uani 1 1 d . . . . . H5' H 0.3341 0.0863 0.5797 0.041 Uiso 1 1 calc R U . . . N6 N 0.3886(11) 0.5122(11) 0.5707(4) 0.045(3) Uani 1 1 d . . . . . H6' H 0.3998 0.5950 0.5759 0.054 Uiso 1 1 calc R U . . . C1 C 0.7740(9) 0.5304(9) 0.2476(3) 0.0168(16) Uani 1 1 d . . . . . H1A H 0.8452 0.6261 0.2393 0.020 Uiso 1 1 calc R U . . . H1B H 0.7816 0.4679 0.2241 0.020 Uiso 1 1 calc R U . . . C2 C 1.0306(9) 0.6687(8) 0.4853(3) 0.0150(15) Uani 1 1 d . . . . . H2A H 1.1245 0.7507 0.4855 0.018 Uiso 1 1 calc R U . . . H2B H 0.9639 0.7020 0.4886 0.018 Uiso 1 1 calc R U . . . C3 C 1.0164(8) 0.5813(8) 0.5285(3) 0.0139(15) Uani 1 1 d . . . . . C4 C 0.8955(9) 0.4524(9) 0.5362(3) 0.0164(16) Uani 1 1 d . . . . . H4 H 0.8198 0.4219 0.5146 0.020 Uiso 1 1 calc R U . . . C5 C 0.8863(8) 0.3694(9) 0.5756(3) 0.0172(16) Uani 1 1 d . . . . . C6 C 0.9979(9) 0.4175(9) 0.6077(3) 0.0198(17) Uani 1 1 d . . . . . H6 H 0.9941 0.3612 0.6341 0.024 Uiso 1 1 calc R U . . . C7 C 1.1128(9) 0.5454(9) 0.6014(3) 0.0207(17) Uani 1 1 d . . . . . H7 H 1.1859 0.5778 0.6243 0.025 Uiso 1 1 calc R U . . . C8 C 1.1243(9) 0.6282(9) 0.5622(3) 0.0186(17) Uani 1 1 d . . . . . H8 H 1.2047 0.7161 0.5583 0.022 Uiso 1 1 calc R U . . . C9 C -0.0288(13) -0.1421(12) 0.1230(4) 0.037(3) Uani 1 1 d . . . . . H9 H 0.0182 -0.1427 0.0944 0.045 Uiso 1 1 calc R U . . . C10 C -0.2355(12) -0.2237(10) 0.1656(4) 0.034(2) Uani 1 1 d . . . . . H10 H -0.3335 -0.2773 0.1656 0.041 Uiso 1 1 calc R U . . . C11 C 0.0438(12) -0.0576(11) 0.1613(4) 0.035(2) Uani 1 1 d . . . . . H11 H 0.1404 0.0038 0.1582 0.042 Uiso 1 1 calc R U . . . C12 C -0.0219(10) -0.0608(9) 0.2045(3) 0.0238(19) Uani 1 1 d . . . . . C13 C -0.1678(11) -0.1475(10) 0.2066(4) 0.029(2) Uani 1 1 d . . . . . H13 H -0.2177 -0.1532 0.2352 0.035 Uiso 1 1 calc R U . . . C14 C 0.1759(9) 0.0794(8) 0.2610(3) 0.0180(16) Uani 1 1 d . . . . . C15 C 0.2811(11) 0.0671(10) 0.2379(3) 0.0258(19) Uani 1 1 d . . . . . H15 H 0.2621 0.0107 0.2100 0.031 Uiso 1 1 calc R U . . . C16 C 0.2073(9) 0.1579(9) 0.3026(3) 0.0196(17) Uani 1 1 d . . . . . H16 H 0.1370 0.1658 0.3191 0.024 Uiso 1 1 calc R U . . . C17 C 0.4107(10) 0.1381(10) 0.2565(4) 0.027(2) Uani 1 1 d . . . . . H17 H 0.4835 0.1339 0.2403 0.032 Uiso 1 1 calc R U . . . C18 C 0.3429(9) 0.2259(9) 0.3205(3) 0.0206(17) Uani 1 1 d . . . . . H18 H 0.3658 0.2801 0.3491 0.025 Uiso 1 1 calc R U . . . C19 C 0.3388(10) -0.0046(10) 0.4300(4) 0.028(2) Uani 1 1 d . . . . . H19 H 0.3096 -0.0007 0.3980 0.034 Uiso 1 1 calc R U . . . C20 C 0.4364(11) -0.0934(11) 0.4834(4) 0.031(2) Uani 1 1 d . . . . . H20 H 0.4729 -0.1528 0.4892 0.037 Uiso 1 1 calc R U . . . C21 C 0.3194(10) 0.0669(10) 0.4656(4) 0.030(2) Uani 1 1 d . . . . . H21 H 0.2760 0.1196 0.4589 0.036 Uiso 1 1 calc R U . . . C22 C 0.4231(11) -0.0213(11) 0.5210(4) 0.030(2) Uani 1 1 d . . . . . H22 H 0.4533 -0.0276 0.5525 0.036 Uiso 1 1 calc R U . . . C23 C 0.3644(11) 0.0617(10) 0.5125(4) 0.028(2) Uani 1 1 d . . . . . C24 C 0.3573(10) 0.2558(11) 0.5552(4) 0.031(2) Uani 1 1 d . . . . . C25 C 0.3817(12) 0.3449(12) 0.5168(5) 0.038(3) Uani 1 1 d . . . . . H25 H 0.3881 0.3176 0.4848 0.046 Uiso 1 1 calc R U . . . C26 C 0.3463(13) 0.2984(14) 0.6027(5) 0.043(3) Uani 1 1 d . . . . . H26 H 0.3272 0.2380 0.6294 0.052 Uiso 1 1 calc R U . . . C27 C 0.3966(12) 0.4746(12) 0.5252(5) 0.044(3) Uani 1 1 d . . . . . H27 H 0.4123 0.5359 0.4991 0.053 Uiso 1 1 calc R U . . . C28 C 0.3634(12) 0.4262(14) 0.6094(5) 0.045(3) Uani 1 1 d . . . . . H28 H 0.3579 0.4561 0.6411 0.054 Uiso 1 1 calc R 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 Mo1 0.0161(3) 0.0140(3) 0.0137(3) 0.0011(3) 0.0021(3) 0.0035(3) Mo2 0.0213(4) 0.0154(3) 0.0163(3) -0.0014(3) -0.0038(3) 0.0096(3) Mo3 0.0146(3) 0.0225(4) 0.0176(3) -0.0043(3) -0.0003(3) 0.0099(3) Mo4 0.0160(3) 0.0174(3) 0.0172(3) 0.0018(3) 0.0031(3) 0.0097(3) Mo5 0.0131(3) 0.0148(3) 0.0156(3) 0.0003(3) 0.0024(3) 0.0030(3) P1 0.0128(10) 0.0156(10) 0.0141(9) -0.0015(7) -0.0022(7) 0.0062(8) P2 0.0124(9) 0.0138(9) 0.0119(9) 0.0006(7) -0.0001(7) 0.0053(8) O1 0.025(3) 0.020(3) 0.020(3) -0.001(2) 0.006(3) -0.002(3) O2 0.035(4) 0.023(3) 0.014(3) 0.002(2) 0.002(3) 0.009(3) O3 0.014(3) 0.016(3) 0.019(3) 0.001(2) -0.003(2) 0.008(2) O4 0.010(3) 0.019(3) 0.018(3) 0.002(2) 0.000(2) 0.005(2) O5 0.021(3) 0.027(3) 0.020(3) -0.001(2) 0.000(2) 0.014(3) O6 0.024(3) 0.021(3) 0.025(3) -0.001(2) -0.001(3) 0.014(3) O7 0.015(3) 0.013(3) 0.022(3) 0.001(2) 0.004(2) 0.005(2) O8 0.016(3) 0.015(3) 0.016(3) 0.001(2) 0.001(2) 0.008(2) O9 0.024(3) 0.018(3) 0.021(3) 0.001(2) 0.004(3) 0.004(3) O10 0.013(3) 0.026(3) 0.020(3) -0.004(2) 0.001(2) 0.006(3) O11 0.014(3) 0.019(3) 0.020(3) -0.002(2) -0.001(2) 0.006(2) O12 0.013(3) 0.016(3) 0.015(3) 0.003(2) 0.000(2) 0.006(2) O13 0.020(3) 0.039(4) 0.033(4) -0.008(3) -0.003(3) 0.021(3) O14 0.019(3) 0.015(3) 0.014(3) 0.004(2) 0.003(2) 0.010(2) O15 0.024(3) 0.018(3) 0.025(3) -0.005(3) 0.004(3) 0.003(3) O16 0.032(4) 0.021(3) 0.028(3) -0.004(3) -0.008(3) 0.016(3) O17 0.028(4) 0.033(4) 0.020(3) -0.008(3) 0.001(3) 0.009(3) O18 0.015(3) 0.012(3) 0.017(3) 0.000(2) -0.002(2) 0.009(2) O19 0.022(3) 0.015(3) 0.017(3) -0.006(2) -0.003(2) 0.008(2) O20 0.031(4) 0.018(3) 0.025(3) -0.004(3) -0.005(3) 0.012(3) O21 0.027(3) 0.017(3) 0.014(3) 0.003(2) -0.001(2) 0.011(3) N1 0.051(6) 0.025(4) 0.030(5) -0.003(4) -0.016(4) 0.011(4) N2 0.021(4) 0.022(4) 0.024(4) -0.003(3) -0.008(3) 0.011(3) N3 0.011(3) 0.023(4) 0.027(4) 0.004(3) -0.001(3) 0.005(3) N4 0.032(5) 0.027(4) 0.035(5) -0.007(4) 0.000(4) 0.013(4) N5 0.041(5) 0.030(5) 0.028(4) 0.002(4) 0.007(4) 0.016(4) N6 0.033(5) 0.039(6) 0.075(8) -0.022(5) -0.016(5) 0.027(5) C1 0.019(4) 0.023(4) 0.013(4) -0.001(3) -0.005(3) 0.013(3) C2 0.017(4) 0.014(4) 0.011(3) 0.002(3) -0.001(3) 0.005(3) C3 0.015(4) 0.014(4) 0.012(4) 0.001(3) 0.004(3) 0.007(3) C4 0.016(4) 0.024(4) 0.012(4) 0.000(3) -0.001(3) 0.011(3) C5 0.012(4) 0.016(4) 0.021(4) 0.000(3) 0.004(3) 0.005(3) C6 0.023(4) 0.020(4) 0.015(4) 0.004(3) 0.000(3) 0.010(4) C7 0.013(4) 0.022(4) 0.021(4) -0.002(3) -0.004(3) 0.004(3) C8 0.015(4) 0.017(4) 0.020(4) 0.002(3) 0.004(3) 0.005(3) C9 0.049(7) 0.034(6) 0.022(5) -0.004(4) -0.005(4) 0.015(5) C10 0.035(6) 0.018(5) 0.046(6) -0.002(4) -0.013(5) 0.011(4) C11 0.038(6) 0.024(5) 0.027(5) 0.002(4) -0.003(4) 0.004(5) C12 0.030(5) 0.018(4) 0.020(4) 0.005(3) -0.005(4) 0.010(4) C13 0.029(5) 0.020(4) 0.039(5) -0.002(4) -0.016(4) 0.013(4) C14 0.016(4) 0.007(4) 0.022(4) 0.005(3) 0.002(3) -0.001(3) C15 0.034(5) 0.021(5) 0.020(4) -0.002(3) 0.006(4) 0.012(4) C16 0.020(4) 0.015(4) 0.023(4) 0.002(3) -0.002(3) 0.008(3) C17 0.024(5) 0.025(5) 0.033(5) 0.001(4) 0.008(4) 0.014(4) C18 0.021(4) 0.023(4) 0.018(4) -0.002(3) -0.004(3) 0.011(4) C19 0.021(5) 0.029(5) 0.022(4) 0.001(4) -0.001(4) 0.003(4) C20 0.030(5) 0.024(5) 0.038(6) -0.004(4) -0.002(4) 0.013(4) C21 0.019(5) 0.022(5) 0.041(6) 0.001(4) -0.003(4) 0.004(4) C22 0.029(5) 0.025(5) 0.026(5) 0.001(4) 0.001(4) 0.006(4) C23 0.031(5) 0.021(5) 0.027(5) 0.002(4) 0.008(4) 0.010(4) C24 0.015(4) 0.025(5) 0.041(6) -0.009(4) 0.002(4) 0.000(4) C25 0.030(6) 0.037(6) 0.050(7) -0.001(5) 0.001(5) 0.019(5) C26 0.043(7) 0.052(7) 0.040(6) -0.011(5) -0.015(5) 0.028(6) C27 0.029(6) 0.027(6) 0.071(9) -0.004(5) 0.001(6) 0.011(5) C28 0.031(6) 0.054(8) 0.051(7) -0.023(6) -0.015(5) 0.021(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 1.711(7) . ? Mo1 O2 1.728(6) . ? Mo1 O21 1.898(6) . ? Mo1 O4 1.950(6) . ? Mo1 O3 2.214(6) . ? Mo1 O14 2.370(6) . ? Mo2 O20 1.702(7) . ? Mo2 O16 1.726(7) . ? Mo2 O19 1.897(6) . ? Mo2 O21 1.941(6) . ? Mo2 O14 2.304(6) . ? Mo2 O18 2.306(6) . ? Mo3 O17 1.698(7) . ? Mo3 O13 1.714(6) . ? Mo3 O10 1.919(6) . ? Mo3 O19 1.952(6) . ? Mo3 O12 2.234(6) . ? Mo3 O18 2.326(6) . ? Mo4 O6 1.700(6) . ? Mo4 O5 1.714(6) . ? Mo4 O4 1.888(6) . ? Mo4 O7 1.919(6) . ? Mo4 O8 2.304(6) . ? Mo5 O15 1.708(6) . ? Mo5 O9 1.710(7) . ? Mo5 O10 1.940(6) . ? Mo5 O7 1.950(6) . ? Mo5 O11 2.330(6) . ? Mo5 O12 2.339(6) . ? P1 O11 1.524(6) . ? P1 O3 1.541(6) . ? P1 O18 1.543(6) . ? P1 C1 1.803(8) . ? P2 O8 1.516(6) . ? P2 O14 1.539(6) . ? P2 O12 1.550(6) . ? P2 C2 1.811(8) . ? N1 C10 1.328(16) . ? N1 C9 1.345(16) . ? N1 H1' 0.8800 . ? N2 C12 1.382(12) . ? N2 C14 1.391(11) . ? N2 H2' 0.8800 . ? N3 C17 1.319(13) . ? N3 C18 1.337(12) . ? N3 H3' 0.8800 . ? N4 C20 1.323(14) . ? N4 C19 1.357(14) . ? N4 H4' 0.8800 . ? N5 C24 1.362(14) . ? N5 C23 1.394(13) . ? N5 H5' 0.8800 . ? N6 C27 1.343(18) . ? N6 C28 1.370(19) . ? N6 H6' 0.8800 . ? C1 C5 1.540(11) 2_654 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.501(11) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.402(12) . ? C3 C4 1.415(12) . ? C4 C5 1.399(12) . ? C4 H4 0.9500 . ? C5 C6 1.401(12) . ? C5 C1 1.540(11) 3_665 ? C6 C7 1.374(12) . ? C6 H6 0.9500 . ? C7 C8 1.390(12) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C11 1.380(15) . ? C9 H9 0.9500 . ? C10 C13 1.393(14) . ? C10 H10 0.9500 . ? C11 C12 1.394(15) . ? C11 H11 0.9500 . ? C12 C13 1.422(14) . ? C13 H13 0.9500 . ? C14 C16 1.380(12) . ? C14 C15 1.405(13) . ? C15 C17 1.357(14) . ? C15 H15 0.9500 . ? C16 C18 1.403(12) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.351(15) . ? C19 H19 0.9500 . ? C20 C22 1.369(15) . ? C20 H20 0.9500 . ? C21 C23 1.403(15) . ? C21 H21 0.9500 . ? C22 C23 1.398(15) . ? C22 H22 0.9500 . ? C24 C25 1.388(16) . ? C24 C26 1.421(16) . ? C25 C27 1.394(17) . ? C25 H25 0.9500 . ? C26 C28 1.356(19) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? 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 O1 Mo1 O2 102.7(3) . . ? O1 Mo1 O21 101.7(3) . . ? O2 Mo1 O21 100.3(3) . . ? O1 Mo1 O4 95.2(3) . . ? O2 Mo1 O4 99.6(3) . . ? O21 Mo1 O4 150.3(2) . . ? O1 Mo1 O3 161.2(3) . . ? O2 Mo1 O3 94.5(3) . . ? O21 Mo1 O3 82.4(2) . . ? O4 Mo1 O3 74.2(2) . . ? O1 Mo1 O14 88.1(3) . . ? O2 Mo1 O14 168.0(3) . . ? O21 Mo1 O14 72.1(2) . . ? O4 Mo1 O14 84.4(2) . . ? O3 Mo1 O14 75.6(2) . . ? O20 Mo2 O16 102.9(3) . . ? O20 Mo2 O19 99.3(3) . . ? O16 Mo2 O19 102.8(3) . . ? O20 Mo2 O21 102.0(3) . . ? O16 Mo2 O21 96.7(3) . . ? O19 Mo2 O21 147.0(2) . . ? O20 Mo2 O14 88.5(3) . . ? O16 Mo2 O14 166.1(3) . . ? O19 Mo2 O14 82.8(2) . . ? O21 Mo2 O14 72.9(2) . . ? O20 Mo2 O18 164.0(3) . . ? O16 Mo2 O18 92.3(3) . . ? O19 Mo2 O18 71.9(2) . . ? O21 Mo2 O18 81.1(2) . . ? O14 Mo2 O18 77.3(2) . . ? O17 Mo3 O13 104.5(3) . . ? O17 Mo3 O10 101.3(3) . . ? O13 Mo3 O10 97.3(3) . . ? O17 Mo3 O19 94.8(3) . . ? O13 Mo3 O19 99.9(3) . . ? O10 Mo3 O19 152.5(3) . . ? O17 Mo3 O12 93.0(3) . . ? O13 Mo3 O12 161.6(3) . . ? O10 Mo3 O12 73.5(2) . . ? O19 Mo3 O12 83.7(2) . . ? O17 Mo3 O18 159.6(3) . . ? O13 Mo3 O18 92.4(3) . . ? O10 Mo3 O18 87.6(2) . . ? O19 Mo3 O18 70.6(2) . . ? O12 Mo3 O18 71.7(2) . . ? O6 Mo4 O5 101.6(3) . . ? O6 Mo4 O4 103.5(3) . . ? O5 Mo4 O4 101.2(3) . . ? O6 Mo4 O7 102.4(3) . . ? O5 Mo4 O7 98.7(3) . . ? O4 Mo4 O7 143.1(3) . . ? O6 Mo4 O8 84.7(3) . . ? O5 Mo4 O8 173.5(3) . . ? O4 Mo4 O8 78.2(2) . . ? O7 Mo4 O8 78.6(2) . . ? O15 Mo5 O9 102.0(3) . . ? O15 Mo5 O10 101.5(3) . . ? O9 Mo5 O10 101.6(3) . . ? O15 Mo5 O7 101.8(3) . . ? O9 Mo5 O7 98.3(3) . . ? O10 Mo5 O7 145.3(3) . . ? O15 Mo5 O11 81.4(3) . . ? O9 Mo5 O11 176.4(3) . . ? O10 Mo5 O11 76.4(2) . . ? O7 Mo5 O11 82.2(2) . . ? O15 Mo5 O12 168.4(3) . . ? O9 Mo5 O12 88.2(3) . . ? O10 Mo5 O12 70.7(2) . . ? O7 Mo5 O12 81.9(2) . . ? O11 Mo5 O12 88.3(2) . . ? O11 P1 O3 108.8(3) . . ? O11 P1 O18 111.4(3) . . ? O3 P1 O18 111.3(3) . . ? O11 P1 C1 109.8(4) . . ? O3 P1 C1 109.1(4) . . ? O18 P1 C1 106.5(4) . . ? O8 P2 O14 111.1(3) . . ? O8 P2 O12 109.6(3) . . ? O14 P2 O12 110.9(3) . . ? O8 P2 C2 111.5(4) . . ? O14 P2 C2 106.7(4) . . ? O12 P2 C2 107.0(4) . . ? P1 O3 Mo1 130.4(3) . . ? Mo4 O4 Mo1 125.9(3) . . ? Mo4 O7 Mo5 149.2(3) . . ? P2 O8 Mo4 117.8(3) . . ? Mo3 O10 Mo5 121.1(3) . . ? P1 O11 Mo5 119.9(3) . . ? P2 O12 Mo3 128.2(3) . . ? P2 O12 Mo5 135.5(3) . . ? Mo3 O12 Mo5 94.5(2) . . ? P2 O14 Mo2 126.4(3) . . ? P2 O14 Mo1 131.3(3) . . ? Mo2 O14 Mo1 92.1(2) . . ? P1 O18 Mo2 127.9(3) . . ? P1 O18 Mo3 130.8(3) . . ? Mo2 O18 Mo3 94.0(2) . . ? Mo2 O19 Mo3 123.3(3) . . ? Mo1 O21 Mo2 122.6(3) . . ? C10 N1 C9 121.7(9) . . ? C10 N1 H1' 119.1 . . ? C9 N1 H1' 119.1 . . ? C12 N2 C14 130.0(9) . . ? C12 N2 H2' 115.0 . . ? C14 N2 H2' 115.0 . . ? C17 N3 C18 122.2(8) . . ? C17 N3 H3' 118.9 . . ? C18 N3 H3' 118.9 . . ? C20 N4 C19 121.0(9) . . ? C20 N4 H4' 119.5 . . ? C19 N4 H4' 119.5 . . ? C24 N5 C23 131.0(9) . . ? C24 N5 H5' 114.5 . . ? C23 N5 H5' 114.5 . . ? C27 N6 C28 122.2(11) . . ? C27 N6 H6' 118.9 . . ? C28 N6 H6' 118.9 . . ? C5 C1 P1 114.5(6) 2_654 . ? C5 C1 H1A 108.6 2_654 . ? P1 C1 H1A 108.6 . . ? C5 C1 H1B 108.6 2_654 . ? P1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C3 C2 P2 115.5(6) . . ? C3 C2 H2A 108.4 . . ? P2 C2 H2A 108.4 . . ? C3 C2 H2B 108.4 . . ? P2 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? C8 C3 C4 119.0(7) . . ? C8 C3 C2 119.7(7) . . ? C4 C3 C2 121.3(7) . . ? C5 C4 C3 120.6(7) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 118.8(8) . . ? C4 C5 C1 118.9(8) . 3_665 ? C6 C5 C1 122.2(8) . 3_665 ? C7 C6 C5 120.6(8) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 121.2(8) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C3 119.6(8) . . ? C7 C8 H8 120.2 . . ? C3 C8 H8 120.2 . . ? N1 C9 C11 119.5(11) . . ? N1 C9 H9 120.3 . . ? C11 C9 H9 120.3 . . ? N1 C10 C13 121.7(11) . . ? N1 C10 H10 119.2 . . ? C13 C10 H10 119.2 . . ? C9 C11 C12 121.2(10) . . ? C9 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? N2 C12 C11 127.2(9) . . ? N2 C12 C13 115.3(9) . . ? C11 C12 C13 117.5(9) . . ? C10 C13 C12 118.1(11) . . ? C10 C13 H13 120.9 . . ? C12 C13 H13 120.9 . . ? C16 C14 N2 116.4(8) . . ? C16 C14 C15 118.8(8) . . ? N2 C14 C15 124.7(8) . . ? C17 C15 C14 118.1(8) . . ? C17 C15 H15 120.9 . . ? C14 C15 H15 120.9 . . ? C14 C16 C18 120.0(9) . . ? C14 C16 H16 120.0 . . ? C18 C16 H16 120.0 . . ? N3 C17 C15 122.4(9) . . ? N3 C17 H17 118.8 . . ? C15 C17 H17 118.8 . . ? N3 C18 C16 118.4(8) . . ? N3 C18 H18 120.8 . . ? C16 C18 H18 120.8 . . ? C21 C19 N4 121.2(9) . . ? C21 C19 H19 119.4 . . ? N4 C19 H19 119.4 . . ? N4 C20 C22 120.9(10) . . ? N4 C20 H20 119.6 . . ? C22 C20 H20 119.6 . . ? C19 C21 C23 118.8(10) . . ? C19 C21 H21 120.6 . . ? C23 C21 H21 120.6 . . ? C20 C22 C23 119.2(10) . . ? C20 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? N5 C23 C22 117.2(9) . . ? N5 C23 C21 124.1(10) . . ? C22 C23 C21 118.7(9) . . ? N5 C24 C25 125.2(10) . . ? N5 C24 C26 115.6(11) . . ? C25 C24 C26 119.0(11) . . ? C24 C25 C27 119.8(12) . . ? C24 C25 H25 120.1 . . ? C27 C25 H25 120.1 . . ? C28 C26 C24 119.3(13) . . ? C28 C26 H26 120.3 . . ? C24 C26 H26 120.3 . . ? N6 C27 C25 119.4(13) . . ? N6 C27 H27 120.3 . . ? C25 C27 H27 120.3 . . ? C26 C28 N6 120.3(12) . . ? C26 C28 H28 119.9 . . ? N6 C28 H28 119.9 . . ? 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 O11 P1 O3 Mo1 -164.9(4) . . . . ? O18 P1 O3 Mo1 -41.8(5) . . . . ? C1 P1 O3 Mo1 75.4(5) . . . . ? O6 Mo4 O4 Mo1 -170.2(4) . . . . ? O5 Mo4 O4 Mo1 84.8(4) . . . . ? O7 Mo4 O4 Mo1 -36.6(6) . . . . ? O8 Mo4 O4 Mo1 -88.6(4) . . . . ? O14 P2 O8 Mo4 -59.0(4) . . . . ? O12 P2 O8 Mo4 63.9(4) . . . . ? C2 P2 O8 Mo4 -177.8(3) . . . . ? O3 P1 O11 Mo5 70.2(4) . . . . ? O18 P1 O11 Mo5 -52.8(5) . . . . ? C1 P1 O11 Mo5 -170.5(4) . . . . ? O8 P2 O12 Mo3 -174.3(4) . . . . ? O14 P2 O12 Mo3 -51.3(5) . . . . ? C2 P2 O12 Mo3 64.7(5) . . . . ? O8 P2 O12 Mo5 -13.7(6) . . . . ? O14 P2 O12 Mo5 109.3(5) . . . . ? C2 P2 O12 Mo5 -134.7(5) . . . . ? O8 P2 O14 Mo2 161.6(4) . . . . ? O12 P2 O14 Mo2 39.4(5) . . . . ? C2 P2 O14 Mo2 -76.8(5) . . . . ? O8 P2 O14 Mo1 26.4(5) . . . . ? O12 P2 O14 Mo1 -95.7(5) . . . . ? C2 P2 O14 Mo1 148.1(4) . . . . ? O11 P1 O18 Mo2 157.8(4) . . . . ? O3 P1 O18 Mo2 36.2(5) . . . . ? C1 P1 O18 Mo2 -82.6(5) . . . . ? O11 P1 O18 Mo3 15.6(5) . . . . ? O3 P1 O18 Mo3 -106.0(4) . . . . ? C1 P1 O18 Mo3 135.2(4) . . . . ? O20 Mo2 O19 Mo3 -169.8(4) . . . . ? O16 Mo2 O19 Mo3 84.6(4) . . . . ? O21 Mo2 O19 Mo3 -40.1(7) . . . . ? O14 Mo2 O19 Mo3 -82.5(4) . . . . ? O18 Mo2 O19 Mo3 -3.6(3) . . . . ? O1 Mo1 O21 Mo2 -79.2(4) . . . . ? O2 Mo1 O21 Mo2 175.4(4) . . . . ? O4 Mo1 O21 Mo2 44.0(7) . . . . ? O3 Mo1 O21 Mo2 82.2(4) . . . . ? O14 Mo1 O21 Mo2 4.9(3) . . . . ? O11 P1 C1 C5 64.9(7) . . . 2_654 ? O3 P1 C1 C5 -176.0(6) . . . 2_654 ? O18 P1 C1 C5 -55.8(7) . . . 2_654 ? O8 P2 C2 C3 -45.1(7) . . . . ? O14 P2 C2 C3 -166.5(6) . . . . ? O12 P2 C2 C3 74.8(7) . . . . ? P2 C2 C3 C8 126.2(7) . . . . ? P2 C2 C3 C4 -54.4(10) . . . . ? C8 C3 C4 C5 -3.4(12) . . . . ? C2 C3 C4 C5 177.2(8) . . . . ? C3 C4 C5 C6 1.3(12) . . . . ? C3 C4 C5 C1 -176.3(7) . . . 3_665 ? C4 C5 C6 C7 1.7(13) . . . . ? C1 C5 C6 C7 179.2(8) 3_665 . . . ? C5 C6 C7 C8 -2.6(14) . . . . ? C6 C7 C8 C3 0.4(14) . . . . ? C4 C3 C8 C7 2.5(12) . . . . ? C2 C3 C8 C7 -178.1(8) . . . . ? C10 N1 C9 C11 0.9(17) . . . . ? C9 N1 C10 C13 -4.9(16) . . . . ? N1 C9 C11 C12 3.7(18) . . . . ? C14 N2 C12 C11 -19.5(16) . . . . ? C14 N2 C12 C13 162.0(9) . . . . ? C9 C11 C12 N2 177.5(10) . . . . ? C9 C11 C12 C13 -4.0(16) . . . . ? N1 C10 C13 C12 4.2(15) . . . . ? N2 C12 C13 C10 178.8(8) . . . . ? C11 C12 C13 C10 0.2(14) . . . . ? C12 N2 C14 C16 174.0(8) . . . . ? C12 N2 C14 C15 -8.2(14) . . . . ? C16 C14 C15 C17 -2.7(13) . . . . ? N2 C14 C15 C17 179.5(9) . . . . ? N2 C14 C16 C18 179.3(8) . . . . ? C15 C14 C16 C18 1.3(13) . . . . ? C18 N3 C17 C15 -1.6(15) . . . . ? C14 C15 C17 N3 2.9(15) . . . . ? C17 N3 C18 C16 0.0(13) . . . . ? C14 C16 C18 N3 0.1(13) . . . . ? C20 N4 C19 C21 2.5(15) . . . . ? C19 N4 C20 C22 -4.1(16) . . . . ? N4 C19 C21 C23 0.8(15) . . . . ? N4 C20 C22 C23 2.4(16) . . . . ? C24 N5 C23 C22 147.2(11) . . . . ? C24 N5 C23 C21 -35.1(18) . . . . ? C20 C22 C23 N5 178.7(10) . . . . ? C20 C22 C23 C21 0.8(15) . . . . ? C19 C21 C23 N5 179.9(10) . . . . ? C19 C21 C23 C22 -2.4(15) . . . . ? C23 N5 C24 C25 0.1(19) . . . . ? C23 N5 C24 C26 -176.2(11) . . . . ? N5 C24 C25 C27 -175.3(10) . . . . ? C26 C24 C25 C27 0.8(16) . . . . ? N5 C24 C26 C28 174.8(11) . . . . ? C25 C24 C26 C28 -1.7(17) . . . . ? C28 N6 C27 C25 -1.3(17) . . . . ? C24 C25 C27 N6 0.7(17) . . . . ? C24 C26 C28 N6 1.1(18) . . . . ? C27 N6 C28 C26 0.4(18) . . . . ? _refine_diff_density_max 1.133 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.143 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957890' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H8 Mo5 O21 P2, C30 H22 Co N6, H2 O, H3 O' _chemical_formula_sum 'C38 H35 Co Mo5 N6 O23 P2' _chemical_formula_weight 1544.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 23.327(3) _cell_length_b 21.115(3) _cell_length_c 9.7462(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4800.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1005 _cell_measurement_theta_min 2.2728 _cell_measurement_theta_max 24.6117 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas 2.15(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.137 _exptl_crystal_F_000 3024 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.291 _exptl_crystal_size_mid 0.099 _exptl_crystal_size_min 0.059 _exptl_absorpt_coefficient_mu 1.763 _shelx_estimated_absorpt_T_min 0.628 _shelx_estimated_absorpt_T_max 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 0.90 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56796 _diffrn_reflns_av_unetI/netI 0.0512 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.995 _diffrn_reflns_theta_max 27.119 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 10565 _reflns_number_gt 9133 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.888 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.5799P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.50(4) _chemical_absolute_configuration ? _refine_ls_number_reflns 10565 _refine_ls_number_parameters 677 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.0903 _refine_ls_wR_factor_gt 0.0864 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.75696(3) -0.07686(4) 0.32527(8) 0.01853(18) Uani 1 1 d . . . . . Mo2 Mo 0.61693(3) -0.06515(4) 0.23037(7) 0.01616(17) Uani 1 1 d . . . . . Mo3 Mo 0.61298(3) 0.07301(4) -0.00162(7) 0.01656(17) Uani 1 1 d . . . . . Mo4 Mo 0.75036(3) 0.09118(4) -0.10536(8) 0.01780(17) Uani 1 1 d . . . . . Mo5 Mo 0.83816(3) 0.00636(4) 0.10279(10) 0.01834(16) Uani 1 1 d . . . . . Co1 Co 0.49721(5) 0.26827(4) 0.36109(15) 0.0127(2) Uani 1 1 d . . . . . P1 P 0.71081(10) 0.07357(10) 0.2376(2) 0.0153(5) Uani 1 1 d . . . . . P2 P 0.78928(10) 0.43757(10) 0.4819(2) 0.0142(5) Uani 1 1 d . . . . . O1 O 0.6986(3) 0.0042(3) 0.2806(6) 0.0142(13) Uani 1 1 d . . . . . O2 O 0.6802(3) -0.1126(3) 0.2978(6) 0.0198(14) Uani 1 1 d . . . . . O3 O 0.7550(3) -0.0660(3) 0.5004(7) 0.0276(16) Uani 1 1 d . . . . . O4 O 0.7927(3) -0.1470(3) 0.3053(7) 0.0245(15) Uani 1 1 d . . . . . O5 O 0.8162(3) -0.0161(3) 0.2878(6) 0.0201(14) Uani 1 1 d . . . . . O6 O 0.5942(3) -0.0347(3) 0.3914(7) 0.0246(14) Uani 1 1 d . . . . . O7 O 0.5651(3) -0.1211(3) 0.2036(7) 0.0233(15) Uani 1 1 d . . . . . O8 O 0.5926(2) 0.0036(3) 0.1123(8) 0.0188(11) Uani 1 1 d . . . . . O9 O 0.5895(3) 0.0428(3) -0.1647(7) 0.0216(14) Uani 1 1 d . . . . . O10 O 0.5607(3) 0.1266(3) 0.0274(7) 0.0267(16) Uani 1 1 d . . . . . O11 O 0.6551(3) 0.1029(3) 0.1858(6) 0.0181(13) Uani 1 1 d . . . . . O12 O 0.6732(3) 0.1234(3) -0.0712(6) 0.0201(14) Uani 1 1 d . . . . . O13 O 0.7454(3) 0.0814(3) -0.2793(7) 0.0264(16) Uani 1 1 d . . . . . O14 O 0.7858(3) 0.1616(3) -0.0867(7) 0.0268(15) Uani 1 1 d . . . . . O15 O 0.8116(3) 0.0305(3) -0.0777(6) 0.0212(14) Uani 1 1 d . . . . . O16 O 0.7594(3) 0.0756(3) 0.1288(6) 0.0173(14) Uani 1 1 d . . . . . O17 O 0.8828(3) -0.0542(3) 0.0597(8) 0.0308(17) Uani 1 1 d . . . . . O18 O 0.8831(3) 0.0678(3) 0.1388(8) 0.0289(17) Uani 1 1 d . . . . . O19 O 0.7403(3) 0.4362(3) 0.5879(7) 0.0186(13) Uani 1 1 d . . . . . O20 O 0.8042(3) 0.5068(3) 0.4405(6) 0.0160(14) Uani 1 1 d . . . . . O21 O 0.8427(3) 0.4062(3) 0.5386(6) 0.0171(13) Uani 1 1 d . . . . . C1 C 0.7342(4) 0.1175(4) 0.3871(9) 0.0203(19) Uani 1 1 d . . . . . H1A H 0.7068 0.1101 0.4603 0.024 Uiso 1 1 calc R U . . . H1B H 0.7707 0.1002 0.4168 0.024 Uiso 1 1 calc R U . . . C2 C 0.7412(4) 0.1891(4) 0.3697(9) 0.0174(19) Uani 1 1 d . . . . . C3 C 0.7807(4) 0.2152(4) 0.2761(10) 0.021(2) Uani 1 1 d . . . . . H3 H 0.8016 0.1883 0.2197 0.025 Uiso 1 1 calc R U . . . C4 C 0.7114(4) 0.2315(5) 0.4493(10) 0.021(2) Uani 1 1 d . . . . . H4 H 0.6852 0.2153 0.5122 0.025 Uiso 1 1 calc R U . . . C5 C 0.7892(4) 0.2804(4) 0.2660(10) 0.020(2) Uani 1 1 d . . . . . H5 H 0.8162 0.2959 0.2044 0.024 Uiso 1 1 calc R U . . . C6 C 0.7177(4) 0.2974(4) 0.4421(9) 0.0186(19) Uani 1 1 d . . . . . H6 H 0.6961 0.3237 0.4984 0.022 Uiso 1 1 calc R U . . . C7 C 0.7576(4) 0.3234(4) 0.3473(9) 0.0197(19) Uani 1 1 d . . . . . C8 C 0.7660(4) 0.3942(4) 0.3322(9) 0.0178(18) Uani 1 1 d . . . . . H8A H 0.7300 0.4124 0.3017 0.021 Uiso 1 1 calc R U . . . H8B H 0.7938 0.4013 0.2599 0.021 Uiso 1 1 calc R U . . . N1 N 0.4266(3) 0.2770(3) 0.4651(7) 0.0153(16) Uani 1 1 d . . . . . N2 N 0.4940(3) 0.3565(3) 0.3582(9) 0.0160(14) Uani 1 1 d . . . . . N3 N 0.5671(3) 0.2817(3) 0.2574(7) 0.0136(15) Uani 1 1 d . . . . . N4 N 0.5405(3) 0.2601(3) 0.5308(7) 0.0154(16) Uani 1 1 d . . . . . N5 N 0.4991(3) 0.1802(3) 0.3643(9) 0.0138(12) Uani 1 1 d . . . . . N6 N 0.4545(3) 0.2534(3) 0.1930(7) 0.0149(16) Uani 1 1 d . . . . . C9 C 0.3937(4) 0.2304(4) 0.5168(9) 0.0168(19) Uani 1 1 d . . . . . H9 H 0.4037 0.1885 0.4990 0.020 Uiso 1 1 calc R U . . . C10 C 0.3457(4) 0.2427(4) 0.5954(9) 0.0176(18) Uani 1 1 d . . . . . H10 H 0.3237 0.2096 0.6301 0.021 Uiso 1 1 calc R U . . . C11 C 0.3306(4) 0.3057(5) 0.6220(9) 0.023(2) Uani 1 1 d . . . . . H11 H 0.2986 0.3153 0.6748 0.027 Uiso 1 1 calc R U . . . C12 C 0.3640(4) 0.3531(4) 0.5687(9) 0.020(2) Uani 1 1 d . . . . . H12 H 0.3548 0.3951 0.5865 0.024 Uiso 1 1 calc R U . . . C13 C 0.4115(4) 0.3389(4) 0.4883(9) 0.0188(19) Uani 1 1 d . . . . . C14 C 0.4500(4) 0.3850(4) 0.4233(8) 0.0181(19) Uani 1 1 d . . . . . C15 C 0.4465(4) 0.4512(4) 0.4226(10) 0.024(2) Uani 1 1 d . . . . . H15 H 0.4172 0.4722 0.4682 0.029 Uiso 1 1 calc R U . . . C16 C 0.4882(4) 0.4842(4) 0.3517(12) 0.032(2) Uani 1 1 d . . . . . H16 H 0.4862 0.5281 0.3484 0.038 Uiso 1 1 calc R U . . . C17 C 0.5335(4) 0.4535(4) 0.2847(9) 0.025(2) Uani 1 1 d . . . . . H17 H 0.5615 0.4766 0.2387 0.030 Uiso 1 1 calc R U . . . C18 C 0.5356(4) 0.3876(4) 0.2884(9) 0.0172(19) Uani 1 1 d . . . . . C19 C 0.5775(4) 0.3444(4) 0.2269(9) 0.0173(18) Uani 1 1 d . . . . . C20 C 0.6238(4) 0.3620(5) 0.1503(10) 0.024(2) Uani 1 1 d . . . . . H20 H 0.6312 0.4046 0.1332 0.028 Uiso 1 1 calc R U . . . C21 C 0.6605(4) 0.3142(4) 0.0970(11) 0.023(2) Uani 1 1 d . . . . . H21 H 0.6916 0.3253 0.0425 0.028 Uiso 1 1 calc R U . . . C22 C 0.6022(4) 0.2375(4) 0.2084(9) 0.0148(18) Uani 1 1 d . . . . . H22 H 0.5949 0.1953 0.2294 0.018 Uiso 1 1 calc R U . . . C23 C 0.6500(4) 0.2522(4) 0.1257(8) 0.019(2) Uani 1 1 d . . . . . H23 H 0.6737 0.2204 0.0919 0.022 Uiso 1 1 calc R U . . . C24 C 0.5623(4) 0.3065(5) 0.6070(10) 0.025(2) Uani 1 1 d . . . . . H24 H 0.5570 0.3483 0.5795 0.029 Uiso 1 1 calc R U . . . C25 C 0.5928(4) 0.2942(5) 0.7268(11) 0.029(2) Uani 1 1 d . . . . . H25 H 0.6076 0.3273 0.7787 0.035 Uiso 1 1 calc R U . . . C26 C 0.6007(5) 0.2322(5) 0.7678(11) 0.034(3) Uani 1 1 d . . . . . H26 H 0.6205 0.2230 0.8482 0.041 Uiso 1 1 calc R U . . . C27 C 0.5788(5) 0.1841(6) 0.6879(12) 0.036(3) Uani 1 1 d . . . . . H27 H 0.5843 0.1420 0.7132 0.043 Uiso 1 1 calc R U . . . C28 C 0.5486(4) 0.1986(4) 0.5701(9) 0.0173(19) Uani 1 1 d . . . . . C29 C 0.5244(4) 0.1518(4) 0.4728(10) 0.0189(19) Uani 1 1 d . . . . . C30 C 0.5247(4) 0.0867(4) 0.4812(12) 0.025(2) Uani 1 1 d . . . . . H30 H 0.5412 0.0662 0.5558 0.030 Uiso 1 1 calc R U . . . C31 C 0.4998(4) 0.0526(4) 0.3756(14) 0.030(2) Uani 1 1 d . . . . . H31 H 0.5008 0.0086 0.3788 0.036 Uiso 1 1 calc R U . . . C32 C 0.4733(4) 0.0819(4) 0.2656(12) 0.025(2) Uani 1 1 d . . . . . H32 H 0.4559 0.0584 0.1965 0.031 Uiso 1 1 calc R U . . . C33 C 0.4739(4) 0.1479(4) 0.2621(10) 0.0168(19) Uani 1 1 d . . . . . C34 C 0.4487(4) 0.1912(4) 0.1612(10) 0.018(2) Uani 1 1 d . . . . . C35 C 0.4200(4) 0.1717(5) 0.0411(9) 0.024(2) Uani 1 1 d . . . . . H35 H 0.4170 0.1290 0.0189 0.029 Uiso 1 1 calc R U . . . C36 C 0.3966(5) 0.2173(5) -0.0422(10) 0.032(3) Uani 1 1 d . . . . . H36 H 0.3762 0.2055 -0.1202 0.038 Uiso 1 1 calc R U . . . C37 C 0.4032(4) 0.2807(5) -0.0106(11) 0.031(2) Uani 1 1 d . . . . . H37 H 0.3883 0.3117 -0.0684 0.037 Uiso 1 1 calc R U . . . C38 C 0.4325(4) 0.2980(4) 0.1093(10) 0.021(2) Uani 1 1 d . . . . . H38 H 0.4368 0.3406 0.1313 0.025 Uiso 1 1 calc R U . . . O90 O 0.6491(3) 0.0016(5) 0.6209(11) 0.062(2) Uani 1 1 d . . . . . H90A H 0.6269 0.0011 0.5519 0.093 Uiso 1 1 d R U . . . H90B H 0.6829 0.0131 0.5969 0.093 Uiso 1 1 d R U . . . O91 O 0.8432(3) 0.0018(3) 0.6504(6) 0.0317(16) 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 0.0209(4) 0.0205(4) 0.0142(4) 0.0043(3) 0.0020(3) 0.0080(3) Mo2 0.0159(4) 0.0157(4) 0.0170(4) 0.0009(3) 0.0026(3) 0.0008(3) Mo3 0.0177(4) 0.0145(4) 0.0174(4) 0.0010(3) -0.0032(3) -0.0007(3) Mo4 0.0204(4) 0.0194(4) 0.0135(3) 0.0034(3) -0.0021(3) -0.0081(3) Mo5 0.0147(3) 0.0219(4) 0.0185(3) 0.0013(3) -0.0013(4) -0.0013(4) Co1 0.0166(5) 0.0088(5) 0.0127(4) -0.0002(4) -0.0049(3) 0.0009(5) P1 0.0194(12) 0.0123(11) 0.0141(10) -0.0011(9) -0.0018(9) -0.0005(9) P2 0.0165(12) 0.0131(11) 0.0129(10) -0.0005(9) -0.0038(9) 0.0001(9) O1 0.016(3) 0.011(3) 0.015(3) 0.001(2) -0.001(2) 0.002(2) O2 0.028(4) 0.009(3) 0.022(3) 0.002(2) 0.003(3) 0.004(2) O3 0.031(4) 0.037(4) 0.015(3) 0.005(3) 0.004(3) 0.012(3) O4 0.026(3) 0.023(4) 0.025(3) 0.005(3) 0.005(3) 0.015(3) O5 0.020(3) 0.025(4) 0.015(3) -0.003(3) -0.005(2) 0.000(3) O6 0.027(4) 0.029(4) 0.018(3) -0.002(3) 0.005(3) 0.006(3) O7 0.021(4) 0.021(4) 0.028(4) -0.001(3) 0.005(3) -0.003(3) O8 0.016(2) 0.019(3) 0.022(2) -0.001(2) 0.002(3) 0.005(3) O9 0.020(3) 0.020(3) 0.025(3) 0.000(3) -0.007(3) -0.003(3) O10 0.029(4) 0.025(4) 0.027(4) 0.008(3) -0.006(3) 0.001(3) O11 0.022(3) 0.015(3) 0.017(3) -0.001(2) -0.003(3) 0.004(3) O12 0.019(3) 0.020(3) 0.022(3) 0.003(3) -0.006(3) -0.005(3) O13 0.033(4) 0.029(4) 0.017(3) 0.007(3) -0.005(3) -0.012(3) O14 0.029(4) 0.027(4) 0.025(3) 0.008(3) -0.002(3) -0.012(3) O15 0.018(3) 0.026(4) 0.020(3) 0.002(3) 0.008(3) -0.009(3) O16 0.021(3) 0.018(3) 0.013(3) -0.002(2) -0.004(2) -0.008(3) O17 0.021(4) 0.037(4) 0.034(4) 0.008(3) 0.006(3) 0.003(3) O18 0.027(4) 0.028(4) 0.032(4) 0.002(3) -0.009(3) -0.011(3) O19 0.020(3) 0.021(3) 0.015(3) 0.001(3) 0.001(3) -0.003(3) O20 0.016(3) 0.014(3) 0.018(3) -0.001(2) 0.000(2) 0.004(2) O21 0.020(3) 0.013(3) 0.018(3) -0.001(2) -0.008(2) 0.001(3) C1 0.025(5) 0.021(5) 0.015(4) -0.003(4) -0.007(4) -0.004(4) C2 0.018(4) 0.022(5) 0.012(4) -0.002(3) -0.008(3) 0.000(4) C3 0.022(5) 0.017(5) 0.023(5) -0.016(4) -0.006(4) 0.001(4) C4 0.018(5) 0.028(5) 0.017(4) -0.003(4) -0.001(4) -0.003(4) C5 0.014(4) 0.024(5) 0.020(5) -0.001(4) -0.002(4) -0.007(4) C6 0.020(5) 0.022(5) 0.013(4) 0.001(3) -0.001(3) -0.002(4) C7 0.014(4) 0.023(5) 0.021(5) -0.012(4) 0.002(4) -0.005(4) C8 0.019(4) 0.024(5) 0.011(4) -0.001(4) 0.004(4) 0.000(4) N1 0.018(4) 0.010(4) 0.017(4) -0.003(3) -0.007(3) 0.007(3) N2 0.022(4) 0.012(3) 0.015(3) -0.001(3) -0.004(2) -0.003(3) N3 0.016(4) 0.016(4) 0.009(3) 0.003(3) -0.005(3) 0.000(3) N4 0.016(4) 0.013(4) 0.017(4) 0.007(3) -0.007(3) -0.008(3) N5 0.012(3) 0.009(3) 0.020(3) 0.003(3) -0.001(2) -0.003(3) N6 0.015(4) 0.019(4) 0.011(3) 0.000(3) -0.002(3) 0.004(3) C9 0.024(5) 0.008(4) 0.018(4) 0.000(3) -0.009(4) 0.000(3) C10 0.028(5) 0.010(4) 0.015(4) -0.002(4) -0.003(4) 0.000(4) C11 0.020(5) 0.035(6) 0.014(5) -0.002(4) -0.005(3) 0.003(4) C12 0.032(5) 0.013(4) 0.016(4) -0.004(3) 0.000(4) 0.007(4) C13 0.027(5) 0.014(4) 0.016(4) -0.001(4) -0.002(4) 0.001(4) C14 0.024(5) 0.021(5) 0.009(4) -0.006(3) -0.004(3) 0.002(4) C15 0.033(6) 0.013(4) 0.027(5) 0.000(4) 0.004(4) 0.003(4) C16 0.044(7) 0.010(4) 0.042(5) -0.001(4) 0.002(5) 0.003(4) C17 0.035(6) 0.013(5) 0.027(5) 0.004(4) 0.009(4) -0.001(4) C18 0.022(5) 0.014(4) 0.016(4) 0.000(3) -0.005(3) 0.005(4) C19 0.027(5) 0.013(4) 0.012(4) 0.000(3) -0.004(4) 0.000(4) C20 0.035(6) 0.018(5) 0.019(4) 0.005(4) 0.004(4) -0.003(4) C21 0.019(5) 0.030(5) 0.021(4) 0.003(4) 0.003(4) -0.010(4) C22 0.016(4) 0.015(4) 0.014(4) 0.001(3) -0.003(3) 0.000(3) C23 0.019(5) 0.022(5) 0.015(4) -0.002(4) -0.006(3) -0.003(4) C24 0.028(5) 0.031(6) 0.015(4) 0.005(4) -0.002(4) -0.010(4) C25 0.030(6) 0.036(6) 0.023(5) 0.001(5) -0.015(4) -0.009(4) C26 0.037(6) 0.041(7) 0.024(5) -0.003(5) -0.014(4) 0.004(5) C27 0.028(6) 0.035(6) 0.044(7) 0.016(5) -0.009(5) 0.004(5) C28 0.014(4) 0.023(5) 0.016(5) 0.010(4) -0.004(3) -0.001(4) C29 0.007(4) 0.020(5) 0.030(5) 0.007(4) 0.002(3) 0.003(4) C30 0.008(4) 0.023(5) 0.043(6) 0.010(4) 0.001(4) -0.006(4) C31 0.019(4) 0.007(4) 0.063(7) 0.006(5) 0.010(4) -0.003(4) C32 0.020(5) 0.014(5) 0.042(6) -0.012(4) 0.010(4) -0.005(4) C33 0.011(4) 0.010(4) 0.030(5) -0.012(4) 0.004(4) 0.001(3) C34 0.014(5) 0.015(5) 0.025(5) -0.006(4) -0.002(4) 0.003(4) C35 0.025(5) 0.028(5) 0.019(5) -0.014(4) -0.003(4) 0.000(4) C36 0.030(6) 0.042(7) 0.024(5) -0.016(5) -0.008(4) 0.003(5) C37 0.022(5) 0.052(7) 0.020(5) 0.002(5) -0.005(4) 0.016(5) C38 0.022(5) 0.018(5) 0.023(5) -0.001(4) -0.006(4) 0.006(4) O90 0.032(4) 0.108(7) 0.046(5) -0.027(4) -0.003(5) -0.012(5) O91 0.034(4) 0.025(4) 0.036(4) 0.006(3) 0.005(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O4 1.710(6) . ? Mo1 O3 1.723(7) . ? Mo1 O5 1.920(7) . ? Mo1 O2 1.962(6) . ? Mo1 O1 2.230(6) . ? Mo1 O19 2.331(6) 3_644 ? Mo2 O7 1.711(6) . ? Mo2 O6 1.777(6) . ? Mo2 O2 1.900(6) . ? Mo2 O8 1.937(7) . ? Mo2 O21 2.179(6) 3_644 ? Mo2 O1 2.453(6) . ? Mo3 O10 1.688(7) . ? Mo3 O9 1.798(6) . ? Mo3 O12 1.888(6) . ? Mo3 O8 1.900(7) . ? Mo3 O11 2.169(6) . ? Mo3 O20 2.450(6) 3_644 ? Mo4 O14 1.711(6) . ? Mo4 O13 1.712(7) . ? Mo4 O15 1.938(7) . ? Mo4 O12 1.954(6) . ? Mo4 O20 2.236(6) 3_644 ? Mo4 O16 2.316(6) . ? Mo5 O17 1.700(7) . ? Mo5 O18 1.704(6) . ? Mo5 O5 1.934(6) . ? Mo5 O15 1.933(6) . ? Mo5 O19 2.358(6) 3_644 ? Mo5 O16 2.362(7) . ? Co1 N5 1.860(6) . ? Co1 N2 1.864(6) . ? Co1 N3 1.938(7) . ? Co1 N1 1.942(8) . ? Co1 N6 1.943(7) . ? Co1 N4 1.946(7) . ? P1 O11 1.525(6) . ? P1 O1 1.550(6) . ? P1 O16 1.553(7) . ? P1 C1 1.812(9) . ? P2 O21 1.515(6) . ? P2 O19 1.541(7) . ? P2 O20 1.555(6) . ? P2 C8 1.806(9) . ? O19 Mo1 2.331(6) 3_655 ? O19 Mo5 2.358(6) 3_655 ? O20 Mo4 2.236(6) 3_655 ? O20 Mo3 2.451(6) 3_655 ? O21 Mo2 2.179(6) 3_655 ? C1 C2 1.529(12) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.373(12) . ? C2 C3 1.409(13) . ? C3 C5 1.395(12) . ? C3 H3 0.9300 . ? C4 C6 1.401(13) . ? C4 H4 0.9300 . ? C5 C7 1.412(12) . ? C5 H5 0.9300 . ? C6 C7 1.422(12) . ? C6 H6 0.9300 . ? C7 C8 1.516(12) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N1 C9 1.346(11) . ? N1 C13 1.373(11) . ? N2 C14 1.349(11) . ? N2 C18 1.354(12) . ? N3 C22 1.329(11) . ? N3 C19 1.379(11) . ? N4 C24 1.330(12) . ? N4 C28 1.367(11) . ? N5 C33 1.343(12) . ? N5 C29 1.352(12) . ? N6 C38 1.347(11) . ? N6 C34 1.355(11) . ? C9 C10 1.383(13) . ? C9 H9 0.9300 . ? C10 C11 1.401(12) . ? C10 H10 0.9300 . ? C11 C12 1.369(13) . ? C11 H11 0.9300 . ? C12 C13 1.389(12) . ? C12 H12 0.9300 . ? C13 C14 1.466(12) . ? C14 C15 1.400(12) . ? C15 C16 1.382(13) . ? C15 H15 0.9300 . ? C16 C17 1.401(14) . ? C16 H16 0.9300 . ? C17 C18 1.393(12) . ? C17 H17 0.9300 . ? C18 C19 1.466(12) . ? C19 C20 1.364(13) . ? C20 C21 1.422(13) . ? C20 H20 0.9300 . ? C21 C23 1.362(12) . ? C21 H21 0.9300 . ? C22 C23 1.411(12) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.392(13) . ? C24 H24 0.9300 . ? C25 C26 1.381(15) . ? C25 H25 0.9300 . ? C26 C27 1.378(16) . ? C26 H26 0.9300 . ? C27 C28 1.383(14) . ? C27 H27 0.9300 . ? C28 C29 1.481(13) . ? C29 C30 1.377(13) . ? C30 C31 1.384(16) . ? C30 H30 0.9300 . ? C31 C32 1.383(16) . ? C31 H31 0.9300 . ? C32 C33 1.395(12) . ? C32 H32 0.9300 . ? C33 C34 1.465(13) . ? C34 C35 1.410(13) . ? C35 C36 1.374(14) . ? C35 H35 0.9300 . ? C36 C37 1.382(15) . ? C36 H36 0.9300 . ? C37 C38 1.402(13) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? O90 H90A 0.8488 . ? O90 H90B 0.8575 . ? 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 O4 Mo1 O3 103.9(3) . . ? O4 Mo1 O5 101.9(3) . . ? O3 Mo1 O5 96.8(3) . . ? O4 Mo1 O2 95.6(3) . . ? O3 Mo1 O2 99.4(3) . . ? O5 Mo1 O2 152.6(3) . . ? O4 Mo1 O1 160.0(3) . . ? O3 Mo1 O1 94.3(3) . . ? O5 Mo1 O1 83.6(3) . . ? O2 Mo1 O1 73.2(2) . . ? O4 Mo1 O19 88.6(3) . 3_644 ? O3 Mo1 O19 165.5(3) . 3_644 ? O5 Mo1 O19 73.3(2) . 3_644 ? O2 Mo1 O19 86.3(2) . 3_644 ? O1 Mo1 O19 74.4(2) . 3_644 ? O7 Mo2 O6 100.0(3) . . ? O7 Mo2 O2 103.8(3) . . ? O6 Mo2 O2 96.7(3) . . ? O7 Mo2 O8 102.7(3) . . ? O6 Mo2 O8 99.6(3) . . ? O2 Mo2 O8 145.9(2) . . ? O7 Mo2 O21 89.0(3) . 3_644 ? O6 Mo2 O21 170.8(3) . 3_644 ? O2 Mo2 O21 79.3(2) . 3_644 ? O8 Mo2 O21 79.9(3) . 3_644 ? O7 Mo2 O1 172.8(3) . . ? O6 Mo2 O1 80.7(3) . . ? O2 Mo2 O1 69.1(2) . . ? O8 Mo2 O1 84.2(2) . . ? O21 Mo2 O1 90.0(2) 3_644 . ? O10 Mo3 O9 99.6(3) . . ? O10 Mo3 O12 102.6(3) . . ? O9 Mo3 O12 96.3(3) . . ? O10 Mo3 O8 103.8(3) . . ? O9 Mo3 O8 99.6(3) . . ? O12 Mo3 O8 146.2(2) . . ? O10 Mo3 O11 89.5(3) . . ? O9 Mo3 O11 170.4(3) . . ? O12 Mo3 O11 78.5(2) . . ? O8 Mo3 O11 81.1(3) . . ? O10 Mo3 O20 172.2(3) . 3_644 ? O9 Mo3 O20 80.4(2) . 3_644 ? O12 Mo3 O20 69.7(2) . 3_644 ? O8 Mo3 O20 83.8(2) . 3_644 ? O11 Mo3 O20 90.1(2) . 3_644 ? O14 Mo4 O13 104.0(3) . . ? O14 Mo4 O15 101.7(3) . . ? O13 Mo4 O15 96.2(3) . . ? O14 Mo4 O12 97.1(3) . . ? O13 Mo4 O12 98.6(3) . . ? O15 Mo4 O12 152.4(3) . . ? O14 Mo4 O20 161.2(3) . 3_644 ? O13 Mo4 O20 93.7(3) . 3_644 ? O15 Mo4 O20 82.3(2) . 3_644 ? O12 Mo4 O20 73.7(2) . 3_644 ? O14 Mo4 O16 88.5(3) . . ? O13 Mo4 O16 164.9(3) . . ? O15 Mo4 O16 72.6(2) . . ? O12 Mo4 O16 88.0(2) . . ? O20 Mo4 O16 75.0(2) 3_644 . ? O17 Mo5 O18 104.3(3) . . ? O17 Mo5 O5 102.0(3) . . ? O18 Mo5 O5 99.1(3) . . ? O17 Mo5 O15 99.8(3) . . ? O18 Mo5 O15 100.6(3) . . ? O5 Mo5 O15 145.9(2) . . ? O17 Mo5 O19 89.3(3) . 3_644 ? O18 Mo5 O19 165.4(3) . 3_644 ? O5 Mo5 O19 72.4(2) . 3_644 ? O15 Mo5 O19 82.0(2) . 3_644 ? O17 Mo5 O16 165.4(3) . . ? O18 Mo5 O16 89.1(3) . . ? O5 Mo5 O16 81.1(2) . . ? O15 Mo5 O16 71.6(2) . . ? O19 Mo5 O16 78.00(17) 3_644 . ? N5 Co1 N2 179.1(3) . . ? N5 Co1 N3 97.7(3) . . ? N2 Co1 N3 83.1(3) . . ? N5 Co1 N1 96.1(3) . . ? N2 Co1 N1 83.1(3) . . ? N3 Co1 N1 166.2(3) . . ? N5 Co1 N6 82.2(3) . . ? N2 Co1 N6 97.4(3) . . ? N3 Co1 N6 90.9(3) . . ? N1 Co1 N6 91.2(3) . . ? N5 Co1 N4 83.4(3) . . ? N2 Co1 N4 97.0(3) . . ? N3 Co1 N4 91.1(3) . . ? N1 Co1 N4 90.3(3) . . ? N6 Co1 N4 165.6(3) . . ? O11 P1 O1 108.5(4) . . ? O11 P1 O16 112.6(4) . . ? O1 P1 O16 110.2(3) . . ? O11 P1 C1 108.3(4) . . ? O1 P1 C1 108.8(4) . . ? O16 P1 C1 108.4(4) . . ? O21 P2 O19 111.0(4) . . ? O21 P2 O20 108.7(4) . . ? O19 P2 O20 110.9(3) . . ? O21 P2 C8 108.7(4) . . ? O19 P2 C8 108.0(4) . . ? O20 P2 C8 109.5(4) . . ? P1 O1 Mo1 131.8(4) . . ? P1 O1 Mo2 130.8(3) . . ? Mo1 O1 Mo2 93.14(19) . . ? Mo2 O2 Mo1 123.6(3) . . ? Mo1 O5 Mo5 122.2(3) . . ? Mo3 O8 Mo2 148.4(3) . . ? P1 O11 Mo3 123.1(4) . . ? Mo3 O12 Mo4 123.4(3) . . ? Mo5 O15 Mo4 122.5(3) . . ? P1 O16 Mo4 127.6(4) . . ? P1 O16 Mo5 128.6(4) . . ? Mo4 O16 Mo5 93.0(2) . . ? P2 O19 Mo1 130.3(4) . 3_655 ? P2 O19 Mo5 127.3(4) . 3_655 ? Mo1 O19 Mo5 92.0(2) 3_655 3_655 ? P2 O20 Mo4 132.3(4) . 3_655 ? P2 O20 Mo3 130.8(3) . 3_655 ? Mo4 O20 Mo3 92.3(2) 3_655 3_655 ? P2 O21 Mo2 123.2(3) . 3_655 ? C2 C1 P1 116.7(6) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C4 C2 C3 116.2(8) . . ? C4 C2 C1 121.8(8) . . ? C3 C2 C1 121.9(8) . . ? C5 C3 C2 121.7(8) . . ? C5 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C2 C4 C6 124.5(9) . . ? C2 C4 H4 117.8 . . ? C6 C4 H4 117.8 . . ? C3 C5 C7 121.4(9) . . ? C3 C5 H5 119.3 . . ? C7 C5 H5 119.3 . . ? C4 C6 C7 119.0(8) . . ? C4 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C5 C7 C6 117.3(8) . . ? C5 C7 C8 120.8(8) . . ? C6 C7 C8 121.9(8) . . ? C7 C8 P2 117.4(6) . . ? C7 C8 H8A 107.9 . . ? P2 C8 H8A 107.9 . . ? C7 C8 H8B 107.9 . . ? P2 C8 H8B 107.9 . . ? H8A C8 H8B 107.2 . . ? C9 N1 C13 119.2(8) . . ? C9 N1 Co1 127.5(6) . . ? C13 N1 Co1 113.2(6) . . ? C14 N2 C18 124.4(7) . . ? C14 N2 Co1 117.9(6) . . ? C18 N2 Co1 117.6(6) . . ? C22 N3 C19 119.2(8) . . ? C22 N3 Co1 127.1(6) . . ? C19 N3 Co1 113.6(6) . . ? C24 N4 C28 119.4(8) . . ? C24 N4 Co1 127.4(6) . . ? C28 N4 Co1 113.2(6) . . ? C33 N5 C29 123.1(6) . . ? C33 N5 Co1 119.0(6) . . ? C29 N5 Co1 117.9(6) . . ? C38 N6 C34 120.0(8) . . ? C38 N6 Co1 126.3(6) . . ? C34 N6 Co1 113.6(6) . . ? N1 C9 C10 122.2(8) . . ? N1 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C9 C10 C11 118.9(9) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 118.7(9) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 120.7(9) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? N1 C13 C12 120.1(8) . . ? N1 C13 C14 113.8(8) . . ? C12 C13 C14 126.1(8) . . ? N2 C14 C15 119.1(8) . . ? N2 C14 C13 111.9(7) . . ? C15 C14 C13 129.0(8) . . ? C16 C15 C14 117.8(9) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C15 C16 C17 122.0(8) . . ? C15 C16 H16 119.0 . . ? C17 C16 H16 119.0 . . ? C18 C17 C16 118.4(9) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? N2 C18 C17 118.3(8) . . ? N2 C18 C19 112.4(8) . . ? C17 C18 C19 129.3(8) . . ? C20 C19 N3 121.3(8) . . ? C20 C19 C18 125.6(8) . . ? N3 C19 C18 113.1(8) . . ? C19 C20 C21 118.8(9) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C23 C21 C20 120.0(9) . . ? C23 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? N3 C22 C23 122.6(8) . . ? N3 C22 H22 118.7 . . ? C23 C22 H22 118.7 . . ? C21 C23 C22 118.0(9) . . ? C21 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? N4 C24 C25 121.7(9) . . ? N4 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C26 C25 C24 119.2(9) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C27 C26 C25 119.1(10) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C26 C27 C28 119.6(10) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? N4 C28 C27 120.9(9) . . ? N4 C28 C29 113.8(7) . . ? C27 C28 C29 125.3(9) . . ? N5 C29 C30 119.5(9) . . ? N5 C29 C28 111.7(7) . . ? C30 C29 C28 128.8(9) . . ? C29 C30 C31 118.2(9) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C30 C31 C32 122.1(8) . . ? C30 C31 H31 118.9 . . ? C32 C31 H31 118.9 . . ? C31 C32 C33 117.5(9) . . ? C31 C32 H32 121.2 . . ? C33 C32 H32 121.2 . . ? N5 C33 C32 119.6(9) . . ? N5 C33 C34 110.9(7) . . ? C32 C33 C34 129.5(9) . . ? N6 C34 C35 121.4(9) . . ? N6 C34 C33 114.3(8) . . ? C35 C34 C33 124.4(8) . . ? C36 C35 C34 118.3(9) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C35 C36 C37 120.3(9) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C36 C37 C38 119.4(10) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? N6 C38 C37 120.6(9) . . ? N6 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? H90A O90 H90B 110.4 . . ? 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 O11 P1 O1 Mo1 165.7(4) . . . . ? O16 P1 O1 Mo1 41.9(6) . . . . ? C1 P1 O1 Mo1 -76.7(5) . . . . ? O11 P1 O1 Mo2 15.5(5) . . . . ? O16 P1 O1 Mo2 -108.2(5) . . . . ? C1 P1 O1 Mo2 133.1(5) . . . . ? O7 Mo2 O2 Mo1 171.6(4) . . . . ? O6 Mo2 O2 Mo1 -86.3(4) . . . . ? O8 Mo2 O2 Mo1 31.8(7) . . . . ? O21 Mo2 O2 Mo1 85.2(4) 3_644 . . . ? O1 Mo2 O2 Mo1 -9.0(3) . . . . ? O1 P1 O11 Mo3 -67.5(5) . . . . ? O16 P1 O11 Mo3 54.8(5) . . . . ? C1 P1 O11 Mo3 174.6(4) . . . . ? O10 Mo3 O12 Mo4 172.4(4) . . . . ? O9 Mo3 O12 Mo4 -86.3(4) . . . . ? O8 Mo3 O12 Mo4 31.5(7) . . . . ? O11 Mo3 O12 Mo4 85.6(4) . . . . ? O20 Mo3 O12 Mo4 -8.9(3) 3_644 . . . ? O11 P1 O16 Mo4 -17.8(5) . . . . ? O1 P1 O16 Mo4 103.5(4) . . . . ? C1 P1 O16 Mo4 -137.6(4) . . . . ? O11 P1 O16 Mo5 -152.3(4) . . . . ? O1 P1 O16 Mo5 -31.0(5) . . . . ? C1 P1 O16 Mo5 87.9(5) . . . . ? O21 P2 O19 Mo1 20.3(6) . . . 3_655 ? O20 P2 O19 Mo1 -100.7(5) . . . 3_655 ? C8 P2 O19 Mo1 139.3(4) . . . 3_655 ? O21 P2 O19 Mo5 154.9(4) . . . 3_655 ? O20 P2 O19 Mo5 34.0(5) . . . 3_655 ? C8 P2 O19 Mo5 -86.0(5) . . . 3_655 ? O21 P2 O20 Mo4 -164.1(4) . . . 3_655 ? O19 P2 O20 Mo4 -41.8(6) . . . 3_655 ? C8 P2 O20 Mo4 77.2(5) . . . 3_655 ? O21 P2 O20 Mo3 -15.2(5) . . . 3_655 ? O19 P2 O20 Mo3 107.1(5) . . . 3_655 ? C8 P2 O20 Mo3 -133.8(5) . . . 3_655 ? O19 P2 O21 Mo2 -55.3(5) . . . 3_655 ? O20 P2 O21 Mo2 67.0(5) . . . 3_655 ? C8 P2 O21 Mo2 -173.9(4) . . . 3_655 ? O11 P1 C1 C2 -54.9(8) . . . . ? O1 P1 C1 C2 -172.6(6) . . . . ? O16 P1 C1 C2 67.6(8) . . . . ? P1 C1 C2 C4 121.7(8) . . . . ? P1 C1 C2 C3 -61.6(10) . . . . ? C4 C2 C3 C5 0.4(12) . . . . ? C1 C2 C3 C5 -176.4(8) . . . . ? C3 C2 C4 C6 0.4(13) . . . . ? C1 C2 C4 C6 177.3(8) . . . . ? C2 C3 C5 C7 -1.3(13) . . . . ? C2 C4 C6 C7 -0.4(13) . . . . ? C3 C5 C7 C6 1.3(13) . . . . ? C3 C5 C7 C8 -178.2(8) . . . . ? C4 C6 C7 C5 -0.5(12) . . . . ? C4 C6 C7 C8 179.0(8) . . . . ? C5 C7 C8 P2 -120.4(8) . . . . ? C6 C7 C8 P2 60.1(10) . . . . ? O21 P2 C8 C7 52.8(7) . . . . ? O19 P2 C8 C7 -67.7(7) . . . . ? O20 P2 C8 C7 171.4(6) . . . . ? N3 Co1 N2 C14 -178.9(7) . . . . ? N1 Co1 N2 C14 0.8(7) . . . . ? N6 Co1 N2 C14 91.1(7) . . . . ? N4 Co1 N2 C14 -88.6(7) . . . . ? N3 Co1 N2 C18 2.4(7) . . . . ? N1 Co1 N2 C18 -177.8(7) . . . . ? N6 Co1 N2 C18 -87.6(7) . . . . ? N4 Co1 N2 C18 92.7(7) . . . . ? N3 Co1 N5 C33 -89.4(7) . . . . ? N1 Co1 N5 C33 90.8(7) . . . . ? N6 Co1 N5 C33 0.4(7) . . . . ? N4 Co1 N5 C33 -179.6(7) . . . . ? N3 Co1 N5 C29 92.8(7) . . . . ? N1 Co1 N5 C29 -87.0(7) . . . . ? N6 Co1 N5 C29 -177.4(7) . . . . ? N4 Co1 N5 C29 2.6(7) . . . . ? C13 N1 C9 C10 -1.4(13) . . . . ? Co1 N1 C9 C10 176.7(6) . . . . ? N1 C9 C10 C11 0.1(13) . . . . ? C9 C10 C11 C12 0.2(13) . . . . ? C10 C11 C12 C13 0.8(14) . . . . ? C9 N1 C13 C12 2.4(13) . . . . ? Co1 N1 C13 C12 -175.9(7) . . . . ? C9 N1 C13 C14 -178.4(7) . . . . ? Co1 N1 C13 C14 3.3(9) . . . . ? C11 C12 C13 N1 -2.1(14) . . . . ? C11 C12 C13 C14 178.7(9) . . . . ? C18 N2 C14 C15 -1.3(14) . . . . ? Co1 N2 C14 C15 -179.9(6) . . . . ? C18 N2 C14 C13 179.3(8) . . . . ? Co1 N2 C14 C13 0.7(10) . . . . ? N1 C13 C14 N2 -2.6(11) . . . . ? C12 C13 C14 N2 176.5(9) . . . . ? N1 C13 C14 C15 178.1(8) . . . . ? C12 C13 C14 C15 -2.7(15) . . . . ? N2 C14 C15 C16 1.5(13) . . . . ? C13 C14 C15 C16 -179.3(9) . . . . ? C14 C15 C16 C17 -1.4(15) . . . . ? C15 C16 C17 C18 1.1(15) . . . . ? C14 N2 C18 C17 1.0(14) . . . . ? Co1 N2 C18 C17 179.6(6) . . . . ? C14 N2 C18 C19 -179.3(8) . . . . ? Co1 N2 C18 C19 -0.7(10) . . . . ? C16 C17 C18 N2 -0.8(13) . . . . ? C16 C17 C18 C19 179.6(9) . . . . ? C22 N3 C19 C20 -1.5(12) . . . . ? Co1 N3 C19 C20 -177.6(7) . . . . ? C22 N3 C19 C18 -179.7(7) . . . . ? Co1 N3 C19 C18 4.2(9) . . . . ? N2 C18 C19 C20 179.6(9) . . . . ? C17 C18 C19 C20 -0.7(15) . . . . ? N2 C18 C19 N3 -2.3(10) . . . . ? C17 C18 C19 N3 177.3(9) . . . . ? N3 C19 C20 C21 2.4(14) . . . . ? C18 C19 C20 C21 -179.7(9) . . . . ? C19 C20 C21 C23 -1.7(15) . . . . ? C19 N3 C22 C23 -0.1(12) . . . . ? Co1 N3 C22 C23 175.5(6) . . . . ? C20 C21 C23 C22 0.3(14) . . . . ? N3 C22 C23 C21 0.7(13) . . . . ? C28 N4 C24 C25 -0.5(14) . . . . ? Co1 N4 C24 C25 -179.8(7) . . . . ? N4 C24 C25 C26 0.0(16) . . . . ? C24 C25 C26 C27 0.8(17) . . . . ? C25 C26 C27 C28 -1.1(17) . . . . ? C24 N4 C28 C27 0.2(14) . . . . ? Co1 N4 C28 C27 179.6(8) . . . . ? C24 N4 C28 C29 -177.3(8) . . . . ? Co1 N4 C28 C29 2.1(10) . . . . ? C26 C27 C28 N4 0.7(16) . . . . ? C26 C27 C28 C29 177.9(10) . . . . ? C33 N5 C29 C30 -0.1(15) . . . . ? Co1 N5 C29 C30 177.6(7) . . . . ? C33 N5 C29 C28 -179.7(7) . . . . ? Co1 N5 C29 C28 -2.1(10) . . . . ? N4 C28 C29 N5 -0.1(11) . . . . ? C27 C28 C29 N5 -177.5(9) . . . . ? N4 C28 C29 C30 -179.7(9) . . . . ? C27 C28 C29 C30 2.9(16) . . . . ? N5 C29 C30 C31 1.2(14) . . . . ? C28 C29 C30 C31 -179.2(9) . . . . ? C29 C30 C31 C32 -2.0(16) . . . . ? C30 C31 C32 C33 1.7(16) . . . . ? C29 N5 C33 C32 -0.3(15) . . . . ? Co1 N5 C33 C32 -177.9(7) . . . . ? C29 N5 C33 C34 178.2(7) . . . . ? Co1 N5 C33 C34 0.6(10) . . . . ? C31 C32 C33 N5 -0.5(14) . . . . ? C31 C32 C33 C34 -178.7(9) . . . . ? C38 N6 C34 C35 0.2(13) . . . . ? Co1 N6 C34 C35 -178.6(7) . . . . ? C38 N6 C34 C33 -179.2(8) . . . . ? Co1 N6 C34 C33 2.1(10) . . . . ? N5 C33 C34 N6 -1.7(11) . . . . ? C32 C33 C34 N6 176.6(9) . . . . ? N5 C33 C34 C35 178.9(9) . . . . ? C32 C33 C34 C35 -2.8(16) . . . . ? N6 C34 C35 C36 -1.6(14) . . . . ? C33 C34 C35 C36 177.7(9) . . . . ? C34 C35 C36 C37 2.4(15) . . . . ? C35 C36 C37 C38 -1.9(16) . . . . ? C34 N6 C38 C37 0.4(13) . . . . ? Co1 N6 C38 C37 179.0(7) . . . . ? C36 C37 C38 N6 0.5(15) . . . . ? _refine_diff_density_max 1.212 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.126 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957891' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ' C8 H8 Mo5 O21 P2, C30 H24 Co N6, 6(H2 O), H3 O' _chemical_formula_sum 'C38 H47 Co Mo5 N6 O28 P2' _chemical_formula_weight 1636.38 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' 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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.574(3) _cell_length_b 17.358(3) _cell_length_c 20.413(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5164.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 371 _cell_measurement_theta_min 3.1410 _cell_measurement_theta_max 19.5026 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_density_meas 2.05(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.106 _exptl_crystal_F_000 3236 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_absorpt_coefficient_mu 1.652 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.97 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 54251 _diffrn_reflns_av_unetI/netI 0.0655 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.717 _diffrn_reflns_theta_max 25.681 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 9786 _reflns_number_gt 8527 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.811 _reflns_Friedel_fraction_max 0.996 _reflns_Friedel_fraction_full 0.997 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 3425 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.537(16) _chemical_absolute_configuration unk _refine_ls_number_reflns 9786 _refine_ls_number_parameters 757 _refine_ls_number_restraints 273 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.46730(5) 1.05527(4) 0.04360(3) 0.00945(17) Uani 1 1 d . U . . . Mo2 Mo 0.41800(5) 1.20117(4) 0.14679(4) 0.01001(17) Uani 1 1 d . U . . . Mo3 Mo 0.22436(5) 1.16188(4) 0.22870(4) 0.00943(17) Uani 1 1 d . U . . . Mo4 Mo 0.12277(5) 0.99822(4) 0.15184(3) 0.00906(16) Uani 1 1 d . U . . . Mo5 Mo 0.31402(5) 0.91297(4) 0.06053(4) 0.00916(17) Uani 1 1 d . U . . . Co1 Co 0.77506(8) 0.91804(7) 0.89269(5) 0.0082(2) Uani 1 1 d . U . . . P1 P 0.36256(15) 1.01276(13) 0.19342(10) 0.0085(5) Uani 1 1 d . U . . . P2 P 0.25662(15) 0.88578(12) 0.56068(11) 0.0085(5) Uani 1 1 d . U . . . O1 O 0.4377(4) 0.9494(3) 0.0505(3) 0.0112(12) Uani 1 1 d . U . . . O2 O 0.4729(4) 1.0668(3) -0.0396(3) 0.0146(13) Uani 1 1 d . U . . . O3 O 0.5791(4) 1.0493(3) 0.0668(3) 0.0153(13) Uani 1 1 d . U . . . O4 O 0.4447(4) 1.1638(3) 0.0616(3) 0.0095(12) Uani 1 1 d . U . . . O5 O 0.4252(4) 1.0667(3) 0.1541(3) 0.0090(12) Uani 1 1 d . U . . . O6 O 0.5239(4) 1.2070(4) 0.1821(3) 0.0158(14) Uani 1 1 d . U . . . O7 O 0.3912(4) 1.2943(3) 0.1296(3) 0.0154(14) Uani 1 1 d . U . . . O8 O 0.3485(4) 1.1861(3) 0.2280(3) 0.0116(13) Uani 1 1 d . U . . . O9 O 0.1708(4) 1.2490(3) 0.2193(3) 0.0169(14) Uani 1 1 d . U . . . O10 O 0.2135(4) 1.1435(3) 0.3095(3) 0.0161(14) Uani 1 1 d . U . . . O11 O 0.1088(4) 1.1042(3) 0.1960(3) 0.0097(12) Uani 1 1 d . U . . . O12 O 0.2645(4) 1.0469(3) 0.1997(3) 0.0087(12) Uani 1 1 d . U . . . O13 O 0.0149(4) 0.9870(3) 0.1215(3) 0.0151(14) Uani 1 1 d . U . . . O14 O 0.1152(4) 0.9495(3) 0.2247(3) 0.0118(12) Uani 1 1 d . U . . . O15 O 0.1936(4) 0.9305(3) 0.1018(3) 0.0104(12) Uani 1 1 d . U . . . O16 O 0.3561(4) 0.9337(3) 0.1638(3) 0.0111(13) Uani 1 1 d . U . . . O17 O 0.3348(4) 0.8179(3) 0.0735(3) 0.0145(14) Uani 1 1 d . U . . . O18 O 0.2793(4) 0.9135(3) -0.0191(3) 0.0139(13) Uani 1 1 d . U . . . O19 O 0.1854(4) 0.9502(3) 0.5503(3) 0.0092(12) Uani 1 1 d . U . . . O20 O 0.2295(4) 0.8317(3) 0.6175(3) 0.0096(12) Uani 1 1 d . U . . . O21 O 0.3497(4) 0.9216(3) 0.5725(3) 0.0085(12) Uani 1 1 d . U . . . O90 O 0.4835(5) 0.8130(4) 0.1982(3) 0.0220(16) Uani 1 1 d D . . . . H90A H 0.453(6) 0.853(3) 0.203(4) 0.026 Uiso 1 1 d D U . . . H90B H 0.493(7) 0.797(5) 0.237(2) 0.026 Uiso 1 1 d D U . . . O91 O 0.9524(6) 0.3041(5) 0.4367(4) 0.048(2) Uani 1 1 d D . . . . H91A H 0.987(7) 0.305(6) 0.403(4) 0.058 Uiso 1 1 d D U . . . H91B H 0.931(8) 0.349(3) 0.442(6) 0.058 Uiso 1 1 d D U . . . O92 O 0.9587(6) 0.3605(4) 0.1703(3) 0.0353(19) Uani 1 1 d D . . . . H92A H 0.926(7) 0.388(5) 0.194(4) 0.042 Uiso 1 1 d D U . . . H92B H 0.954(8) 0.380(5) 0.132(2) 0.042 Uiso 1 1 d D U . . . O93 O 0.9836(5) 0.1968(4) 0.1491(3) 0.0246(16) Uani 1 1 d D . . . . H93A H 0.961(7) 0.155(3) 0.158(4) 0.030 Uiso 1 1 d D U . . . H93B H 0.983(7) 0.225(4) 0.182(3) 0.030 Uiso 1 1 d D U . . . O94 O 0.0421(7) 0.2577(5) 0.0356(4) 0.043(2) Uani 1 1 d D . . . . H94A H 0.005(6) 0.281(5) 0.012(5) 0.051 Uiso 1 1 d D U . . . H94B H 0.070(7) 0.283(5) 0.064(4) 0.051 Uiso 1 1 d D U . . . O95A O 0.1656(16) 0.3304(14) 0.1059(11) 0.024(8) Uiso 0.34(3) 1 d . . P A 1 O95B O 0.1340(9) 0.3612(8) 0.1265(6) 0.028(4) Uiso 0.66(3) 1 d . . P A 2 O96 O 0.0390(10) 0.3169(7) 0.3104(5) 0.095(4) Uani 1 1 d D . . . . H96A H 0.030(13) 0.276(5) 0.333(6) 0.114 Uiso 1 1 d D U . . . H96B H 0.060(12) 0.302(8) 0.273(4) 0.114 Uiso 1 1 d D U . . . N1 N 0.6430(5) 0.9270(4) 0.8920(3) 0.0082(14) Uani 1 1 d . U . . . N2 N 0.7539(5) 0.8567(4) 0.9701(3) 0.0095(15) Uani 1 1 d . U . . . N3 N 0.8000(5) 1.0024(4) 0.9513(3) 0.0104(14) Uani 1 1 d . U . . . N4 N 0.9051(5) 0.9031(4) 0.8980(3) 0.0113(15) Uani 1 1 d . U . . . N5 N 0.7967(5) 0.9797(4) 0.8151(3) 0.0084(15) Uani 1 1 d . U . . . N6 N 0.7574(5) 0.8375(4) 0.8295(3) 0.0090(15) Uani 1 1 d . U . . . C1 C 0.5921(6) 0.9562(5) 0.8440(4) 0.0110(18) Uani 1 1 d . U . . . H1 H 0.6204 0.9849 0.8113 0.013 Uiso 1 1 calc R U . . . C2 C 0.4983(6) 0.9451(5) 0.8413(4) 0.0160(19) Uani 1 1 d . U . . . H2 H 0.4641 0.9665 0.8075 0.019 Uiso 1 1 calc R U . . . C3 C 0.4555(6) 0.9016(5) 0.8899(4) 0.0136(19) Uani 1 1 d . U . . . H3 H 0.3926 0.8927 0.8884 0.016 Uiso 1 1 calc R U . . . C4 C 0.5073(6) 0.8721(5) 0.9399(4) 0.0128(19) Uani 1 1 d . U . . . H4 H 0.4803 0.8433 0.9731 0.015 Uiso 1 1 calc R U . . . C5 C 0.6017(6) 0.8862(4) 0.9400(4) 0.0083(17) Uani 1 1 d . U . . . C6 C 0.6644(6) 0.8539(5) 0.9897(4) 0.0108(18) Uani 1 1 d . U . . . C7 C 0.6379(6) 0.8262(5) 1.0493(4) 0.0136(19) Uani 1 1 d . U . . . H7 H 0.5765 0.8267 1.0617 0.016 Uiso 1 1 calc R U . . . C8 C 0.7050(7) 0.7973(5) 1.0910(4) 0.020(2) Uani 1 1 d . U . . . H8 H 0.6892 0.7794 1.1325 0.023 Uiso 1 1 calc R U . . . C9 C 0.7959(6) 0.7953(5) 1.0704(4) 0.019(2) Uani 1 1 d . U . . . H9 H 0.8414 0.7738 1.0966 0.023 Uiso 1 1 calc R U . . . C10 C 0.8164(6) 0.8259(5) 1.0102(4) 0.0125(18) Uani 1 1 d . U . . . H10 H 0.8772 0.8251 0.9964 0.015 Uiso 1 1 calc R U . . . C11 C 0.7383(6) 1.0499(5) 0.9767(4) 0.0109(18) Uani 1 1 d . U . . . H11 H 0.6768 1.0425 0.9666 0.013 Uiso 1 1 calc R U . . . C12 C 0.7621(7) 1.1094(5) 1.0176(4) 0.018(2) Uani 1 1 d . U . . . H12 H 0.7171 1.1407 1.0359 0.021 Uiso 1 1 calc R U . . . C13 C 0.8537(6) 1.1224(5) 1.0312(4) 0.017(2) Uani 1 1 d . U . . . H13 H 0.8714 1.1638 1.0573 0.021 Uiso 1 1 calc R U . . . C14 C 0.9189(7) 1.0726(5) 1.0053(4) 0.0144(19) Uani 1 1 d . U . . . H14 H 0.9808 1.0794 1.0148 0.017 Uiso 1 1 calc R U . . . C15 C 0.8907(6) 1.0133(5) 0.9656(4) 0.0124(18) Uani 1 1 d . U . . . C16 C 0.9505(6) 0.9546(5) 0.9369(4) 0.0106(17) Uani 1 1 d . U . . . C17 C 1.0448(6) 0.9484(5) 0.9470(4) 0.0147(19) Uani 1 1 d . U . . . H17 H 1.0751 0.9833 0.9740 0.018 Uiso 1 1 calc R U . . . C18 C 1.0919(6) 0.8908(5) 0.9170(4) 0.018(2) Uani 1 1 d . U . . . H18 H 1.1549 0.8861 0.9230 0.021 Uiso 1 1 calc R U . . . C19 C 1.0448(6) 0.8387(6) 0.8771(4) 0.018(2) Uani 1 1 d . U . . . H19 H 1.0764 0.7993 0.8560 0.021 Uiso 1 1 calc R U . . . C20 C 0.9524(6) 0.8460(5) 0.8692(4) 0.0143(19) Uani 1 1 d . U . . . H20 H 0.9213 0.8105 0.8433 0.017 Uiso 1 1 calc R U . . . C21 C 0.8124(6) 1.0556(5) 0.8127(4) 0.0126(18) Uani 1 1 d . U . . . H21 H 0.8039 1.0854 0.8501 0.015 Uiso 1 1 calc R U . . . C22 C 0.8412(6) 1.0905(5) 0.7553(4) 0.016(2) Uani 1 1 d . U . . . H22 H 0.8499 1.1436 0.7541 0.019 Uiso 1 1 calc R U . . . C23 C 0.8568(6) 1.0476(5) 0.7006(4) 0.015(2) Uani 1 1 d . U . . . H23 H 0.8791 1.0704 0.6626 0.018 Uiso 1 1 calc R U . . . C24 C 0.8386(6) 0.9692(5) 0.7030(4) 0.016(2) Uani 1 1 d . U . . . H24 H 0.8477 0.9387 0.6661 0.019 Uiso 1 1 calc R U . . . C25 C 0.8074(6) 0.9372(5) 0.7598(4) 0.0097(17) Uani 1 1 d . U . . . C26 C 0.7806(6) 0.8561(5) 0.7678(4) 0.0097(17) Uani 1 1 d . U . . . C27 C 0.7756(6) 0.8039(5) 0.7168(4) 0.0132(18) Uani 1 1 d . U . . . H27 H 0.7929 0.8179 0.6746 0.016 Uiso 1 1 calc R U . . . C28 C 0.7445(6) 0.7309(5) 0.7302(5) 0.017(2) Uani 1 1 d . U . . . H28 H 0.7424 0.6942 0.6971 0.021 Uiso 1 1 calc R U . . . C29 C 0.7166(6) 0.7123(5) 0.7919(4) 0.0147(19) Uani 1 1 d . U . . . H29 H 0.6933 0.6636 0.8009 0.018 Uiso 1 1 calc R U . . . C30 C 0.7235(6) 0.7665(5) 0.8410(4) 0.0144(19) Uani 1 1 d . U . . . H30 H 0.7043 0.7539 0.8831 0.017 Uiso 1 1 calc R U . . . C31 C 0.4139(6) 1.0063(5) 0.2731(4) 0.0115(17) Uani 1 1 d . U . . . H31A H 0.4768 0.9892 0.2673 0.014 Uiso 1 1 calc R U . . . H31B H 0.4164 1.0579 0.2912 0.014 Uiso 1 1 calc R U . . . C32 C 0.3697(6) 0.9547(5) 0.3235(4) 0.0097(17) Uani 1 1 d . U . . . C33 C 0.2821(6) 0.9696(5) 0.3470(4) 0.0109(17) Uani 1 1 d . U . . . H33 H 0.2471 1.0081 0.3276 0.013 Uiso 1 1 calc R U . . . C34 C 0.4182(6) 0.8953(5) 0.3525(4) 0.0106(17) Uani 1 1 d . U . . . H34 H 0.4761 0.8830 0.3364 0.013 Uiso 1 1 calc R U . . . C35 C 0.2460(6) 0.9281(5) 0.3988(4) 0.0121(19) Uani 1 1 d . U . . . H35 H 0.1871 0.9392 0.4136 0.015 Uiso 1 1 calc R U . . . C36 C 0.3834(6) 0.8537(5) 0.4044(4) 0.0108(18) Uani 1 1 d . U . . . H36 H 0.4181 0.8145 0.4230 0.013 Uiso 1 1 calc R U . . . C37 C 0.2963(6) 0.8703(5) 0.4291(4) 0.0120(18) Uani 1 1 d . U . . . C38 C 0.2599(6) 0.8280(5) 0.4882(4) 0.0115(18) Uani 1 1 d . U . . . H38A H 0.2981 0.7832 0.4963 0.014 Uiso 1 1 calc R U . . . H38B H 0.1983 0.8099 0.4787 0.014 Uiso 1 1 calc R 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 Mo1 0.0082(4) 0.0110(4) 0.0091(4) 0.0002(3) 0.0007(3) -0.0018(3) Mo2 0.0105(4) 0.0093(4) 0.0102(4) -0.0007(3) 0.0001(3) -0.0038(3) Mo3 0.0101(4) 0.0080(4) 0.0102(4) -0.0004(3) -0.0002(3) -0.0005(3) Mo4 0.0074(4) 0.0075(4) 0.0123(4) 0.0010(3) 0.0002(3) -0.0006(3) Mo5 0.0086(4) 0.0085(4) 0.0104(4) -0.0014(3) 0.0004(3) -0.0008(3) Co1 0.0060(6) 0.0081(6) 0.0105(5) 0.0002(5) 0.0005(5) -0.0011(5) P1 0.0076(11) 0.0093(12) 0.0085(10) 0.0007(9) 0.0005(8) -0.0010(9) P2 0.0099(12) 0.0073(10) 0.0082(10) 0.0006(9) 0.0016(9) -0.0009(9) O1 0.011(3) 0.012(3) 0.011(3) 0.000(3) 0.001(2) 0.000(2) O2 0.019(3) 0.011(3) 0.014(3) -0.003(3) 0.003(3) 0.000(3) O3 0.008(3) 0.023(3) 0.015(3) -0.003(3) 0.002(2) -0.002(3) O4 0.012(3) 0.011(3) 0.006(3) 0.002(2) 0.000(2) -0.003(2) O5 0.009(3) 0.008(3) 0.010(3) 0.001(2) 0.001(2) -0.003(2) O6 0.010(3) 0.021(3) 0.016(3) -0.004(3) -0.005(3) -0.006(3) O7 0.019(4) 0.009(3) 0.018(3) 0.000(3) 0.003(3) -0.003(3) O8 0.012(3) 0.014(3) 0.009(3) -0.002(3) 0.000(2) -0.004(2) O9 0.020(4) 0.012(3) 0.018(3) -0.001(3) -0.001(3) 0.003(3) O10 0.016(3) 0.017(3) 0.016(3) 0.001(3) -0.001(3) -0.001(3) O11 0.010(3) 0.006(3) 0.012(3) 0.001(2) 0.002(2) 0.000(2) O12 0.007(3) 0.006(3) 0.013(3) 0.000(2) 0.002(2) 0.001(2) O13 0.008(3) 0.016(3) 0.021(3) -0.002(3) -0.003(2) -0.002(3) O14 0.012(3) 0.008(3) 0.015(3) 0.001(3) 0.006(3) 0.001(3) O15 0.011(3) 0.008(3) 0.012(3) -0.001(2) 0.002(2) -0.002(2) O16 0.012(3) 0.010(3) 0.012(3) 0.002(2) 0.000(2) 0.003(2) O17 0.014(3) 0.012(3) 0.018(3) -0.002(3) 0.002(3) 0.000(3) O18 0.015(3) 0.014(3) 0.013(3) -0.002(3) 0.001(2) -0.006(3) O19 0.009(3) 0.007(3) 0.012(3) -0.002(2) -0.002(2) 0.000(2) O20 0.007(3) 0.011(3) 0.011(3) 0.001(2) 0.002(2) -0.001(3) O21 0.009(3) 0.005(3) 0.011(3) -0.001(2) 0.002(2) -0.002(2) O90 0.025(4) 0.013(4) 0.028(4) 0.002(3) -0.004(3) 0.004(3) O91 0.054(6) 0.039(5) 0.052(6) 0.003(5) 0.005(5) 0.001(5) O92 0.060(6) 0.025(4) 0.021(4) 0.002(3) 0.009(4) 0.007(4) O93 0.023(4) 0.012(3) 0.039(4) -0.004(3) -0.014(4) 0.000(3) O94 0.065(7) 0.040(5) 0.023(4) -0.001(4) -0.005(4) 0.037(5) O96 0.095(9) 0.127(11) 0.063(7) 0.030(7) 0.027(7) 0.073(9) N1 0.005(3) 0.008(4) 0.011(3) -0.001(3) 0.000(3) -0.001(3) N2 0.009(4) 0.007(4) 0.013(3) 0.000(3) -0.001(3) -0.003(3) N3 0.013(4) 0.011(3) 0.007(3) 0.001(3) -0.002(3) -0.006(3) N4 0.007(3) 0.013(4) 0.014(4) 0.002(3) -0.001(3) -0.002(3) N5 0.004(4) 0.010(3) 0.011(3) 0.001(3) 0.001(3) -0.005(3) N6 0.006(4) 0.008(3) 0.012(3) -0.004(3) 0.000(3) 0.003(3) C1 0.007(4) 0.011(4) 0.015(4) -0.001(4) 0.002(3) 0.002(4) C2 0.006(4) 0.020(5) 0.022(5) 0.000(4) -0.004(4) 0.007(4) C3 0.005(4) 0.015(5) 0.021(5) 0.002(4) 0.000(3) 0.002(4) C4 0.007(4) 0.015(5) 0.016(4) -0.004(4) 0.006(3) -0.005(4) C5 0.008(4) 0.004(4) 0.013(4) -0.006(3) -0.001(3) 0.002(3) C6 0.008(4) 0.010(5) 0.014(4) -0.003(3) 0.000(3) 0.003(4) C7 0.011(5) 0.018(5) 0.013(4) -0.003(4) -0.001(3) -0.010(4) C8 0.024(5) 0.016(5) 0.019(5) 0.005(4) 0.000(4) -0.004(4) C9 0.021(5) 0.015(5) 0.021(5) 0.004(4) -0.008(4) -0.008(4) C10 0.009(4) 0.009(5) 0.020(4) 0.001(4) -0.006(4) 0.000(4) C11 0.011(4) 0.014(4) 0.008(4) -0.002(3) -0.001(3) -0.005(4) C12 0.019(5) 0.020(5) 0.014(5) -0.001(4) 0.004(4) 0.005(4) C13 0.022(5) 0.012(5) 0.018(5) -0.009(4) -0.001(4) -0.009(4) C14 0.018(5) 0.006(4) 0.019(5) 0.001(4) -0.008(4) -0.003(4) C15 0.010(4) 0.013(4) 0.014(4) 0.005(3) -0.003(3) -0.002(4) C16 0.008(4) 0.013(4) 0.010(4) 0.005(3) 0.002(3) -0.003(3) C17 0.005(4) 0.018(5) 0.021(5) 0.005(4) -0.005(4) -0.006(4) C18 0.006(5) 0.025(5) 0.022(5) 0.010(4) 0.003(4) 0.003(4) C19 0.012(5) 0.019(5) 0.022(5) 0.006(4) 0.006(4) 0.005(4) C20 0.014(5) 0.019(5) 0.010(4) 0.004(4) -0.001(4) 0.000(4) C21 0.011(5) 0.010(4) 0.017(4) -0.002(4) 0.000(4) 0.002(4) C22 0.017(5) 0.010(4) 0.021(5) 0.006(4) -0.003(4) 0.000(4) C23 0.014(5) 0.015(5) 0.016(4) 0.004(4) 0.001(4) -0.002(4) C24 0.017(5) 0.017(5) 0.014(4) -0.004(4) 0.004(4) 0.001(4) C25 0.003(4) 0.011(4) 0.015(4) -0.001(3) -0.002(3) 0.001(3) C26 0.003(4) 0.009(4) 0.017(4) -0.008(3) -0.001(4) -0.001(3) C27 0.012(5) 0.015(4) 0.013(4) 0.001(4) 0.000(4) 0.001(4) C28 0.023(6) 0.012(4) 0.017(4) -0.004(4) -0.005(4) 0.001(4) C29 0.018(5) 0.004(4) 0.022(5) -0.002(3) 0.002(4) -0.002(4) C30 0.009(5) 0.013(4) 0.021(5) 0.001(4) 0.005(4) 0.002(4) C31 0.011(4) 0.013(4) 0.010(4) 0.000(4) -0.002(3) 0.001(4) C32 0.006(4) 0.015(5) 0.008(4) -0.003(3) 0.001(3) -0.005(4) C33 0.005(4) 0.010(4) 0.018(4) 0.000(4) -0.005(4) -0.001(3) C34 0.010(4) 0.010(4) 0.011(4) -0.005(3) 0.003(4) 0.003(3) C35 0.012(5) 0.012(5) 0.012(4) -0.003(4) 0.000(3) 0.003(4) C36 0.011(4) 0.006(4) 0.015(4) -0.003(3) -0.003(4) 0.004(4) C37 0.015(5) 0.008(4) 0.013(4) -0.002(3) 0.002(3) -0.006(4) C38 0.013(5) 0.005(4) 0.016(4) -0.002(3) 0.005(3) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O3 1.700(6) . ? Mo1 O2 1.712(6) . ? Mo1 O1 1.893(6) . ? Mo1 O4 1.947(6) . ? Mo1 O19 2.231(6) 2_574 ? Mo1 O5 2.346(5) . ? Mo2 O7 1.699(6) . ? Mo2 O6 1.706(6) . ? Mo2 O4 1.897(5) . ? Mo2 O8 1.961(6) . ? Mo2 O20 2.303(6) 2_574 ? Mo2 O5 2.341(5) . ? Mo3 O10 1.688(6) . ? Mo3 O9 1.712(6) . ? Mo3 O8 1.857(6) . ? Mo3 O11 2.070(6) . ? Mo3 O12 2.163(6) . ? Mo3 O20 2.370(5) 2_574 ? Mo4 O13 1.701(6) . ? Mo4 O14 1.715(6) . ? Mo4 O15 1.868(6) . ? Mo4 O11 2.059(5) . ? Mo4 O21 2.173(5) 2_574 ? Mo4 O12 2.436(6) . ? Mo5 O17 1.698(6) . ? Mo5 O18 1.702(6) . ? Mo5 O1 1.922(6) . ? Mo5 O15 1.970(6) . ? Mo5 O16 2.225(6) . ? Mo5 O19 2.384(5) 2_574 ? Co1 N4 1.916(7) . ? Co1 N6 1.921(7) . ? Co1 N3 1.926(7) . ? Co1 N2 1.931(7) . ? Co1 N1 1.931(7) . ? Co1 N5 1.937(7) . ? P1 O16 1.503(6) . ? P1 O5 1.535(6) . ? P1 O12 1.552(6) . ? P1 C31 1.793(8) . ? P2 O21 1.511(6) . ? P2 O19 1.540(6) . ? P2 O20 1.544(6) . ? P2 C38 1.788(8) . ? O19 Mo1 2.232(6) 2_575 ? O19 Mo5 2.384(5) 2_575 ? O20 Mo2 2.303(6) 2_575 ? O20 Mo3 2.370(5) 2_575 ? O21 Mo4 2.173(5) 2_575 ? O90 H90A 0.84(3) . ? O90 H90B 0.84(3) . ? O91 H91A 0.86(3) . ? O91 H91B 0.86(3) . ? O92 H92A 0.84(3) . ? O92 H92B 0.85(3) . ? O93 H93A 0.82(3) . ? O93 H93B 0.84(3) . ? O94 H94A 0.82(3) . ? O94 H94B 0.84(3) . ? O96 H96A 0.85(3) . ? O96 H96B 0.85(3) . ? N1 C1 1.330(11) . ? N1 C5 1.351(10) . ? N2 C10 1.335(11) . ? N2 C6 1.365(11) . ? N3 C11 1.325(11) . ? N3 C15 1.366(11) . ? N4 C20 1.343(11) . ? N4 C16 1.367(11) . ? N5 C21 1.339(10) . ? N5 C25 1.358(10) . ? N6 C26 1.343(11) . ? N6 C30 1.347(10) . ? C1 C2 1.381(12) . ? C1 H1 0.9300 . ? C2 C3 1.394(12) . ? C2 H2 0.9300 . ? C3 C4 1.369(12) . ? C3 H3 0.9300 . ? C4 C5 1.396(11) . ? C4 H4 0.9300 . ? C5 C6 1.475(11) . ? C6 C7 1.364(12) . ? C7 C8 1.391(12) . ? C7 H7 0.9300 . ? C8 C9 1.391(13) . ? C8 H8 0.9300 . ? C9 C10 1.372(12) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.372(12) . ? C11 H11 0.9300 . ? C12 C13 1.383(13) . ? C12 H12 0.9300 . ? C13 C14 1.388(13) . ? C13 H13 0.9300 . ? C14 C15 1.374(12) . ? C14 H14 0.9300 . ? C15 C16 1.463(12) . ? C16 C17 1.393(12) . ? C17 C18 1.359(13) . ? C17 H17 0.9300 . ? C18 C19 1.397(13) . ? C18 H18 0.9300 . ? C19 C20 1.362(12) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.383(12) . ? C21 H21 0.9300 . ? C22 C23 1.361(12) . ? C22 H22 0.9300 . ? C23 C24 1.387(12) . ? C23 H23 0.9300 . ? C24 C25 1.364(12) . ? C24 H24 0.9300 . ? C25 C26 1.470(11) . ? C26 C27 1.381(11) . ? C27 C28 1.373(12) . ? C27 H27 0.9300 . ? C28 C29 1.363(12) . ? C28 H28 0.9300 . ? C29 C30 1.378(12) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.510(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C34 1.382(12) . ? C32 C33 1.387(11) . ? C33 C35 1.384(12) . ? C33 H33 0.9300 . ? C34 C36 1.379(12) . ? C34 H34 0.9300 . ? C35 C37 1.387(12) . ? C35 H35 0.9300 . ? C36 C37 1.395(12) . ? C36 H36 0.9300 . ? C37 C38 1.510(11) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? 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 O3 Mo1 O2 103.8(3) . . ? O3 Mo1 O1 98.0(3) . . ? O2 Mo1 O1 101.4(3) . . ? O3 Mo1 O4 99.7(3) . . ? O2 Mo1 O4 94.7(2) . . ? O1 Mo1 O4 152.5(2) . . ? O3 Mo1 O19 159.4(2) . 2_574 ? O2 Mo1 O19 96.5(3) . 2_574 ? O1 Mo1 O19 74.2(2) . 2_574 ? O4 Mo1 O19 82.0(2) . 2_574 ? O3 Mo1 O5 89.3(2) . . ? O2 Mo1 O5 163.0(2) . . ? O1 Mo1 O5 87.2(2) . . ? O4 Mo1 O5 72.1(2) . . ? O19 Mo1 O5 71.56(19) 2_574 . ? O7 Mo2 O6 103.8(3) . . ? O7 Mo2 O4 100.6(3) . . ? O6 Mo2 O4 102.8(3) . . ? O7 Mo2 O8 100.5(3) . . ? O6 Mo2 O8 96.8(3) . . ? O4 Mo2 O8 146.7(2) . . ? O7 Mo2 O20 88.2(3) . 2_574 ? O6 Mo2 O20 165.6(2) . 2_574 ? O4 Mo2 O20 82.5(2) . 2_574 ? O8 Mo2 O20 72.8(2) . 2_574 ? O7 Mo2 O5 166.3(3) . . ? O6 Mo2 O5 89.5(3) . . ? O4 Mo2 O5 73.0(2) . . ? O8 Mo2 O5 80.6(2) . . ? O20 Mo2 O5 79.13(19) 2_574 . ? O10 Mo3 O9 103.5(3) . . ? O10 Mo3 O8 98.1(3) . . ? O9 Mo3 O8 104.1(3) . . ? O10 Mo3 O11 98.5(3) . . ? O9 Mo3 O11 91.2(3) . . ? O8 Mo3 O11 154.1(2) . . ? O10 Mo3 O12 96.8(2) . . ? O9 Mo3 O12 155.2(3) . . ? O8 Mo3 O12 86.8(2) . . ? O11 Mo3 O12 71.7(2) . . ? O10 Mo3 O20 166.4(3) . 2_574 ? O9 Mo3 O20 88.9(2) . 2_574 ? O8 Mo3 O20 72.9(2) . 2_574 ? O11 Mo3 O20 86.8(2) . 2_574 ? O12 Mo3 O20 72.8(2) . 2_574 ? O13 Mo4 O14 101.6(3) . . ? O13 Mo4 O15 103.9(3) . . ? O14 Mo4 O15 101.5(3) . . ? O13 Mo4 O11 99.8(3) . . ? O14 Mo4 O11 93.1(2) . . ? O15 Mo4 O11 148.9(2) . . ? O13 Mo4 O21 88.4(2) . 2_574 ? O14 Mo4 O21 167.0(2) . 2_574 ? O15 Mo4 O21 83.9(2) . 2_574 ? O11 Mo4 O21 76.8(2) . 2_574 ? O13 Mo4 O12 165.8(2) . . ? O14 Mo4 O12 82.9(2) . . ? O15 Mo4 O12 88.2(2) . . ? O11 Mo4 O12 66.3(2) . . ? O21 Mo4 O12 85.42(19) 2_574 . ? O17 Mo5 O18 101.9(3) . . ? O17 Mo5 O1 99.7(3) . . ? O18 Mo5 O1 100.1(3) . . ? O17 Mo5 O15 104.0(3) . . ? O18 Mo5 O15 98.2(3) . . ? O1 Mo5 O15 146.1(2) . . ? O17 Mo5 O16 87.7(2) . . ? O18 Mo5 O16 170.3(3) . . ? O1 Mo5 O16 77.8(2) . . ? O15 Mo5 O16 79.3(2) . . ? O17 Mo5 O19 168.8(3) . 2_574 ? O18 Mo5 O19 85.0(2) . 2_574 ? O1 Mo5 O19 70.1(2) . 2_574 ? O15 Mo5 O19 83.5(2) . 2_574 ? O16 Mo5 O19 85.46(19) . 2_574 ? N4 Co1 N6 94.1(3) . . ? N4 Co1 N3 83.2(3) . . ? N6 Co1 N3 175.3(3) . . ? N4 Co1 N2 92.1(3) . . ? N6 Co1 N2 97.3(3) . . ? N3 Co1 N2 86.6(3) . . ? N4 Co1 N1 175.7(3) . . ? N6 Co1 N1 85.4(3) . . ? N3 Co1 N1 97.6(3) . . ? N2 Co1 N1 83.7(3) . . ? N4 Co1 N5 87.7(3) . . ? N6 Co1 N5 82.8(3) . . ? N3 Co1 N5 93.3(3) . . ? N2 Co1 N5 179.8(3) . . ? N1 Co1 N5 96.5(3) . . ? O16 P1 O5 112.6(3) . . ? O16 P1 O12 108.9(3) . . ? O5 P1 O12 111.0(3) . . ? O16 P1 C31 109.5(4) . . ? O5 P1 C31 105.3(4) . . ? O12 P1 C31 109.5(4) . . ? O21 P2 O19 109.2(3) . . ? O21 P2 O20 111.1(3) . . ? O19 P2 O20 111.8(3) . . ? O21 P2 C38 109.8(4) . . ? O19 P2 C38 108.1(4) . . ? O20 P2 C38 106.7(4) . . ? Mo1 O1 Mo5 122.8(3) . . ? Mo2 O4 Mo1 122.6(3) . . ? P1 O5 Mo2 128.0(3) . . ? P1 O5 Mo1 127.4(3) . . ? Mo2 O5 Mo1 92.01(19) . . ? Mo3 O8 Mo2 122.7(3) . . ? Mo4 O11 Mo3 119.5(3) . . ? P1 O12 Mo3 128.6(3) . . ? P1 O12 Mo4 128.0(3) . . ? Mo3 O12 Mo4 101.6(2) . . ? Mo4 O15 Mo5 145.4(3) . . ? P1 O16 Mo5 123.1(3) . . ? P2 O19 Mo1 130.5(3) . 2_575 ? P2 O19 Mo5 135.1(3) . 2_575 ? Mo1 O19 Mo5 92.9(2) 2_575 2_575 ? P2 O20 Mo2 125.8(3) . 2_575 ? P2 O20 Mo3 128.2(3) . 2_575 ? Mo2 O20 Mo3 91.60(19) 2_575 2_575 ? P2 O21 Mo4 123.2(3) . 2_575 ? H90A O90 H90B 105(6) . . ? H91A O91 H91B 108(7) . . ? H92A O92 H92B 105(6) . . ? H93A O93 H93B 110(6) . . ? H94A O94 H94B 117(7) . . ? H96A O96 H96B 106(7) . . ? C1 N1 C5 119.1(7) . . ? C1 N1 Co1 126.3(6) . . ? C5 N1 Co1 113.4(5) . . ? C10 N2 C6 117.4(7) . . ? C10 N2 Co1 127.8(6) . . ? C6 N2 Co1 114.3(6) . . ? C11 N3 C15 119.1(7) . . ? C11 N3 Co1 126.0(6) . . ? C15 N3 Co1 114.9(6) . . ? C20 N4 C16 119.2(7) . . ? C20 N4 Co1 125.7(6) . . ? C16 N4 Co1 115.1(6) . . ? C21 N5 C25 119.0(7) . . ? C21 N5 Co1 127.0(6) . . ? C25 N5 Co1 113.5(5) . . ? C26 N6 C30 118.5(7) . . ? C26 N6 Co1 114.9(5) . . ? C30 N6 Co1 126.6(6) . . ? N1 C1 C2 121.8(8) . . ? N1 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C1 C2 C3 119.4(8) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.1(8) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 118.7(8) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.9(8) . . ? N1 C5 C6 114.9(7) . . ? C4 C5 C6 123.0(8) . . ? C7 C6 N2 122.9(8) . . ? C7 C6 C5 124.9(8) . . ? N2 C6 C5 112.2(7) . . ? C6 C7 C8 118.4(8) . . ? C6 C7 H7 120.8 . . ? C8 C7 H7 120.8 . . ? C9 C8 C7 119.5(8) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C10 C9 C8 118.0(9) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? N2 C10 C9 123.7(9) . . ? N2 C10 H10 118.2 . . ? C9 C10 H10 118.2 . . ? N3 C11 C12 122.4(8) . . ? N3 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 119.3(9) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C12 C13 C14 118.8(8) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 119.1(9) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N3 C15 C14 121.3(8) . . ? N3 C15 C16 113.3(7) . . ? C14 C15 C16 125.4(8) . . ? N4 C16 C17 120.9(8) . . ? N4 C16 C15 113.5(7) . . ? C17 C16 C15 125.6(8) . . ? C18 C17 C16 119.2(8) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 119.4(9) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 119.6(9) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? N4 C20 C19 121.6(9) . . ? N4 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? N5 C21 C22 120.9(8) . . ? N5 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 120.4(9) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 118.5(9) . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 C23 119.5(9) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? N5 C25 C24 121.6(8) . . ? N5 C25 C26 113.4(7) . . ? C24 C25 C26 125.0(8) . . ? N6 C26 C27 122.3(8) . . ? N6 C26 C25 113.7(7) . . ? C27 C26 C25 123.9(8) . . ? C28 C27 C26 118.2(8) . . ? C28 C27 H27 120.9 . . ? C26 C27 H27 120.9 . . ? C29 C28 C27 120.0(8) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 119.3(8) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? N6 C30 C29 121.5(8) . . ? N6 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C32 C31 P1 118.5(6) . . ? C32 C31 H31A 107.7 . . ? P1 C31 H31A 107.7 . . ? C32 C31 H31B 107.7 . . ? P1 C31 H31B 107.7 . . ? H31A C31 H31B 107.1 . . ? C34 C32 C33 117.5(8) . . ? C34 C32 C31 121.1(8) . . ? C33 C32 C31 121.2(8) . . ? C35 C33 C32 121.1(8) . . ? C35 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C36 C34 C32 122.1(8) . . ? C36 C34 H34 119.0 . . ? C32 C34 H34 119.0 . . ? C33 C35 C37 121.0(8) . . ? C33 C35 H35 119.5 . . ? C37 C35 H35 119.5 . . ? C34 C36 C37 120.2(8) . . ? C34 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C35 C37 C36 118.0(8) . . ? C35 C37 C38 121.4(8) . . ? C36 C37 C38 120.6(8) . . ? C37 C38 P2 113.5(6) . . ? C37 C38 H38A 108.9 . . ? P2 C38 H38A 108.9 . . ? C37 C38 H38B 108.9 . . ? P2 C38 H38B 108.9 . . ? H38A C38 H38B 107.7 . . ? 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 O3 Mo1 O1 Mo5 158.4(3) . . . . ? O2 Mo1 O1 Mo5 -95.7(4) . . . . ? O4 Mo1 O1 Mo5 28.9(7) . . . . ? O19 Mo1 O1 Mo5 -2.1(3) 2_574 . . . ? O5 Mo1 O1 Mo5 69.5(3) . . . . ? O7 Mo2 O4 Mo1 -172.6(3) . . . . ? O6 Mo2 O4 Mo1 80.5(4) . . . . ? O8 Mo2 O4 Mo1 -44.1(6) . . . . ? O20 Mo2 O4 Mo1 -85.9(3) 2_574 . . . ? O5 Mo2 O4 Mo1 -5.0(3) . . . . ? O16 P1 O5 Mo2 152.5(3) . . . . ? O12 P1 O5 Mo2 30.2(5) . . . . ? C31 P1 O5 Mo2 -88.2(5) . . . . ? O16 P1 O5 Mo1 21.9(5) . . . . ? O12 P1 O5 Mo1 -100.5(4) . . . . ? C31 P1 O5 Mo1 141.1(4) . . . . ? O10 Mo3 O8 Mo2 171.4(4) . . . . ? O9 Mo3 O8 Mo2 -82.4(4) . . . . ? O11 Mo3 O8 Mo2 42.0(7) . . . . ? O12 Mo3 O8 Mo2 75.0(3) . . . . ? O20 Mo3 O8 Mo2 2.0(3) 2_574 . . . ? O16 P1 O12 Mo3 -173.1(4) . . . . ? O5 P1 O12 Mo3 -48.6(5) . . . . ? C31 P1 O12 Mo3 67.2(5) . . . . ? O16 P1 O12 Mo4 -11.6(5) . . . . ? O5 P1 O12 Mo4 112.9(4) . . . . ? C31 P1 O12 Mo4 -131.3(4) . . . . ? O13 Mo4 O15 Mo5 145.1(5) . . . . ? O14 Mo4 O15 Mo5 -109.8(5) . . . . ? O11 Mo4 O15 Mo5 6.6(9) . . . . ? O21 Mo4 O15 Mo5 58.2(5) 2_574 . . . ? O12 Mo4 O15 Mo5 -27.3(5) . . . . ? O5 P1 O16 Mo5 -55.0(5) . . . . ? O12 P1 O16 Mo5 68.5(4) . . . . ? C31 P1 O16 Mo5 -171.9(4) . . . . ? O21 P2 O19 Mo1 -170.8(4) . . . 2_575 ? O20 P2 O19 Mo1 -47.5(5) . . . 2_575 ? C38 P2 O19 Mo1 69.7(5) . . . 2_575 ? O21 P2 O19 Mo5 -8.3(5) . . . 2_575 ? O20 P2 O19 Mo5 115.1(4) . . . 2_575 ? C38 P2 O19 Mo5 -127.7(5) . . . 2_575 ? O21 P2 O20 Mo2 155.3(3) . . . 2_575 ? O19 P2 O20 Mo2 33.1(5) . . . 2_575 ? C38 P2 O20 Mo2 -85.0(5) . . . 2_575 ? O21 P2 O20 Mo3 27.7(5) . . . 2_575 ? O19 P2 O20 Mo3 -94.6(4) . . . 2_575 ? C38 P2 O20 Mo3 147.3(4) . . . 2_575 ? O19 P2 O21 Mo4 58.0(4) . . . 2_575 ? O20 P2 O21 Mo4 -65.8(4) . . . 2_575 ? C38 P2 O21 Mo4 176.4(4) . . . 2_575 ? C5 N1 C1 C2 -1.0(12) . . . . ? Co1 N1 C1 C2 165.6(6) . . . . ? N1 C1 C2 C3 -0.5(13) . . . . ? C1 C2 C3 C4 1.3(13) . . . . ? C2 C3 C4 C5 -0.6(13) . . . . ? C1 N1 C5 C4 1.7(12) . . . . ? Co1 N1 C5 C4 -166.5(6) . . . . ? C1 N1 C5 C6 177.9(7) . . . . ? Co1 N1 C5 C6 9.7(9) . . . . ? C3 C4 C5 N1 -0.9(12) . . . . ? C3 C4 C5 C6 -176.8(8) . . . . ? C10 N2 C6 C7 4.6(12) . . . . ? Co1 N2 C6 C7 -167.3(7) . . . . ? C10 N2 C6 C5 -177.2(7) . . . . ? Co1 N2 C6 C5 10.9(9) . . . . ? N1 C5 C6 C7 164.6(8) . . . . ? C4 C5 C6 C7 -19.3(13) . . . . ? N1 C5 C6 N2 -13.6(10) . . . . ? C4 C5 C6 N2 162.6(8) . . . . ? N2 C6 C7 C8 -2.1(13) . . . . ? C5 C6 C7 C8 179.9(8) . . . . ? C6 C7 C8 C9 -1.9(13) . . . . ? C7 C8 C9 C10 3.3(13) . . . . ? C6 N2 C10 C9 -3.1(12) . . . . ? Co1 N2 C10 C9 167.5(7) . . . . ? C8 C9 C10 N2 -0.7(13) . . . . ? C15 N3 C11 C12 -0.5(12) . . . . ? Co1 N3 C11 C12 -179.1(6) . . . . ? N3 C11 C12 C13 2.2(13) . . . . ? C11 C12 C13 C14 -2.7(13) . . . . ? C12 C13 C14 C15 1.7(13) . . . . ? C11 N3 C15 C14 -0.5(12) . . . . ? Co1 N3 C15 C14 178.2(6) . . . . ? C11 N3 C15 C16 177.2(7) . . . . ? Co1 N3 C15 C16 -4.1(9) . . . . ? C13 C14 C15 N3 -0.1(13) . . . . ? C13 C14 C15 C16 -177.5(8) . . . . ? C20 N4 C16 C17 -0.1(12) . . . . ? Co1 N4 C16 C17 177.5(6) . . . . ? C20 N4 C16 C15 -179.4(7) . . . . ? Co1 N4 C16 C15 -1.8(9) . . . . ? N3 C15 C16 N4 3.8(10) . . . . ? C14 C15 C16 N4 -178.6(8) . . . . ? N3 C15 C16 C17 -175.4(8) . . . . ? C14 C15 C16 C17 2.2(13) . . . . ? N4 C16 C17 C18 0.8(12) . . . . ? C15 C16 C17 C18 -180.0(8) . . . . ? C16 C17 C18 C19 -0.5(13) . . . . ? C17 C18 C19 C20 -0.5(13) . . . . ? C16 N4 C20 C19 -0.9(12) . . . . ? Co1 N4 C20 C19 -178.2(6) . . . . ? C18 C19 C20 N4 1.2(13) . . . . ? C25 N5 C21 C22 -1.5(12) . . . . ? Co1 N5 C21 C22 169.7(6) . . . . ? N5 C21 C22 C23 -2.0(13) . . . . ? C21 C22 C23 C24 3.3(13) . . . . ? C22 C23 C24 C25 -1.1(13) . . . . ? C21 N5 C25 C24 3.8(12) . . . . ? Co1 N5 C25 C24 -168.5(7) . . . . ? C21 N5 C25 C26 -175.1(7) . . . . ? Co1 N5 C25 C26 12.5(9) . . . . ? C23 C24 C25 N5 -2.5(13) . . . . ? C23 C24 C25 C26 176.3(8) . . . . ? C30 N6 C26 C27 -3.6(12) . . . . ? Co1 N6 C26 C27 177.3(7) . . . . ? C30 N6 C26 C25 173.9(7) . . . . ? Co1 N6 C26 C25 -5.2(9) . . . . ? N5 C25 C26 N6 -4.9(10) . . . . ? C24 C25 C26 N6 176.1(8) . . . . ? N5 C25 C26 C27 172.5(8) . . . . ? C24 C25 C26 C27 -6.4(14) . . . . ? N6 C26 C27 C28 1.0(13) . . . . ? C25 C26 C27 C28 -176.3(8) . . . . ? C26 C27 C28 C29 2.1(13) . . . . ? C27 C28 C29 C30 -2.5(14) . . . . ? C26 N6 C30 C29 3.2(12) . . . . ? Co1 N6 C30 C29 -177.9(6) . . . . ? C28 C29 C30 N6 -0.2(13) . . . . ? O16 P1 C31 C32 -56.8(7) . . . . ? O5 P1 C31 C32 -178.1(6) . . . . ? O12 P1 C31 C32 62.5(7) . . . . ? P1 C31 C32 C34 122.2(8) . . . . ? P1 C31 C32 C33 -64.0(10) . . . . ? C34 C32 C33 C35 2.0(12) . . . . ? C31 C32 C33 C35 -172.0(8) . . . . ? C33 C32 C34 C36 -2.4(12) . . . . ? C31 C32 C34 C36 171.6(8) . . . . ? C32 C33 C35 C37 0.1(13) . . . . ? C32 C34 C36 C37 0.7(13) . . . . ? C33 C35 C37 C36 -1.8(12) . . . . ? C33 C35 C37 C38 176.3(8) . . . . ? C34 C36 C37 C35 1.5(12) . . . . ? C34 C36 C37 C38 -176.7(8) . . . . ? C35 C37 C38 P2 -70.7(10) . . . . ? C36 C37 C38 P2 107.4(8) . . . . ? O21 P2 C38 C37 -52.7(7) . . . . ? O19 P2 C38 C37 66.4(7) . . . . ? O20 P2 C38 C37 -173.1(6) . . . . ? _refine_diff_density_max 1.219 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.121 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 957892' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mo_compound5 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H40 Cu2 Mo5 N8 O21 P2, 6(H2 O)' _chemical_formula_sum 'C48 H52 Cu2 Mo5 N8 O27 P2' _chemical_formula_weight 1841.69 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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0366(13) _cell_length_b 13.0703(13) _cell_length_c 20.989(2) _cell_angle_alpha 76.271(3) _cell_angle_beta 85.514(3) _cell_angle_gamma 60.541(3) _cell_volume 3021.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 728 _cell_measurement_theta_min 1.8989 _cell_measurement_theta_max 22.4666 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_density_meas 2.05(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.024 _exptl_crystal_F_000 1820 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.123 _exptl_crystal_size_mid 0.064 _exptl_crystal_size_min 0.063 _exptl_absorpt_coefficient_mu 1.840 _shelx_estimated_absorpt_T_min 0.805 _shelx_estimated_absorpt_T_max 0.893 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.89 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33166 _diffrn_reflns_av_unetI/netI 0.0590 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.796 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.973 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.973 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.973 _reflns_number_total 10663 _reflns_number_gt 8149 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 1.000 39 5 ' ' 2 0.120 0.699 0.571 12 1 ' ' 3 0.500 1.000 1.000 158 46 ' ' 4 0.343 0.171 0.475 29 3 ' ' 5 0.657 0.829 0.525 29 3 ' ' 6 0.879 0.301 0.429 12 1 ' ' _platon_squeeze_details ; The unit cell contains 3 water molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 10663 _refine_ls_number_parameters 821 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0678 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1533 _refine_ls_wR_factor_gt 0.1376 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 -0.08068(5) 0.89274(5) 0.27789(3) 0.01280(16) Uani 1 1 d . . . A 4 Mo2 Mo 0.19443(5) 0.77422(5) 0.34394(3) 0.00834(15) Uani 1 1 d . . . A 4 Mo3 Mo 0.38579(5) 0.56473(5) 0.26304(3) 0.00981(15) Uani 1 1 d . . . A 4 Mo4 Mo 0.23354(5) 0.52309(5) 0.15857(3) 0.01128(16) Uani 1 1 d . . . A 4 Mo5 Mo -0.05583(5) 0.67800(5) 0.18351(3) 0.01306(16) Uani 1 1 d . . . A 4 Cu1 Cu 0.31923(7) 0.92753(7) 0.38978(4) 0.0116(2) Uani 1 1 d . . . A 4 Cu2 Cu 0.38905(8) 0.23735(8) 0.12500(4) 0.0122(2) Uani 1 1 d . . . A 4 P1 P 0.13559(17) 0.80830(16) 0.17695(9) 0.0111(4) Uani 1 1 d . . . A 4 P2 P 0.12336(15) 0.57032(15) 0.31521(9) 0.0088(4) Uani 1 1 d . . . A 4 O1 O -0.1381(4) 0.8507(4) 0.3491(3) 0.0186(12) Uani 1 1 d . . . A 4 O2 O -0.1839(4) 1.0387(4) 0.2503(3) 0.0201(12) Uani 1 1 d . . . A 4 O3 O 0.0422(4) 0.9079(4) 0.3154(2) 0.0110(10) Uani 1 1 d . . . A 4 O4 O 0.0216(4) 0.9138(4) 0.1908(2) 0.0144(11) Uani 1 1 d . . . A 4 O5 O -0.1118(4) 0.8092(4) 0.2252(2) 0.0153(11) Uani 1 1 d . . . A 4 O6 O 0.1804(4) 0.7489(4) 0.4267(2) 0.0129(10) Uani 1 1 d . . . A 4 O7 O 0.2713(4) 0.8559(4) 0.3300(2) 0.0121(10) Uani 1 1 d . . . A 4 O8 O 0.3221(4) 0.6163(4) 0.3423(2) 0.0090(10) Uani 1 1 d . . . A 4 O9 O 0.2307(4) 0.7598(4) 0.2320(2) 0.0119(10) Uani 1 1 d . . . A 4 O10 O 0.4809(4) 0.6215(4) 0.2456(2) 0.0159(11) Uani 1 1 d . . . A 4 O11 O 0.4796(4) 0.4150(4) 0.2948(2) 0.0151(11) Uani 1 1 d . . . A 4 O12 O 0.3498(4) 0.5641(4) 0.1764(2) 0.0138(11) Uani 1 1 d . . . A 4 O13 O 0.2325(4) 0.5196(4) 0.2729(2) 0.0091(10) Uani 1 1 d . . . A 4 O14 O 0.2385(5) 0.5544(5) 0.0756(2) 0.0193(12) Uani 1 1 d . . . A 4 O15 O 0.3155(4) 0.3657(4) 0.1827(2) 0.0147(11) Uani 1 1 d . . . A 4 O16 O 0.0828(4) 0.5341(4) 0.1685(2) 0.0135(11) Uani 1 1 d . . . A 4 O17 O 0.1105(4) 0.7082(4) 0.1681(2) 0.0118(10) Uani 1 1 d . . . A 4 O18 O -0.1006(5) 0.7555(5) 0.1037(2) 0.0220(12) Uani 1 1 d . . . A 4 O19 O -0.1545(4) 0.6260(4) 0.2042(3) 0.0179(11) Uani 1 1 d . . . A 4 O20 O 0.0185(4) 0.5733(4) 0.2885(2) 0.0120(10) Uani 1 1 d . . . A 4 O21 O 0.0905(4) 0.6986(4) 0.3213(2) 0.0108(10) Uani 1 1 d . . . A 4 O90 O 0.7728(7) 0.7087(7) 0.4160(5) 0.065(2) Uani 1 1 d D . . B 4 H90A H 0.789(11) 0.759(9) 0.390(5) 0.078 Uiso 1 1 d D U . C 4 H90B H 0.827(8) 0.635(4) 0.430(6) 0.078 Uiso 1 1 d D U . D 4 O91 O 0.7206(7) 0.4175(8) 0.2933(5) 0.070(3) Uani 1 1 d D . . E 4 H91A H 0.740(12) 0.470(9) 0.276(7) 0.084 Uiso 1 1 d D U . F 4 H91B H 0.649(4) 0.448(11) 0.304(7) 0.084 Uiso 1 1 d D U . G 4 O92 O 0.7836(9) 0.5694(8) 0.3321(5) 0.077(3) Uani 1 1 d D . . H 4 H92A H 0.797(13) 0.619(10) 0.347(7) 0.092 Uiso 1 1 d D U . I 4 H92B H 0.781(13) 0.506(7) 0.352(6) 0.092 Uiso 1 1 d D U . J 4 N1 N 0.4227(5) 1.0077(5) 0.3690(3) 0.0138(13) Uani 1 1 d . . . A 4 N2 N 0.1987(5) 1.0898(5) 0.3452(3) 0.0122(13) Uani 1 1 d . . . A 4 N3 N 0.4361(5) 0.7637(5) 0.4375(3) 0.0141(13) Uani 1 1 d . . . A 4 N4 N 0.2466(5) 0.9269(5) 0.4810(3) 0.0129(13) Uani 1 1 d . . . A 4 N5 N 0.3814(6) 0.2881(6) 0.0256(3) 0.0206(15) Uani 1 1 d . . . A 4 N6 N 0.5217(5) 0.2727(5) 0.1143(3) 0.0158(13) Uani 1 1 d . . . A 4 N7 N 0.4633(5) 0.0670(5) 0.1849(3) 0.0133(13) Uani 1 1 d . . . A 4 N8 N 0.2476(6) 0.2148(6) 0.1355(3) 0.0155(13) Uani 1 1 d . . . A 4 C1 C 0.5365(6) 0.9606(7) 0.3853(4) 0.0181(17) Uani 1 1 d . . . A 4 H1 H 0.5794 0.8774 0.4064 0.022 Uiso 1 1 calc R U . A 4 C2 C 0.5947(7) 1.0264(7) 0.3729(4) 0.0196(17) Uani 1 1 d . . . A 4 H2 H 0.6762 0.9891 0.3848 0.024 Uiso 1 1 calc R U . A 4 C3 C 0.5335(7) 1.1464(6) 0.3433(4) 0.0163(16) Uani 1 1 d . . . A 4 H3 H 0.5717 1.1940 0.3348 0.020 Uiso 1 1 calc R U . A 4 C4 C 0.4141(7) 1.1983(6) 0.3258(3) 0.0141(15) Uani 1 1 d . . . A 4 H4 H 0.3699 1.2814 0.3050 0.017 Uiso 1 1 calc R U . A 4 C5 C 0.3609(6) 1.1264(6) 0.3392(3) 0.0117(15) Uani 1 1 d . . . A 4 C6 C 0.2358(6) 1.1710(6) 0.3240(3) 0.0094(14) Uani 1 1 d . . . A 4 C7 C 0.1586(7) 1.2881(6) 0.2902(3) 0.0153(16) Uani 1 1 d . . . A 4 H7 H 0.1870 1.3430 0.2725 0.018 Uiso 1 1 calc R U . A 4 C8 C 0.0401(6) 1.3243(6) 0.2823(4) 0.0144(16) Uani 1 1 d . . . A 4 H8 H -0.0147 1.4050 0.2616 0.017 Uiso 1 1 calc R U . A 4 C9 C 0.0036(7) 1.2381(6) 0.3056(4) 0.0186(17) Uani 1 1 d . . . A 4 H9 H -0.0769 1.2595 0.3011 0.022 Uiso 1 1 calc R U . A 4 C10 C 0.0855(7) 1.1229(7) 0.3351(4) 0.0179(17) Uani 1 1 d . . . A 4 H10 H 0.0609 1.0640 0.3490 0.021 Uiso 1 1 calc R U . A 4 C11 C 0.5294(7) 0.6854(7) 0.4097(4) 0.0191(17) Uani 1 1 d . . . A 4 H11 H 0.5397 0.7075 0.3642 0.023 Uiso 1 1 calc R U . A 4 C12 C 0.6104(6) 0.5735(6) 0.4460(4) 0.0162(16) Uani 1 1 d . . . A 4 H12 H 0.6760 0.5194 0.4258 0.019 Uiso 1 1 calc R U . A 4 C13 C 0.5949(7) 0.5422(7) 0.5112(4) 0.0200(17) Uani 1 1 d . . . A 4 H13 H 0.6494 0.4656 0.5370 0.024 Uiso 1 1 calc R U . A 4 C14 C 0.4985(6) 0.6235(6) 0.5399(4) 0.0157(16) Uani 1 1 d . . . A 4 H14 H 0.4876 0.6038 0.5855 0.019 Uiso 1 1 calc R U . A 4 C15 C 0.4197(7) 0.7322(6) 0.5014(3) 0.0145(16) Uani 1 1 d . . . A 4 C16 C 0.3088(6) 0.8224(6) 0.5256(4) 0.0140(15) Uani 1 1 d . . . A 4 C17 C 0.2713(7) 0.8028(7) 0.5891(4) 0.0185(17) Uani 1 1 d . . . A 4 H17 H 0.3145 0.7274 0.6193 0.022 Uiso 1 1 calc R U . A 4 C18 C 0.1713(7) 0.8939(7) 0.6076(4) 0.0172(16) Uani 1 1 d . . . A 4 H18 H 0.1457 0.8825 0.6510 0.021 Uiso 1 1 calc R U . A 4 C19 C 0.1078(7) 1.0022(7) 0.5628(4) 0.0207(17) Uani 1 1 d . . . A 4 H19 H 0.0385 1.0666 0.5747 0.025 Uiso 1 1 calc R U . A 4 C20 C 0.1486(7) 1.0138(7) 0.4999(4) 0.0172(16) Uani 1 1 d . . . A 4 H20 H 0.1045 1.0873 0.4686 0.021 Uiso 1 1 calc R U . A 4 C21 C 0.3086(8) 0.2869(9) -0.0158(4) 0.033(2) Uani 1 1 d . . . A 4 H21 H 0.2518 0.2637 0.0019 0.039 Uiso 1 1 calc R U . A 4 C22 C 0.3135(9) 0.3176(10) -0.0823(4) 0.038(2) Uani 1 1 d . . . A 4 H22 H 0.2599 0.3177 -0.1105 0.046 Uiso 1 1 calc R U . A 4 C23 C 0.3985(9) 0.3490(9) -0.1081(4) 0.039(2) Uani 1 1 d . . . A 4 H23 H 0.4037 0.3710 -0.1543 0.047 Uiso 1 1 calc R U . A 4 C24 C 0.4753(8) 0.3477(7) -0.0656(4) 0.0266(19) Uani 1 1 d . . . A 4 H24 H 0.5350 0.3672 -0.0822 0.032 Uiso 1 1 calc R U . A 4 C25 C 0.4641(7) 0.3178(7) 0.0009(4) 0.0213(17) Uani 1 1 d . . . A 4 C26 C 0.5410(7) 0.3131(6) 0.0504(4) 0.0172(16) Uani 1 1 d . . . A 4 C27 C 0.6261(7) 0.3485(7) 0.0355(4) 0.028(2) Uani 1 1 d . . . A 4 H27 H 0.6410 0.3737 -0.0089 0.034 Uiso 1 1 calc R U . A 4 C28 C 0.6890(8) 0.3464(8) 0.0866(5) 0.033(2) Uani 1 1 d . . . A 4 H28 H 0.7463 0.3721 0.0775 0.040 Uiso 1 1 calc R U . A 4 C29 C 0.6680(8) 0.3064(8) 0.1511(5) 0.033(2) Uani 1 1 d . . . A 4 H29 H 0.7109 0.3033 0.1867 0.039 Uiso 1 1 calc R U . A 4 C30 C 0.5821(7) 0.2711(7) 0.1621(4) 0.0190(17) Uani 1 1 d . . . A 4 H30 H 0.5665 0.2447 0.2061 0.023 Uiso 1 1 calc R U . A 4 C31 C 0.5769(7) -0.0048(7) 0.2061(4) 0.0169(16) Uani 1 1 d . . . A 4 H31 H 0.6272 0.0297 0.2017 0.020 Uiso 1 1 calc R U . A 4 C32 C 0.6233(7) -0.1258(7) 0.2336(4) 0.0199(17) Uani 1 1 d . . . A 4 H32 H 0.7032 -0.1735 0.2496 0.024 Uiso 1 1 calc R U . A 4 C33 C 0.5511(7) -0.1767(7) 0.2376(4) 0.0196(17) Uani 1 1 d . . . A 4 H33 H 0.5819 -0.2610 0.2544 0.024 Uiso 1 1 calc R U . A 4 C34 C 0.4323(7) -0.1029(6) 0.2169(3) 0.0148(16) Uani 1 1 d . . . A 4 H34 H 0.3810 -0.1360 0.2199 0.018 Uiso 1 1 calc R U . A 4 C35 C 0.3913(6) 0.0181(7) 0.1920(3) 0.0135(15) Uani 1 1 d . . . A 4 C36 C 0.2676(6) 0.1050(6) 0.1701(3) 0.0132(15) Uani 1 1 d . . . A 4 C37 C 0.1757(7) 0.0790(7) 0.1839(4) 0.0201(17) Uani 1 1 d . . . A 4 H37 H 0.1911 0.0015 0.2086 0.024 Uiso 1 1 calc R U . A 4 C38 C 0.0634(7) 0.1653(8) 0.1620(4) 0.0254(19) Uani 1 1 d . . . A 4 H38 H 0.0003 0.1480 0.1703 0.030 Uiso 1 1 calc R U . A 4 C39 C 0.0425(7) 0.2796(7) 0.1270(4) 0.0207(17) Uani 1 1 d . . . A 4 H39 H -0.0349 0.3412 0.1114 0.025 Uiso 1 1 calc R U . A 4 C40 C 0.1368(7) 0.3011(7) 0.1156(4) 0.0176(16) Uani 1 1 d . . . A 4 H40 H 0.1228 0.3792 0.0930 0.021 Uiso 1 1 calc R U . A 4 C41 C 0.1904(7) 0.8560(6) 0.1005(3) 0.0164(16) Uani 1 1 d . . . A 4 H41A H 0.2261 0.9044 0.1074 0.020 Uiso 1 1 calc R U . A 4 H41B H 0.2528 0.7840 0.0862 0.020 Uiso 1 1 calc R U . A 4 C42 C 0.0934(7) 0.9305(7) 0.0470(3) 0.0171(16) Uani 1 1 d . . . A 4 C43 C 0.0447(7) 0.8763(7) 0.0192(4) 0.0208(18) Uani 1 1 d . . . A 4 H43 H 0.0752 0.7914 0.0318 0.025 Uiso 1 1 calc R U . A 4 C44 C 0.0480(7) 1.0538(7) 0.0268(3) 0.0194(17) Uani 1 1 d . . . A 4 H44 H 0.0813 1.0914 0.0450 0.023 Uiso 1 1 calc R U . A 4 C45 C 0.1694(6) 0.4687(6) 0.3957(3) 0.0111(14) Uani 1 1 d . . . A 4 H45A H 0.2006 0.3857 0.3898 0.013 Uiso 1 1 calc R U . A 4 H45B H 0.2361 0.4724 0.4126 0.013 Uiso 1 1 calc R U . A 4 C46 C 0.0800(6) 0.4878(6) 0.4483(3) 0.0115(14) Uani 1 1 d . . . A 4 C47 C 0.0210(7) 0.4199(6) 0.4616(4) 0.0163(16) Uani 1 1 d . . . A 4 H47 H 0.0341 0.3653 0.4350 0.020 Uiso 1 1 calc R U . A 4 C48 C 0.0553(7) 0.5696(6) 0.4878(4) 0.0173(16) Uani 1 1 d . . . A 4 H48 H 0.0919 0.6186 0.4796 0.021 Uiso 1 1 calc R U . A 4 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 0.0087(3) 0.0103(3) 0.0169(3) -0.0048(3) -0.0020(3) -0.0016(3) Mo2 0.0084(3) 0.0074(3) 0.0081(3) -0.0010(2) 0.0000(2) -0.0032(2) Mo3 0.0097(3) 0.0077(3) 0.0103(3) -0.0017(2) 0.0029(2) -0.0035(2) Mo4 0.0154(3) 0.0088(3) 0.0090(3) -0.0022(2) 0.0025(2) -0.0057(3) Mo5 0.0133(3) 0.0103(3) 0.0135(3) -0.0025(2) -0.0036(3) -0.0038(3) Cu1 0.0114(5) 0.0077(4) 0.0126(5) 0.0002(3) -0.0010(4) -0.0031(4) Cu2 0.0137(5) 0.0141(4) 0.0110(4) -0.0024(4) 0.0021(4) -0.0089(4) P1 0.0154(10) 0.0082(8) 0.0080(9) 0.0011(7) -0.0017(7) -0.0055(8) P2 0.0088(9) 0.0080(8) 0.0082(9) -0.0006(7) 0.0007(7) -0.0036(7) O1 0.015(3) 0.018(3) 0.026(3) -0.011(2) 0.005(2) -0.008(2) O2 0.015(3) 0.011(3) 0.027(3) -0.005(2) -0.007(2) 0.000(2) O3 0.014(3) 0.007(2) 0.009(2) -0.0015(19) -0.001(2) -0.003(2) O4 0.025(3) 0.010(2) 0.008(2) 0.000(2) 0.001(2) -0.009(2) O5 0.011(3) 0.015(3) 0.021(3) -0.009(2) -0.001(2) -0.005(2) O6 0.014(3) 0.012(2) 0.013(3) -0.004(2) 0.003(2) -0.006(2) O7 0.012(3) 0.012(2) 0.013(3) -0.004(2) 0.002(2) -0.006(2) O8 0.009(2) 0.010(2) 0.006(2) 0.0006(19) -0.0007(19) -0.003(2) O9 0.011(3) 0.007(2) 0.012(3) 0.0022(19) -0.004(2) -0.001(2) O10 0.017(3) 0.016(3) 0.017(3) -0.005(2) 0.006(2) -0.010(2) O11 0.013(3) 0.014(3) 0.017(3) -0.006(2) 0.004(2) -0.005(2) O12 0.018(3) 0.012(2) 0.015(3) -0.006(2) 0.004(2) -0.009(2) O13 0.011(3) 0.008(2) 0.009(2) -0.0016(19) 0.0020(19) -0.005(2) O14 0.025(3) 0.021(3) 0.012(3) -0.004(2) 0.002(2) -0.011(2) O15 0.015(3) 0.016(3) 0.016(3) -0.007(2) 0.006(2) -0.008(2) O16 0.014(3) 0.012(2) 0.013(3) -0.005(2) 0.002(2) -0.005(2) O17 0.015(3) 0.013(2) 0.008(2) -0.004(2) 0.002(2) -0.007(2) O18 0.036(3) 0.017(3) 0.013(3) -0.001(2) -0.010(2) -0.012(3) O19 0.014(3) 0.017(3) 0.022(3) -0.002(2) -0.005(2) -0.007(2) O20 0.012(3) 0.013(2) 0.012(3) -0.002(2) -0.001(2) -0.007(2) O21 0.010(3) 0.010(2) 0.013(3) -0.004(2) 0.003(2) -0.004(2) O90 0.035(5) 0.044(5) 0.089(7) 0.024(4) -0.007(4) -0.014(4) O91 0.024(4) 0.062(6) 0.084(7) 0.005(5) -0.012(4) 0.001(4) O92 0.077(6) 0.050(5) 0.074(7) 0.007(5) 0.032(5) -0.022(5) N1 0.014(3) 0.006(3) 0.021(3) -0.006(3) 0.003(3) -0.003(3) N2 0.010(3) 0.013(3) 0.014(3) -0.002(2) -0.001(2) -0.006(3) N3 0.012(3) 0.013(3) 0.013(3) 0.001(2) -0.002(3) -0.004(3) N4 0.012(3) 0.011(3) 0.013(3) -0.002(2) 0.000(3) -0.004(3) N5 0.024(4) 0.029(4) 0.011(3) -0.002(3) 0.004(3) -0.016(3) N6 0.015(3) 0.010(3) 0.022(3) -0.004(3) 0.000(3) -0.005(3) N7 0.017(3) 0.019(3) 0.008(3) -0.005(3) 0.004(3) -0.011(3) N8 0.023(4) 0.025(3) 0.007(3) -0.006(3) 0.003(3) -0.017(3) C1 0.012(4) 0.012(4) 0.020(4) 0.002(3) -0.006(3) 0.000(3) C2 0.012(4) 0.020(4) 0.025(4) -0.004(3) -0.003(3) -0.007(3) C3 0.018(4) 0.017(4) 0.019(4) -0.008(3) 0.004(3) -0.012(3) C4 0.019(4) 0.016(4) 0.012(4) -0.003(3) 0.001(3) -0.012(3) C5 0.014(4) 0.015(4) 0.005(3) -0.006(3) 0.003(3) -0.005(3) C6 0.013(4) 0.010(3) 0.004(3) -0.003(3) -0.002(3) -0.004(3) C7 0.023(4) 0.011(4) 0.012(4) -0.002(3) -0.001(3) -0.008(3) C8 0.008(4) 0.009(3) 0.022(4) -0.008(3) 0.004(3) 0.000(3) C9 0.017(4) 0.015(4) 0.023(4) -0.002(3) 0.000(3) -0.007(3) C10 0.019(4) 0.017(4) 0.018(4) 0.002(3) 0.001(3) -0.012(3) C11 0.023(4) 0.015(4) 0.013(4) 0.001(3) 0.000(3) -0.006(3) C12 0.012(4) 0.014(4) 0.016(4) -0.002(3) 0.000(3) -0.003(3) C13 0.017(4) 0.014(4) 0.023(4) 0.005(3) -0.011(3) -0.005(3) C14 0.019(4) 0.018(4) 0.013(4) 0.001(3) -0.001(3) -0.013(3) C15 0.024(4) 0.011(3) 0.013(4) -0.001(3) 0.001(3) -0.013(3) C16 0.014(4) 0.014(4) 0.019(4) -0.005(3) -0.002(3) -0.010(3) C17 0.022(4) 0.023(4) 0.018(4) -0.004(3) 0.007(3) -0.018(4) C18 0.023(4) 0.032(4) 0.009(4) -0.006(3) 0.003(3) -0.023(4) C19 0.021(4) 0.029(4) 0.021(4) -0.015(4) 0.006(3) -0.016(4) C20 0.014(4) 0.019(4) 0.020(4) -0.005(3) -0.002(3) -0.008(3) C21 0.041(6) 0.056(6) 0.017(4) -0.012(4) 0.006(4) -0.035(5) C22 0.041(6) 0.070(7) 0.009(4) -0.008(4) 0.005(4) -0.033(6) C23 0.058(7) 0.046(6) 0.017(5) -0.002(4) 0.002(4) -0.030(5) C24 0.029(5) 0.028(5) 0.016(4) 0.002(4) 0.006(4) -0.013(4) C25 0.018(4) 0.017(4) 0.028(5) -0.005(3) 0.005(3) -0.008(3) C26 0.018(4) 0.009(3) 0.019(4) 0.000(3) 0.004(3) -0.004(3) C27 0.020(5) 0.028(5) 0.033(5) 0.000(4) 0.009(4) -0.013(4) C28 0.024(5) 0.038(5) 0.043(6) 0.002(4) -0.001(4) -0.024(4) C29 0.020(5) 0.032(5) 0.044(6) 0.000(4) -0.009(4) -0.014(4) C30 0.016(4) 0.019(4) 0.022(4) -0.003(3) 0.000(3) -0.009(3) C31 0.019(4) 0.019(4) 0.016(4) -0.001(3) 0.001(3) -0.013(3) C32 0.014(4) 0.023(4) 0.023(4) -0.010(3) 0.002(3) -0.007(3) C33 0.031(5) 0.017(4) 0.011(4) -0.001(3) 0.001(3) -0.013(4) C34 0.023(4) 0.019(4) 0.011(4) -0.006(3) 0.010(3) -0.017(3) C35 0.014(4) 0.021(4) 0.008(4) -0.009(3) 0.002(3) -0.008(3) C36 0.017(4) 0.013(4) 0.012(4) -0.006(3) 0.005(3) -0.009(3) C37 0.023(4) 0.021(4) 0.022(4) -0.009(3) 0.001(3) -0.013(4) C38 0.024(5) 0.036(5) 0.025(5) -0.009(4) 0.008(4) -0.022(4) C39 0.014(4) 0.023(4) 0.027(4) -0.009(3) -0.001(3) -0.008(3) C40 0.017(4) 0.016(4) 0.020(4) -0.004(3) 0.000(3) -0.007(3) C41 0.018(4) 0.015(4) 0.013(4) 0.002(3) -0.001(3) -0.007(3) C42 0.021(4) 0.020(4) 0.005(3) 0.000(3) 0.001(3) -0.007(3) C43 0.040(5) 0.010(4) 0.013(4) -0.003(3) -0.002(4) -0.012(4) C44 0.035(5) 0.018(4) 0.008(4) -0.005(3) 0.002(3) -0.014(4) C45 0.012(4) 0.011(3) 0.007(3) 0.003(3) -0.002(3) -0.004(3) C46 0.011(4) 0.010(3) 0.010(4) -0.001(3) -0.004(3) -0.002(3) C47 0.022(4) 0.015(4) 0.013(4) -0.008(3) 0.002(3) -0.007(3) C48 0.020(4) 0.014(4) 0.023(4) -0.005(3) 0.004(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.691(5) . ? Mo1 O1 1.714(5) . ? Mo1 O5 1.912(5) . ? Mo1 O3 1.952(5) . ? Mo1 O4 2.221(5) . ? Mo1 O21 2.429(5) . ? Mo2 O6 1.702(5) . ? Mo2 O7 1.757(5) . ? Mo2 O3 1.905(5) . ? Mo2 O8 1.918(5) . ? Mo2 O21 2.164(5) . ? Mo2 O9 2.393(5) . ? Mo3 O11 1.710(5) . ? Mo3 O10 1.712(5) . ? Mo3 O12 1.916(5) . ? Mo3 O8 1.918(4) . ? Mo3 O9 2.315(4) . ? Mo3 O13 2.328(5) . ? Mo4 O14 1.695(5) . ? Mo4 O15 1.749(5) . ? Mo4 O16 1.897(5) . ? Mo4 O12 1.926(5) . ? Mo4 O17 2.198(5) . ? Mo4 O13 2.388(5) . ? Mo5 O19 1.714(5) . ? Mo5 O18 1.714(5) . ? Mo5 O5 1.904(5) . ? Mo5 O16 1.936(5) . ? Mo5 O20 2.294(5) . ? Mo5 O17 2.374(5) . ? Cu1 N2 1.963(6) . ? Cu1 N3 1.980(6) . ? Cu1 O7 2.025(5) . ? Cu1 N1 2.047(6) . ? Cu1 N4 2.069(6) . ? Cu2 N6 1.983(6) . ? Cu2 N8 1.994(6) . ? Cu2 N5 2.028(6) . ? Cu2 N7 2.053(6) . ? Cu2 O15 2.098(5) . ? P1 O4 1.518(5) . ? P1 O9 1.542(5) . ? P1 O17 1.548(5) . ? P1 C41 1.806(7) . ? P2 O20 1.498(5) . ? P2 O21 1.548(5) . ? P2 O13 1.552(5) . ? P2 C45 1.813(7) . ? O90 H90A 0.86(2) . ? O90 H90B 0.86(2) . ? O91 H91A 0.84(2) . ? O91 H91B 0.84(2) . ? O92 H92A 0.87(3) . ? O92 H92B 0.84(2) . ? N1 C1 1.332(9) . ? N1 C5 1.355(9) . ? N2 C10 1.337(9) . ? N2 C6 1.344(9) . ? N3 C11 1.347(10) . ? N3 C15 1.339(9) . ? N4 C20 1.337(9) . ? N4 C16 1.350(9) . ? N5 C21 1.343(11) . ? N5 C25 1.345(10) . ? N6 C30 1.313(10) . ? N6 C26 1.371(9) . ? N7 C31 1.346(10) . ? N7 C35 1.354(9) . ? N8 C40 1.343(10) . ? N8 C36 1.350(9) . ? C1 C2 1.375(11) . ? C1 H1 0.9500 . ? C2 C3 1.366(10) . ? C2 H2 0.9500 . ? C3 C4 1.397(10) . ? C3 H3 0.9500 . ? C4 C5 1.388(10) . ? C4 H4 0.9500 . ? C5 C6 1.469(10) . ? C6 C7 1.393(10) . ? C7 C8 1.386(10) . ? C7 H7 0.9500 . ? C8 C9 1.401(10) . ? C8 H8 0.9500 . ? C9 C10 1.367(10) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.383(10) . ? C11 H11 0.9500 . ? C12 C13 1.362(11) . ? C12 H12 0.9500 . ? C13 C14 1.393(11) . ? C13 H13 0.9500 . ? C14 C15 1.369(10) . ? C14 H14 0.9500 . ? C15 C16 1.493(10) . ? C16 C17 1.393(10) . ? C17 C18 1.371(11) . ? C17 H17 0.9500 . ? C18 C19 1.383(11) . ? C18 H18 0.9500 . ? C19 C20 1.386(11) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.364(11) . ? C21 H21 0.9500 . ? C22 C23 1.392(13) . ? C22 H22 0.9500 . ? C23 C24 1.384(13) . ? C23 H23 0.9500 . ? C24 C25 1.375(11) . ? C24 H24 0.9500 . ? C25 C26 1.470(11) . ? C26 C27 1.388(11) . ? C27 C28 1.387(13) . ? C27 H27 0.9500 . ? C28 C29 1.389(13) . ? C28 H28 0.9500 . ? C29 C30 1.391(11) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.371(11) . ? C31 H31 0.9500 . ? C32 C33 1.383(11) . ? C32 H32 0.9500 . ? C33 C34 1.399(11) . ? C33 H33 0.9500 . ? C34 C35 1.371(10) . ? C34 H34 0.9500 . ? C35 C36 1.472(10) . ? C36 C37 1.390(10) . ? C37 C38 1.365(12) . ? C37 H37 0.9500 . ? C38 C39 1.398(11) . ? C38 H38 0.9500 . ? C39 C40 1.381(11) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.516(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C44 1.379(10) . ? C42 C43 1.394(11) . ? C43 C44 1.380(11) 2_575 ? C43 H43 0.9500 . ? C44 C43 1.380(11) 2_575 ? C44 H44 0.9500 . ? C45 C46 1.512(9) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C48 1.405(10) . ? C46 C47 1.406(10) . ? C47 C48 1.380(10) 2_566 ? C47 H47 0.9500 . ? C48 C47 1.380(10) 2_566 ? C48 H48 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 102.3(2) . . ? O2 Mo1 O5 103.8(2) . . ? O1 Mo1 O5 98.1(2) . . ? O2 Mo1 O3 102.0(2) . . ? O1 Mo1 O3 99.1(2) . . ? O5 Mo1 O3 145.0(2) . . ? O2 Mo1 O4 88.1(2) . . ? O1 Mo1 O4 169.6(2) . . ? O5 Mo1 O4 79.82(19) . . ? O3 Mo1 O4 77.81(19) . . ? O2 Mo1 O21 169.3(2) . . ? O1 Mo1 O21 81.6(2) . . ? O5 Mo1 O21 85.38(19) . . ? O3 Mo1 O21 67.33(17) . . ? O4 Mo1 O21 88.03(16) . . ? O6 Mo2 O7 103.6(2) . . ? O6 Mo2 O3 100.3(2) . . ? O7 Mo2 O3 96.9(2) . . ? O6 Mo2 O8 96.8(2) . . ? O7 Mo2 O8 99.8(2) . . ? O3 Mo2 O8 152.4(2) . . ? O6 Mo2 O21 97.6(2) . . ? O7 Mo2 O21 158.2(2) . . ? O3 Mo2 O21 74.11(18) . . ? O8 Mo2 O21 82.38(18) . . ? O6 Mo2 O9 166.49(19) . . ? O7 Mo2 O9 85.36(19) . . ? O3 Mo2 O9 88.45(18) . . ? O8 Mo2 O9 71.37(17) . . ? O21 Mo2 O9 74.75(16) . . ? O11 Mo3 O10 102.0(2) . . ? O11 Mo3 O12 102.0(2) . . ? O10 Mo3 O12 100.2(2) . . ? O11 Mo3 O8 100.0(2) . . ? O10 Mo3 O8 100.7(2) . . ? O12 Mo3 O8 145.6(2) . . ? O11 Mo3 O9 168.4(2) . . ? O10 Mo3 O9 88.6(2) . . ? O12 Mo3 O9 80.36(19) . . ? O8 Mo3 O9 73.19(17) . . ? O11 Mo3 O13 87.9(2) . . ? O10 Mo3 O13 169.4(2) . . ? O12 Mo3 O13 73.85(18) . . ? O8 Mo3 O13 80.84(18) . . ? O9 Mo3 O13 81.81(16) . . ? O14 Mo4 O15 104.6(2) . . ? O14 Mo4 O16 100.7(2) . . ? O15 Mo4 O16 96.4(2) . . ? O14 Mo4 O12 97.1(2) . . ? O15 Mo4 O12 99.8(2) . . ? O16 Mo4 O12 152.1(2) . . ? O14 Mo4 O17 97.2(2) . . ? O15 Mo4 O17 157.4(2) . . ? O16 Mo4 O17 73.83(18) . . ? O12 Mo4 O17 82.69(19) . . ? O14 Mo4 O13 166.4(2) . . ? O15 Mo4 O13 85.77(19) . . ? O16 Mo4 O13 86.52(18) . . ? O12 Mo4 O13 72.26(17) . . ? O17 Mo4 O13 73.54(16) . . ? O19 Mo5 O18 101.5(3) . . ? O19 Mo5 O5 103.6(2) . . ? O18 Mo5 O5 100.1(2) . . ? O19 Mo5 O16 101.2(2) . . ? O18 Mo5 O16 99.4(2) . . ? O5 Mo5 O16 144.4(2) . . ? O19 Mo5 O20 82.8(2) . . ? O18 Mo5 O20 175.4(2) . . ? O5 Mo5 O20 80.31(19) . . ? O16 Mo5 O20 77.96(19) . . ? O19 Mo5 O17 167.6(2) . . ? O18 Mo5 O17 88.1(2) . . ? O5 Mo5 O17 82.14(18) . . ? O16 Mo5 O17 69.12(18) . . ? O20 Mo5 O17 87.50(16) . . ? N2 Cu1 N3 177.6(2) . . ? N2 Cu1 O7 89.7(2) . . ? N3 Cu1 O7 90.5(2) . . ? N2 Cu1 N1 81.3(2) . . ? N3 Cu1 N1 100.5(2) . . ? O7 Cu1 N1 127.9(2) . . ? N2 Cu1 N4 97.1(2) . . ? N3 Cu1 N4 80.7(2) . . ? O7 Cu1 N4 115.3(2) . . ? N1 Cu1 N4 116.7(2) . . ? N6 Cu2 N8 175.7(2) . . ? N6 Cu2 N5 81.4(3) . . ? N8 Cu2 N5 98.2(2) . . ? N6 Cu2 N7 102.8(2) . . ? N8 Cu2 N7 80.7(2) . . ? N5 Cu2 N7 129.3(2) . . ? N6 Cu2 O15 86.2(2) . . ? N8 Cu2 O15 90.4(2) . . ? N5 Cu2 O15 121.3(2) . . ? N7 Cu2 O15 109.4(2) . . ? O4 P1 O9 111.2(3) . . ? O4 P1 O17 109.3(3) . . ? O9 P1 O17 111.2(3) . . ? O4 P1 C41 109.6(3) . . ? O9 P1 C41 108.5(3) . . ? O17 P1 C41 106.8(3) . . ? O20 P2 O21 109.5(3) . . ? O20 P2 O13 112.4(3) . . ? O21 P2 O13 110.7(3) . . ? O20 P2 C45 110.1(3) . . ? O21 P2 C45 109.0(3) . . ? O13 P2 C45 105.0(3) . . ? Mo2 O3 Mo1 122.9(2) . . ? P1 O4 Mo1 121.6(3) . . ? Mo5 O5 Mo1 149.5(3) . . ? Mo2 O7 Cu1 132.1(3) . . ? Mo2 O8 Mo3 123.6(2) . . ? P1 O9 Mo3 126.8(3) . . ? P1 O9 Mo2 125.7(3) . . ? Mo3 O9 Mo2 91.77(16) . . ? Mo3 O12 Mo4 122.6(2) . . ? P2 O13 Mo3 126.4(3) . . ? P2 O13 Mo4 127.3(3) . . ? Mo3 O13 Mo4 91.19(15) . . ? Mo4 O15 Cu2 129.5(3) . . ? Mo4 O16 Mo5 122.4(2) . . ? P1 O17 Mo4 130.0(3) . . ? P1 O17 Mo5 134.3(3) . . ? Mo4 O17 Mo5 94.50(17) . . ? P2 O20 Mo5 120.6(3) . . ? P2 O21 Mo2 132.5(3) . . ? P2 O21 Mo1 130.5(3) . . ? Mo2 O21 Mo1 94.91(16) . . ? H90A O90 H90B 120(10) . . ? H91A O91 H91B 112(10) . . ? H92A O92 H92B 131(10) . . ? C1 N1 C5 118.7(6) . . ? C1 N1 Cu1 128.4(5) . . ? C5 N1 Cu1 112.7(5) . . ? C10 N2 C6 119.5(6) . . ? C10 N2 Cu1 124.6(5) . . ? C6 N2 Cu1 115.9(5) . . ? C11 N3 C15 119.6(6) . . ? C11 N3 Cu1 124.0(5) . . ? C15 N3 Cu1 116.4(5) . . ? C20 N4 C16 118.1(6) . . ? C20 N4 Cu1 128.8(5) . . ? C16 N4 Cu1 113.1(5) . . ? C21 N5 C25 119.2(7) . . ? C21 N5 Cu2 126.5(5) . . ? C25 N5 Cu2 114.2(5) . . ? C30 N6 C26 119.5(6) . . ? C30 N6 Cu2 125.7(5) . . ? C26 N6 Cu2 114.5(5) . . ? C31 N7 C35 118.6(6) . . ? C31 N7 Cu2 127.4(5) . . ? C35 N7 Cu2 112.7(5) . . ? C40 N8 C36 119.3(6) . . ? C40 N8 Cu2 125.4(5) . . ? C36 N8 Cu2 115.1(5) . . ? N1 C1 C2 123.2(7) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C3 C2 C1 118.9(7) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.1(7) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 119.0(7) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 121.1(7) . . ? N1 C5 C6 114.9(6) . . ? C4 C5 C6 123.9(6) . . ? N2 C6 C7 120.8(6) . . ? N2 C6 C5 115.1(6) . . ? C7 C6 C5 124.1(6) . . ? C6 C7 C8 119.8(7) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C7 C8 C9 118.0(7) . . ? C7 C8 H8 121.0 . . ? C9 C8 H8 121.0 . . ? C10 C9 C8 119.0(7) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? N2 C10 C9 122.7(7) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C12 121.5(7) . . ? N3 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 119.0(7) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 119.4(7) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 119.2(7) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N3 C15 C14 121.3(7) . . ? N3 C15 C16 114.8(6) . . ? C14 C15 C16 123.9(7) . . ? N4 C16 C17 121.6(7) . . ? N4 C16 C15 114.7(6) . . ? C17 C16 C15 123.6(7) . . ? C18 C17 C16 119.1(7) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 119.9(7) . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 C18 117.7(7) . . ? C20 C19 H19 121.1 . . ? C18 C19 H19 121.1 . . ? N4 C20 C19 123.5(7) . . ? N4 C20 H20 118.2 . . ? C19 C20 H20 118.2 . . ? N5 C21 C22 122.4(8) . . ? N5 C21 H21 118.8 . . ? C22 C21 H21 118.8 . . ? C21 C22 C23 118.7(9) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 119.1(8) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C23 C24 C25 119.1(8) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? N5 C25 C24 121.5(8) . . ? N5 C25 C26 114.8(7) . . ? C24 C25 C26 123.7(7) . . ? N6 C26 C27 121.0(8) . . ? N6 C26 C25 115.1(6) . . ? C27 C26 C25 123.9(7) . . ? C26 C27 C28 118.7(8) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C29 C28 C27 119.8(8) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 118.1(8) . . ? C28 C29 H29 121.0 . . ? C30 C29 H29 121.0 . . ? N6 C30 C29 122.9(8) . . ? N6 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N7 C31 C32 122.7(7) . . ? N7 C31 H31 118.6 . . ? C32 C31 H31 118.6 . . ? C33 C32 C31 118.5(7) . . ? C33 C32 H32 120.7 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 119.4(7) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 118.7(7) . . ? C35 C34 H34 120.7 . . ? C33 C34 H34 120.7 . . ? N7 C35 C34 121.9(7) . . ? N7 C35 C36 114.5(6) . . ? C34 C35 C36 123.6(7) . . ? N8 C36 C37 121.1(7) . . ? N8 C36 C35 115.3(6) . . ? C37 C36 C35 123.7(7) . . ? C38 C37 C36 119.8(7) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 119.1(7) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 118.7(7) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? N8 C40 C39 122.0(7) . . ? N8 C40 H40 119.0 . . ? C39 C40 H40 119.0 . . ? C42 C41 P1 111.8(5) . . ? C42 C41 H41A 109.3 . . ? P1 C41 H41A 109.3 . . ? C42 C41 H41B 109.3 . . ? P1 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? C44 C42 C43 118.5(7) . . ? C44 C42 C41 120.9(7) . . ? C43 C42 C41 120.5(7) . . ? C44 C43 C42 119.8(7) 2_575 . ? C44 C43 H43 120.1 2_575 . ? C42 C43 H43 120.1 . . ? C42 C44 C43 121.6(7) . 2_575 ? C42 C44 H44 119.2 . . ? C43 C44 H44 119.2 2_575 . ? C46 C45 P2 118.8(5) . . ? C46 C45 H45A 107.6 . . ? P2 C45 H45A 107.6 . . ? C46 C45 H45B 107.6 . . ? P2 C45 H45B 107.6 . . ? H45A C45 H45B 107.1 . . ? C48 C46 C47 116.9(6) . . ? C48 C46 C45 122.2(6) . . ? C47 C46 C45 120.8(6) . . ? C48 C47 C46 121.7(7) 2_566 . ? C48 C47 H47 119.1 2_566 . ? C46 C47 H47 119.1 . . ? C47 C48 C46 121.3(7) 2_566 . ? C47 C48 H48 119.3 2_566 . ? C46 C48 H48 119.3 . . ? 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 O9 P1 O4 Mo1 -62.9(4) . . . . ? O17 P1 O4 Mo1 60.2(4) . . . . ? C41 P1 O4 Mo1 177.0(3) . . . . ? O6 Mo2 O7 Cu1 -7.2(4) . . . . ? O3 Mo2 O7 Cu1 95.2(3) . . . . ? O8 Mo2 O7 Cu1 -106.8(3) . . . . ? O21 Mo2 O7 Cu1 159.2(4) . . . . ? O9 Mo2 O7 Cu1 -176.9(3) . . . . ? O4 P1 O9 Mo3 152.6(3) . . . . ? O17 P1 O9 Mo3 30.5(4) . . . . ? C41 P1 O9 Mo3 -86.7(4) . . . . ? O4 P1 O9 Mo2 26.7(4) . . . . ? O17 P1 O9 Mo2 -95.3(3) . . . . ? C41 P1 O9 Mo2 147.4(3) . . . . ? O20 P2 O13 Mo3 152.8(3) . . . . ? O21 P2 O13 Mo3 30.0(4) . . . . ? C45 P2 O13 Mo3 -87.5(4) . . . . ? O20 P2 O13 Mo4 26.3(4) . . . . ? O21 P2 O13 Mo4 -96.5(3) . . . . ? C45 P2 O13 Mo4 146.0(3) . . . . ? O14 Mo4 O15 Cu2 -6.6(4) . . . . ? O16 Mo4 O15 Cu2 96.2(3) . . . . ? O12 Mo4 O15 Cu2 -106.6(3) . . . . ? O17 Mo4 O15 Cu2 158.9(4) . . . . ? O13 Mo4 O15 Cu2 -177.8(3) . . . . ? O14 Mo4 O16 Mo5 -97.9(3) . . . . ? O15 Mo4 O16 Mo5 155.9(3) . . . . ? O12 Mo4 O16 Mo5 30.6(6) . . . . ? O17 Mo4 O16 Mo5 -3.3(3) . . . . ? O13 Mo4 O16 Mo5 70.5(3) . . . . ? O4 P1 O17 Mo4 -172.0(3) . . . . ? O9 P1 O17 Mo4 -48.8(4) . . . . ? C41 P1 O17 Mo4 69.5(4) . . . . ? O4 P1 O17 Mo5 -8.3(5) . . . . ? O9 P1 O17 Mo5 114.8(4) . . . . ? C41 P1 O17 Mo5 -126.9(4) . . . . ? O21 P2 O20 Mo5 65.9(3) . . . . ? O13 P2 O20 Mo5 -57.6(4) . . . . ? C45 P2 O20 Mo5 -174.3(3) . . . . ? O20 P2 O21 Mo2 -171.5(3) . . . . ? O13 P2 O21 Mo2 -47.0(4) . . . . ? C45 P2 O21 Mo2 68.1(4) . . . . ? O20 P2 O21 Mo1 -12.3(4) . . . . ? O13 P2 O21 Mo1 112.3(3) . . . . ? C45 P2 O21 Mo1 -132.7(3) . . . . ? C5 N1 C1 C2 -0.3(11) . . . . ? Cu1 N1 C1 C2 -174.8(6) . . . . ? N1 C1 C2 C3 0.8(12) . . . . ? C1 C2 C3 C4 -0.8(11) . . . . ? C2 C3 C4 C5 0.2(11) . . . . ? C1 N1 C5 C4 -0.3(10) . . . . ? Cu1 N1 C5 C4 175.1(5) . . . . ? C1 N1 C5 C6 -179.0(6) . . . . ? Cu1 N1 C5 C6 -3.7(7) . . . . ? C3 C4 C5 N1 0.3(10) . . . . ? C3 C4 C5 C6 179.0(6) . . . . ? C10 N2 C6 C7 -1.9(10) . . . . ? Cu1 N2 C6 C7 178.2(5) . . . . ? C10 N2 C6 C5 178.4(6) . . . . ? Cu1 N2 C6 C5 -1.5(7) . . . . ? N1 C5 C6 N2 3.5(9) . . . . ? C4 C5 C6 N2 -175.2(6) . . . . ? N1 C5 C6 C7 -176.2(6) . . . . ? C4 C5 C6 C7 5.1(11) . . . . ? N2 C6 C7 C8 4.8(10) . . . . ? C5 C6 C7 C8 -175.5(6) . . . . ? C6 C7 C8 C9 -3.8(10) . . . . ? C7 C8 C9 C10 0.1(11) . . . . ? C6 N2 C10 C9 -2.0(11) . . . . ? Cu1 N2 C10 C9 177.8(6) . . . . ? C8 C9 C10 N2 2.9(12) . . . . ? C15 N3 C11 C12 -1.4(11) . . . . ? Cu1 N3 C11 C12 177.8(6) . . . . ? N3 C11 C12 C13 0.3(12) . . . . ? C11 C12 C13 C14 -0.4(11) . . . . ? C12 C13 C14 C15 1.6(11) . . . . ? C11 N3 C15 C14 2.6(11) . . . . ? Cu1 N3 C15 C14 -176.6(5) . . . . ? C11 N3 C15 C16 -175.7(6) . . . . ? Cu1 N3 C15 C16 5.1(8) . . . . ? C13 C14 C15 N3 -2.8(11) . . . . ? C13 C14 C15 C16 175.4(7) . . . . ? C20 N4 C16 C17 1.9(10) . . . . ? Cu1 N4 C16 C17 -177.3(6) . . . . ? C20 N4 C16 C15 -177.6(6) . . . . ? Cu1 N4 C16 C15 3.2(7) . . . . ? N3 C15 C16 N4 -5.5(9) . . . . ? C14 C15 C16 N4 176.2(7) . . . . ? N3 C15 C16 C17 175.1(7) . . . . ? C14 C15 C16 C17 -3.2(11) . . . . ? N4 C16 C17 C18 -2.7(11) . . . . ? C15 C16 C17 C18 176.7(7) . . . . ? C16 C17 C18 C19 1.5(11) . . . . ? C17 C18 C19 C20 0.4(11) . . . . ? C16 N4 C20 C19 0.1(11) . . . . ? Cu1 N4 C20 C19 179.2(5) . . . . ? C18 C19 C20 N4 -1.3(11) . . . . ? C25 N5 C21 C22 -1.7(14) . . . . ? Cu2 N5 C21 C22 -177.0(7) . . . . ? N5 C21 C22 C23 1.3(15) . . . . ? C21 C22 C23 C24 0.2(15) . . . . ? C22 C23 C24 C25 -1.3(14) . . . . ? C21 N5 C25 C24 0.5(12) . . . . ? Cu2 N5 C25 C24 176.3(6) . . . . ? C21 N5 C25 C26 -178.4(7) . . . . ? Cu2 N5 C25 C26 -2.5(8) . . . . ? C23 C24 C25 N5 1.0(13) . . . . ? C23 C24 C25 C26 179.8(8) . . . . ? C30 N6 C26 C27 2.1(10) . . . . ? Cu2 N6 C26 C27 176.0(6) . . . . ? C30 N6 C26 C25 -176.6(6) . . . . ? Cu2 N6 C26 C25 -2.7(8) . . . . ? N5 C25 C26 N6 3.5(10) . . . . ? C24 C25 C26 N6 -175.4(7) . . . . ? N5 C25 C26 C27 -175.2(7) . . . . ? C24 C25 C26 C27 5.9(12) . . . . ? N6 C26 C27 C28 -2.2(12) . . . . ? C25 C26 C27 C28 176.5(8) . . . . ? C26 C27 C28 C29 1.5(13) . . . . ? C27 C28 C29 C30 -0.8(13) . . . . ? C26 N6 C30 C29 -1.4(11) . . . . ? Cu2 N6 C30 C29 -174.6(6) . . . . ? C28 C29 C30 N6 0.8(12) . . . . ? C35 N7 C31 C32 0.9(11) . . . . ? Cu2 N7 C31 C32 -165.2(6) . . . . ? N7 C31 C32 C33 2.4(11) . . . . ? C31 C32 C33 C34 -3.3(11) . . . . ? C32 C33 C34 C35 1.0(11) . . . . ? C31 N7 C35 C34 -3.4(10) . . . . ? Cu2 N7 C35 C34 164.7(5) . . . . ? C31 N7 C35 C36 177.3(6) . . . . ? Cu2 N7 C35 C36 -14.6(7) . . . . ? C33 C34 C35 N7 2.4(10) . . . . ? C33 C34 C35 C36 -178.4(6) . . . . ? C40 N8 C36 C37 1.7(10) . . . . ? Cu2 N8 C36 C37 176.8(5) . . . . ? C40 N8 C36 C35 -177.7(6) . . . . ? Cu2 N8 C36 C35 -2.6(8) . . . . ? N7 C35 C36 N8 11.7(9) . . . . ? C34 C35 C36 N8 -167.6(6) . . . . ? N7 C35 C36 C37 -167.7(7) . . . . ? C34 C35 C36 C37 13.0(11) . . . . ? N8 C36 C37 C38 0.4(11) . . . . ? C35 C36 C37 C38 179.7(7) . . . . ? C36 C37 C38 C39 -1.4(12) . . . . ? C37 C38 C39 C40 0.3(12) . . . . ? C36 N8 C40 C39 -2.8(11) . . . . ? Cu2 N8 C40 C39 -177.4(6) . . . . ? C38 C39 C40 N8 1.8(12) . . . . ? O4 P1 C41 C42 -45.3(6) . . . . ? O9 P1 C41 C42 -166.9(5) . . . . ? O17 P1 C41 C42 73.0(6) . . . . ? P1 C41 C42 C44 106.0(7) . . . . ? P1 C41 C42 C43 -71.3(8) . . . . ? C44 C42 C43 C44 -0.9(12) . . . 2_575 ? C41 C42 C43 C44 176.4(7) . . . 2_575 ? C43 C42 C44 C43 0.9(12) . . . 2_575 ? C41 C42 C44 C43 -176.4(7) . . . 2_575 ? O20 P2 C45 C46 -54.7(6) . . . . ? O21 P2 C45 C46 65.3(6) . . . . ? O13 P2 C45 C46 -176.0(5) . . . . ? P2 C45 C46 C48 -84.6(8) . . . . ? P2 C45 C46 C47 98.0(7) . . . . ? C48 C46 C47 C48 -1.7(12) . . . 2_566 ? C45 C46 C47 C48 175.8(7) . . . 2_566 ? C47 C46 C48 C47 1.7(12) . . . 2_566 ? C45 C46 C48 C47 -175.8(7) . . . 2_566 ? _refine_diff_density_max 2.145 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.185 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957893' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound6 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H32 Cu2 Mo5 N4 O25 P2, 4(H2 O)' _chemical_formula_sum 'C32 H40 Cu2 Mo5 N4 O29 P2' _chemical_formula_weight 1613.40 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4404(14) _cell_length_b 21.237(2) _cell_length_c 18.1894(14) _cell_angle_alpha 90 _cell_angle_beta 118.357(6) _cell_angle_gamma 90 _cell_volume 4568.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6598 _cell_measurement_theta_min 1.6906 _cell_measurement_theta_max 33.0412 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_density_meas 2.36(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.346 _exptl_crystal_F_000 3160 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.332 _exptl_crystal_size_mid 0.147 _exptl_crystal_size_min 0.127 _exptl_absorpt_coefficient_mu 2.416 _shelx_estimated_absorpt_T_min 0.501 _shelx_estimated_absorpt_T_max 0.749 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 86173 _diffrn_reflns_av_unetI/netI 0.0326 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.722 _diffrn_reflns_theta_max 34.165 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measured_fraction_theta_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_point_group_measured_fraction_full 0.993 _reflns_number_total 17963 _reflns_number_gt 14688 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+21.3187P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 17963 _refine_ls_number_parameters 715 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0743 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 1.25011(2) 0.71780(2) 0.88020(2) 0.00818(4) Uani 1 1 d . . . . . Mo2 Mo 1.32390(2) 0.63808(2) 0.75412(2) 0.00868(4) Uani 1 1 d . . . . . Mo3 Mo 1.10166(2) 0.55259(2) 0.61561(2) 0.00798(4) Uani 1 1 d . . . . . Mo4 Mo 0.87314(2) 0.59728(2) 0.63040(2) 0.00813(4) Uani 1 1 d . . . . . Mo5 Mo 0.98604(2) 0.67466(2) 0.83768(2) 0.00787(4) Uani 1 1 d . . . . . Cu1 Cu 0.82358(3) 0.81329(2) 0.82056(2) 0.01037(6) Uani 1 1 d . . . . . Cu2 Cu 0.73862(3) 0.45654(2) 0.64505(2) 0.01020(6) Uani 1 1 d . . . . . P1 P 1.05749(6) 0.70785(3) 0.67279(4) 0.00787(11) Uani 1 1 d . . . . . P2 P 0.85937(6) 1.06728(3) 0.68598(4) 0.00746(11) Uani 1 1 d . . . . . O1 O 1.13779(16) 0.69560(10) 0.91600(12) 0.0089(3) Uani 1 1 d . . . . . O2 O 1.23915(18) 0.79772(10) 0.88380(14) 0.0127(4) Uani 1 1 d . . . . . O3 O 1.36770(17) 0.70083(10) 0.97281(13) 0.0122(4) Uani 1 1 d . . . . . O4 O 1.30727(17) 0.71478(10) 0.80218(13) 0.0106(4) Uani 1 1 d . . . . . O5 O 1.08426(16) 0.70744(10) 0.76547(12) 0.0097(3) Uani 1 1 d . . . . . O6 O 1.45059(17) 0.61062(11) 0.83144(14) 0.0141(4) Uani 1 1 d . . . . . O7 O 1.35760(18) 0.66741(11) 0.68094(14) 0.0152(4) Uani 1 1 d . . . . . O8 O 1.25296(16) 0.56045(10) 0.70544(12) 0.0098(3) Uani 1 1 d . . . . . O9 O 1.13679(16) 0.66277(10) 0.65799(12) 0.0092(3) Uani 1 1 d . . . . . O10 O 1.12548(17) 0.56748(10) 0.53275(13) 0.0118(4) Uani 1 1 d . . . . . O11 O 1.08975(17) 0.47286(10) 0.61600(13) 0.0123(4) Uani 1 1 d . . . . . O12 O 0.94230(16) 0.57670(10) 0.56471(12) 0.0097(3) Uani 1 1 d . . . . . O13 O 0.84219(17) 0.52125(10) 0.65185(13) 0.0123(4) Uani 1 1 d . . . . . O14 O 0.74263(17) 0.62150(11) 0.55812(13) 0.0135(4) Uani 1 1 d . . . . . O15 O 0.93416(16) 0.69050(10) 0.61860(12) 0.0097(3) Uani 1 1 d . . . . . O16 O 0.88748(16) 0.63637(10) 0.73122(12) 0.0095(3) Uani 1 1 d . . . . . O17 O 0.93417(18) 0.64604(11) 0.89938(13) 0.0131(4) Uani 1 1 d . . . . . O18 O 0.92557(17) 0.75035(10) 0.81644(13) 0.0111(4) Uani 1 1 d . . . . . O19 O 0.9422(2) 0.84512(13) 0.92713(16) 0.0225(5) Uani 1 1 d D . . . . H19C H 0.919(4) 0.824(2) 0.953(3) 0.027 Uiso 1 1 d D U . . . H19D H 1.008(2) 0.830(2) 0.947(3) 0.027 Uiso 1 1 d D U . . . O20 O 0.7712(2) 0.75436(14) 0.90043(19) 0.0259(5) Uani 1 1 d D . . . . H20C H 0.732(4) 0.737(2) 0.8539(19) 0.031 Uiso 1 1 d D U . . . H20D H 0.759(4) 0.7156(10) 0.903(3) 0.031 Uiso 1 1 d D U . . . O21 O 0.92830(16) 1.08313(10) 0.64258(12) 0.0092(3) Uani 1 1 d . . . . . O22 O 0.93884(16) 1.06640(10) 0.78116(12) 0.0087(3) Uani 1 1 d . . . . . O23 O 0.76055(16) 1.11392(10) 0.66258(13) 0.0095(3) Uani 1 1 d . . . . . O24 O 0.74350(19) 0.41630(11) 0.54727(14) 0.0145(4) Uani 1 1 d D . . . . H24C H 0.783(3) 0.425(2) 0.525(2) 0.017 Uiso 1 1 d D U . . . H24D H 0.752(4) 0.3780(9) 0.552(3) 0.017 Uiso 1 1 d D U . . . O25 O 0.5922(2) 0.52392(15) 0.5789(2) 0.0396(8) Uani 1 1 d D . . . . H25C H 0.602(5) 0.5572(17) 0.605(3) 0.047 Uiso 1 1 d D U . . . H25D H 0.573(5) 0.517(3) 0.5297(16) 0.047 Uiso 1 1 d D U . . . O90 O 0.6724(2) 0.86250(17) 0.3564(2) 0.0344(7) Uani 1 1 d D . . . . H90A H 0.606(2) 0.872(3) 0.348(3) 0.041 Uiso 1 1 d D U . . . H90B H 0.666(5) 0.871(3) 0.3085(19) 0.041 Uiso 1 1 d D U . . . O91 O 0.6545(2) 0.87676(15) 0.19520(19) 0.0270(6) Uani 1 1 d D . . . . H91A H 0.679(4) 0.8439(16) 0.226(3) 0.032 Uiso 1 1 d D U . . . H91B H 0.608(4) 0.8474(19) 0.167(3) 0.032 Uiso 1 1 d D U . . . O92 O 0.5231(2) 0.30168(14) 0.40767(17) 0.0228(5) Uani 1 1 d . . . . . H92A H 0.549(4) 0.276(3) 0.442(3) 0.027 Uiso 1 1 d . U . . . H92B H 0.561(4) 0.313(2) 0.387(3) 0.027 Uiso 1 1 d . U . . . O93 O 0.1520(2) 0.69726(12) 0.50521(15) 0.0172(4) Uani 1 1 d D . . . . H93A H 0.178(3) 0.696(2) 0.5571(12) 0.021 Uiso 1 1 d D U . . . H93B H 0.160(4) 0.7351(11) 0.496(3) 0.021 Uiso 1 1 d D U . . . N1 N 0.7126(2) 0.87998(12) 0.81167(16) 0.0119(4) Uani 1 1 d . . . . . N2 N 0.7327(2) 0.81422(12) 0.69718(16) 0.0122(4) Uani 1 1 d . . . . . N3 N 0.6314(2) 0.39292(12) 0.64591(15) 0.0110(4) Uani 1 1 d . . . . . N4 N 0.7799(2) 0.46410(12) 0.76555(15) 0.0112(4) Uani 1 1 d . . . . . C1 C 0.7042(2) 0.91058(15) 0.87198(19) 0.0149(5) Uani 1 1 d . . . . . H1 H 0.7524 0.8999 0.9273 0.018 Uiso 1 1 calc R U . . . C2 C 0.6239(3) 0.95887(15) 0.8544(2) 0.0166(5) Uani 1 1 d . . . . . H2 H 0.6184 0.9789 0.8978 0.020 Uiso 1 1 calc R U . . . C3 C 0.5541(3) 0.97617(15) 0.7735(2) 0.0178(6) Uani 1 1 d . . . . . H3 H 0.5019 1.0084 0.7618 0.021 Uiso 1 1 calc R U . . . C4 C 0.6413(2) 0.89567(14) 0.73121(18) 0.0113(5) Uani 1 1 d . . . . . C5 C 0.5617(2) 0.94485(15) 0.7080(2) 0.0145(5) Uani 1 1 d . . . . . C6 C 0.4951(2) 0.95893(15) 0.6207(2) 0.0169(6) Uani 1 1 d . . . . . H6 H 0.4432 0.9918 0.6044 0.020 Uiso 1 1 calc R U . . . C7 C 0.5062(3) 0.92533(16) 0.5611(2) 0.0175(6) Uani 1 1 d . . . . . H7 H 0.4611 0.9352 0.5050 0.021 Uiso 1 1 calc R U . . . C8 C 0.5866(2) 0.87490(15) 0.58402(18) 0.0135(5) Uani 1 1 d . . . . . C9 C 0.6527(2) 0.86044(14) 0.66888(18) 0.0117(5) Uani 1 1 d . . . . . C10 C 0.7514(2) 0.78235(15) 0.64178(19) 0.0142(5) Uani 1 1 d . . . . . H10 H 0.8065 0.7511 0.6607 0.017 Uiso 1 1 calc R U . . . C11 C 0.6903(3) 0.79457(16) 0.55578(19) 0.0164(5) Uani 1 1 d . . . . . H11 H 0.7060 0.7721 0.5186 0.020 Uiso 1 1 calc R U . . . C12 C 0.6070(3) 0.84003(16) 0.52659(19) 0.0164(6) Uani 1 1 d . . . . . H12 H 0.5647 0.8476 0.4696 0.020 Uiso 1 1 calc R U . . . C13 C 0.5498(2) 0.36202(15) 0.58267(19) 0.0141(5) Uani 1 1 d . . . . . H13 H 0.5365 0.3706 0.5286 0.017 Uiso 1 1 calc R U . . . C14 C 0.4832(2) 0.31698(15) 0.5948(2) 0.0171(6) Uani 1 1 d . . . . . H14 H 0.4249 0.2972 0.5489 0.020 Uiso 1 1 calc R U . . . C15 C 0.5032(2) 0.30180(15) 0.6738(2) 0.0170(6) Uani 1 1 d . . . . . H15 H 0.4607 0.2708 0.6820 0.020 Uiso 1 1 calc R U . . . C16 C 0.5893(2) 0.33385(14) 0.7427(2) 0.0138(5) Uani 1 1 d . . . . . C17 C 0.6486(2) 0.38027(14) 0.72420(18) 0.0113(5) Uani 1 1 d . . . . . C18 C 0.7301(2) 0.41882(14) 0.78984(18) 0.0112(5) Uani 1 1 d . . . . . C19 C 0.6174(3) 0.32380(15) 0.8283(2) 0.0162(5) Uani 1 1 d . . . . . H19A H 0.5805 0.2922 0.8415 0.019 Uiso 1 1 calc R U . . . C20 C 0.6967(3) 0.35931(15) 0.8906(2) 0.0161(5) Uani 1 1 d . . . . . H20A H 0.7143 0.3512 0.9457 0.019 Uiso 1 1 calc R U . . . C21 C 0.7539(2) 0.40943(15) 0.87249(18) 0.0133(5) Uani 1 1 d . . . . . C22 C 0.8303(3) 0.45163(15) 0.93252(18) 0.0148(5) Uani 1 1 d . . . . . H22 H 0.8490 0.4475 0.9885 0.018 Uiso 1 1 calc R U . . . C23 C 0.8768(3) 0.49905(15) 0.90704(19) 0.0156(5) Uani 1 1 d . . . . . H23 H 0.9251 0.5282 0.9456 0.019 Uiso 1 1 calc R U . . . C24 C 0.8514(2) 0.50342(15) 0.82283(18) 0.0135(5) Uani 1 1 d . . . . . H24 H 0.8857 0.5347 0.8069 0.016 Uiso 1 1 calc R U . . . C25 C 1.0844(2) 0.78609(13) 0.64805(18) 0.0106(5) Uani 1 1 d . . . . . H25A H 1.1623 0.7967 0.6864 0.013 Uiso 1 1 calc R U . . . H25B H 1.0768 0.7853 0.5923 0.013 Uiso 1 1 calc R U . . . C26 C 1.0096(2) 0.83855(13) 0.65122(17) 0.0096(4) Uani 1 1 d . . . . . C27 C 0.9309(2) 0.86740(14) 0.57722(18) 0.0118(5) Uani 1 1 d . . . . . H27 H 0.9239 0.8537 0.5264 0.014 Uiso 1 1 calc R U . . . C28 C 1.0186(2) 0.86041(14) 0.72660(18) 0.0117(5) Uani 1 1 d . . . . . H28 H 1.0700 0.8416 0.7765 0.014 Uiso 1 1 calc R U . . . C29 C 0.8629(2) 0.91633(14) 0.57856(18) 0.0118(5) Uani 1 1 d . . . . . H29 H 0.8102 0.9345 0.5286 0.014 Uiso 1 1 calc R U . . . C30 C 0.9518(2) 0.91007(14) 0.72811(18) 0.0121(5) Uani 1 1 d . . . . . H30 H 0.9599 0.9244 0.7790 0.015 Uiso 1 1 calc R U . . . C31 C 0.8728(2) 0.93855(13) 0.65403(18) 0.0099(4) Uani 1 1 d . . . . . C32 C 0.7958(2) 0.99082(13) 0.65348(18) 0.0102(5) Uani 1 1 d . . . . . H32A H 0.7645 0.9785 0.6896 0.012 Uiso 1 1 calc R U . . . H32B H 0.7333 0.9945 0.5973 0.012 Uiso 1 1 calc R 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 Mo1 0.00814(9) 0.00641(10) 0.00938(9) -0.00083(7) 0.00366(7) -0.00091(7) Mo2 0.00807(9) 0.00767(10) 0.01062(10) -0.00084(7) 0.00470(8) -0.00077(7) Mo3 0.00862(9) 0.00669(10) 0.00866(9) -0.00041(7) 0.00414(7) -0.00021(7) Mo4 0.00756(9) 0.00778(10) 0.00831(9) -0.00017(7) 0.00317(7) -0.00079(7) Mo5 0.00803(9) 0.00705(10) 0.00875(9) -0.00036(7) 0.00415(7) 0.00022(7) Cu1 0.00940(14) 0.00918(16) 0.01110(15) -0.00034(11) 0.00369(12) 0.00169(11) Cu2 0.01098(14) 0.00901(16) 0.01068(15) -0.00078(11) 0.00519(12) -0.00264(11) P1 0.0085(3) 0.0059(3) 0.0092(3) 0.0002(2) 0.0042(2) 0.0002(2) P2 0.0073(3) 0.0058(3) 0.0087(3) -0.0001(2) 0.0033(2) 0.0003(2) O1 0.0106(8) 0.0070(9) 0.0091(8) -0.0007(6) 0.0045(7) 0.0004(6) O2 0.0154(9) 0.0076(9) 0.0166(10) -0.0009(7) 0.0089(8) -0.0011(7) O3 0.0114(8) 0.0123(10) 0.0112(9) 0.0008(7) 0.0040(7) 0.0000(7) O4 0.0126(8) 0.0070(9) 0.0133(9) -0.0027(7) 0.0070(7) -0.0024(7) O5 0.0094(8) 0.0097(9) 0.0090(8) -0.0004(7) 0.0037(7) -0.0004(6) O6 0.0105(8) 0.0135(11) 0.0165(10) -0.0018(8) 0.0050(8) -0.0002(7) O7 0.0161(9) 0.0143(11) 0.0177(10) -0.0007(8) 0.0102(8) -0.0004(8) O8 0.0100(8) 0.0082(9) 0.0109(9) -0.0011(7) 0.0047(7) 0.0012(6) O9 0.0092(8) 0.0069(9) 0.0108(8) -0.0002(6) 0.0042(7) 0.0008(6) O10 0.0123(8) 0.0126(10) 0.0114(9) -0.0001(7) 0.0064(7) 0.0004(7) O11 0.0132(9) 0.0077(10) 0.0157(10) -0.0007(7) 0.0066(8) -0.0006(7) O12 0.0101(8) 0.0100(9) 0.0088(8) -0.0004(7) 0.0043(7) 0.0003(7) O13 0.0132(9) 0.0103(10) 0.0127(9) -0.0017(7) 0.0056(7) -0.0033(7) O14 0.0093(8) 0.0160(11) 0.0130(9) 0.0016(7) 0.0035(7) 0.0010(7) O15 0.0095(8) 0.0067(9) 0.0118(9) 0.0008(7) 0.0041(7) 0.0004(6) O16 0.0099(8) 0.0094(9) 0.0095(8) -0.0008(7) 0.0048(7) -0.0002(6) O17 0.0142(9) 0.0142(11) 0.0127(9) 0.0005(7) 0.0078(8) 0.0000(7) O18 0.0107(8) 0.0097(10) 0.0125(9) 0.0001(7) 0.0051(7) 0.0021(7) O19 0.0160(10) 0.0211(13) 0.0197(12) -0.0068(9) -0.0003(9) 0.0055(9) O20 0.0279(13) 0.0224(14) 0.0349(15) 0.0100(11) 0.0211(12) 0.0052(10) O21 0.0103(8) 0.0072(9) 0.0110(8) -0.0003(6) 0.0059(7) 0.0009(6) O22 0.0088(8) 0.0088(9) 0.0079(8) 0.0001(6) 0.0035(7) 0.0003(6) O23 0.0096(8) 0.0072(9) 0.0119(9) 0.0013(7) 0.0050(7) 0.0019(6) O24 0.0202(10) 0.0089(10) 0.0181(10) -0.0012(8) 0.0122(8) -0.0018(8) O25 0.0184(12) 0.0205(15) 0.052(2) -0.0118(14) -0.0058(13) 0.0058(10) O90 0.0229(13) 0.048(2) 0.0364(16) 0.0036(14) 0.0172(12) 0.0085(13) O91 0.0212(12) 0.0286(15) 0.0326(15) 0.0019(11) 0.0138(11) -0.0026(10) O92 0.0239(12) 0.0255(14) 0.0264(13) 0.0077(10) 0.0179(11) 0.0076(10) O93 0.0207(10) 0.0140(11) 0.0154(10) 0.0040(8) 0.0075(9) -0.0028(8) N1 0.0112(10) 0.0104(11) 0.0138(11) -0.0002(8) 0.0057(8) -0.0001(8) N2 0.0110(10) 0.0112(12) 0.0139(11) -0.0006(8) 0.0055(8) 0.0002(8) N3 0.0100(9) 0.0093(11) 0.0128(10) -0.0021(8) 0.0048(8) -0.0011(8) N4 0.0106(9) 0.0096(11) 0.0131(10) 0.0002(8) 0.0055(8) -0.0011(8) C1 0.0149(12) 0.0144(14) 0.0169(13) -0.0031(10) 0.0089(10) -0.0008(10) C2 0.0161(12) 0.0134(14) 0.0226(15) -0.0035(11) 0.0112(11) -0.0015(10) C3 0.0153(12) 0.0113(14) 0.0300(17) -0.0013(11) 0.0134(12) -0.0004(10) C4 0.0090(10) 0.0094(12) 0.0146(12) 0.0000(9) 0.0051(9) -0.0007(8) C5 0.0095(11) 0.0105(13) 0.0231(14) 0.0036(10) 0.0075(10) 0.0017(9) C6 0.0119(11) 0.0130(14) 0.0234(15) 0.0046(11) 0.0065(11) 0.0013(10) C7 0.0123(12) 0.0167(15) 0.0188(14) 0.0054(11) 0.0035(11) -0.0018(10) C8 0.0115(11) 0.0131(14) 0.0135(12) 0.0022(10) 0.0039(10) -0.0031(9) C9 0.0097(10) 0.0099(13) 0.0141(12) 0.0010(9) 0.0045(9) -0.0012(9) C10 0.0136(12) 0.0135(14) 0.0158(13) -0.0023(10) 0.0071(10) -0.0017(10) C11 0.0161(12) 0.0184(15) 0.0133(13) -0.0037(10) 0.0057(10) -0.0058(10) C12 0.0137(12) 0.0199(16) 0.0122(12) 0.0003(10) 0.0034(10) -0.0058(10) C13 0.0115(11) 0.0105(13) 0.0177(13) -0.0044(10) 0.0048(10) -0.0015(9) C14 0.0108(11) 0.0110(14) 0.0257(15) -0.0030(11) 0.0056(11) -0.0029(9) C15 0.0109(11) 0.0091(13) 0.0310(16) -0.0005(11) 0.0100(11) -0.0018(9) C16 0.0129(11) 0.0070(12) 0.0247(15) 0.0018(10) 0.0114(11) 0.0005(9) C17 0.0120(11) 0.0075(12) 0.0160(12) 0.0000(9) 0.0079(10) -0.0004(9) C18 0.0116(11) 0.0090(12) 0.0140(12) 0.0001(9) 0.0069(9) 0.0003(9) C19 0.0165(12) 0.0118(14) 0.0251(15) 0.0066(11) 0.0138(12) 0.0035(10) C20 0.0188(13) 0.0147(14) 0.0183(13) 0.0062(11) 0.0118(11) 0.0056(10) C21 0.0145(12) 0.0122(13) 0.0136(12) 0.0036(9) 0.0070(10) 0.0034(9) C22 0.0169(12) 0.0153(14) 0.0115(12) 0.0013(10) 0.0061(10) 0.0038(10) C23 0.0169(12) 0.0148(14) 0.0109(12) -0.0020(10) 0.0032(10) -0.0004(10) C24 0.0131(11) 0.0118(13) 0.0140(12) -0.0018(9) 0.0052(10) -0.0005(9) C25 0.0129(11) 0.0059(12) 0.0159(12) 0.0018(9) 0.0093(10) 0.0001(8) C26 0.0100(10) 0.0064(12) 0.0131(11) 0.0011(9) 0.0061(9) 0.0008(8) C27 0.0156(12) 0.0092(13) 0.0113(11) 0.0011(9) 0.0068(10) 0.0012(9) C28 0.0123(11) 0.0087(12) 0.0129(12) 0.0005(9) 0.0048(9) 0.0011(9) C29 0.0127(11) 0.0099(13) 0.0115(12) 0.0002(9) 0.0047(9) 0.0022(9) C30 0.0153(12) 0.0077(12) 0.0126(12) -0.0013(9) 0.0060(10) 0.0007(9) C31 0.0109(10) 0.0050(11) 0.0143(12) 0.0001(9) 0.0063(9) 0.0000(8) C32 0.0092(10) 0.0058(12) 0.0157(12) -0.0015(9) 0.0059(9) -0.0010(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.708(2) . ? Mo1 O3 1.714(2) . ? Mo1 O4 1.909(2) . ? Mo1 O1 1.964(2) . ? Mo1 O5 2.226(2) . ? Mo1 O23 2.321(2) 2_746 ? Mo2 O7 1.714(2) . ? Mo2 O6 1.715(2) . ? Mo2 O8 1.900(2) . ? Mo2 O4 1.911(2) . ? Mo2 O9 2.341(2) . ? Mo2 O23 2.341(2) 2_746 ? Mo3 O11 1.701(2) . ? Mo3 O10 1.713(2) . ? Mo3 O8 1.917(2) . ? Mo3 O12 1.955(2) . ? Mo3 O22 2.2088(19) 2_746 ? Mo3 O9 2.439(2) . ? Mo4 O14 1.697(2) . ? Mo4 O13 1.757(2) . ? Mo4 O12 1.881(2) . ? Mo4 O16 1.937(2) . ? Mo4 O15 2.192(2) . ? Mo4 O22 2.3542(19) 2_746 ? Mo5 O17 1.691(2) . ? Mo5 O18 1.759(2) . ? Mo5 O1 1.904(2) . ? Mo5 O16 1.931(2) . ? Mo5 O21 2.200(2) 2_746 ? Mo5 O5 2.366(2) . ? Cu1 O18 1.941(2) . ? Cu1 O19 1.954(2) . ? Cu1 N2 1.981(3) . ? Cu1 N1 2.007(3) . ? Cu1 O20 2.268(3) . ? Cu2 O13 1.918(2) . ? Cu2 N3 1.981(2) . ? Cu2 N4 1.996(2) . ? Cu2 O24 2.002(2) . ? Cu2 O25 2.262(3) . ? P1 O15 1.518(2) . ? P1 O5 1.548(2) . ? P1 O9 1.548(2) . ? P1 C25 1.802(3) . ? P2 O21 1.513(2) . ? P2 O22 1.543(2) . ? P2 O23 1.546(2) . ? P2 C32 1.799(3) . ? O19 H19C 0.807(19) . ? O19 H19D 0.837(19) . ? O20 H20C 0.844(19) . ? O20 H20D 0.844(19) . ? O21 Mo5 2.200(2) 2_756 ? O22 Mo3 2.2088(19) 2_756 ? O22 Mo4 2.3542(19) 2_756 ? O23 Mo1 2.321(2) 2_756 ? O23 Mo2 2.341(2) 2_756 ? O24 H24C 0.829(19) . ? O24 H24D 0.820(19) . ? O25 H25C 0.829(19) . ? O25 H25D 0.818(19) . ? O90 H90A 0.852(19) . ? O90 H90B 0.854(19) . ? O91 H91A 0.855(19) . ? O91 H91B 0.861(19) . ? O92 H92A 0.77(5) . ? O92 H92B 0.80(5) . ? O93 H93A 0.837(19) . ? O93 H93B 0.837(19) . ? N1 C1 1.326(4) . ? N1 C4 1.356(4) . ? N2 C10 1.333(4) . ? N2 C9 1.363(4) . ? N3 C13 1.326(4) . ? N3 C17 1.357(4) . ? N4 C24 1.325(4) . ? N4 C18 1.360(4) . ? C1 C2 1.411(4) . ? C1 H1 0.9300 . ? C2 C3 1.366(5) . ? C2 H2 0.9300 . ? C3 C5 1.410(5) . ? C3 H3 0.9300 . ? C4 C5 1.409(4) . ? C4 C9 1.426(4) . ? C5 C6 1.436(4) . ? C6 C7 1.364(5) . ? C6 H6 0.9300 . ? C7 C8 1.436(4) . ? C7 H7 0.9300 . ? C8 C9 1.401(4) . ? C8 C12 1.410(5) . ? C10 C11 1.403(4) . ? C10 H10 0.9300 . ? C11 C12 1.380(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.397(4) . ? C13 H13 0.9300 . ? C14 C15 1.370(5) . ? C14 H14 0.9300 . ? C15 C16 1.412(4) . ? C15 H15 0.9300 . ? C16 C17 1.406(4) . ? C16 C19 1.433(4) . ? C17 C18 1.433(4) . ? C18 C21 1.395(4) . ? C19 C20 1.357(5) . ? C19 H19A 0.9300 . ? C20 C21 1.440(4) . ? C20 H20A 0.9300 . ? C21 C22 1.409(4) . ? C22 C23 1.377(5) . ? C22 H22 0.9300 . ? C23 C24 1.405(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.519(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C28 1.397(4) . ? C26 C27 1.398(4) . ? C27 C29 1.392(4) . ? C27 H27 0.9300 . ? C28 C30 1.394(4) . ? C28 H28 0.9300 . ? C29 C31 1.397(4) . ? C29 H29 0.9300 . ? C30 C31 1.396(4) . ? C30 H30 0.9300 . ? C31 C32 1.515(4) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O3 103.14(11) . . ? O2 Mo1 O4 97.73(10) . . ? O3 Mo1 O4 102.40(9) . . ? O2 Mo1 O1 97.58(9) . . ? O3 Mo1 O1 96.82(9) . . ? O4 Mo1 O1 151.93(8) . . ? O2 Mo1 O5 93.90(9) . . ? O3 Mo1 O5 161.14(9) . . ? O4 Mo1 O5 82.94(8) . . ? O1 Mo1 O5 72.66(8) . . ? O2 Mo1 O23 164.78(9) . 2_746 ? O3 Mo1 O23 90.63(9) . 2_746 ? O4 Mo1 O23 72.62(8) . 2_746 ? O1 Mo1 O23 87.03(8) . 2_746 ? O5 Mo1 O23 73.55(7) . 2_746 ? O7 Mo2 O6 103.57(11) . . ? O7 Mo2 O8 102.27(10) . . ? O6 Mo2 O8 99.80(10) . . ? O7 Mo2 O4 100.19(10) . . ? O6 Mo2 O4 101.59(10) . . ? O8 Mo2 O4 144.19(8) . . ? O7 Mo2 O9 85.69(9) . . ? O6 Mo2 O9 169.89(9) . . ? O8 Mo2 O9 73.91(8) . . ? O4 Mo2 O9 80.40(8) . . ? O7 Mo2 O23 166.04(9) . 2_746 ? O6 Mo2 O23 89.58(9) . 2_746 ? O8 Mo2 O23 79.70(8) . 2_746 ? O4 Mo2 O23 72.11(8) . 2_746 ? O9 Mo2 O23 81.57(7) . 2_746 ? O11 Mo3 O10 104.17(10) . . ? O11 Mo3 O8 98.45(9) . . ? O10 Mo3 O8 99.66(9) . . ? O11 Mo3 O12 100.29(9) . . ? O10 Mo3 O12 98.95(9) . . ? O8 Mo3 O12 149.38(8) . . ? O11 Mo3 O22 93.85(9) . 2_746 ? O10 Mo3 O22 161.48(9) . 2_746 ? O8 Mo3 O22 81.60(8) . 2_746 ? O12 Mo3 O22 73.20(8) . 2_746 ? O11 Mo3 O9 163.39(9) . . ? O10 Mo3 O9 90.68(9) . . ? O8 Mo3 O9 71.29(8) . . ? O12 Mo3 O9 84.41(8) . . ? O22 Mo3 O9 72.11(7) 2_746 . ? O14 Mo4 O13 100.60(10) . . ? O14 Mo4 O12 102.66(10) . . ? O13 Mo4 O12 99.67(10) . . ? O14 Mo4 O16 101.83(10) . . ? O13 Mo4 O16 96.38(9) . . ? O12 Mo4 O16 147.56(8) . . ? O14 Mo4 O15 87.00(9) . . ? O13 Mo4 O15 172.23(9) . . ? O12 Mo4 O15 80.04(8) . . ? O16 Mo4 O15 80.33(8) . . ? O14 Mo4 O22 173.22(9) . 2_746 ? O13 Mo4 O22 83.26(8) . 2_746 ? O12 Mo4 O22 71.06(8) . 2_746 ? O16 Mo4 O22 83.14(8) . 2_746 ? O15 Mo4 O22 89.34(7) . 2_746 ? O17 Mo5 O18 100.44(10) . . ? O17 Mo5 O1 102.72(9) . . ? O18 Mo5 O1 99.78(9) . . ? O17 Mo5 O16 102.21(10) . . ? O18 Mo5 O16 98.00(9) . . ? O1 Mo5 O16 146.02(8) . . ? O17 Mo5 O21 85.57(9) . 2_746 ? O18 Mo5 O21 173.95(8) . 2_746 ? O1 Mo5 O21 78.04(8) . 2_746 ? O16 Mo5 O21 81.26(8) . 2_746 ? O17 Mo5 O5 171.45(9) . . ? O18 Mo5 O5 86.03(8) . . ? O1 Mo5 O5 70.42(8) . . ? O16 Mo5 O5 82.25(8) . . ? O21 Mo5 O5 87.93(7) 2_746 . ? O18 Cu1 O19 91.05(10) . . ? O18 Cu1 N2 91.71(10) . . ? O19 Cu1 N2 153.33(12) . . ? O18 Cu1 N1 173.81(10) . . ? O19 Cu1 N1 93.47(10) . . ? N2 Cu1 N1 82.36(10) . . ? O18 Cu1 O20 94.85(10) . . ? O19 Cu1 O20 84.87(12) . . ? N2 Cu1 O20 121.28(11) . . ? N1 Cu1 O20 89.77(10) . . ? O13 Cu2 N3 175.35(10) . . ? O13 Cu2 N4 93.26(10) . . ? N3 Cu2 N4 82.52(10) . . ? O13 Cu2 O24 91.96(9) . . ? N3 Cu2 O24 92.69(10) . . ? N4 Cu2 O24 154.25(10) . . ? O13 Cu2 O25 90.13(11) . . ? N3 Cu2 O25 89.05(12) . . ? N4 Cu2 O25 104.54(12) . . ? O24 Cu2 O25 100.65(12) . . ? O15 P1 O5 108.86(11) . . ? O15 P1 O9 111.51(12) . . ? O5 P1 O9 111.27(11) . . ? O15 P1 C25 110.38(12) . . ? O5 P1 C25 107.86(13) . . ? O9 P1 C25 106.89(12) . . ? O21 P2 O22 108.60(11) . . ? O21 P2 O23 111.89(11) . . ? O22 P2 O23 111.28(11) . . ? O21 P2 C32 110.01(12) . . ? O22 P2 C32 108.99(13) . . ? O23 P2 C32 106.02(12) . . ? Mo5 O1 Mo1 121.78(10) . . ? Mo1 O4 Mo2 122.99(11) . . ? P1 O5 Mo1 129.19(11) . . ? P1 O5 Mo5 134.74(11) . . ? Mo1 O5 Mo5 94.76(7) . . ? Mo2 O8 Mo3 124.55(11) . . ? P1 O9 Mo2 126.34(11) . . ? P1 O9 Mo3 127.04(11) . . ? Mo2 O9 Mo3 89.96(7) . . ? Mo4 O12 Mo3 121.38(10) . . ? Mo4 O13 Cu2 152.30(13) . . ? P1 O15 Mo4 119.98(11) . . ? Mo5 O16 Mo4 147.36(11) . . ? Mo5 O18 Cu1 151.84(13) . . ? Cu1 O19 H19C 91(4) . . ? Cu1 O19 H19D 119(3) . . ? H19C O19 H19D 99(5) . . ? Cu1 O20 H20C 81(4) . . ? Cu1 O20 H20D 134(4) . . ? H20C O20 H20D 64(4) . . ? P2 O21 Mo5 120.93(11) . 2_756 ? P2 O22 Mo3 129.53(11) . 2_756 ? P2 O22 Mo4 135.20(11) . 2_756 ? Mo3 O22 Mo4 94.25(7) 2_756 2_756 ? P2 O23 Mo1 127.56(11) . 2_756 ? P2 O23 Mo2 125.42(11) . 2_756 ? Mo1 O23 Mo2 92.12(7) 2_756 2_756 ? Cu2 O24 H24C 129(3) . . ? Cu2 O24 H24D 113(3) . . ? H24C O24 H24D 101(4) . . ? Cu2 O25 H25C 112(4) . . ? Cu2 O25 H25D 102(4) . . ? H25C O25 H25D 132(6) . . ? H90A O90 H90B 100(5) . . ? H91A O91 H91B 75(4) . . ? H92A O92 H92B 116(5) . . ? H93A O93 H93B 104(4) . . ? C1 N1 C4 118.6(3) . . ? C1 N1 Cu1 129.2(2) . . ? C4 N1 Cu1 112.18(19) . . ? C10 N2 C9 118.5(3) . . ? C10 N2 Cu1 128.0(2) . . ? C9 N2 Cu1 112.7(2) . . ? C13 N3 C17 118.1(3) . . ? C13 N3 Cu2 129.5(2) . . ? C17 N3 Cu2 112.41(19) . . ? C24 N4 C18 118.4(3) . . ? C24 N4 Cu2 129.3(2) . . ? C18 N4 Cu2 112.15(19) . . ? N1 C1 C2 121.7(3) . . ? N1 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C5 119.6(3) . . ? C2 C3 H3 120.2 . . ? C5 C3 H3 120.2 . . ? N1 C4 C5 123.5(3) . . ? N1 C4 C9 116.2(3) . . ? C5 C4 C9 120.3(3) . . ? C4 C5 C3 116.5(3) . . ? C4 C5 C6 118.1(3) . . ? C3 C5 C6 125.4(3) . . ? C7 C6 C5 121.6(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 120.7(3) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C12 117.2(3) . . ? C9 C8 C7 118.6(3) . . ? C12 C8 C7 124.2(3) . . ? N2 C9 C8 123.2(3) . . ? N2 C9 C4 116.2(3) . . ? C8 C9 C4 120.6(3) . . ? N2 C10 C11 121.9(3) . . ? N2 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C8 119.4(3) . . ? C11 C12 H12 120.3 . . ? C8 C12 H12 120.3 . . ? N3 C13 C14 122.0(3) . . ? N3 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 120.3(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.2(3) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C17 C16 C15 116.4(3) . . ? C17 C16 C19 118.5(3) . . ? C15 C16 C19 125.1(3) . . ? N3 C17 C16 123.8(3) . . ? N3 C17 C18 116.3(2) . . ? C16 C17 C18 119.8(3) . . ? N4 C18 C21 123.7(3) . . ? N4 C18 C17 115.6(3) . . ? C21 C18 C17 120.7(3) . . ? C20 C19 C16 121.5(3) . . ? C20 C19 H19A 119.3 . . ? C16 C19 H19A 119.3 . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C18 C21 C22 117.0(3) . . ? C18 C21 C20 118.6(3) . . ? C22 C21 C20 124.4(3) . . ? C23 C22 C21 119.0(3) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 120.1(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? N4 C24 C23 121.7(3) . . ? N4 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C26 C25 P1 116.88(19) . . ? C26 C25 H25A 108.1 . . ? P1 C25 H25A 108.1 . . ? C26 C25 H25B 108.1 . . ? P1 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? C28 C26 C27 118.2(3) . . ? C28 C26 C25 122.0(2) . . ? C27 C26 C25 119.8(2) . . ? C29 C27 C26 120.9(3) . . ? C29 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C30 C28 C26 121.0(3) . . ? C30 C28 H28 119.5 . . ? C26 C28 H28 119.5 . . ? C27 C29 C31 120.8(3) . . ? C27 C29 H29 119.6 . . ? C31 C29 H29 119.6 . . ? C28 C30 C31 120.7(3) . . ? C28 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C30 C31 C29 118.4(3) . . ? C30 C31 C32 121.9(3) . . ? C29 C31 C32 119.7(2) . . ? C31 C32 P2 116.29(19) . . ? C31 C32 H32A 108.2 . . ? P2 C32 H32A 108.2 . . ? C31 C32 H32B 108.2 . . ? P2 C32 H32B 108.2 . . ? H32A C32 H32B 107.4 . . ? 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 O15 P1 O5 Mo1 172.62(14) . . . . ? O9 P1 O5 Mo1 49.34(18) . . . . ? C25 P1 O5 Mo1 -67.60(17) . . . . ? O15 P1 O5 Mo5 9.1(2) . . . . ? O9 P1 O5 Mo5 -114.15(16) . . . . ? C25 P1 O5 Mo5 128.91(16) . . . . ? O7 Mo2 O8 Mo3 -76.63(14) . . . . ? O6 Mo2 O8 Mo3 177.04(13) . . . . ? O4 Mo2 O8 Mo3 51.0(2) . . . . ? O9 Mo2 O8 Mo3 5.16(11) . . . . ? O23 Mo2 O8 Mo3 89.27(12) 2_746 . . . ? O15 P1 O9 Mo2 -153.05(12) . . . . ? O5 P1 O9 Mo2 -31.30(17) . . . . ? C25 P1 O9 Mo2 86.23(16) . . . . ? O15 P1 O9 Mo3 -29.42(17) . . . . ? O5 P1 O9 Mo3 92.33(15) . . . . ? C25 P1 O9 Mo3 -150.14(14) . . . . ? O14 Mo4 O12 Mo3 174.35(12) . . . . ? O13 Mo4 O12 Mo3 -82.38(13) . . . . ? O16 Mo4 O12 Mo3 36.2(2) . . . . ? O15 Mo4 O12 Mo3 89.75(12) . . . . ? O22 Mo4 O12 Mo3 -3.00(10) 2_746 . . . ? O14 Mo4 O13 Cu2 -11.8(3) . . . . ? O12 Mo4 O13 Cu2 -116.7(3) . . . . ? O16 Mo4 O13 Cu2 91.6(3) . . . . ? O22 Mo4 O13 Cu2 173.8(3) 2_746 . . . ? O5 P1 O15 Mo4 -63.24(15) . . . . ? O9 P1 O15 Mo4 59.89(15) . . . . ? C25 P1 O15 Mo4 178.55(12) . . . . ? O17 Mo5 O18 Cu1 -8.5(3) . . . . ? O1 Mo5 O18 Cu1 -113.5(3) . . . . ? O16 Mo5 O18 Cu1 95.6(3) . . . . ? O5 Mo5 O18 Cu1 177.1(3) . . . . ? O22 P2 O21 Mo5 -63.25(15) . . . 2_756 ? O23 P2 O21 Mo5 59.98(16) . . . 2_756 ? C32 P2 O21 Mo5 177.55(12) . . . 2_756 ? O21 P2 O22 Mo3 176.00(13) . . . 2_756 ? O23 P2 O22 Mo3 52.41(18) . . . 2_756 ? C32 P2 O22 Mo3 -64.16(18) . . . 2_756 ? O21 P2 O22 Mo4 10.7(2) . . . 2_756 ? O23 P2 O22 Mo4 -112.87(16) . . . 2_756 ? C32 P2 O22 Mo4 130.56(16) . . . 2_756 ? O21 P2 O23 Mo1 -26.57(18) . . . 2_756 ? O22 P2 O23 Mo1 95.12(15) . . . 2_756 ? C32 P2 O23 Mo1 -146.51(14) . . . 2_756 ? O21 P2 O23 Mo2 -153.73(12) . . . 2_756 ? O22 P2 O23 Mo2 -32.04(17) . . . 2_756 ? C32 P2 O23 Mo2 86.33(16) . . . 2_756 ? C4 N1 C1 C2 -0.4(4) . . . . ? Cu1 N1 C1 C2 176.6(2) . . . . ? N1 C1 C2 C3 -1.6(5) . . . . ? C1 C2 C3 C5 1.0(5) . . . . ? C1 N1 C4 C5 2.9(4) . . . . ? Cu1 N1 C4 C5 -174.6(2) . . . . ? C1 N1 C4 C9 -178.9(3) . . . . ? Cu1 N1 C4 C9 3.6(3) . . . . ? N1 C4 C5 C3 -3.4(4) . . . . ? C9 C4 C5 C3 178.5(3) . . . . ? N1 C4 C5 C6 176.8(3) . . . . ? C9 C4 C5 C6 -1.3(4) . . . . ? C2 C3 C5 C4 1.3(4) . . . . ? C2 C3 C5 C6 -178.9(3) . . . . ? C4 C5 C6 C7 1.2(4) . . . . ? C3 C5 C6 C7 -178.6(3) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? C6 C7 C8 C9 0.7(4) . . . . ? C6 C7 C8 C12 -176.8(3) . . . . ? C10 N2 C9 C8 2.0(4) . . . . ? Cu1 N2 C9 C8 172.8(2) . . . . ? C10 N2 C9 C4 -176.2(3) . . . . ? Cu1 N2 C9 C4 -5.3(3) . . . . ? C12 C8 C9 N2 -1.2(4) . . . . ? C7 C8 C9 N2 -178.9(3) . . . . ? C12 C8 C9 C4 176.8(3) . . . . ? C7 C8 C9 C4 -0.8(4) . . . . ? N1 C4 C9 N2 1.1(4) . . . . ? C5 C4 C9 N2 179.4(3) . . . . ? N1 C4 C9 C8 -177.1(3) . . . . ? C5 C4 C9 C8 1.2(4) . . . . ? C9 N2 C10 C11 -0.8(4) . . . . ? Cu1 N2 C10 C11 -170.0(2) . . . . ? N2 C10 C11 C12 -1.1(5) . . . . ? C10 C11 C12 C8 1.8(5) . . . . ? C9 C8 C12 C11 -0.7(4) . . . . ? C7 C8 C12 C11 176.8(3) . . . . ? C17 N3 C13 C14 -0.7(4) . . . . ? Cu2 N3 C13 C14 178.2(2) . . . . ? N3 C13 C14 C15 -2.2(5) . . . . ? C13 C14 C15 C16 2.3(5) . . . . ? C14 C15 C16 C17 0.4(4) . . . . ? C14 C15 C16 C19 178.4(3) . . . . ? C13 N3 C17 C16 3.7(4) . . . . ? Cu2 N3 C17 C16 -175.5(2) . . . . ? C13 N3 C17 C18 -174.2(3) . . . . ? Cu2 N3 C17 C18 6.6(3) . . . . ? C15 C16 C17 N3 -3.5(4) . . . . ? C19 C16 C17 N3 178.3(3) . . . . ? C15 C16 C17 C18 174.4(3) . . . . ? C19 C16 C17 C18 -3.8(4) . . . . ? C24 N4 C18 C21 -3.1(4) . . . . ? Cu2 N4 C18 C21 173.1(2) . . . . ? C24 N4 C18 C17 176.4(3) . . . . ? Cu2 N4 C18 C17 -7.4(3) . . . . ? N3 C17 C18 N4 0.6(4) . . . . ? C16 C17 C18 N4 -177.4(3) . . . . ? N3 C17 C18 C21 -179.9(3) . . . . ? C16 C17 C18 C21 2.1(4) . . . . ? C17 C16 C19 C20 2.2(4) . . . . ? C15 C16 C19 C20 -175.8(3) . . . . ? C16 C19 C20 C21 1.3(5) . . . . ? N4 C18 C21 C22 3.0(4) . . . . ? C17 C18 C21 C22 -176.5(3) . . . . ? N4 C18 C21 C20 -179.2(3) . . . . ? C17 C18 C21 C20 1.3(4) . . . . ? C19 C20 C21 C18 -3.0(4) . . . . ? C19 C20 C21 C22 174.7(3) . . . . ? C18 C21 C22 C23 -0.1(4) . . . . ? C20 C21 C22 C23 -177.8(3) . . . . ? C21 C22 C23 C24 -2.5(4) . . . . ? C18 N4 C24 C23 0.3(4) . . . . ? Cu2 N4 C24 C23 -175.1(2) . . . . ? C22 C23 C24 N4 2.5(5) . . . . ? O15 P1 C25 C26 53.9(2) . . . . ? O5 P1 C25 C26 -64.9(2) . . . . ? O9 P1 C25 C26 175.3(2) . . . . ? P1 C25 C26 C28 71.2(3) . . . . ? P1 C25 C26 C27 -110.4(3) . . . . ? C28 C26 C27 C29 -0.4(4) . . . . ? C25 C26 C27 C29 -178.8(3) . . . . ? C27 C26 C28 C30 -0.7(4) . . . . ? C25 C26 C28 C30 177.8(3) . . . . ? C26 C27 C29 C31 1.0(4) . . . . ? C26 C28 C30 C31 1.0(4) . . . . ? C28 C30 C31 C29 -0.4(4) . . . . ? C28 C30 C31 C32 177.5(3) . . . . ? C27 C29 C31 C30 -0.6(4) . . . . ? C27 C29 C31 C32 -178.6(3) . . . . ? C30 C31 C32 P2 76.0(3) . . . . ? C29 C31 C32 P2 -106.2(3) . . . . ? O21 P2 C32 C31 47.3(2) . . . . ? O22 P2 C32 C31 -71.6(2) . . . . ? O23 P2 C32 C31 168.5(2) . . . . ? _refine_diff_density_max 1.875 _refine_diff_density_min -1.210 _refine_diff_density_rms 0.178 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957894' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound7 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H19 Cu Mo5 N2 O22 P2, C16 H15 Cu N2 O4 P' _chemical_formula_sum 'C36 H34 Cu2 Mo5 N4 O26 P3' _chemical_formula_weight 1638.36 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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 53.884(3) _cell_length_b 9.5839(5) _cell_length_c 18.7832(9) _cell_angle_alpha 90 _cell_angle_beta 91.5890(10) _cell_angle_gamma 90 _cell_volume 9696.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 856 _cell_measurement_theta_min 2.2930 _cell_measurement_theta_max 27.2582 _exptl_crystal_description block _exptl_crystal_colour green-blue _exptl_crystal_density_meas 2.28(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.245 _exptl_crystal_F_000 6392 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.121 _exptl_crystal_size_mid 0.121 _exptl_crystal_size_min 0.076 _exptl_absorpt_coefficient_mu 2.306 _shelx_estimated_absorpt_T_min 0.768 _shelx_estimated_absorpt_T_max 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55032 _diffrn_reflns_av_unetI/netI 0.0434 _diffrn_reflns_av_R_equivalents 0.0619 _diffrn_reflns_limit_h_min -67 _diffrn_reflns_limit_h_max 67 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.158 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 9899 _reflns_number_gt 7966 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+10.5994P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9899 _refine_ls_number_parameters 703 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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 0.40593(2) 0.57178(4) 0.27422(2) 0.00991(8) Uani 1 1 d . U . . . Mo2 Mo 0.39149(2) 0.31642(4) 0.38596(2) 0.01020(8) Uani 1 1 d . U . . . Mo3 Mo 0.32635(2) 0.30677(4) 0.40175(2) 0.00982(8) Uani 1 1 d . U . . . Mo4 Mo 0.30417(2) 0.50314(4) 0.24442(2) 0.00934(8) Uani 1 1 d . U . . . Mo5 Mo 0.35344(2) 0.69458(3) 0.19184(2) 0.00916(8) Uani 1 1 d . U . . . Cu1 Cu 0.46926(2) 0.36339(5) 0.07308(3) 0.01019(11) Uani 1 1 d . U . . . Cu2 Cu 0.31561(2) 0.26293(5) 0.11493(2) 0.01055(11) Uani 1 1 d . U . . . P1 P 0.49304(2) 0.38306(10) -0.08701(5) 0.0098(2) Uani 1 1 d . U . . . P2 P 0.35899(2) 0.32977(10) 0.23506(5) 0.0081(2) Uani 1 1 d . U . . . P3 P 0.35277(2) 0.38662(10) -0.13130(5) 0.0087(2) Uani 1 1 d . U . . . O1 O 0.43789(5) 0.5078(3) 0.06614(16) 0.0191(7) Uani 1 1 d D U . . . H1A H 0.4302(8) 0.542(5) 0.0324(18) 0.023 Uiso 1 1 d D U . . . H1B H 0.4318(8) 0.542(5) 0.1016(17) 0.023 Uiso 1 1 d D U . . . O2 O 0.47609(5) 0.4023(3) -0.02570(14) 0.0125(6) Uani 1 1 d . U . . . O3 O 0.47758(5) 0.3183(3) -0.15198(15) 0.0143(6) Uani 1 1 d D U . . . H3' H 0.4628(4) 0.335(5) -0.156(2) 0.017 Uiso 1 1 d D U . . . O4 O 0.50511(5) 0.5148(3) -0.11318(14) 0.0121(6) Uani 1 1 d . U . . . O5 O 0.42225(5) 0.5542(3) 0.19842(15) 0.0179(6) Uani 1 1 d . U . . . O6 O 0.42635(5) 0.6548(3) 0.33165(15) 0.0165(6) Uani 1 1 d . U . . . O7 O 0.40868(5) 0.3809(3) 0.30746(14) 0.0116(6) Uani 1 1 d . U . . . O8 O 0.37157(5) 0.4664(3) 0.21442(14) 0.0105(6) Uani 1 1 d . U . . . O9 O 0.38380(5) 0.7167(3) 0.24822(14) 0.0111(6) Uani 1 1 d . U . . . O10 O 0.36377(5) 0.6921(3) 0.10625(14) 0.0156(6) Uani 1 1 d . U . . . O11 O 0.34250(5) 0.8582(3) 0.20396(14) 0.0139(6) Uani 1 1 d . U . . . O12 O 0.32267(5) 0.5953(3) 0.17189(14) 0.0101(6) Uani 1 1 d . U . . . O13 O 0.28554(5) 0.6296(3) 0.27626(15) 0.0162(6) Uani 1 1 d . U . . . O14 O 0.28460(5) 0.4086(3) 0.18927(14) 0.0128(6) Uani 1 1 d . U . . . O15 O 0.30700(4) 0.3862(3) 0.32778(14) 0.0107(6) Uani 1 1 d . U . . . O16 O 0.35784(5) 0.3118(3) 0.31745(13) 0.0093(5) Uani 1 1 d . U . . . O17 O 0.32352(5) 0.1337(3) 0.38299(14) 0.0161(6) Uani 1 1 d . U . . . O18 O 0.30967(5) 0.3238(3) 0.47614(15) 0.0166(6) Uani 1 1 d . U . . . O19 O 0.36092(5) 0.2962(3) 0.44992(14) 0.0121(6) Uani 1 1 d D U . . . H19' H 0.3631(8) 0.318(4) 0.4918(12) 0.015 Uiso 1 1 d D U . . . O20 O 0.40977(5) 0.3637(3) 0.45756(14) 0.0159(6) Uani 1 1 d . U . . . O21 O 0.39645(5) 0.1434(3) 0.37491(15) 0.0161(6) Uani 1 1 d . U . . . O22 O 0.33221(5) 0.3252(3) 0.20531(13) 0.0095(5) Uani 1 1 d . U . . . O23 O 0.32865(6) 0.4205(3) 0.06470(15) 0.0161(6) Uani 1 1 d D U . . . H23A H 0.3261(8) 0.492(3) 0.088(2) 0.019 Uiso 1 1 d D U . . . H23B H 0.3318(8) 0.438(5) 0.0233(12) 0.019 Uiso 1 1 d D U . . . O24 O 0.33697(4) 0.4640(3) -0.07833(13) 0.0092(6) Uani 1 1 d . U . . . O25 O 0.33916(5) 0.3868(3) -0.20488(13) 0.0093(6) Uani 1 1 d . U . . . O26 O 0.37876(5) 0.4550(3) -0.13474(13) 0.0092(6) Uani 1 1 d . U . . . N1 N 0.44889(6) 0.1946(3) 0.04769(17) 0.0118(7) Uani 1 1 d . U . . . N2 N 0.46315(6) 0.2934(3) 0.17253(17) 0.0111(7) Uani 1 1 d . U . . . N3 N 0.29337(6) 0.2040(3) 0.03308(17) 0.0112(7) Uani 1 1 d . U . . . N4 N 0.29925(6) 0.1072(3) 0.16397(17) 0.0106(7) Uani 1 1 d . U . . . C1 C 0.44043(7) 0.1554(4) -0.0159(2) 0.0181(9) Uani 1 1 d . U . . . H1 H 0.4443 0.2104 -0.0562 0.022 Uiso 1 1 calc R U . . . C2 C 0.42593(8) 0.0349(5) -0.0259(2) 0.0213(10) Uani 1 1 d . U . . . H2 H 0.4200 0.0095 -0.0722 0.026 Uiso 1 1 calc R U . . . C3 C 0.42033(8) -0.0458(5) 0.0317(2) 0.0199(10) Uani 1 1 d . U . . . H3 H 0.4107 -0.1283 0.0254 0.024 Uiso 1 1 calc R U . . . C4 C 0.42883(7) -0.0060(4) 0.1002(2) 0.0141(8) Uani 1 1 d . U . . . C5 C 0.44271(7) 0.1164(4) 0.1051(2) 0.0114(8) Uani 1 1 d . U . . . C6 C 0.42363(8) -0.0791(4) 0.1647(2) 0.0197(9) Uani 1 1 d . U . . . H6 H 0.4144 -0.1634 0.1621 0.024 Uiso 1 1 calc R U . . . C7 C 0.43147(7) -0.0313(4) 0.2288(2) 0.0186(9) Uani 1 1 d . U . . . H7 H 0.4280 -0.0834 0.2703 0.022 Uiso 1 1 calc R U . . . C8 C 0.44507(7) 0.0981(4) 0.2352(2) 0.0146(9) Uani 1 1 d . U . . . C9 C 0.45063(7) 0.1699(4) 0.1728(2) 0.0120(8) Uani 1 1 d . U . . . C10 C 0.45273(7) 0.1596(4) 0.3002(2) 0.0170(9) Uani 1 1 d . U . . . H10 H 0.4497 0.1140 0.3440 0.020 Uiso 1 1 calc R U . . . C11 C 0.46468(7) 0.2862(4) 0.2996(2) 0.0149(9) Uani 1 1 d . U . . . H11 H 0.4696 0.3298 0.3431 0.018 Uiso 1 1 calc R U . . . C12 C 0.46956(7) 0.3507(4) 0.2346(2) 0.0134(8) Uani 1 1 d . U . . . H12 H 0.4777 0.4385 0.2349 0.016 Uiso 1 1 calc R U . . . C13 C 0.29028(7) 0.2592(4) -0.0313(2) 0.0134(8) Uani 1 1 d . U . . . H13 H 0.3003 0.3362 -0.0443 0.016 Uiso 1 1 calc R U . . . C14 C 0.27270(7) 0.2077(4) -0.0807(2) 0.0153(9) Uani 1 1 d . U . . . H14 H 0.2709 0.2502 -0.1263 0.018 Uiso 1 1 calc R U . . . C15 C 0.25816(8) 0.0966(5) -0.0639(2) 0.0190(9) Uani 1 1 d . U . . . H15 H 0.2463 0.0611 -0.0976 0.023 Uiso 1 1 calc R U . . . C16 C 0.26098(7) 0.0351(4) 0.0041(2) 0.0148(9) Uani 1 1 d . U . . . C17 C 0.24564(8) -0.0749(5) 0.0296(2) 0.0209(10) Uani 1 1 d . U . . . H17 H 0.2337 -0.1170 -0.0018 0.025 Uiso 1 1 calc R U . . . C18 C 0.24782(7) -0.1201(5) 0.0977(2) 0.0198(9) Uani 1 1 d . U . . . H18 H 0.2372 -0.1921 0.1135 0.024 Uiso 1 1 calc R U . . . C19 C 0.26602(7) -0.0605(4) 0.1467(2) 0.0140(8) Uani 1 1 d . U . . . C20 C 0.27872(7) 0.0946(4) 0.0508(2) 0.0124(8) Uani 1 1 d . U . . . C21 C 0.28144(7) 0.0442(4) 0.1224(2) 0.0113(8) Uani 1 1 d . U . . . C22 C 0.26894(7) -0.0982(4) 0.2193(2) 0.0173(9) Uani 1 1 d . U . . . H22 H 0.2585 -0.1669 0.2393 0.021 Uiso 1 1 calc R U . . . C23 C 0.28696(8) -0.0348(5) 0.2603(2) 0.0198(10) Uani 1 1 d . U . . . H23 H 0.2894 -0.0608 0.3088 0.024 Uiso 1 1 calc R U . . . C24 C 0.30178(7) 0.0678(4) 0.2310(2) 0.0137(9) Uani 1 1 d . U . . . H24 H 0.3142 0.1112 0.2603 0.016 Uiso 1 1 calc R U . . . C25 C 0.51671(7) 0.2544(4) -0.0690(2) 0.0171(9) Uani 1 1 d . U . . . H25A H 0.5244 0.2295 -0.1146 0.021 Uiso 1 1 calc R U . . . H25B H 0.5298 0.2973 -0.0381 0.021 Uiso 1 1 calc R U . . . C26 C 0.50821(7) 0.1224(4) -0.0342(2) 0.0132(8) Uani 1 1 d . U . . . C27 C 0.49859(7) 0.0113(4) -0.0738(2) 0.0160(9) Uani 1 1 d . U . . . H27 H 0.4974 0.0175 -0.1243 0.019 Uiso 1 1 calc R U . . . C28 C 0.49070(7) -0.1087(4) -0.0395(2) 0.0154(9) Uani 1 1 d . U . . . H28 H 0.4844 -0.1840 -0.0675 0.018 Uiso 1 1 calc R U . . . C29 C 0.37569(7) 0.1836(4) 0.2013(2) 0.0116(8) Uani 1 1 d . U . . . H29A H 0.3935 0.1915 0.2157 0.014 Uiso 1 1 calc R U . . . H29B H 0.3691 0.0963 0.2219 0.014 Uiso 1 1 calc R U . . . C30 C 0.37312(7) 0.1781(4) 0.1208(2) 0.0102(8) Uani 1 1 d . U . . . C31 C 0.38628(7) 0.2719(4) 0.0798(2) 0.0123(8) Uani 1 1 d . U . . . H31 H 0.3982 0.3318 0.1020 0.015 Uiso 1 1 calc R U . . . C32 C 0.38207(7) 0.2783(4) 0.0068(2) 0.0124(8) Uani 1 1 d . U . . . H32 H 0.3914 0.3417 -0.0207 0.015 Uiso 1 1 calc R U . . . C33 C 0.35648(7) 0.0875(4) 0.0872(2) 0.0111(8) Uani 1 1 d . U . . . H33 H 0.3481 0.0198 0.1145 0.013 Uiso 1 1 calc R U . . . C34 C 0.35198(7) 0.0949(4) 0.0137(2) 0.0116(8) Uani 1 1 d . U . . . H34 H 0.3404 0.0329 -0.0087 0.014 Uiso 1 1 calc R U . . . C35 C 0.36434(7) 0.1927(4) -0.0267(2) 0.0103(8) Uani 1 1 d . U . . . C36 C 0.35765(7) 0.2078(4) -0.1055(2) 0.0113(8) Uani 1 1 d . U . . . H36A H 0.3424 0.1538 -0.1165 0.014 Uiso 1 1 calc R U . . . H36B H 0.3712 0.1680 -0.1337 0.014 Uiso 1 1 calc R 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 Mo1 0.00969(16) 0.01294(18) 0.00717(17) 0.00018(14) 0.00111(13) -0.00001(14) Mo2 0.01079(16) 0.01254(18) 0.00715(17) 0.00091(14) -0.00224(13) 0.00190(14) Mo3 0.01121(16) 0.01161(18) 0.00662(17) 0.00198(14) -0.00015(13) -0.00051(14) Mo4 0.00977(16) 0.01099(17) 0.00722(17) 0.00130(14) -0.00070(13) 0.00114(13) Mo5 0.01187(16) 0.00983(17) 0.00580(17) 0.00177(14) 0.00062(13) 0.00011(13) Cu1 0.0116(2) 0.0098(2) 0.0091(3) 0.00094(19) -0.00066(19) -0.00272(19) Cu2 0.0133(2) 0.0117(3) 0.0066(2) 0.00136(19) -0.00186(19) -0.00342(19) P1 0.0125(5) 0.0084(5) 0.0083(5) 0.0005(4) -0.0006(4) -0.0027(4) P2 0.0097(5) 0.0088(5) 0.0057(5) -0.0003(4) -0.0008(4) 0.0011(4) P3 0.0113(5) 0.0097(5) 0.0050(5) 0.0004(4) 0.0007(4) -0.0006(4) O1 0.0187(16) 0.0302(18) 0.0083(16) -0.0005(14) 0.0006(12) 0.0104(14) O2 0.0146(14) 0.0150(15) 0.0079(14) -0.0014(11) 0.0002(11) -0.0018(11) O3 0.0140(14) 0.0158(15) 0.0130(15) -0.0047(12) -0.0008(12) -0.0034(12) O4 0.0136(13) 0.0112(14) 0.0115(15) 0.0033(11) -0.0015(11) -0.0051(11) O5 0.0167(14) 0.0211(16) 0.0162(16) 0.0017(13) 0.0052(12) 0.0040(12) O6 0.0150(14) 0.0215(16) 0.0131(15) -0.0011(12) -0.0001(12) -0.0019(12) O7 0.0109(13) 0.0139(14) 0.0099(14) 0.0005(11) 0.0003(11) 0.0037(11) O8 0.0115(13) 0.0120(14) 0.0079(14) 0.0008(11) -0.0002(11) 0.0009(11) O9 0.0145(13) 0.0107(14) 0.0083(14) 0.0001(11) 0.0033(11) -0.0006(11) O10 0.0171(14) 0.0200(16) 0.0099(15) 0.0033(12) 0.0003(11) 0.0006(12) O11 0.0174(14) 0.0111(14) 0.0130(15) 0.0022(12) -0.0003(12) 0.0005(12) O12 0.0125(13) 0.0098(14) 0.0082(14) 0.0011(11) -0.0001(11) 0.0025(11) O13 0.0167(14) 0.0173(15) 0.0148(16) 0.0014(12) 0.0032(12) 0.0038(12) O14 0.0121(13) 0.0170(15) 0.0091(14) 0.0029(12) -0.0018(11) -0.0006(11) O15 0.0090(13) 0.0149(15) 0.0082(14) 0.0018(11) 0.0001(11) 0.0000(11) O16 0.0120(13) 0.0100(14) 0.0058(13) 0.0001(11) -0.0003(10) 0.0004(11) O17 0.0235(15) 0.0147(15) 0.0101(15) 0.0037(12) -0.0020(12) -0.0020(12) O18 0.0162(14) 0.0209(16) 0.0128(15) 0.0046(12) 0.0019(12) 0.0000(12) O19 0.0171(14) 0.0144(15) 0.0047(14) 0.0008(12) -0.0023(11) -0.0005(12) O20 0.0171(14) 0.0219(16) 0.0084(15) 0.0024(12) -0.0039(12) 0.0003(12) O21 0.0170(14) 0.0159(15) 0.0153(16) 0.0017(12) -0.0033(12) 0.0013(12) O22 0.0131(13) 0.0096(14) 0.0058(13) 0.0006(11) 0.0001(10) 0.0008(11) O23 0.0300(17) 0.0107(15) 0.0077(15) 0.0003(12) 0.0017(13) -0.0046(13) O24 0.0103(13) 0.0114(14) 0.0059(14) 0.0003(11) -0.0002(10) 0.0023(11) O25 0.0125(13) 0.0090(14) 0.0064(14) -0.0005(11) 0.0019(11) -0.0005(11) O26 0.0107(13) 0.0111(14) 0.0059(14) 0.0006(11) 0.0010(11) -0.0004(11) N1 0.0108(16) 0.0121(17) 0.0124(17) -0.0040(14) 0.0012(13) -0.0034(13) N2 0.0086(15) 0.0130(17) 0.0117(17) 0.0019(14) -0.0021(13) -0.0017(13) N3 0.0103(16) 0.0141(18) 0.0090(17) -0.0005(14) -0.0010(13) -0.0002(13) N4 0.0120(16) 0.0105(17) 0.0092(17) 0.0001(13) 0.0004(13) -0.0003(13) C1 0.017(2) 0.020(2) 0.017(2) -0.0070(18) 0.0022(18) -0.0020(17) C2 0.024(2) 0.023(2) 0.017(2) -0.0112(19) 0.0026(19) -0.0071(19) C3 0.018(2) 0.017(2) 0.024(2) -0.0096(19) 0.0054(18) -0.0046(18) C4 0.0096(19) 0.009(2) 0.024(2) -0.0038(17) 0.0067(17) 0.0007(16) C5 0.0101(18) 0.0070(19) 0.017(2) 0.0011(16) 0.0048(16) 0.0017(15) C6 0.019(2) 0.010(2) 0.030(3) 0.0023(18) 0.0023(19) -0.0042(17) C7 0.017(2) 0.015(2) 0.024(2) 0.0065(18) 0.0057(18) 0.0003(17) C8 0.0093(19) 0.016(2) 0.019(2) 0.0051(17) 0.0000(17) 0.0012(16) C9 0.0074(18) 0.013(2) 0.016(2) 0.0027(16) 0.0020(16) 0.0005(15) C10 0.014(2) 0.020(2) 0.018(2) 0.0089(18) 0.0006(17) -0.0006(17) C11 0.0118(19) 0.023(2) 0.010(2) 0.0013(17) -0.0024(16) -0.0009(17) C12 0.0103(19) 0.014(2) 0.016(2) 0.0034(17) -0.0013(16) 0.0005(16) C13 0.0132(19) 0.016(2) 0.011(2) -0.0020(17) 0.0003(16) -0.0001(16) C14 0.017(2) 0.024(2) 0.005(2) -0.0007(17) 0.0015(16) 0.0036(18) C15 0.016(2) 0.028(3) 0.013(2) -0.0083(18) -0.0025(17) 0.0009(18) C16 0.0094(19) 0.019(2) 0.016(2) -0.0068(17) 0.0019(16) 0.0006(16) C17 0.016(2) 0.020(2) 0.027(3) -0.0055(19) -0.0047(19) -0.0031(18) C18 0.014(2) 0.015(2) 0.031(3) -0.0029(19) 0.0023(18) -0.0047(17) C19 0.0093(19) 0.011(2) 0.021(2) -0.0023(17) 0.0021(16) -0.0003(16) C20 0.0090(18) 0.015(2) 0.013(2) -0.0028(16) -0.0005(15) 0.0014(15) C21 0.0097(18) 0.010(2) 0.014(2) -0.0025(16) 0.0022(16) -0.0006(15) C22 0.015(2) 0.014(2) 0.024(2) 0.0087(18) 0.0047(17) -0.0019(17) C23 0.024(2) 0.022(2) 0.014(2) 0.0034(18) 0.0020(18) 0.0025(18) C24 0.016(2) 0.014(2) 0.011(2) 0.0009(17) -0.0014(16) 0.0009(16) C25 0.016(2) 0.012(2) 0.023(2) 0.0032(18) 0.0013(18) 0.0019(17) C26 0.0098(19) 0.0096(19) 0.020(2) 0.0011(17) 0.0021(17) 0.0047(16) C27 0.020(2) 0.015(2) 0.012(2) -0.0008(17) -0.0008(17) 0.0051(17) C28 0.017(2) 0.008(2) 0.021(2) -0.0045(17) -0.0031(18) 0.0009(16) C29 0.016(2) 0.0105(19) 0.0081(19) 0.0030(16) 0.0011(16) 0.0014(16) C30 0.0108(18) 0.010(2) 0.0095(19) 0.0009(16) 0.0007(15) 0.0058(15) C31 0.0128(19) 0.013(2) 0.011(2) -0.0005(16) -0.0015(16) -0.0012(16) C32 0.015(2) 0.013(2) 0.009(2) 0.0031(16) 0.0037(16) -0.0014(16) C33 0.0145(19) 0.009(2) 0.010(2) 0.0006(16) 0.0056(16) 0.0013(15) C34 0.0121(19) 0.010(2) 0.012(2) -0.0018(16) 0.0003(16) -0.0013(15) C35 0.0149(19) 0.010(2) 0.0064(19) 0.0004(15) 0.0006(15) 0.0038(16) C36 0.016(2) 0.010(2) 0.008(2) 0.0009(16) 0.0020(16) -0.0004(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O5 1.703(3) . ? Mo1 O6 1.715(3) . ? Mo1 O9 1.886(3) . ? Mo1 O7 1.938(3) . ? Mo1 O26 2.296(3) 6_566 ? Mo1 O8 2.365(2) . ? Mo2 O21 1.693(3) . ? Mo2 O20 1.706(3) . ? Mo2 O7 1.868(3) . ? Mo2 O19 2.075(3) . ? Mo2 O16 2.195(2) . ? Mo2 O26 2.326(3) 6_566 ? Mo3 O18 1.690(3) . ? Mo3 O17 1.702(3) . ? Mo3 O15 1.875(2) . ? Mo3 O19 2.051(3) . ? Mo3 O24 2.298(3) 6_566 ? Mo3 O16 2.353(3) . ? Mo4 O13 1.693(3) . ? Mo4 O14 1.716(3) . ? Mo4 O12 1.925(3) . ? Mo4 O15 1.928(3) . ? Mo4 O25 2.340(2) 6_566 ? Mo4 O22 2.407(3) . ? Mo5 O11 1.693(3) . ? Mo5 O10 1.716(3) . ? Mo5 O9 1.935(3) . ? Mo5 O12 1.939(3) . ? Mo5 O25 2.246(3) 6_566 ? Mo5 O8 2.427(3) . ? Cu1 O2 1.938(3) . ? Cu1 O4 1.945(3) 5_665 ? Cu1 N1 2.005(3) . ? Cu1 N2 2.021(3) . ? Cu1 O1 2.186(3) . ? Cu2 O23 1.924(3) . ? Cu2 N4 1.975(3) . ? Cu2 O22 1.988(3) . ? Cu2 N3 2.004(3) . ? P1 O2 1.501(3) . ? P1 O4 1.508(3) . ? P1 O3 1.585(3) . ? P1 C25 1.799(4) . ? P2 O8 1.530(3) . ? P2 O22 1.533(3) . ? P2 O16 1.560(3) . ? P2 C29 1.791(4) . ? P3 O24 1.520(3) . ? P3 O25 1.546(3) . ? P3 O26 1.549(3) . ? P3 C36 1.798(4) . ? O1 H1A 0.816(19) . ? O1 H1B 0.821(19) . ? O3 H3' 0.815(19) . ? O4 Cu1 1.945(3) 5_665 ? O19 H19' 0.820(19) . ? O23 H23A 0.821(19) . ? O23 H23B 0.818(19) . ? O24 Mo3 2.298(3) 6_565 ? O25 Mo5 2.246(3) 6_565 ? O25 Mo4 2.340(2) 6_565 ? O26 Mo1 2.296(3) 6_565 ? O26 Mo2 2.325(3) 6_565 ? N1 C1 1.322(5) . ? N1 C5 1.362(5) . ? N2 C12 1.325(5) . ? N2 C9 1.362(5) . ? N3 C13 1.327(5) . ? N3 C20 1.360(5) . ? N4 C24 1.317(5) . ? N4 C21 1.362(5) . ? C1 C2 1.404(6) . ? C1 H1 0.9500 . ? C2 C3 1.370(6) . ? C2 H2 0.9500 . ? C3 C4 1.406(6) . ? C3 H3 0.9500 . ? C4 C5 1.393(5) . ? C4 C6 1.434(6) . ? C5 C9 1.427(6) . ? C6 C7 1.345(6) . ? C6 H6 0.9500 . ? C7 C8 1.444(6) . ? C7 H7 0.9500 . ? C8 C9 1.398(6) . ? C8 C10 1.408(6) . ? C10 C11 1.374(6) . ? C10 H10 0.9500 . ? C11 C12 1.400(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.398(5) . ? C13 H13 0.9500 . ? C14 C15 1.364(6) . ? C14 H14 0.9500 . ? C15 C16 1.412(6) . ? C15 H15 0.9500 . ? C16 C20 1.400(5) . ? C16 C17 1.431(6) . ? C17 C18 1.351(6) . ? C17 H17 0.9500 . ? C18 C19 1.444(6) . ? C18 H18 0.9500 . ? C19 C21 1.388(5) . ? C19 C22 1.416(6) . ? C20 C21 1.432(5) . ? C22 C23 1.365(6) . ? C22 H22 0.9500 . ? C23 C24 1.391(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.501(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C28 1.391(6) 5_655 ? C26 C27 1.391(6) . ? C27 C28 1.391(6) . ? C27 H27 0.9500 . ? C28 C26 1.391(6) 5_655 ? C28 H28 0.9500 . ? C29 C30 1.517(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.387(5) . ? C30 C31 1.390(5) . ? C31 C32 1.384(5) . ? C31 H31 0.9500 . ? C32 C35 1.396(5) . ? C32 H32 0.9500 . ? C33 C34 1.398(5) . ? C33 H33 0.9500 . ? C34 C35 1.387(5) . ? C34 H34 0.9500 . ? C35 C36 1.520(5) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? 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 O5 Mo1 O6 103.55(13) . . ? O5 Mo1 O9 101.19(12) . . ? O6 Mo1 O9 102.20(12) . . ? O5 Mo1 O7 97.99(12) . . ? O6 Mo1 O7 101.15(12) . . ? O9 Mo1 O7 145.19(11) . . ? O5 Mo1 O26 165.15(12) . 6_566 ? O6 Mo1 O26 89.70(11) . 6_566 ? O9 Mo1 O26 82.15(10) . 6_566 ? O7 Mo1 O26 72.50(10) . 6_566 ? O5 Mo1 O8 88.64(11) . . ? O6 Mo1 O8 167.67(12) . . ? O9 Mo1 O8 73.16(10) . . ? O7 Mo1 O8 78.57(10) . . ? O26 Mo1 O8 78.42(9) 6_566 . ? O21 Mo2 O20 105.50(13) . . ? O21 Mo2 O7 98.26(13) . . ? O20 Mo2 O7 104.25(12) . . ? O21 Mo2 O19 96.31(12) . . ? O20 Mo2 O19 91.07(12) . . ? O7 Mo2 O19 155.11(11) . . ? O21 Mo2 O16 92.23(11) . . ? O20 Mo2 O16 156.51(12) . . ? O7 Mo2 O16 87.91(10) . . ? O19 Mo2 O16 71.42(10) . . ? O21 Mo2 O26 161.63(11) . 6_566 ? O20 Mo2 O26 92.44(11) . 6_566 ? O7 Mo2 O26 72.95(10) . 6_566 ? O19 Mo2 O26 87.12(10) . 6_566 ? O16 Mo2 O26 71.70(9) . 6_566 ? O18 Mo3 O17 102.63(14) . . ? O18 Mo3 O15 106.02(12) . . ? O17 Mo3 O15 101.41(12) . . ? O18 Mo3 O19 97.89(12) . . ? O17 Mo3 O19 96.79(12) . . ? O15 Mo3 O19 145.74(11) . . ? O18 Mo3 O24 84.77(12) . 6_566 ? O17 Mo3 O24 170.38(11) . 6_566 ? O15 Mo3 O24 82.14(10) . 6_566 ? O19 Mo3 O24 75.90(10) . 6_566 ? O18 Mo3 O16 164.62(11) . . ? O17 Mo3 O16 86.72(11) . . ? O15 Mo3 O16 83.66(10) . . ? O19 Mo3 O16 68.58(10) . . ? O24 Mo3 O16 84.78(9) 6_566 . ? O13 Mo4 O14 103.34(13) . . ? O13 Mo4 O12 104.20(12) . . ? O14 Mo4 O12 97.86(12) . . ? O13 Mo4 O15 99.41(12) . . ? O14 Mo4 O15 102.53(12) . . ? O12 Mo4 O15 144.14(10) . . ? O13 Mo4 O25 90.72(11) . 6_566 ? O14 Mo4 O25 163.40(11) . 6_566 ? O12 Mo4 O25 69.74(10) . 6_566 ? O15 Mo4 O25 83.49(10) . 6_566 ? O13 Mo4 O22 176.62(11) . . ? O14 Mo4 O22 79.74(11) . . ? O12 Mo4 O22 76.55(10) . . ? O15 Mo4 O22 78.45(10) . . ? O25 Mo4 O22 86.46(9) 6_566 . ? O11 Mo5 O10 105.19(13) . . ? O11 Mo5 O9 96.73(12) . . ? O10 Mo5 O9 102.89(12) . . ? O11 Mo5 O12 100.45(12) . . ? O10 Mo5 O12 96.31(12) . . ? O9 Mo5 O12 149.84(11) . . ? O11 Mo5 O25 94.38(11) . 6_566 ? O10 Mo5 O25 158.76(12) . 6_566 ? O9 Mo5 O25 82.53(10) . 6_566 ? O12 Mo5 O25 71.65(10) . 6_566 ? O11 Mo5 O8 161.96(11) . . ? O10 Mo5 O8 90.68(11) . . ? O9 Mo5 O8 70.91(10) . . ? O12 Mo5 O8 85.97(9) . . ? O25 Mo5 O8 71.48(9) 6_566 . ? O2 Cu1 O4 95.94(11) . 5_665 ? O2 Cu1 N1 92.58(12) . . ? O4 Cu1 N1 162.74(12) 5_665 . ? O2 Cu1 N2 171.62(12) . . ? O4 Cu1 N2 88.48(12) 5_665 . ? N1 Cu1 N2 81.36(13) . . ? O2 Cu1 O1 89.32(11) . . ? O4 Cu1 O1 100.52(12) 5_665 . ? N1 Cu1 O1 94.55(13) . . ? N2 Cu1 O1 96.89(12) . . ? O23 Cu2 N4 174.90(13) . . ? O23 Cu2 O22 91.23(11) . . ? N4 Cu2 O22 91.40(12) . . ? O23 Cu2 N3 93.65(13) . . ? N4 Cu2 N3 83.09(13) . . ? O22 Cu2 N3 169.97(12) . . ? O2 P1 O4 115.09(16) . . ? O2 P1 O3 108.72(15) . . ? O4 P1 O3 107.39(15) . . ? O2 P1 C25 112.55(18) . . ? O4 P1 C25 108.97(17) . . ? O3 P1 C25 103.36(18) . . ? O8 P2 O22 110.58(15) . . ? O8 P2 O16 112.08(15) . . ? O22 P2 O16 107.19(15) . . ? O8 P2 C29 110.47(17) . . ? O22 P2 C29 109.02(17) . . ? O16 P2 C29 107.36(16) . . ? O24 P3 O25 108.91(14) . . ? O24 P3 O26 110.14(15) . . ? O25 P3 O26 111.68(14) . . ? O24 P3 C36 111.62(17) . . ? O25 P3 C36 107.71(16) . . ? O26 P3 C36 106.78(16) . . ? Cu1 O1 H1A 132(3) . . ? Cu1 O1 H1B 122(3) . . ? H1A O1 H1B 105(5) . . ? P1 O2 Cu1 147.86(17) . . ? P1 O3 H3' 120(3) . . ? P1 O4 Cu1 133.18(16) . 5_665 ? Mo2 O7 Mo1 122.10(14) . . ? P2 O8 Mo1 126.29(14) . . ? P2 O8 Mo5 129.52(14) . . ? Mo1 O8 Mo5 90.25(9) . . ? Mo1 O9 Mo5 125.44(14) . . ? Mo4 O12 Mo5 123.04(13) . . ? Mo3 O15 Mo4 150.19(14) . . ? P2 O16 Mo2 121.65(14) . . ? P2 O16 Mo3 135.96(14) . . ? Mo2 O16 Mo3 101.85(10) . . ? Mo3 O19 Mo2 117.77(13) . . ? Mo3 O19 H19' 121(3) . . ? Mo2 O19 H19' 116(3) . . ? P2 O22 Cu2 135.74(16) . . ? P2 O22 Mo4 117.43(14) . . ? Cu2 O22 Mo4 101.65(10) . . ? Cu2 O23 H23A 109(3) . . ? Cu2 O23 H23B 136(3) . . ? H23A O23 H23B 112(5) . . ? P3 O24 Mo3 120.07(15) . 6_565 ? P3 O25 Mo5 127.31(14) . 6_565 ? P3 O25 Mo4 136.13(15) . 6_565 ? Mo5 O25 Mo4 95.53(9) 6_565 6_565 ? P3 O26 Mo1 125.44(14) . 6_565 ? P3 O26 Mo2 130.87(15) . 6_565 ? Mo1 O26 Mo2 92.20(9) 6_565 6_565 ? C1 N1 C5 118.2(3) . . ? C1 N1 Cu1 128.1(3) . . ? C5 N1 Cu1 113.6(3) . . ? C12 N2 C9 118.3(3) . . ? C12 N2 Cu1 129.0(3) . . ? C9 N2 Cu1 112.7(3) . . ? C13 N3 C20 118.2(3) . . ? C13 N3 Cu2 130.1(3) . . ? C20 N3 Cu2 111.6(2) . . ? C24 N4 C21 118.3(3) . . ? C24 N4 Cu2 128.8(3) . . ? C21 N4 Cu2 112.6(3) . . ? N1 C1 C2 122.1(4) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C3 C2 C1 119.5(4) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? C2 C3 C4 119.7(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 116.7(4) . . ? C5 C4 C6 118.2(4) . . ? C3 C4 C6 125.1(4) . . ? N1 C5 C4 123.7(4) . . ? N1 C5 C9 115.8(3) . . ? C4 C5 C9 120.6(4) . . ? C7 C6 C4 121.7(4) . . ? C7 C6 H6 119.1 . . ? C4 C6 H6 119.1 . . ? C6 C7 C8 120.9(4) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C10 117.2(4) . . ? C9 C8 C7 118.2(4) . . ? C10 C8 C7 124.6(4) . . ? N2 C9 C8 123.3(4) . . ? N2 C9 C5 116.4(3) . . ? C8 C9 C5 120.3(4) . . ? C11 C10 C8 119.2(4) . . ? C11 C10 H10 120.4 . . ? C8 C10 H10 120.4 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? N2 C12 C11 122.2(4) . . ? N2 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? N3 C13 C14 122.0(4) . . ? N3 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.2(4) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C20 C16 C15 116.8(4) . . ? C20 C16 C17 118.7(4) . . ? C15 C16 C17 124.2(4) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 121.1(4) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C21 C19 C22 116.7(4) . . ? C21 C19 C18 118.6(4) . . ? C22 C19 C18 124.7(4) . . ? N3 C20 C16 123.5(4) . . ? N3 C20 C21 116.4(3) . . ? C16 C20 C21 120.1(4) . . ? N4 C21 C19 123.4(4) . . ? N4 C21 C20 116.2(3) . . ? C19 C21 C20 120.4(4) . . ? C23 C22 C19 119.2(4) . . ? C23 C22 H22 120.4 . . ? C19 C22 H22 120.4 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? N4 C24 C23 122.4(4) . . ? N4 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C26 C25 P1 115.8(3) . . ? C26 C25 H25A 108.3 . . ? P1 C25 H25A 108.3 . . ? C26 C25 H25B 108.3 . . ? P1 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C28 C26 C27 117.7(4) 5_655 . ? C28 C26 C25 120.6(4) 5_655 . ? C27 C26 C25 121.7(4) . . ? C28 C27 C26 120.0(4) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C26 C28 C27 122.3(4) 5_655 . ? C26 C28 H28 118.9 5_655 . ? C27 C28 H28 118.9 . . ? C30 C29 P2 110.3(3) . . ? C30 C29 H29A 109.6 . . ? P2 C29 H29A 109.6 . . ? C30 C29 H29B 109.6 . . ? P2 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C33 C30 C31 119.1(4) . . ? C33 C30 C29 121.0(3) . . ? C31 C30 C29 119.7(3) . . ? C32 C31 C30 120.3(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C35 120.8(4) . . ? C31 C32 H32 119.6 . . ? C35 C32 H32 119.6 . . ? C30 C33 C34 120.6(4) . . ? C30 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34 119.9 . . ? C33 C34 H34 119.9 . . ? C34 C35 C32 118.9(3) . . ? C34 C35 C36 119.5(3) . . ? C32 C35 C36 121.6(3) . . ? C35 C36 P3 112.5(3) . . ? C35 C36 H36A 109.1 . . ? P3 C36 H36A 109.1 . . ? C35 C36 H36B 109.1 . . ? P3 C36 H36B 109.1 . . ? H36A C36 H36B 107.8 . . ? _refine_diff_density_max 1.627 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.122 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957895' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound8 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H25 Mo5 N2 Ni O25 P2, C10 H9 N2, 4(H2 O)' _chemical_formula_sum 'C28 H42 Mo5 N4 Ni O29 P2' _chemical_formula_weight 1499.00 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' Ni Ni 0.3393 1.1124 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.6642(11) _cell_length_b 17.0366(13) _cell_length_c 18.1045(13) _cell_angle_alpha 90 _cell_angle_beta 110.3660(10) _cell_angle_gamma 90 _cell_volume 4529.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 4666 _cell_measurement_theta_min 1.8152 _cell_measurement_theta_max 28.6829 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_density_meas 2.20(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.198 _exptl_crystal_F_000 2952 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.086 _exptl_absorpt_coefficient_mu 1.922 _shelx_estimated_absorpt_T_min 0.514 _shelx_estimated_absorpt_T_max 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31509 _diffrn_reflns_av_unetI/netI 0.0201 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.831 _diffrn_reflns_theta_max 25.680 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8602 _reflns_number_gt 7675 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+5.9249P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8602 _refine_ls_number_parameters 677 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0183 _refine_ls_wR_factor_ref 0.0448 _refine_ls_wR_factor_gt 0.0428 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.11372(2) 0.13930(2) -0.07139(2) 0.00886(5) Uani 1 1 d . . . . . Mo2 Mo 0.04462(2) 0.31458(2) -0.02583(2) 0.00877(5) Uani 1 1 d . . . . . Mo3 Mo 0.23245(2) 0.42683(2) 0.05549(2) 0.00785(5) Uani 1 1 d . . . . . Mo4 Mo 0.42252(2) 0.32077(2) 0.07984(2) 0.00891(5) Uani 1 1 d . . . . . Mo5 Mo 0.36168(2) 0.13227(2) 0.03320(2) 0.00884(5) Uani 1 1 d . . . . . Ni1 Ni 0.33465(2) 0.49020(2) 0.26712(2) 0.00902(7) Uani 1 1 d . . . . . P1 P 0.23556(4) 0.29390(3) -0.08585(3) 0.00821(12) Uani 1 1 d . . . . . P2 P 0.23390(4) 0.23197(3) 0.11265(3) 0.00771(12) Uani 1 1 d . . . . . O1 O 0.23896(11) 0.10683(10) -0.02623(9) 0.0114(3) Uani 1 1 d . . . . . O2 O 0.08138(11) 0.09345(10) -0.16065(9) 0.0121(3) Uani 1 1 d . . . . . O3 O 0.17666(11) 0.22721(9) -0.13074(9) 0.0113(3) Uani 1 1 d . . . . . O4 O 0.02864(11) 0.22633(9) -0.09623(9) 0.0111(3) Uani 1 1 d . . . . . O5 O 0.06657(11) 0.08112(10) -0.01849(10) 0.0132(4) Uani 1 1 d . . . . . O6 O 0.15129(11) 0.22691(9) 0.03412(9) 0.0090(3) Uani 1 1 d . . . . . O7 O 0.18075(11) 0.34930(9) -0.05100(9) 0.0092(3) Uani 1 1 d . . . . . O8 O -0.01133(11) 0.38351(10) -0.09498(10) 0.0143(4) Uani 1 1 d . . . . . O9 O -0.03169(11) 0.28808(10) 0.01730(10) 0.0149(4) Uani 1 1 d . . . . . O10 O 0.12084(11) 0.38176(9) 0.05773(9) 0.0094(3) Uani 1 1 d . . . . . O11 O 0.19580(12) 0.50927(10) 0.00068(10) 0.0133(4) Uani 1 1 d . . . . . O12 O 0.29080(11) 0.30612(9) 0.11437(9) 0.0088(3) Uani 1 1 d . . . . . O13 O 0.34502(11) 0.41092(9) 0.03807(9) 0.0102(3) Uani 1 1 d . . . . . O14 O 0.27036(11) 0.46198(9) 0.15147(9) 0.0104(3) Uani 1 1 d . . . . . O15 O 0.47690(11) 0.35184(10) 0.17561(10) 0.0139(4) Uani 1 1 d . . . . . O16 O 0.49897(12) 0.33961(10) 0.03445(11) 0.0172(4) Uani 1 1 d . . . . . O17 O 0.43989(11) 0.20974(9) 0.10038(9) 0.0106(3) Uani 1 1 d . . . . . O18 O 0.32012(11) 0.26109(9) -0.01982(9) 0.0100(3) Uani 1 1 d . . . . . O19 O 0.40756(11) 0.12457(10) -0.04071(10) 0.0136(4) Uani 1 1 d . . . . . O20 O 0.40210(11) 0.04848(10) 0.08589(10) 0.0136(4) Uani 1 1 d . . . . . O21 O 0.28973(11) 0.15720(9) 0.12097(9) 0.0097(3) Uani 1 1 d . . . . . O22 O 0.35097(13) 0.37138(11) 0.29573(12) 0.0173(4) Uani 1 1 d . . . . . H22C H 0.369(2) 0.3391(19) 0.2743(18) 0.021 Uiso 1 1 d . U . . . H22D H 0.371(2) 0.3614(18) 0.3390(19) 0.021 Uiso 1 1 d . U . . . O23 O 0.45700(12) 0.48569(12) 0.25107(11) 0.0154(4) Uani 1 1 d . . . . . H23C H 0.471(2) 0.5178(18) 0.2259(18) 0.019 Uiso 1 1 d . U . . . H23D H 0.461(2) 0.4418(19) 0.2312(17) 0.019 Uiso 1 1 d . U . . . O24 O 0.41047(13) 0.51558(11) 0.38475(10) 0.0129(4) Uani 1 1 d . . . . . H24C H 0.463(2) 0.5182(17) 0.3907(17) 0.015 Uiso 1 1 d . U . . . H24D H 0.4127(19) 0.4782(18) 0.4117(17) 0.015 Uiso 1 1 d . U . . . O25 O 0.21502(13) 0.48835(11) 0.29081(12) 0.0165(4) Uani 1 1 d . . . . . H25C H 0.210(2) 0.4600(18) 0.3196(19) 0.020 Uiso 1 1 d . U . . . H25D H 0.168(2) 0.4842(17) 0.2507(18) 0.020 Uiso 1 1 d . U . . . O90 O 0.39587(15) 0.51311(12) 0.93275(12) 0.0270(5) Uani 1 1 d D . . . . H90A H 0.424(2) 0.5546(14) 0.9515(18) 0.032 Uiso 1 1 d D U . . . H90B H 0.388(2) 0.4907(18) 0.9711(15) 0.032 Uiso 1 1 d D U . . . O91 O 0.06509(13) 0.46705(11) 0.16265(11) 0.0172(4) Uani 1 1 d D . . . . H91A H 0.0408(19) 0.5067(13) 0.1412(16) 0.021 Uiso 1 1 d D U . . . H91B H 0.074(2) 0.4407(16) 0.1285(14) 0.021 Uiso 1 1 d D U . . . O92 O 0.43625(14) 0.22607(13) 0.27870(13) 0.0285(5) Uani 1 1 d D . . . . H92A H 0.4844(17) 0.2482(19) 0.3110(17) 0.034 Uiso 1 1 d D U . . . H92B H 0.447(2) 0.217(2) 0.2371(14) 0.034 Uiso 1 1 d D U . . . O93 O 0.53195(15) 0.56976(13) 0.16777(14) 0.0305(5) Uani 1 1 d D . . . . H93A H 0.546(2) 0.6185(12) 0.1825(19) 0.037 Uiso 1 1 d D U . . . H93B H 0.554(2) 0.5486(19) 0.1358(17) 0.037 Uiso 1 1 d D U . . . N1 N 0.30976(13) 0.60891(12) 0.23993(11) 0.0109(4) Uani 1 1 d . . . . . N2 N 0.22089(15) 1.00332(12) 0.12687(13) 0.0163(5) Uani 1 1 d D . . . . H2' H 0.2129(19) 1.0529(11) 0.1115(16) 0.020 Uiso 1 1 d D U . . . N3 N 0.58696(17) 0.27022(17) 0.40881(16) 0.0321(6) Uani 1 1 d . . . . . N4 N 0.9834(2) 0.24759(17) 0.74567(15) 0.0428(8) Uani 1 1 d D . . . . H4' H 1.032(2) 0.245(2) 0.7898(16) 0.062(13) Uiso 1 1 d D . . . . C1 C 0.27312(16) 0.15064(14) 0.34672(13) 0.0100(5) Uani 1 1 d . . . . . H1A H 0.3110 0.1843 0.3259 0.012 Uiso 1 1 calc R U . . . H1B H 0.3109 0.1059 0.3747 0.012 Uiso 1 1 calc R U . . . C2 C 0.19230(16) 0.12057(14) 0.27944(14) 0.0101(5) Uani 1 1 d . . . . . C3 C 0.15336(17) 0.04939(14) 0.29097(14) 0.0139(5) Uani 1 1 d . . . . . H3 H 0.1809 0.0209 0.3384 0.017 Uiso 1 1 calc R U . . . C4 C 0.07563(18) 0.02012(15) 0.23449(15) 0.0164(5) Uani 1 1 d . . . . . H4 H 0.0502 -0.0280 0.2433 0.020 Uiso 1 1 calc R U . . . C5 C 0.03468(17) 0.06133(15) 0.16463(15) 0.0155(5) Uani 1 1 d . . . . . H5 H -0.0187 0.0414 0.1257 0.019 Uiso 1 1 calc R U . . . C6 C 0.07223(17) 0.13154(15) 0.15224(14) 0.0141(5) Uani 1 1 d . . . . . H6 H 0.0440 0.1595 0.1045 0.017 Uiso 1 1 calc R U . . . C7 C 0.15084(16) 0.16209(14) 0.20858(14) 0.0105(5) Uani 1 1 d . . . . . C8 C 0.18865(16) 0.23927(13) 0.19152(13) 0.0099(5) Uani 1 1 d . . . . . H8A H 0.2375 0.2573 0.2399 0.012 Uiso 1 1 calc R U . . . H8B H 0.1397 0.2792 0.1774 0.012 Uiso 1 1 calc R U . . . C9 C 0.24408(17) 0.63005(14) 0.17198(14) 0.0130(5) Uani 1 1 d . . . . . H9 H 0.2121 0.5900 0.1366 0.016 Uiso 1 1 calc R U . . . C10 C 0.35263(17) 0.66648(14) 0.28967(15) 0.0137(5) Uani 1 1 d . . . . . H10 H 0.3983 0.6525 0.3382 0.016 Uiso 1 1 calc R U . . . C11 C 0.22130(17) 0.70757(14) 0.15153(15) 0.0135(5) Uani 1 1 d . . . . . H11 H 0.1747 0.7198 0.1030 0.016 Uiso 1 1 calc R U . . . C12 C 0.33320(17) 0.74575(14) 0.27345(15) 0.0147(5) Uani 1 1 d . . . . . H12 H 0.3648 0.7846 0.3105 0.018 Uiso 1 1 calc R U . . . C13 C 0.26671(16) 0.76749(14) 0.20207(14) 0.0122(5) Uani 1 1 d . . . . . C14 C 0.24778(17) 0.85133(14) 0.17884(14) 0.0129(5) Uani 1 1 d . . . . . C15 C 0.16607(17) 0.87396(15) 0.12082(15) 0.0156(5) Uani 1 1 d . . . . . H15 H 0.1190 0.8365 0.0991 0.019 Uiso 1 1 calc R U . . . C16 C 0.31353(17) 0.90883(15) 0.21252(15) 0.0155(5) Uani 1 1 d . . . . . H16 H 0.3683 0.8956 0.2539 0.019 Uiso 1 1 calc R U . . . C17 C 0.15397(17) 0.95064(15) 0.09524(15) 0.0172(5) Uani 1 1 d . . . . . H17 H 0.0988 0.9663 0.0555 0.021 Uiso 1 1 calc R U . . . C18 C 0.29827(18) 0.98482(15) 0.18520(15) 0.0169(5) Uani 1 1 d . . . . . H18 H 0.3427 1.0242 0.2078 0.020 Uiso 1 1 calc R U . . . C19 C 0.6234(2) 0.20092(19) 0.43976(18) 0.0282(7) Uani 1 1 d . . . . . H19 H 0.5957 0.1542 0.4137 0.034 Uiso 1 1 calc R U . . . C20 C 0.6257(2) 0.3349(2) 0.4478(2) 0.0358(8) Uani 1 1 d . . . . . H20 H 0.5996 0.3843 0.4279 0.043 Uiso 1 1 calc R U . . . C21 C 0.69943(19) 0.19431(18) 0.50772(17) 0.0239(6) Uani 1 1 d . . . . . H21 H 0.7229 0.1441 0.5274 0.029 Uiso 1 1 calc R U . . . C22 C 0.7018(2) 0.33379(19) 0.5154(2) 0.0336(7) Uani 1 1 d . . . . . H22A H 0.7274 0.3815 0.5405 0.040 Uiso 1 1 calc R U . . . C23 C 0.74078(19) 0.26194(17) 0.54662(17) 0.0236(6) Uani 1 1 d . . . . . C24 C 0.82488(19) 0.25719(17) 0.61745(16) 0.0214(6) Uani 1 1 d . . . . . C25 C 0.8521(2) 0.31874(18) 0.67234(19) 0.0320(8) Uani 1 1 d . . . . . H25A H 0.8160 0.3648 0.6656 0.038 Uiso 1 1 calc R U . . . C26 C 0.88061(19) 0.19111(16) 0.63095(15) 0.0201(6) Uani 1 1 d . . . . . H26 H 0.8638 0.1480 0.5955 0.024 Uiso 1 1 calc R U . . . C27 C 0.9319(3) 0.3114(2) 0.73626(17) 0.0412(10) Uani 1 1 d . . . . . H27 H 0.9502 0.3525 0.7739 0.049 Uiso 1 1 calc R U . . . C28 C 0.9599(2) 0.18775(18) 0.69533(17) 0.0307(7) Uani 1 1 d . . . . . H28 H 0.9978 0.1427 0.7038 0.037 Uiso 1 1 calc R 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 Mo1 0.01064(10) 0.00630(10) 0.00790(10) -0.00072(8) 0.00104(8) -0.00041(8) Mo2 0.00957(10) 0.00818(10) 0.00752(10) -0.00086(8) 0.00168(8) 0.00090(8) Mo3 0.01070(10) 0.00577(10) 0.00696(10) -0.00031(7) 0.00294(8) 0.00003(8) Mo4 0.00938(10) 0.00728(10) 0.01011(10) -0.00097(8) 0.00343(8) -0.00077(8) Mo5 0.00994(10) 0.00663(10) 0.00908(10) -0.00069(8) 0.00222(8) 0.00093(8) Ni1 0.01181(15) 0.00734(15) 0.00796(14) -0.00038(12) 0.00350(12) -0.00074(12) P1 0.0113(3) 0.0069(3) 0.0065(3) -0.0003(2) 0.0032(2) 0.0002(2) P2 0.0096(3) 0.0062(3) 0.0065(3) 0.0004(2) 0.0019(2) -0.0005(2) O1 0.0111(8) 0.0095(8) 0.0120(8) -0.0008(7) 0.0020(7) -0.0001(7) O2 0.0137(9) 0.0107(8) 0.0104(8) -0.0011(7) 0.0024(7) -0.0009(7) O3 0.0152(9) 0.0108(8) 0.0086(8) -0.0013(7) 0.0049(7) -0.0026(7) O4 0.0114(8) 0.0105(8) 0.0093(8) -0.0011(7) 0.0011(7) 0.0006(7) O5 0.0161(9) 0.0103(8) 0.0128(8) 0.0001(7) 0.0044(7) -0.0005(7) O6 0.0101(8) 0.0075(8) 0.0081(8) -0.0001(6) 0.0014(6) -0.0005(6) O7 0.0128(8) 0.0073(8) 0.0075(8) -0.0006(6) 0.0037(7) 0.0003(6) O8 0.0166(9) 0.0103(9) 0.0125(8) -0.0005(7) 0.0009(7) 0.0022(7) O9 0.0136(9) 0.0170(9) 0.0139(9) -0.0032(7) 0.0047(7) -0.0018(7) O10 0.0107(8) 0.0094(8) 0.0087(8) -0.0018(7) 0.0039(7) 0.0004(7) O11 0.0180(9) 0.0093(8) 0.0127(8) 0.0008(7) 0.0054(7) 0.0020(7) O12 0.0106(8) 0.0075(8) 0.0087(8) 0.0001(6) 0.0037(6) 0.0000(6) O13 0.0144(9) 0.0071(8) 0.0104(8) 0.0007(7) 0.0060(7) 0.0001(7) O14 0.0126(8) 0.0084(8) 0.0108(8) -0.0017(7) 0.0047(7) -0.0003(7) O15 0.0122(9) 0.0123(9) 0.0144(9) -0.0022(7) 0.0013(7) 0.0005(7) O16 0.0188(9) 0.0135(9) 0.0239(10) -0.0010(8) 0.0132(8) -0.0013(7) O17 0.0101(8) 0.0103(8) 0.0097(8) -0.0007(7) 0.0012(7) -0.0006(7) O18 0.0138(8) 0.0074(8) 0.0087(8) -0.0002(6) 0.0037(7) 0.0007(7) O19 0.0151(9) 0.0109(9) 0.0153(9) -0.0025(7) 0.0060(7) 0.0004(7) O20 0.0153(9) 0.0092(8) 0.0154(9) 0.0009(7) 0.0043(7) 0.0023(7) O21 0.0122(8) 0.0066(8) 0.0100(8) 0.0005(6) 0.0036(7) 0.0001(6) O22 0.0257(11) 0.0104(9) 0.0134(9) -0.0019(8) 0.0036(8) 0.0002(8) O23 0.0170(9) 0.0145(10) 0.0158(9) -0.0025(8) 0.0070(8) -0.0013(8) O24 0.0148(9) 0.0110(9) 0.0121(9) 0.0027(7) 0.0037(7) -0.0009(7) O25 0.0187(10) 0.0166(10) 0.0170(10) 0.0005(8) 0.0095(8) -0.0038(8) O90 0.0404(13) 0.0221(11) 0.0216(11) -0.0038(9) 0.0147(10) -0.0150(9) O91 0.0244(10) 0.0131(9) 0.0165(10) -0.0011(8) 0.0100(8) 0.0067(8) O92 0.0267(11) 0.0353(13) 0.0257(11) 0.0062(10) 0.0121(9) 0.0027(9) O93 0.0356(12) 0.0218(11) 0.0426(13) 0.0020(10) 0.0245(11) -0.0019(10) N1 0.0109(10) 0.0107(10) 0.0118(10) 0.0005(8) 0.0046(8) -0.0004(8) N2 0.0213(12) 0.0079(10) 0.0225(12) 0.0049(9) 0.0114(10) 0.0022(9) N3 0.0213(13) 0.0438(17) 0.0353(15) 0.0105(13) 0.0149(11) 0.0056(12) N4 0.075(2) 0.0272(15) 0.0125(13) 0.0067(11) -0.0012(14) -0.0219(16) C1 0.0132(12) 0.0085(11) 0.0088(11) 0.0007(9) 0.0047(9) -0.0001(9) C2 0.0123(12) 0.0103(12) 0.0098(11) -0.0037(9) 0.0066(9) -0.0006(9) C3 0.0200(13) 0.0121(12) 0.0105(12) 0.0010(10) 0.0063(10) -0.0004(10) C4 0.0241(14) 0.0127(13) 0.0159(13) -0.0015(10) 0.0112(11) -0.0077(11) C5 0.0169(13) 0.0161(13) 0.0129(12) -0.0045(10) 0.0046(10) -0.0068(10) C6 0.0168(13) 0.0153(13) 0.0102(12) 0.0005(10) 0.0047(10) -0.0009(10) C7 0.0135(12) 0.0109(12) 0.0097(11) -0.0021(9) 0.0073(10) -0.0013(9) C8 0.0122(12) 0.0086(11) 0.0082(11) 0.0005(9) 0.0029(9) -0.0006(9) C9 0.0145(12) 0.0127(12) 0.0115(12) -0.0016(10) 0.0040(10) -0.0019(10) C10 0.0125(12) 0.0121(12) 0.0140(12) 0.0019(10) 0.0016(10) -0.0014(10) C11 0.0139(12) 0.0126(12) 0.0136(12) 0.0027(10) 0.0044(10) 0.0015(10) C12 0.0141(12) 0.0101(12) 0.0168(13) -0.0008(10) 0.0015(10) -0.0027(10) C13 0.0109(12) 0.0122(12) 0.0150(12) 0.0026(10) 0.0067(10) -0.0001(10) C14 0.0143(12) 0.0110(12) 0.0145(12) 0.0023(10) 0.0066(10) 0.0011(10) C15 0.0140(13) 0.0125(13) 0.0204(13) 0.0020(10) 0.0060(10) 0.0001(10) C16 0.0148(13) 0.0127(12) 0.0184(13) 0.0016(10) 0.0049(10) -0.0007(10) C17 0.0151(13) 0.0175(13) 0.0195(13) 0.0034(11) 0.0066(11) 0.0034(10) C18 0.0186(13) 0.0119(13) 0.0219(13) -0.0011(11) 0.0090(11) -0.0022(10) C19 0.0209(15) 0.0339(17) 0.0329(17) -0.0009(14) 0.0132(13) -0.0035(13) C20 0.0318(18) 0.0292(17) 0.052(2) 0.0079(16) 0.0220(16) 0.0060(14) C21 0.0205(14) 0.0268(16) 0.0269(15) 0.0007(13) 0.0114(12) -0.0009(12) C22 0.0274(17) 0.0278(17) 0.051(2) -0.0035(15) 0.0206(16) -0.0003(13) C23 0.0206(14) 0.0263(15) 0.0321(16) -0.0021(13) 0.0196(13) -0.0010(12) C24 0.0257(15) 0.0249(15) 0.0210(14) -0.0051(12) 0.0174(12) -0.0086(12) C25 0.050(2) 0.0239(16) 0.0372(18) -0.0109(14) 0.0349(17) -0.0155(14) C26 0.0273(15) 0.0226(15) 0.0130(13) -0.0024(11) 0.0102(11) -0.0089(12) C27 0.075(3) 0.041(2) 0.0129(15) -0.0137(14) 0.0223(16) -0.0357(19) C28 0.0447(19) 0.0246(16) 0.0189(15) 0.0068(12) 0.0060(14) -0.0126(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.7055(16) . ? Mo1 O5 1.7140(17) . ? Mo1 O1 1.9253(16) . ? Mo1 O4 1.9389(16) . ? Mo1 O3 2.2597(16) . ? Mo1 O6 2.3325(16) . ? Mo2 O9 1.7005(17) . ? Mo2 O8 1.7177(16) . ? Mo2 O4 1.9301(16) . ? Mo2 O10 1.9408(16) . ? Mo2 O6 2.2223(16) . ? Mo2 O7 2.4044(16) . ? Mo3 O11 1.7001(16) . ? Mo3 O14 1.7356(16) . ? Mo3 O13 1.9155(16) . ? Mo3 O10 1.9228(16) . ? Mo3 O7 2.2429(16) . ? Mo3 O12 2.3501(16) . ? Mo4 O16 1.7021(17) . ? Mo4 O15 1.7275(17) . ? Mo4 O17 1.9287(16) . ? Mo4 O13 1.9405(16) . ? Mo4 O18 2.2016(16) . ? Mo4 O12 2.3681(16) . ? Mo5 O20 1.7112(16) . ? Mo5 O19 1.7301(17) . ? Mo5 O1 1.8977(16) . ? Mo5 O17 1.9197(16) . ? Mo5 O21 2.2851(16) . ? Mo5 O18 2.3930(16) . ? Ni1 O23 2.0374(19) . ? Ni1 O14 2.0401(16) . ? Ni1 O25 2.0630(19) . ? Ni1 O22 2.0831(19) . ? Ni1 N1 2.086(2) . ? Ni1 O24 2.0911(18) . ? P1 O3 1.5103(17) . ? P1 O18 1.5473(17) . ? P1 O7 1.5502(16) . ? P1 C1 1.797(2) 4_565 ? P2 O21 1.5226(17) . ? P2 O12 1.5400(16) . ? P2 O6 1.5566(16) . ? P2 C8 1.806(2) . ? O22 H22C 0.78(3) . ? O22 H22D 0.75(3) . ? O23 H23C 0.79(3) . ? O23 H23D 0.84(3) . ? O24 H24C 0.80(3) . ? O24 H24D 0.80(3) . ? O25 H25C 0.73(3) . ? O25 H25D 0.84(3) . ? O90 H90A 0.841(18) . ? O90 H90B 0.839(18) . ? O91 H91A 0.806(17) . ? O91 H91B 0.817(17) . ? O92 H92A 0.863(18) . ? O92 H92B 0.842(18) . ? O93 H93A 0.876(18) . ? O93 H93B 0.849(18) . ? N1 C10 1.343(3) . ? N1 C9 1.349(3) . ? N2 C18 1.339(3) . ? N2 C17 1.347(3) . ? N2 H2' 0.884(17) . ? N3 C20 1.335(4) . ? N3 C19 1.346(4) . ? N4 C27 1.329(5) . ? N4 C28 1.331(4) . ? N4 H4' 0.889(19) . ? C1 C2 1.509(3) . ? C1 P1 1.797(2) 4_566 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.405(3) . ? C2 C7 1.410(3) . ? C3 C4 1.382(4) . ? C3 H3 0.9500 . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(3) . ? C5 H5 0.9500 . ? C6 C7 1.398(3) . ? C6 H6 0.9500 . ? C7 C8 1.517(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.384(3) . ? C9 H9 0.9500 . ? C10 C12 1.393(3) . ? C10 H10 0.9500 . ? C11 C13 1.390(3) . ? C11 H11 0.9500 . ? C12 C13 1.398(3) . ? C12 H12 0.9500 . ? C13 C14 1.489(3) . ? C14 C15 1.398(3) . ? C14 C16 1.398(4) . ? C15 C17 1.377(4) . ? C15 H15 0.9500 . ? C16 C18 1.377(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.387(4) . ? C19 H19 0.9500 . ? C20 C22 1.379(5) . ? C20 H20 0.9500 . ? C21 C23 1.388(4) . ? C21 H21 0.9500 . ? C22 C23 1.397(4) . ? C22 H22A 0.9500 . ? C23 C24 1.487(4) . ? C24 C26 1.393(4) . ? C24 C25 1.405(4) . ? C25 C27 1.383(5) . ? C25 H25A 0.9500 . ? C26 C28 1.377(4) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O5 102.77(8) . . ? O2 Mo1 O1 101.16(7) . . ? O5 Mo1 O1 99.79(7) . . ? O2 Mo1 O4 100.20(7) . . ? O5 Mo1 O4 100.18(7) . . ? O1 Mo1 O4 146.59(7) . . ? O2 Mo1 O3 83.56(7) . . ? O5 Mo1 O3 173.27(7) . . ? O1 Mo1 O3 81.01(6) . . ? O4 Mo1 O3 76.20(6) . . ? O2 Mo1 O6 167.47(7) . . ? O5 Mo1 O6 86.98(7) . . ? O1 Mo1 O6 84.64(6) . . ? O4 Mo1 O6 69.99(6) . . ? O3 Mo1 O6 86.44(6) . . ? O9 Mo2 O8 104.73(8) . . ? O9 Mo2 O4 98.39(8) . . ? O8 Mo2 O4 97.77(7) . . ? O9 Mo2 O10 97.97(7) . . ? O8 Mo2 O10 100.63(7) . . ? O4 Mo2 O10 151.31(7) . . ? O9 Mo2 O6 97.26(7) . . ? O8 Mo2 O6 157.16(7) . . ? O4 Mo2 O6 72.64(6) . . ? O10 Mo2 O6 82.04(6) . . ? O9 Mo2 O7 164.54(7) . . ? O8 Mo2 O7 87.42(7) . . ? O4 Mo2 O7 89.21(6) . . ? O10 Mo2 O7 69.94(6) . . ? O6 Mo2 O7 72.07(6) . . ? O11 Mo3 O14 103.16(8) . . ? O11 Mo3 O13 99.44(7) . . ? O14 Mo3 O13 101.53(7) . . ? O11 Mo3 O10 102.55(8) . . ? O14 Mo3 O10 96.51(7) . . ? O13 Mo3 O10 147.44(7) . . ? O11 Mo3 O7 92.13(7) . . ? O14 Mo3 O7 163.56(7) . . ? O13 Mo3 O7 81.54(6) . . ? O10 Mo3 O7 73.98(6) . . ? O11 Mo3 O12 170.65(7) . . ? O14 Mo3 O12 84.50(7) . . ? O13 Mo3 O12 73.49(6) . . ? O10 Mo3 O12 81.60(6) . . ? O7 Mo3 O12 80.89(6) . . ? O16 Mo4 O15 104.05(8) . . ? O16 Mo4 O17 101.67(8) . . ? O15 Mo4 O17 96.88(7) . . ? O16 Mo4 O13 96.46(8) . . ? O15 Mo4 O13 99.89(7) . . ? O17 Mo4 O13 151.47(7) . . ? O16 Mo4 O18 97.23(7) . . ? O15 Mo4 O18 158.15(7) . . ? O17 Mo4 O18 73.67(6) . . ? O13 Mo4 O18 82.39(6) . . ? O16 Mo4 O12 166.25(7) . . ? O15 Mo4 O12 86.44(7) . . ? O17 Mo4 O12 85.59(6) . . ? O13 Mo4 O12 72.66(6) . . ? O18 Mo4 O12 73.41(6) . . ? O20 Mo5 O19 101.26(8) . . ? O20 Mo5 O1 103.34(8) . . ? O19 Mo5 O1 98.96(7) . . ? O20 Mo5 O17 100.93(7) . . ? O19 Mo5 O17 101.35(7) . . ? O1 Mo5 O17 144.43(7) . . ? O20 Mo5 O21 86.78(7) . . ? O19 Mo5 O21 171.88(7) . . ? O1 Mo5 O21 77.83(6) . . ? O17 Mo5 O21 78.00(6) . . ? O20 Mo5 O18 170.02(7) . . ? O19 Mo5 O18 83.54(7) . . ? O1 Mo5 O18 84.35(6) . . ? O17 Mo5 O18 69.40(6) . . ? O21 Mo5 O18 88.70(5) . . ? O23 Ni1 O14 89.86(7) . . ? O23 Ni1 O25 175.33(8) . . ? O14 Ni1 O25 92.87(7) . . ? O23 Ni1 O22 87.63(8) . . ? O14 Ni1 O22 90.01(7) . . ? O25 Ni1 O22 88.58(8) . . ? O23 Ni1 N1 96.36(8) . . ? O14 Ni1 N1 90.08(7) . . ? O25 Ni1 N1 87.43(8) . . ? O22 Ni1 N1 176.01(8) . . ? O23 Ni1 O24 85.64(7) . . ? O14 Ni1 O24 175.26(7) . . ? O25 Ni1 O24 91.52(8) . . ? O22 Ni1 O24 88.32(7) . . ? N1 Ni1 O24 91.90(7) . . ? O3 P1 O18 110.02(9) . . ? O3 P1 O7 110.86(9) . . ? O18 P1 O7 110.60(9) . . ? O3 P1 C1 108.25(10) . 4_565 ? O18 P1 C1 108.67(10) . 4_565 ? O7 P1 C1 108.36(10) . 4_565 ? O21 P2 O12 112.07(9) . . ? O21 P2 O6 108.08(9) . . ? O12 P2 O6 110.80(9) . . ? O21 P2 C8 110.46(10) . . ? O12 P2 C8 108.13(10) . . ? O6 P2 C8 107.20(10) . . ? Mo5 O1 Mo1 148.94(9) . . ? P1 O3 Mo1 121.91(9) . . ? Mo2 O4 Mo1 121.45(8) . . ? P2 O6 Mo2 130.82(9) . . ? P2 O6 Mo1 132.54(9) . . ? Mo2 O6 Mo1 95.60(6) . . ? P1 O7 Mo3 128.54(9) . . ? P1 O7 Mo2 125.49(9) . . ? Mo3 O7 Mo2 93.48(6) . . ? Mo3 O10 Mo2 122.43(8) . . ? P2 O12 Mo3 125.29(9) . . ? P2 O12 Mo4 129.23(9) . . ? Mo3 O12 Mo4 91.43(5) . . ? Mo3 O13 Mo4 122.32(8) . . ? Mo3 O14 Ni1 169.59(10) . . ? Mo5 O17 Mo4 122.41(8) . . ? P1 O18 Mo4 130.54(9) . . ? P1 O18 Mo5 132.96(9) . . ? Mo4 O18 Mo5 94.36(6) . . ? P2 O21 Mo5 119.48(9) . . ? Ni1 O22 H22C 126(2) . . ? Ni1 O22 H22D 117(2) . . ? H22C O22 H22D 105(3) . . ? Ni1 O23 H23C 121(2) . . ? Ni1 O23 H23D 108(2) . . ? H23C O23 H23D 107(3) . . ? Ni1 O24 H24C 110(2) . . ? Ni1 O24 H24D 110(2) . . ? H24C O24 H24D 98(3) . . ? Ni1 O25 H25C 119(2) . . ? Ni1 O25 H25D 114(2) . . ? H25C O25 H25D 106(3) . . ? H90A O90 H90B 105(3) . . ? H91A O91 H91B 106(3) . . ? H92A O92 H92B 107(3) . . ? H93A O93 H93B 119(3) . . ? C10 N1 C9 117.5(2) . . ? C10 N1 Ni1 122.77(16) . . ? C9 N1 Ni1 119.64(16) . . ? C18 N2 C17 122.4(2) . . ? C18 N2 H2' 117.6(19) . . ? C17 N2 H2' 119.9(19) . . ? C20 N3 C19 117.1(3) . . ? C27 N4 C28 121.8(3) . . ? C27 N4 H4' 116(3) . . ? C28 N4 H4' 122(3) . . ? C2 C1 P1 110.24(16) . 4_566 ? C2 C1 H1A 109.6 . . ? P1 C1 H1A 109.6 4_566 . ? C2 C1 H1B 109.6 . . ? P1 C1 H1B 109.6 4_566 . ? H1A C1 H1B 108.1 . . ? C3 C2 C7 118.8(2) . . ? C3 C2 C1 117.3(2) . . ? C7 C2 C1 123.8(2) . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.9(2) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.7(2) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.3(2) . . ? C5 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C6 C7 C2 119.1(2) . . ? C6 C7 C8 118.8(2) . . ? C2 C7 C8 122.1(2) . . ? C7 C8 P2 112.93(16) . . ? C7 C8 H8A 109.0 . . ? P2 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? P2 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 C11 122.8(2) . . ? N1 C9 H9 118.6 . . ? C11 C9 H9 118.6 . . ? N1 C10 C12 123.0(2) . . ? N1 C10 H10 118.5 . . ? C12 C10 H10 118.5 . . ? C9 C11 C13 119.9(2) . . ? C9 C11 H11 120.0 . . ? C13 C11 H11 120.0 . . ? C10 C12 C13 119.3(2) . . ? C10 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? C11 C13 C12 117.4(2) . . ? C11 C13 C14 120.8(2) . . ? C12 C13 C14 121.7(2) . . ? C15 C14 C16 118.5(2) . . ? C15 C14 C13 121.1(2) . . ? C16 C14 C13 120.3(2) . . ? C17 C15 C14 119.8(2) . . ? C17 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C18 C16 C14 119.5(2) . . ? C18 C16 H16 120.2 . . ? C14 C16 H16 120.2 . . ? N2 C17 C15 119.6(2) . . ? N2 C17 H17 120.2 . . ? C15 C17 H17 120.2 . . ? N2 C18 C16 120.1(2) . . ? N2 C18 H18 120.0 . . ? C16 C18 H18 120.0 . . ? N3 C19 C21 123.3(3) . . ? N3 C19 H19 118.3 . . ? C21 C19 H19 118.3 . . ? N3 C20 C22 123.4(3) . . ? N3 C20 H20 118.3 . . ? C22 C20 H20 118.3 . . ? C19 C21 C23 119.2(3) . . ? C19 C21 H21 120.4 . . ? C23 C21 H21 120.4 . . ? C20 C22 C23 119.5(3) . . ? C20 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C21 C23 C22 117.4(3) . . ? C21 C23 C24 120.6(3) . . ? C22 C23 C24 121.9(3) . . ? C26 C24 C25 117.5(3) . . ? C26 C24 C23 120.6(2) . . ? C25 C24 C23 121.9(3) . . ? C27 C25 C24 119.2(3) . . ? C27 C25 H25A 120.4 . . ? C24 C25 H25A 120.4 . . ? C28 C26 C24 120.5(3) . . ? C28 C26 H26 119.7 . . ? C24 C26 H26 119.7 . . ? N4 C27 C25 120.9(3) . . ? N4 C27 H27 119.6 . . ? C25 C27 H27 119.6 . . ? N4 C28 C26 120.1(3) . . ? N4 C28 H28 120.0 . . ? C26 C28 H28 120.0 . . ? 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 O20 Mo5 O1 Mo1 143.47(18) . . . . ? O19 Mo5 O1 Mo1 -112.62(18) . . . . ? O17 Mo5 O1 Mo1 11.7(3) . . . . ? O21 Mo5 O1 Mo1 59.80(17) . . . . ? O18 Mo5 O1 Mo1 -30.08(18) . . . . ? O18 P1 O3 Mo1 60.73(13) . . . . ? O7 P1 O3 Mo1 -61.93(13) . . . . ? C1 P1 O3 Mo1 179.35(10) 4_565 . . . ? O21 P2 O6 Mo2 -174.47(11) . . . . ? O12 P2 O6 Mo2 -51.32(14) . . . . ? C8 P2 O6 Mo2 66.46(14) . . . . ? O21 P2 O6 Mo1 -9.11(15) . . . . ? O12 P2 O6 Mo1 114.04(12) . . . . ? C8 P2 O6 Mo1 -128.18(12) . . . . ? O3 P1 O7 Mo3 153.47(10) . . . . ? O18 P1 O7 Mo3 31.15(14) . . . . ? C1 P1 O7 Mo3 -87.87(13) 4_565 . . . ? O3 P1 O7 Mo2 21.92(13) . . . . ? O18 P1 O7 Mo2 -100.40(11) . . . . ? C1 P1 O7 Mo2 140.57(11) 4_565 . . . ? O21 P2 O12 Mo3 153.87(9) . . . . ? O6 P2 O12 Mo3 33.06(13) . . . . ? C8 P2 O12 Mo3 -84.15(12) . . . . ? O21 P2 O12 Mo4 25.75(14) . . . . ? O6 P2 O12 Mo4 -95.06(12) . . . . ? C8 P2 O12 Mo4 147.73(11) . . . . ? O11 Mo3 O14 Ni1 -135.8(5) . . . . ? O13 Mo3 O14 Ni1 -33.2(6) . . . . ? O10 Mo3 O14 Ni1 119.6(5) . . . . ? O7 Mo3 O14 Ni1 66.1(7) . . . . ? O12 Mo3 O14 Ni1 38.7(5) . . . . ? O3 P1 O18 Mo4 -168.74(11) . . . . ? O7 P1 O18 Mo4 -45.93(14) . . . . ? C1 P1 O18 Mo4 72.91(14) 4_565 . . . ? O3 P1 O18 Mo5 -9.84(15) . . . . ? O7 P1 O18 Mo5 112.96(12) . . . . ? C1 P1 O18 Mo5 -128.20(13) 4_565 . . . ? O12 P2 O21 Mo5 -56.92(12) . . . . ? O6 P2 O21 Mo5 65.46(11) . . . . ? C8 P2 O21 Mo5 -177.55(10) . . . . ? P1 C1 C2 C3 -85.3(2) 4_566 . . . ? P1 C1 C2 C7 90.4(2) 4_566 . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C1 C2 C3 C4 175.7(2) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? C5 C6 C7 C2 -0.2(4) . . . . ? C5 C6 C7 C8 180.0(2) . . . . ? C3 C2 C7 C6 0.3(3) . . . . ? C1 C2 C7 C6 -175.4(2) . . . . ? C3 C2 C7 C8 -179.9(2) . . . . ? C1 C2 C7 C8 4.3(3) . . . . ? C6 C7 C8 P2 -68.1(3) . . . . ? C2 C7 C8 P2 112.2(2) . . . . ? O21 P2 C8 C7 -43.12(19) . . . . ? O12 P2 C8 C7 -166.09(16) . . . . ? O6 P2 C8 C7 74.40(18) . . . . ? C10 N1 C9 C11 1.4(4) . . . . ? Ni1 N1 C9 C11 177.32(18) . . . . ? C9 N1 C10 C12 -1.1(4) . . . . ? Ni1 N1 C10 C12 -176.83(19) . . . . ? N1 C9 C11 C13 -0.1(4) . . . . ? N1 C10 C12 C13 -0.6(4) . . . . ? C9 C11 C13 C12 -1.5(4) . . . . ? C9 C11 C13 C14 175.8(2) . . . . ? C10 C12 C13 C11 1.8(4) . . . . ? C10 C12 C13 C14 -175.4(2) . . . . ? C11 C13 C14 C15 21.9(4) . . . . ? C12 C13 C14 C15 -161.0(2) . . . . ? C11 C13 C14 C16 -155.3(2) . . . . ? C12 C13 C14 C16 21.8(4) . . . . ? C16 C14 C15 C17 3.4(4) . . . . ? C13 C14 C15 C17 -173.8(2) . . . . ? C15 C14 C16 C18 -3.2(4) . . . . ? C13 C14 C16 C18 174.1(2) . . . . ? C18 N2 C17 C15 -2.8(4) . . . . ? C14 C15 C17 N2 -0.5(4) . . . . ? C17 N2 C18 C16 3.0(4) . . . . ? C14 C16 C18 N2 0.1(4) . . . . ? C20 N3 C19 C21 -1.8(4) . . . . ? C19 N3 C20 C22 2.3(5) . . . . ? N3 C19 C21 C23 0.1(4) . . . . ? N3 C20 C22 C23 -1.0(5) . . . . ? C19 C21 C23 C22 1.2(4) . . . . ? C19 C21 C23 C24 -177.1(2) . . . . ? C20 C22 C23 C21 -0.8(4) . . . . ? C20 C22 C23 C24 177.5(3) . . . . ? C21 C23 C24 C26 21.9(4) . . . . ? C22 C23 C24 C26 -156.4(3) . . . . ? C21 C23 C24 C25 -159.1(3) . . . . ? C22 C23 C24 C25 22.7(4) . . . . ? C26 C24 C25 C27 0.3(4) . . . . ? C23 C24 C25 C27 -178.8(3) . . . . ? C25 C24 C26 C28 -1.0(4) . . . . ? C23 C24 C26 C28 178.1(3) . . . . ? C28 N4 C27 C25 -1.3(5) . . . . ? C24 C25 C27 N4 0.8(4) . . . . ? C27 N4 C28 C26 0.6(5) . . . . ? C24 C26 C28 N4 0.6(4) . . . . ? _refine_diff_density_max 0.699 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.077 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957896' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound9 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H46 Mo6 N12 Ni2 O27 P2, 6(H2 O)' _chemical_formula_sum 'C56 H58 Mo6 N12 Ni2 O33 P2' _chemical_formula_weight 2182.14 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' Ni Ni 0.3393 1.1124 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.3824(13) _cell_length_b 23.955(2) _cell_length_c 20.6777(19) _cell_angle_alpha 90 _cell_angle_beta 100.325(2) _cell_angle_gamma 90 _cell_volume 7008.9(11) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 407 _cell_measurement_theta_min 3.5144 _cell_measurement_theta_max 20.0423 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas 2.08(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.068 _exptl_crystal_F_000 4320 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.040 _exptl_absorpt_coefficient_mu 1.709 _shelx_estimated_absorpt_T_min 0.875 _shelx_estimated_absorpt_T_max 0.935 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.94 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 78703 _diffrn_reflns_av_unetI/netI 0.0893 _diffrn_reflns_av_R_equivalents 0.1103 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.313 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 14313 _reflns_number_gt 9651 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 355 137 ' ' 2 0.014 0.864 0.069 19 3 ' ' 3 -0.014 0.136 0.931 19 3 ' ' 4 0.500 1.000 0.500 356 137 ' ' 5 0.486 0.364 0.431 20 3 ' ' 6 0.514 0.636 0.569 19 2 ' ' _platon_squeeze_details ; The unit cell contains 6 water molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 14313 _refine_ls_number_parameters 1048 _refine_ls_number_restraints 379 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.0981 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.933 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.001 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 0.54943(4) 0.74094(2) 1.08652(3) 0.00833(12) Uani 1 1 d . U . . . Mo2 Mo 0.59482(4) 0.87294(2) 1.18266(3) 0.01210(13) Uani 1 1 d . U . . . Mo3 Mo 0.43381(4) 0.87303(2) 1.27387(3) 0.01289(13) Uani 1 1 d . U . . . Mo4 Mo 0.32262(4) 0.74131(2) 1.29955(3) 0.00857(12) Uani 1 1 d . U . . . Mo5 Mo 0.44391(3) 0.62244(2) 1.29172(3) 0.00856(12) Uani 1 1 d . U . . . Mo6 Mo 0.55699(3) 0.62080(2) 1.16426(3) 0.00810(12) Uani 1 1 d . U . . . Ni1 Ni 0.74573(5) 0.69167(4) 1.01304(4) 0.01115(18) Uani 1 1 d . U . . . Ni2 Ni 0.46615(5) 0.87275(3) 0.82840(4) 0.00928(17) Uani 1 1 d . U . . . P1 P 0.35190(10) 0.69866(7) 1.14372(8) 0.0064(3) Uani 1 1 d . U . . . P2 P 0.05924(11) 0.75579(7) 0.75943(8) 0.0082(3) Uani 1 1 d . U . . . O1 O 0.8318(3) 0.6544(2) 0.9563(2) 0.0178(11) Uani 1 1 d D U . . . H1C H 0.805(4) 0.630(2) 0.930(3) 0.021 Uiso 1 1 d D U . . . H1D H 0.862(4) 0.677(2) 0.936(3) 0.021 Uiso 1 1 d D U . . . O2 O 0.8073(3) 0.64462(19) 1.0901(2) 0.0127(10) Uani 1 1 d D U . . . H2C H 0.827(4) 0.6123(13) 1.083(3) 0.015 Uiso 1 1 d D U . . . H2D H 0.768(4) 0.637(2) 1.115(3) 0.015 Uiso 1 1 d D U . . . O3 O 0.6654(3) 0.72560(18) 1.0778(2) 0.0112(9) Uani 1 1 d . U . . . O4 O 0.4979(3) 0.75556(19) 1.0081(2) 0.0139(10) Uani 1 1 d . U . . . O5 O 0.5168(3) 0.66213(18) 1.0867(2) 0.0115(9) Uani 1 1 d . U . . . O6 O 0.4104(3) 0.74482(18) 1.1188(2) 0.0098(9) Uani 1 1 d . U . . . O7 O 0.5699(3) 0.81284(18) 1.1216(2) 0.0124(9) Uani 1 1 d . U . . . O8 O 0.7084(3) 0.8639(2) 1.2198(2) 0.0221(11) Uani 1 1 d . U . . . O9 O 0.5987(3) 0.92592(19) 1.1290(2) 0.0227(11) Uani 1 1 d . U . . . O10 O 0.5370(3) 0.91151(18) 1.2451(2) 0.0173(10) Uani 1 1 d . U . . . O11 O 0.3502(3) 0.92506(19) 1.2615(2) 0.0207(11) Uani 1 1 d . U . . . O12 O 0.4095(3) 0.85853(19) 1.1563(2) 0.0177(10) Uani 1 1 d . U . . . O13 O 0.4701(3) 0.8723(2) 1.3562(2) 0.0246(11) Uani 1 1 d . U . . . O14 O 0.3520(3) 0.81139(18) 1.2641(2) 0.0128(9) Uani 1 1 d . U . . . O15 O 0.3709(3) 0.75500(18) 1.3792(2) 0.0120(9) Uani 1 1 d . U . . . O16 O 0.2033(3) 0.74779(18) 1.2978(2) 0.0127(10) Uani 1 1 d . U . . . O17 O 0.4939(3) 0.6156(2) 1.3723(2) 0.0165(10) Uani 1 1 d . U . . . O18 O 0.3313(3) 0.66177(18) 1.2998(2) 0.0120(9) Uani 1 1 d . U . . . O19 O 0.3908(3) 0.55869(18) 1.2714(2) 0.0146(10) Uani 1 1 d . U . . . O20 O 0.5577(3) 0.61451(17) 1.2567(2) 0.0098(9) Uani 1 1 d . U . . . O21 O 0.2903(3) 0.72345(18) 1.1896(2) 0.0102(9) Uani 1 1 d . U . . . O22 O 0.4108(3) 0.64998(18) 1.1808(2) 0.0104(9) Uani 1 1 d . U . . . O23 O 0.5175(3) 0.55659(18) 1.1356(2) 0.0125(9) Uani 1 1 d . U . . . O24 O 0.6775(3) 0.61823(18) 1.1669(2) 0.0122(9) Uani 1 1 d . U . . . O25 O 0.0396(3) 0.69341(18) 0.7490(2) 0.0113(9) Uani 1 1 d . U . . . O26 O -0.0229(3) 0.78334(17) 0.7860(2) 0.0093(9) Uani 1 1 d . U . . . O27 O 0.0790(3) 0.78348(17) 0.6961(2) 0.0079(9) Uani 1 1 d . U . . . O90 O 0.2445(6) 0.0065(4) 0.1622(5) 0.099(3) Uani 1 1 d D . . . . H90A H 0.210(7) 0.021(6) 0.124(3) 0.118 Uiso 1 1 d D U . . . H90B H 0.203(6) 0.004(6) 0.187(4) 0.118 Uiso 1 1 d D U . . . O91 O 0.2678(5) 0.4083(3) 0.1414(4) 0.071(3) Uani 1 1 d D . . . . H91B H 0.253(7) 0.405(5) 0.179(2) 0.086 Uiso 1 1 d D U . . . H91A H 0.225(6) 0.428(5) 0.119(4) 0.086 Uiso 1 1 d D U . . . O92 O 0.3413(4) 0.5117(2) 0.1456(3) 0.0305(13) Uani 1 1 d D . . . . H92A H 0.320(5) 0.533(3) 0.115(2) 0.037 Uiso 1 1 d D U . . . H92B H 0.346(5) 0.527(3) 0.1824(17) 0.037 Uiso 1 1 d D U . . . O93 O 0.0999(5) 0.7383(3) 0.1576(3) 0.0538(18) Uani 1 1 d D . . . . H93A H 0.086(7) 0.733(4) 0.196(2) 0.065 Uiso 1 1 d D U . . . H93B H 0.130(7) 0.771(2) 0.163(4) 0.065 Uiso 1 1 d D U . . . O94 O 0.1586(5) 0.8476(3) 0.1958(4) 0.070(2) Uani 1 1 d D . . . . H94A H 0.151(7) 0.816(3) 0.174(5) 0.084 Uiso 1 1 d D U . . . H94B H 0.211(4) 0.844(4) 0.222(4) 0.084 Uiso 1 1 d D U . . . O95 O 0.2422(5) 0.9027(3) 1.1063(3) 0.0536(19) Uani 1 1 d D . . . . H95A H 0.204(6) 0.883(3) 1.125(5) 0.064 Uiso 1 1 d D U . . . H95B H 0.237(7) 0.9360(13) 1.118(5) 0.064 Uiso 1 1 d D U . . . N1 N 0.6364(4) 0.6402(2) 0.9700(3) 0.0124(11) Uani 1 1 d . U . . . N2 N 0.6727(3) 0.7423(2) 0.9452(2) 0.0074(10) Uani 1 1 d . U . . . N3 N 0.8316(3) 0.7621(2) 1.0236(2) 0.0106(11) Uani 1 1 d . U . . . N4 N 0.5586(3) 0.9240(2) 0.8913(3) 0.0115(11) Uani 1 1 d . U . . . N5 N 0.5571(3) 0.8162(2) 0.8764(2) 0.0076(10) Uani 1 1 d . U . . . N6 N 0.4144(3) 0.7962(2) 0.7841(3) 0.0098(11) Uani 1 1 d . U . . . N7 N 0.5328(3) 0.8945(2) 0.7501(3) 0.0115(11) Uani 1 1 d . U . . . N8 N 0.3748(3) 0.9282(2) 0.7805(3) 0.0096(11) Uani 1 1 d . U . . . N9 N 0.3656(3) 0.8785(2) 0.8891(2) 0.0114(11) Uani 1 1 d . U . . . N10 N 0.3484(4) 0.9672(2) 0.5775(3) 0.0153(12) Uani 1 1 d . U . . . N11 N 0.2507(3) 1.0027(2) 0.7134(2) 0.0111(11) Uani 1 1 d . U . . . N12 N 0.1778(4) 1.0236(2) 0.8641(3) 0.0160(12) Uani 1 1 d . U . . . C1 C 0.6246(5) 0.5878(3) 0.9860(3) 0.0177(14) Uani 1 1 d . U . . . H1 H 0.6710 0.5712 1.0188 0.021 Uiso 1 1 calc R U . . . C2 C 0.5479(4) 0.5556(3) 0.9573(3) 0.0163(14) Uani 1 1 d . U . . . H2 H 0.5440 0.5172 0.9682 0.020 Uiso 1 1 calc R U . . . C3 C 0.4774(5) 0.5809(3) 0.9127(3) 0.0159(14) Uani 1 1 d . U . . . H3 H 0.4221 0.5607 0.8939 0.019 Uiso 1 1 calc R U . . . C4 C 0.4889(4) 0.6359(3) 0.8957(3) 0.0133(13) Uani 1 1 d . U . . . H4 H 0.4407 0.6542 0.8657 0.016 Uiso 1 1 calc R U . . . C5 C 0.5705(4) 0.6646(3) 0.9226(3) 0.0095(12) Uani 1 1 d . U . . . C6 C 0.5927(4) 0.7232(3) 0.9079(3) 0.0084(12) Uani 1 1 d . U . . . C7 C 0.5426(4) 0.7620(3) 0.8636(3) 0.0074(12) Uani 1 1 d . U . . . C8 C 0.6970(4) 0.7961(3) 0.9499(3) 0.0101(12) Uani 1 1 d . U . . . C9 C 0.6287(4) 0.8358(3) 0.9220(3) 0.0091(12) Uani 1 1 d . U . . . C10 C 0.7954(4) 0.8046(3) 0.9847(3) 0.0110(13) Uani 1 1 d . U . . . C11 C 0.9219(4) 0.7643(3) 1.0525(3) 0.0143(14) Uani 1 1 d . U . . . H11 H 0.9473 0.7342 1.0800 0.017 Uiso 1 1 calc R U . . . C12 C 0.9803(5) 0.8088(3) 1.0442(3) 0.0194(15) Uani 1 1 d . U . . . H12 H 1.0441 0.8097 1.0665 0.023 Uiso 1 1 calc R U . . . C13 C 0.9443(4) 0.8514(3) 1.0032(3) 0.0158(14) Uani 1 1 d . U . . . H13 H 0.9835 0.8818 0.9956 0.019 Uiso 1 1 calc R U . . . C14 C 0.8498(4) 0.8501(3) 0.9726(3) 0.0129(13) Uani 1 1 d . U . . . H14 H 0.8232 0.8795 0.9444 0.015 Uiso 1 1 calc R U . . . C15 C 0.6228(4) 0.8956(3) 0.9366(3) 0.0119(13) Uani 1 1 d . U . . . C16 C 0.6686(4) 0.9212(3) 0.9927(3) 0.0115(13) Uani 1 1 d . U . . . H16 H 0.7086 0.9002 1.0255 0.014 Uiso 1 1 calc R U . . . C17 C 0.6560(4) 0.9783(3) 1.0013(3) 0.0166(14) Uani 1 1 d . U . . . H17 H 0.6882 0.9967 1.0395 0.020 Uiso 1 1 calc R U . . . C18 C 0.5963(4) 1.0075(3) 0.9537(3) 0.0172(14) Uani 1 1 d . U . . . H18 H 0.5885 1.0467 0.9575 0.021 Uiso 1 1 calc R U . . . C19 C 0.5475(4) 0.9783(3) 0.8997(3) 0.0154(14) Uani 1 1 d . U . . . H19 H 0.5045 0.9982 0.8676 0.018 Uiso 1 1 calc R U . . . C20 C 0.4709(4) 0.7521(3) 0.8027(3) 0.0083(12) Uani 1 1 d . U . . . C21 C 0.4668(4) 0.7036(3) 0.7658(3) 0.0116(13) Uani 1 1 d . U . . . H21 H 0.5115 0.6745 0.7777 0.014 Uiso 1 1 calc R U . . . C22 C 0.3963(4) 0.6986(3) 0.7112(3) 0.0140(14) Uani 1 1 d . U . . . H22 H 0.3900 0.6655 0.6855 0.017 Uiso 1 1 calc R U . . . C23 C 0.3349(4) 0.7430(3) 0.6948(3) 0.0129(14) Uani 1 1 d . U . . . H23 H 0.2845 0.7401 0.6583 0.015 Uiso 1 1 calc R U . . . C24 C 0.3469(4) 0.7907(3) 0.7312(3) 0.0127(13) Uani 1 1 d . U . . . H24 H 0.3056 0.8213 0.7183 0.015 Uiso 1 1 calc R U . . . C25 C 0.6212(4) 0.8808(3) 0.7450(3) 0.0134(14) Uani 1 1 d . U . . . H25 H 0.6502 0.8501 0.7701 0.016 Uiso 1 1 calc R U . . . C26 C 0.6718(4) 0.9089(3) 0.7053(3) 0.0164(15) Uani 1 1 d . U . . . H26 H 0.7339 0.8972 0.7020 0.020 Uiso 1 1 calc R U . . . C27 C 0.6312(4) 0.9544(3) 0.6701(3) 0.0155(14) Uani 1 1 d . U . . . H27 H 0.6661 0.9756 0.6439 0.019 Uiso 1 1 calc R U . . . C28 C 0.5373(4) 0.9690(3) 0.6737(3) 0.0135(14) Uani 1 1 d . U . . . H28 H 0.5072 0.9996 0.6493 0.016 Uiso 1 1 calc R U . . . C29 C 0.4902(4) 0.9375(3) 0.7139(3) 0.0108(13) Uani 1 1 d . U . . . C30 C 0.3940(4) 0.9509(3) 0.7256(3) 0.0117(13) Uani 1 1 d . U . . . C31 C 0.3250(4) 0.9853(3) 0.6880(3) 0.0119(13) Uani 1 1 d . U . . . C32 C 0.2965(4) 0.9411(3) 0.8052(3) 0.0097(12) Uani 1 1 d . U . . . C33 C 0.2382(4) 0.9838(3) 0.7726(3) 0.0109(13) Uani 1 1 d . U . . . C34 C 0.3667(4) 0.8492(3) 0.9439(3) 0.0141(14) Uani 1 1 d . U . . . H34 H 0.4223 0.8290 0.9616 0.017 Uiso 1 1 calc R U . . . C35 C 0.2912(5) 0.8466(3) 0.9763(3) 0.0173(15) Uani 1 1 d . U . . . H35 H 0.2950 0.8263 1.0161 0.021 Uiso 1 1 calc R U . . . C36 C 0.2099(4) 0.8746(3) 0.9489(3) 0.0185(15) Uani 1 1 d . U . . . H36 H 0.1557 0.8726 0.9691 0.022 Uiso 1 1 calc R U . . . C37 C 0.2073(4) 0.9053(3) 0.8925(3) 0.0135(14) Uani 1 1 d . U . . . H37 H 0.1510 0.9241 0.8732 0.016 Uiso 1 1 calc R U . . . C38 C 0.2870(4) 0.9086(3) 0.8637(3) 0.0106(13) Uani 1 1 d . U . . . C39 C 0.3341(4) 1.0057(3) 0.6219(3) 0.0123(13) Uani 1 1 d . U . . . C40 C 0.3372(5) 1.0623(3) 0.6113(3) 0.0187(15) Uani 1 1 d . U . . . H40 H 0.3221 1.0879 0.6429 0.022 Uiso 1 1 calc R U . . . C41 C 0.3629(5) 1.0811(3) 0.5532(4) 0.0278(17) Uani 1 1 d . U . . . H41 H 0.3689 1.1199 0.5452 0.033 Uiso 1 1 calc R U . . . C42 C 0.3793(5) 1.0420(3) 0.5074(4) 0.0272(17) Uani 1 1 d . U . . . H42 H 0.3980 1.0535 0.4677 0.033 Uiso 1 1 calc R U . . . C43 C 0.3683(5) 0.9860(3) 0.5201(3) 0.0227(16) Uani 1 1 d . U . . . H43 H 0.3751 0.9597 0.4869 0.027 Uiso 1 1 calc R U . . . C44 C 0.1610(4) 1.0125(3) 0.7989(3) 0.0112(13) Uani 1 1 d . U . . . C45 C 0.0782(4) 1.0272(3) 0.7583(3) 0.0116(13) Uani 1 1 d . U . . . H45 H 0.0697 1.0194 0.7125 0.014 Uiso 1 1 calc R U . . . C46 C 0.1092(4) 1.0485(3) 0.8884(3) 0.0194(15) Uani 1 1 d . U . . . H46 H 0.1191 1.0556 0.9343 0.023 Uiso 1 1 calc R U . . . C47 C 0.0241(5) 1.0646(3) 0.8509(4) 0.0207(16) Uani 1 1 d . U . . . H47 H -0.0221 1.0833 0.8704 0.025 Uiso 1 1 calc R U . . . C48 C 0.0076(5) 1.0531(3) 0.7842(3) 0.0174(15) Uani 1 1 d . U . . . H48 H -0.0507 1.0628 0.7571 0.021 Uiso 1 1 calc R U . . . C49 C 0.2738(4) 0.6654(3) 1.0763(3) 0.0129(13) Uani 1 1 d . U . . . H49A H 0.3040 0.6300 1.0667 0.015 Uiso 1 1 calc R U . . . H49B H 0.2151 0.6554 1.0924 0.015 Uiso 1 1 calc R U . . . C50 C 0.2450(4) 0.6957(3) 1.0122(3) 0.0133(13) Uani 1 1 d . U . . . C51 C 0.3034(4) 0.6920(3) 0.9653(3) 0.0127(13) Uani 1 1 d . U . . . H51 H 0.3631 0.6741 0.9761 0.015 Uiso 1 1 calc R U . . . C52 C 0.1569(4) 0.7210(3) 0.9934(3) 0.0143(14) Uani 1 1 d . U . . . H52 H 0.1155 0.7228 1.0244 0.017 Uiso 1 1 calc R U . . . C53 C 0.2749(4) 0.7144(3) 0.9030(3) 0.0149(14) Uani 1 1 d . U . . . H53 H 0.3165 0.7125 0.8722 0.018 Uiso 1 1 calc R U . . . C54 C 0.1271(5) 0.7437(3) 0.9308(3) 0.0169(15) Uani 1 1 d . U . . . H54 H 0.0674 0.7615 0.9201 0.020 Uiso 1 1 calc R U . . . C55 C 0.1858(4) 0.7399(3) 0.8845(3) 0.0138(14) Uani 1 1 d . U . . . C56 C 0.1668(4) 0.7663(3) 0.8171(3) 0.0106(13) Uani 1 1 d . U . . . H56A H 0.2189 0.7545 0.7947 0.013 Uiso 1 1 calc R U . . . H56B H 0.1736 0.8071 0.8240 0.013 Uiso 1 1 calc R 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 Mo1 0.0087(3) 0.0097(3) 0.0067(3) 0.0012(2) 0.0020(2) 0.0018(2) Mo2 0.0141(3) 0.0082(3) 0.0149(3) -0.0001(2) 0.0051(2) 0.0010(2) Mo3 0.0133(3) 0.0112(3) 0.0153(3) -0.0034(3) 0.0059(2) -0.0010(2) Mo4 0.0092(3) 0.0100(3) 0.0070(3) -0.0008(2) 0.0027(2) -0.0003(2) Mo5 0.0083(2) 0.0099(3) 0.0074(3) 0.0002(2) 0.0012(2) 0.0000(2) Mo6 0.0088(2) 0.0085(3) 0.0070(3) 0.0002(2) 0.0015(2) 0.0008(2) Ni1 0.0107(4) 0.0129(5) 0.0099(4) 0.0014(4) 0.0018(3) 0.0029(3) Ni2 0.0093(4) 0.0093(4) 0.0090(4) 0.0017(4) 0.0010(3) 0.0021(3) P1 0.0043(7) 0.0077(8) 0.0062(8) -0.0003(7) -0.0013(6) 0.0005(6) P2 0.0080(7) 0.0086(9) 0.0079(8) 0.0004(7) 0.0013(6) 0.0002(6) O1 0.023(3) 0.020(3) 0.014(3) -0.002(2) 0.011(2) 0.002(2) O2 0.013(2) 0.014(2) 0.012(2) 0.0026(19) 0.0035(18) 0.0033(18) O3 0.012(2) 0.014(2) 0.008(2) 0.0002(18) 0.0024(17) 0.0003(17) O4 0.012(2) 0.019(3) 0.012(2) 0.0045(19) 0.0034(18) 0.0049(19) O5 0.016(2) 0.013(2) 0.005(2) 0.0007(18) 0.0018(18) 0.0024(18) O6 0.010(2) 0.014(2) 0.005(2) 0.0021(18) 0.0003(17) 0.0025(17) O7 0.020(2) 0.011(2) 0.008(2) 0.0022(18) 0.0048(18) -0.0002(18) O8 0.016(2) 0.022(3) 0.029(3) -0.004(2) 0.006(2) 0.000(2) O9 0.038(3) 0.010(3) 0.025(3) 0.004(2) 0.016(2) 0.002(2) O10 0.019(2) 0.009(2) 0.026(3) -0.005(2) 0.009(2) -0.0023(18) O11 0.022(2) 0.012(3) 0.031(3) -0.004(2) 0.013(2) 0.002(2) O12 0.029(3) 0.015(3) 0.012(2) -0.0002(19) 0.010(2) 0.002(2) O13 0.019(2) 0.035(3) 0.019(3) -0.006(2) 0.001(2) -0.003(2) O14 0.011(2) 0.012(2) 0.018(2) 0.0031(19) 0.0083(18) 0.0024(17) O15 0.015(2) 0.013(2) 0.008(2) 0.0014(18) 0.0044(18) -0.0021(18) O16 0.012(2) 0.014(3) 0.014(2) -0.0029(19) 0.0053(18) 0.0003(18) O17 0.013(2) 0.028(3) 0.007(2) 0.002(2) 0.0011(17) 0.004(2) O18 0.010(2) 0.013(2) 0.013(2) 0.0016(19) 0.0016(18) 0.0000(17) O19 0.015(2) 0.013(2) 0.017(3) -0.003(2) 0.0081(19) -0.0017(18) O20 0.011(2) 0.011(2) 0.007(2) -0.0013(18) 0.0011(17) 0.0002(17) O21 0.013(2) 0.015(2) 0.003(2) 0.0012(18) 0.0006(17) 0.0049(18) O22 0.011(2) 0.013(2) 0.007(2) 0.0018(18) 0.0012(17) 0.0009(17) O23 0.012(2) 0.014(2) 0.012(2) 0.0008(19) 0.0011(18) 0.0030(18) O24 0.013(2) 0.012(3) 0.011(2) 0.0019(19) 0.0003(17) 0.0028(18) O25 0.013(2) 0.010(2) 0.011(2) 0.0014(19) 0.0047(18) 0.0041(18) O26 0.010(2) 0.008(2) 0.011(2) 0.0018(18) 0.0023(17) -0.0007(17) O27 0.009(2) 0.009(2) 0.005(2) 0.0032(18) 0.0003(16) 0.0027(17) O90 0.088(6) 0.084(7) 0.142(8) -0.050(7) 0.070(6) 0.001(6) O91 0.103(6) 0.071(6) 0.060(5) -0.045(4) 0.068(5) -0.057(5) O92 0.025(3) 0.040(4) 0.027(3) -0.014(3) 0.005(3) -0.006(3) O93 0.045(4) 0.068(5) 0.048(4) 0.010(4) 0.008(3) 0.009(4) O94 0.041(4) 0.077(6) 0.087(7) 0.022(5) -0.005(4) 0.010(4) O95 0.075(5) 0.055(5) 0.030(4) -0.004(4) 0.009(3) 0.032(4) N1 0.014(2) 0.011(3) 0.013(3) 0.000(2) 0.006(2) 0.001(2) N2 0.005(2) 0.012(3) 0.005(3) -0.002(2) -0.0006(18) 0.0029(19) N3 0.008(2) 0.016(3) 0.007(3) -0.003(2) 0.000(2) 0.001(2) N4 0.013(2) 0.011(3) 0.012(3) 0.001(2) 0.005(2) 0.001(2) N5 0.009(2) 0.012(3) 0.003(3) 0.000(2) 0.0041(19) 0.0000(19) N6 0.004(2) 0.013(3) 0.013(3) 0.003(2) 0.0042(19) 0.0044(19) N7 0.012(2) 0.010(3) 0.012(3) -0.001(2) 0.001(2) 0.001(2) N8 0.007(2) 0.009(3) 0.012(3) -0.004(2) -0.0010(19) -0.001(2) N9 0.014(2) 0.012(3) 0.008(3) -0.005(2) 0.002(2) 0.000(2) N10 0.018(3) 0.016(3) 0.012(3) -0.001(2) 0.003(2) -0.005(2) N11 0.011(2) 0.011(3) 0.008(3) -0.004(2) -0.006(2) -0.002(2) N12 0.020(3) 0.013(3) 0.016(3) -0.004(2) 0.004(2) -0.003(2) C1 0.022(3) 0.014(3) 0.018(4) 0.004(3) 0.007(3) 0.005(3) C2 0.021(3) 0.013(4) 0.017(4) 0.000(3) 0.010(3) 0.002(3) C3 0.020(3) 0.018(4) 0.010(4) -0.001(3) 0.005(3) -0.006(3) C4 0.019(3) 0.016(3) 0.006(3) -0.003(3) 0.004(2) 0.000(3) C5 0.017(3) 0.007(3) 0.005(3) -0.003(2) 0.002(2) 0.000(2) C6 0.014(3) 0.011(3) 0.001(3) 0.000(2) 0.002(2) 0.000(2) C7 0.008(3) 0.007(3) 0.009(3) 0.000(2) 0.008(2) -0.002(2) C8 0.014(3) 0.014(3) 0.004(3) -0.003(2) 0.005(2) 0.002(2) C9 0.008(3) 0.014(3) 0.007(3) 0.002(2) 0.004(2) 0.002(2) C10 0.009(3) 0.012(3) 0.011(3) -0.004(3) 0.001(2) -0.002(2) C11 0.011(3) 0.021(4) 0.011(4) -0.004(3) 0.002(2) 0.000(3) C12 0.014(3) 0.032(4) 0.011(4) -0.012(3) -0.001(3) -0.001(3) C13 0.012(3) 0.018(4) 0.019(4) -0.013(3) 0.007(3) -0.003(3) C14 0.014(3) 0.018(4) 0.007(3) -0.005(3) 0.003(2) 0.002(3) C15 0.008(3) 0.010(3) 0.019(4) 0.000(3) 0.005(2) -0.003(2) C16 0.008(3) 0.019(3) 0.007(3) 0.000(3) -0.001(2) 0.003(3) C17 0.020(3) 0.018(4) 0.013(4) -0.008(3) 0.005(3) -0.004(3) C18 0.023(4) 0.011(4) 0.018(4) -0.004(3) 0.005(3) 0.000(3) C19 0.013(3) 0.014(3) 0.019(4) 0.000(3) 0.002(3) 0.004(3) C20 0.008(3) 0.012(3) 0.006(3) -0.001(2) 0.002(2) 0.001(2) C21 0.014(3) 0.008(3) 0.014(3) 0.001(3) 0.004(2) 0.004(2) C22 0.022(3) 0.016(4) 0.005(3) -0.004(3) 0.004(3) -0.001(3) C23 0.005(3) 0.019(4) 0.012(4) -0.001(3) -0.002(2) -0.001(2) C24 0.010(3) 0.016(3) 0.012(3) 0.005(3) 0.002(2) 0.003(3) C25 0.015(3) 0.016(4) 0.009(3) -0.003(3) 0.002(3) 0.003(3) C26 0.012(3) 0.025(4) 0.012(4) -0.002(3) 0.002(3) 0.004(3) C27 0.015(3) 0.022(4) 0.011(4) -0.003(3) 0.004(3) -0.005(3) C28 0.012(3) 0.022(4) 0.006(3) -0.002(3) 0.000(2) 0.002(3) C29 0.010(3) 0.011(3) 0.010(3) -0.005(3) -0.001(2) -0.002(2) C30 0.013(3) 0.011(3) 0.011(3) 0.002(3) 0.003(2) 0.004(2) C31 0.017(3) 0.009(3) 0.009(3) -0.003(3) 0.000(2) -0.004(3) C32 0.009(3) 0.007(3) 0.011(3) -0.004(2) -0.003(2) -0.005(2) C33 0.012(3) 0.009(3) 0.012(3) -0.002(3) 0.001(2) 0.000(2) C34 0.015(3) 0.014(4) 0.011(3) 0.002(3) 0.000(3) 0.005(3) C35 0.022(3) 0.020(4) 0.010(4) 0.004(3) 0.002(3) 0.000(3) C36 0.013(3) 0.023(4) 0.021(4) -0.004(3) 0.008(3) -0.002(3) C37 0.013(3) 0.014(4) 0.014(4) -0.003(3) 0.003(3) -0.001(3) C38 0.013(3) 0.011(3) 0.007(3) -0.004(2) -0.001(2) -0.001(2) C39 0.010(3) 0.019(4) 0.006(3) 0.002(3) -0.004(2) 0.001(3) C40 0.022(3) 0.012(3) 0.023(4) 0.004(3) 0.004(3) 0.001(3) C41 0.031(4) 0.028(4) 0.021(4) 0.011(3) -0.003(3) -0.003(3) C42 0.029(4) 0.033(4) 0.019(4) 0.008(3) 0.001(3) -0.007(3) C43 0.024(4) 0.034(4) 0.010(4) -0.004(3) 0.003(3) -0.011(3) C44 0.012(3) 0.006(3) 0.016(3) 0.002(3) 0.003(2) 0.000(2) C45 0.015(3) 0.003(3) 0.015(3) 0.005(3) -0.003(2) 0.000(2) C46 0.019(3) 0.021(4) 0.017(4) -0.008(3) -0.001(3) 0.008(3) C47 0.017(3) 0.016(4) 0.030(4) -0.006(3) 0.008(3) 0.002(3) C48 0.015(3) 0.010(4) 0.025(4) -0.003(3) -0.001(3) -0.002(3) C49 0.015(3) 0.013(4) 0.010(3) -0.003(3) -0.002(2) -0.002(3) C50 0.013(3) 0.011(3) 0.014(3) -0.005(3) -0.002(2) -0.003(3) C51 0.008(3) 0.013(4) 0.016(3) -0.001(3) -0.002(2) 0.003(3) C52 0.014(3) 0.018(4) 0.013(3) -0.004(3) 0.009(3) 0.004(3) C53 0.014(3) 0.018(4) 0.012(3) 0.003(3) 0.000(3) 0.005(3) C54 0.016(3) 0.017(4) 0.018(4) -0.001(3) 0.002(3) 0.001(3) C55 0.013(3) 0.015(4) 0.013(3) -0.006(3) 0.002(2) -0.002(3) C56 0.008(3) 0.010(3) 0.013(3) -0.002(3) -0.001(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O4 1.695(4) . ? Mo1 O3 1.748(4) . ? Mo1 O7 1.872(4) . ? Mo1 O5 1.946(4) . ? Mo1 O6 2.221(4) . ? Mo1 O27 2.305(4) 4_676 ? Mo2 O8 1.690(5) . ? Mo2 O9 1.693(5) . ? Mo2 O10 1.897(4) . ? Mo2 O7 1.906(4) . ? Mo2 O25 2.330(4) 4_676 ? Mo3 O13 1.688(5) . ? Mo3 O11 1.719(5) . ? Mo3 O14 1.876(4) . ? Mo3 O10 1.930(4) . ? Mo3 O25 2.323(4) 4_676 ? Mo3 O12 2.417(4) . ? Mo4 O15 1.701(4) . ? Mo4 O16 1.717(4) . ? Mo4 O14 1.910(4) . ? Mo4 O18 1.910(4) . ? Mo4 O21 2.277(4) . ? Mo4 O26 2.364(4) 4_676 ? Mo5 O17 1.700(4) . ? Mo5 O19 1.725(4) . ? Mo5 O18 1.906(4) . ? Mo5 O20 1.915(4) . ? Mo5 O26 2.315(4) 4_676 ? Mo5 O22 2.352(4) . ? Mo6 O23 1.709(4) . ? Mo6 O24 1.725(4) . ? Mo6 O5 1.884(4) . ? Mo6 O20 1.915(4) . ? Mo6 O22 2.298(4) . ? Mo6 O27 2.391(4) 4_676 ? Ni1 N2 2.003(5) . ? Ni1 O2 2.022(5) . ? Ni1 O1 2.055(4) . ? Ni1 N1 2.070(5) . ? Ni1 N3 2.080(5) . ? Ni1 O3 2.085(4) . ? Ni2 N8 2.001(5) . ? Ni2 N5 2.017(5) . ? Ni2 N9 2.083(5) . ? Ni2 N4 2.085(5) . ? Ni2 N7 2.090(5) . ? Ni2 N6 2.124(5) . ? P1 O21 1.530(4) . ? P1 O6 1.533(4) . ? P1 O22 1.560(4) . ? P1 C49 1.810(6) . ? P2 O25 1.529(5) . ? P2 O26 1.538(4) . ? P2 O27 1.539(4) . ? P2 C56 1.793(6) . ? O1 H1C 0.84(2) . ? O1 H1D 0.85(2) . ? O2 H2C 0.85(2) . ? O2 H2D 0.84(2) . ? O25 Mo3 2.323(4) 4_575 ? O25 Mo2 2.330(4) 4_575 ? O26 Mo5 2.314(4) 4_575 ? O26 Mo4 2.364(4) 4_575 ? O27 Mo1 2.305(4) 4_575 ? O27 Mo6 2.391(4) 4_575 ? O90 H90A 0.93(4) . ? O90 H90B 0.85(2) . ? O91 H91B 0.84(2) . ? O91 H91A 0.84(2) . ? O92 H92A 0.82(2) . ? O92 H92B 0.84(2) . ? O93 H93A 0.86(2) . ? O93 H93B 0.89(2) . ? O94 H94A 0.88(2) . ? O94 H94B 0.85(2) . ? O95 H95A 0.86(2) . ? O95 H95B 0.84(2) . ? N1 C1 1.317(8) . ? N1 C5 1.366(8) . ? N2 C8 1.333(8) . ? N2 C6 1.345(8) . ? N3 C11 1.329(8) . ? N3 C10 1.343(8) . ? N4 C19 1.327(8) . ? N4 C15 1.371(8) . ? N5 C7 1.333(8) . ? N5 C9 1.350(8) . ? N6 C24 1.333(8) . ? N6 C20 1.348(8) . ? N7 C25 1.336(7) . ? N7 C29 1.354(8) . ? N8 C30 1.331(8) . ? N8 C32 1.354(7) . ? N9 C34 1.330(8) . ? N9 C38 1.365(8) . ? N10 C39 1.343(8) . ? N10 C43 1.348(8) . ? N11 C31 1.339(7) . ? N11 C33 1.348(8) . ? N12 C46 1.328(8) . ? N12 C44 1.351(8) . ? C1 C2 1.389(9) . ? C1 H1 0.9500 . ? C2 C3 1.383(9) . ? C2 H2 0.9500 . ? C3 C4 1.382(9) . ? C3 H3 0.9500 . ? C4 C5 1.387(9) . ? C4 H4 0.9500 . ? C5 C6 1.485(8) . ? C6 C7 1.409(9) . ? C7 C20 1.496(9) . ? C8 C9 1.415(9) . ? C8 C10 1.483(8) . ? C9 C15 1.468(9) . ? C10 C14 1.391(9) . ? C11 C12 1.387(9) . ? C11 H11 0.9500 . ? C12 C13 1.369(10) . ? C12 H12 0.9500 . ? C13 C14 1.392(9) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.372(9) . ? C16 C17 1.396(9) . ? C16 H16 0.9500 . ? C17 C18 1.377(10) . ? C17 H17 0.9500 . ? C18 C19 1.395(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.385(9) . ? C21 C22 1.381(9) . ? C21 H21 0.9500 . ? C22 C23 1.384(9) . ? C22 H22 0.9500 . ? C23 C24 1.363(9) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.367(8) . ? C25 H25 0.9500 . ? C26 C27 1.382(9) . ? C26 H26 0.9500 . ? C27 C28 1.410(8) . ? C27 H27 0.9500 . ? C28 C29 1.386(8) . ? C28 H28 0.9500 . ? C29 C30 1.481(8) . ? C30 C31 1.411(9) . ? C31 C39 1.480(8) . ? C32 C33 1.415(9) . ? C32 C38 1.465(9) . ? C33 C44 1.490(8) . ? C34 C35 1.374(8) . ? C34 H34 0.9500 . ? C35 C36 1.378(9) . ? C35 H35 0.9500 . ? C36 C37 1.374(9) . ? C36 H36 0.9500 . ? C37 C38 1.385(8) . ? C37 H37 0.9500 . ? C39 C40 1.374(9) . ? C40 C41 1.395(9) . ? C40 H40 0.9500 . ? C41 C42 1.381(11) . ? C41 H41 0.9500 . ? C42 C43 1.381(11) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 C45 1.374(9) . ? C45 C48 1.379(8) . ? C45 H45 0.9500 . ? C46 C47 1.381(9) . ? C46 H46 0.9500 . ? C47 C48 1.385(10) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C50 1.503(9) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C52 1.395(9) . ? C50 C51 1.395(8) . ? C51 C53 1.387(9) . ? C51 H51 0.9500 . ? C52 C54 1.398(9) . ? C52 H52 0.9500 . ? C53 C55 1.409(9) . ? C53 H53 0.9500 . ? C54 C55 1.390(8) . ? C54 H54 0.9500 . ? C55 C56 1.509(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? 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 O4 Mo1 O3 101.93(19) . . ? O4 Mo1 O7 101.1(2) . . ? O3 Mo1 O7 98.45(19) . . ? O4 Mo1 O5 98.0(2) . . ? O3 Mo1 O5 91.80(18) . . ? O7 Mo1 O5 155.95(17) . . ? O4 Mo1 O6 90.95(17) . . ? O3 Mo1 O6 165.17(18) . . ? O7 Mo1 O6 86.10(16) . . ? O5 Mo1 O6 79.00(16) . . ? O4 Mo1 O27 164.90(17) . 4_676 ? O3 Mo1 O27 92.08(17) . 4_676 ? O7 Mo1 O27 82.18(16) . 4_676 ? O5 Mo1 O27 75.73(16) . 4_676 ? O6 Mo1 O27 74.48(14) . 4_676 ? O8 Mo2 O9 104.6(2) . . ? O8 Mo2 O10 105.0(2) . . ? O9 Mo2 O10 98.7(2) . . ? O8 Mo2 O7 104.8(2) . . ? O9 Mo2 O7 99.0(2) . . ? O10 Mo2 O7 139.94(18) . . ? O8 Mo2 O25 92.75(19) . 4_676 ? O9 Mo2 O25 162.1(2) . 4_676 ? O10 Mo2 O25 72.19(17) . 4_676 ? O7 Mo2 O25 80.27(16) . 4_676 ? O13 Mo3 O11 103.8(2) . . ? O13 Mo3 O14 100.1(2) . . ? O11 Mo3 O14 98.4(2) . . ? O13 Mo3 O10 101.5(2) . . ? O11 Mo3 O10 99.5(2) . . ? O14 Mo3 O10 147.65(18) . . ? O13 Mo3 O25 96.9(2) . 4_676 ? O11 Mo3 O25 158.89(19) . 4_676 ? O14 Mo3 O25 81.94(16) . 4_676 ? O10 Mo3 O25 71.84(16) . 4_676 ? O13 Mo3 O12 167.1(2) . . ? O11 Mo3 O12 89.07(19) . . ? O14 Mo3 O12 78.65(17) . . ? O10 Mo3 O12 74.91(18) . . ? O25 Mo3 O12 70.23(15) 4_676 . ? O15 Mo4 O16 103.6(2) . . ? O15 Mo4 O14 97.1(2) . . ? O16 Mo4 O14 101.64(19) . . ? O15 Mo4 O18 100.1(2) . . ? O16 Mo4 O18 98.92(19) . . ? O14 Mo4 O18 149.24(17) . . ? O15 Mo4 O21 167.88(17) . . ? O16 Mo4 O21 88.38(17) . . ? O14 Mo4 O21 78.54(17) . . ? O18 Mo4 O21 79.44(17) . . ? O15 Mo4 O26 86.22(17) . 4_676 ? O16 Mo4 O26 167.77(18) . 4_676 ? O14 Mo4 O26 84.06(15) . 4_676 ? O18 Mo4 O26 71.85(15) . 4_676 ? O21 Mo4 O26 82.12(14) . 4_676 ? O17 Mo5 O19 104.1(2) . . ? O17 Mo5 O18 100.29(19) . . ? O19 Mo5 O18 96.49(19) . . ? O17 Mo5 O20 96.97(19) . . ? O19 Mo5 O20 101.02(18) . . ? O18 Mo5 O20 151.57(18) . . ? O17 Mo5 O26 95.15(19) . 4_676 ? O19 Mo5 O26 159.57(19) . 4_676 ? O18 Mo5 O26 73.07(16) . 4_676 ? O20 Mo5 O26 83.06(16) . 4_676 ? O17 Mo5 O22 163.54(19) . . ? O19 Mo5 O22 90.42(18) . . ? O18 Mo5 O22 85.43(16) . . ? O20 Mo5 O22 72.30(16) . . ? O26 Mo5 O22 71.59(15) 4_676 . ? O23 Mo6 O24 104.4(2) . . ? O23 Mo6 O5 98.4(2) . . ? O24 Mo6 O5 101.49(18) . . ? O23 Mo6 O20 102.57(19) . . ? O24 Mo6 O20 98.03(18) . . ? O5 Mo6 O20 146.72(17) . . ? O23 Mo6 O22 94.00(17) . . ? O24 Mo6 O22 161.18(18) . . ? O5 Mo6 O22 79.47(16) . . ? O20 Mo6 O22 73.57(16) . . ? O23 Mo6 O27 168.04(17) . 4_676 ? O24 Mo6 O27 86.72(17) . 4_676 ? O5 Mo6 O27 74.68(17) . 4_676 ? O20 Mo6 O27 79.84(16) . 4_676 ? O22 Mo6 O27 75.33(14) . 4_676 ? N2 Ni1 O2 171.85(18) . . ? N2 Ni1 O1 99.00(19) . . ? O2 Ni1 O1 89.13(18) . . ? N2 Ni1 N1 78.3(2) . . ? O2 Ni1 N1 101.5(2) . . ? O1 Ni1 N1 89.1(2) . . ? N2 Ni1 N3 79.0(2) . . ? O2 Ni1 N3 101.6(2) . . ? O1 Ni1 N3 90.30(19) . . ? N1 Ni1 N3 156.9(2) . . ? N2 Ni1 O3 86.16(18) . . ? O2 Ni1 O3 85.71(17) . . ? O1 Ni1 O3 174.81(19) . . ? N1 Ni1 O3 92.48(18) . . ? N3 Ni1 O3 90.18(18) . . ? N8 Ni2 N5 179.3(2) . . ? N8 Ni2 N9 77.9(2) . . ? N5 Ni2 N9 101.91(19) . . ? N8 Ni2 N4 101.9(2) . . ? N5 Ni2 N4 78.7(2) . . ? N9 Ni2 N4 91.11(19) . . ? N8 Ni2 N7 78.6(2) . . ? N5 Ni2 N7 101.65(19) . . ? N9 Ni2 N7 156.2(2) . . ? N4 Ni2 N7 90.4(2) . . ? N8 Ni2 N6 102.2(2) . . ? N5 Ni2 N6 77.2(2) . . ? N9 Ni2 N6 95.10(19) . . ? N4 Ni2 N6 155.8(2) . . ? N7 Ni2 N6 93.19(19) . . ? O21 P1 O6 110.0(2) . . ? O21 P1 O22 108.0(2) . . ? O6 P1 O22 114.9(2) . . ? O21 P1 C49 107.5(3) . . ? O6 P1 C49 111.1(3) . . ? O22 P1 C49 104.9(3) . . ? O25 P2 O26 109.6(2) . . ? O25 P2 O27 111.0(2) . . ? O26 P2 O27 112.9(2) . . ? O25 P2 C56 110.2(3) . . ? O26 P2 C56 109.2(3) . . ? O27 P2 C56 103.7(3) . . ? Ni1 O1 H1C 114(5) . . ? Ni1 O1 H1D 115(5) . . ? H1C O1 H1D 109(4) . . ? Ni1 O2 H2C 119(5) . . ? Ni1 O2 H2D 110(4) . . ? H2C O2 H2D 101(4) . . ? Mo1 O3 Ni1 142.8(2) . . ? Mo6 O5 Mo1 118.3(2) . . ? P1 O6 Mo1 130.4(2) . . ? Mo1 O7 Mo2 161.8(2) . . ? Mo2 O10 Mo3 115.6(2) . . ? Mo3 O14 Mo4 145.9(3) . . ? Mo5 O18 Mo4 123.3(2) . . ? Mo5 O20 Mo6 121.2(2) . . ? P1 O21 Mo4 130.9(2) . . ? P1 O22 Mo6 125.8(2) . . ? P1 O22 Mo5 133.3(2) . . ? Mo6 O22 Mo5 91.67(15) . . ? P2 O25 Mo3 138.6(2) . 4_575 ? P2 O25 Mo2 132.5(2) . 4_575 ? Mo3 O25 Mo2 88.21(15) 4_575 4_575 ? P2 O26 Mo5 128.0(2) . 4_575 ? P2 O26 Mo4 137.2(2) . 4_575 ? Mo5 O26 Mo4 91.76(14) 4_575 4_575 ? P2 O27 Mo1 134.2(2) . 4_575 ? P2 O27 Mo6 127.8(2) . 4_575 ? Mo1 O27 Mo6 88.89(14) 4_575 4_575 ? H90A O90 H90B 103(5) . . ? H91B O91 H91A 107(5) . . ? H92A O92 H92B 113(5) . . ? H93A O93 H93B 102(4) . . ? H94A O94 H94B 103(5) . . ? H95A O95 H95B 107(5) . . ? C1 N1 C5 118.9(6) . . ? C1 N1 Ni1 125.6(5) . . ? C5 N1 Ni1 115.5(4) . . ? C8 N2 C6 123.7(5) . . ? C8 N2 Ni1 115.8(4) . . ? C6 N2 Ni1 118.9(4) . . ? C11 N3 C10 118.8(6) . . ? C11 N3 Ni1 126.4(5) . . ? C10 N3 Ni1 113.1(4) . . ? C19 N4 C15 118.7(6) . . ? C19 N4 Ni2 125.5(4) . . ? C15 N4 Ni2 114.2(4) . . ? C7 N5 C9 123.5(5) . . ? C7 N5 Ni2 119.4(4) . . ? C9 N5 Ni2 117.1(4) . . ? C24 N6 C20 118.1(6) . . ? C24 N6 Ni2 125.9(4) . . ? C20 N6 Ni2 114.0(4) . . ? C25 N7 C29 119.2(5) . . ? C25 N7 Ni2 125.1(4) . . ? C29 N7 Ni2 113.2(4) . . ? C30 N8 C32 122.8(5) . . ? C30 N8 Ni2 118.4(4) . . ? C32 N8 Ni2 118.8(4) . . ? C34 N9 C38 119.3(5) . . ? C34 N9 Ni2 125.1(4) . . ? C38 N9 Ni2 114.8(4) . . ? C39 N10 C43 117.1(6) . . ? C31 N11 C33 119.8(5) . . ? C46 N12 C44 117.0(6) . . ? N1 C1 C2 123.4(7) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 118.3(7) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C4 C3 C2 118.7(6) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N1 C5 C4 120.3(6) . . ? N1 C5 C6 113.8(5) . . ? C4 C5 C6 125.8(6) . . ? N2 C6 C7 115.8(6) . . ? N2 C6 C5 113.4(5) . . ? C7 C6 C5 130.8(6) . . ? N5 C7 C6 117.9(6) . . ? N5 C7 C20 112.5(5) . . ? C6 C7 C20 129.5(6) . . ? N2 C8 C9 117.9(6) . . ? N2 C8 C10 112.5(5) . . ? C9 C8 C10 129.6(6) . . ? N5 C9 C8 115.8(6) . . ? N5 C9 C15 114.8(5) . . ? C8 C9 C15 129.4(6) . . ? N3 C10 C14 122.1(6) . . ? N3 C10 C8 114.8(5) . . ? C14 C10 C8 122.7(6) . . ? N3 C11 C12 122.7(7) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 118.6(6) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C12 C13 C14 119.6(6) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C10 C14 C13 118.1(6) . . ? C10 C14 H14 121.0 . . ? C13 C14 H14 121.0 . . ? N4 C15 C16 121.2(6) . . ? N4 C15 C9 113.6(6) . . ? C16 C15 C9 124.9(6) . . ? C15 C16 C17 119.4(6) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 119.1(6) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 118.5(6) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? N4 C19 C18 122.8(6) . . ? N4 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? N6 C20 C21 122.4(6) . . ? N6 C20 C7 113.9(5) . . ? C21 C20 C7 123.5(6) . . ? C22 C21 C20 118.4(6) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C21 C22 C23 118.5(6) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C24 C23 C22 119.8(6) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? N6 C24 C23 122.5(6) . . ? N6 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? N7 C25 C26 122.8(6) . . ? N7 C25 H25 118.6 . . ? C26 C25 H25 118.6 . . ? C25 C26 C27 119.1(6) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C26 C27 C28 119.1(6) . . ? C26 C27 H27 120.5 . . ? C28 C27 H27 120.5 . . ? C29 C28 C27 118.2(6) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? N7 C29 C28 121.6(5) . . ? N7 C29 C30 114.7(5) . . ? C28 C29 C30 123.5(6) . . ? N8 C30 C31 118.4(5) . . ? N8 C30 C29 113.2(5) . . ? C31 C30 C29 128.4(6) . . ? N11 C31 C30 119.9(5) . . ? N11 C31 C39 117.9(6) . . ? C30 C31 C39 122.2(5) . . ? N8 C32 C33 116.6(5) . . ? N8 C32 C38 113.4(5) . . ? C33 C32 C38 130.0(5) . . ? N11 C33 C32 120.8(5) . . ? N11 C33 C44 114.0(5) . . ? C32 C33 C44 125.2(5) . . ? N9 C34 C35 123.3(6) . . ? N9 C34 H34 118.4 . . ? C35 C34 H34 118.4 . . ? C34 C35 C36 117.7(6) . . ? C34 C35 H35 121.2 . . ? C36 C35 H35 121.2 . . ? C37 C36 C35 120.1(6) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 119.8(6) . . ? C36 C37 H37 120.1 . . ? C38 C37 H37 120.1 . . ? N9 C38 C37 119.7(6) . . ? N9 C38 C32 114.0(5) . . ? C37 C38 C32 126.3(6) . . ? N10 C39 C40 123.7(6) . . ? N10 C39 C31 117.0(6) . . ? C40 C39 C31 118.9(6) . . ? C39 C40 C41 118.5(7) . . ? C39 C40 H40 120.8 . . ? C41 C40 H40 120.8 . . ? C42 C41 C40 118.4(7) . . ? C42 C41 H41 120.8 . . ? C40 C41 H41 120.8 . . ? C43 C42 C41 119.2(7) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? N10 C43 C42 122.8(7) . . ? N10 C43 H43 118.6 . . ? C42 C43 H43 118.6 . . ? N12 C44 C45 122.8(6) . . ? N12 C44 C33 116.3(5) . . ? C45 C44 C33 121.0(6) . . ? C44 C45 C48 119.7(6) . . ? C44 C45 H45 120.2 . . ? C48 C45 H45 120.2 . . ? N12 C46 C47 123.8(7) . . ? N12 C46 H46 118.1 . . ? C47 C46 H46 118.1 . . ? C46 C47 C48 118.8(6) . . ? C46 C47 H47 120.6 . . ? C48 C47 H47 120.6 . . ? C45 C48 C47 118.0(6) . . ? C45 C48 H48 121.0 . . ? C47 C48 H48 121.0 . . ? C50 C49 P1 120.2(5) . . ? C50 C49 H49A 107.3 . . ? P1 C49 H49A 107.3 . . ? C50 C49 H49B 107.3 . . ? P1 C49 H49B 107.3 . . ? H49A C49 H49B 106.9 . . ? C52 C50 C51 117.7(6) . . ? C52 C50 C49 123.2(6) . . ? C51 C50 C49 118.5(6) . . ? C53 C51 C50 120.4(6) . . ? C53 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C50 C52 C54 122.6(6) . . ? C50 C52 H52 118.7 . . ? C54 C52 H52 118.7 . . ? C51 C53 C55 121.6(6) . . ? C51 C53 H53 119.2 . . ? C55 C53 H53 119.2 . . ? C55 C54 C52 119.3(6) . . ? C55 C54 H54 120.3 . . ? C52 C54 H54 120.3 . . ? C54 C55 C53 118.4(6) . . ? C54 C55 C56 125.2(6) . . ? C53 C55 C56 116.0(5) . . ? C55 C56 P2 123.2(4) . . ? C55 C56 H56A 106.5 . . ? P2 C56 H56A 106.5 . . ? C55 C56 H56B 106.5 . . ? P2 C56 H56B 106.5 . . ? H56A C56 H56B 106.5 . . ? _refine_diff_density_max 1.348 _refine_diff_density_min -0.805 _refine_diff_density_rms 0.165 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 957897' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound10 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H20 Mo2 N3 Ni O13 P2, 2 (H2 O)' _chemical_formula_sum 'C20 H24 Mo2 N3 Ni O15 P2' _chemical_formula_weight 858.95 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' Ni Ni 0.3393 1.1124 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.135(4) _cell_length_b 11.8418(18) _cell_length_c 20.308(3) _cell_angle_alpha 90 _cell_angle_beta 112.140(4) _cell_angle_gamma 90 _cell_volume 5376.0(14) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1223 _cell_measurement_theta_min 1.8381 _cell_measurement_theta_max 30.0137 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_density_meas 2.07(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.122 _exptl_crystal_F_000 3416 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.192 _exptl_crystal_size_mid 0.183 _exptl_crystal_size_min 0.125 _exptl_absorpt_coefficient_mu 1.813 _shelx_estimated_absorpt_T_min 0.722 _shelx_estimated_absorpt_T_max 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20391 _diffrn_reflns_av_unetI/netI 0.0660 _diffrn_reflns_av_R_equivalents 0.1092 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.822 _diffrn_reflns_theta_max 26.361 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 5490 _reflns_number_gt 4573 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0766P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5490 _refine_ls_number_parameters 416 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.29382(2) 1.30454(3) 0.65747(2) 0.01032(12) Uani 1 1 d . U . . . Mo2 Mo 0.34786(2) 1.09466(3) 0.58809(2) 0.00955(12) Uani 1 1 d . U . . . Ni1 Ni 0.41055(2) 0.98536(4) 0.34326(3) 0.01109(15) Uani 1 1 d . U . . . P1 P 0.31253(5) 1.00557(9) 0.42012(5) 0.0099(2) Uani 1 1 d . U . . . P2 P 0.30859(4) 0.34317(9) 0.50230(5) 0.0093(2) Uani 1 1 d . U . . . O1 O 0.26518(13) 1.2121(3) 0.70207(15) 0.0140(6) Uani 1 1 d . U . . . O2 O 0.33311(13) 1.3993(3) 0.71987(16) 0.0167(6) Uani 1 1 d . U . . . O3 O 0.35815(12) 1.2127(2) 0.65542(15) 0.0123(6) Uani 1 1 d . U . . . O4 O 0.33139(13) 0.9889(2) 0.63489(15) 0.0135(6) Uani 1 1 d . U . . . O5 O 0.42151(13) 1.0709(3) 0.60311(15) 0.0163(6) Uani 1 1 d . U . . . O6 O 0.31542(12) 1.0109(2) 0.49724(15) 0.0111(6) Uani 1 1 d . U . . . O7 O 0.28484(12) 1.1152(2) 0.38010(15) 0.0127(6) Uani 1 1 d . U . . . O8 O 0.37382(13) 0.9857(3) 0.41763(15) 0.0149(6) Uani 1 1 d . U . . . O9 O 0.49105(14) 1.0209(3) 0.42905(17) 0.0191(7) Uani 1 1 d D U . . . H9C H 0.5235(15) 0.993(4) 0.429(3) 0.023 Uiso 1 1 d D U . . . H9D H 0.507(2) 1.085(3) 0.436(3) 0.023 Uiso 1 1 d D U . . . O10 O 0.32710(13) 0.9728(3) 0.26460(15) 0.0136(6) Uani 1 1 d D U . . . H10C H 0.327(2) 0.998(4) 0.2271(17) 0.016 Uiso 1 1 d D U . . . H10D H 0.318(2) 0.9047(19) 0.260(3) 0.016 Uiso 1 1 d D U . . . O11 O 0.34434(12) 0.2332(2) 0.51646(14) 0.0117(6) Uani 1 1 d . U . . . O12 O 0.24699(12) 0.3314(2) 0.44097(15) 0.0119(6) Uani 1 1 d . U . . . O13 O 0.30331(12) 0.3894(2) 0.56995(15) 0.0117(6) Uani 1 1 d . U . . . O90A O 0.5219(4) 0.3310(18) 0.4188(5) 0.034(4) Uani 0.46(3) 1 d . . P A 1 O90B O 0.5260(3) 0.2571(17) 0.4248(4) 0.034(4) Uani 0.54(3) 1 d . . P A 2 O91 O 0.44584(17) 0.2140(3) 0.48178(19) 0.0309(8) Uani 1 1 d D . . . . H91A H 0.440(3) 0.148(3) 0.465(3) 0.037 Uiso 1 1 d D U . . . H91B H 0.4145(17) 0.225(5) 0.491(3) 0.037 Uiso 1 1 d D U . . . N1 N 0.40703(15) 1.1559(3) 0.30806(18) 0.0124(7) Uani 1 1 d . U . . . N2 N 0.45981(15) 0.9784(3) 0.28027(17) 0.0112(7) Uani 1 1 d . U . . . N3 N 0.43362(16) 0.8129(3) 0.34675(18) 0.0131(7) Uani 1 1 d . U . . . C1 C 0.37146(18) 1.2380(4) 0.3139(2) 0.0141(8) Uani 1 1 d . U . . . H1 H 0.3493 1.2259 0.3433 0.017 Uiso 1 1 calc R U . . . C2 C 0.36545(19) 1.3412(4) 0.2785(2) 0.0176(9) Uani 1 1 d . U . . . H2 H 0.3415 1.3997 0.2860 0.021 Uiso 1 1 calc R U . . . C3 C 0.39458(19) 1.3568(4) 0.2327(2) 0.0173(9) Uani 1 1 d . U . . . H3 H 0.3899 1.4253 0.2068 0.021 Uiso 1 1 calc R U . . . C4 C 0.43100(18) 1.2712(4) 0.2247(2) 0.0142(8) Uani 1 1 d . U . . . H4 H 0.4508 1.2795 0.1924 0.017 Uiso 1 1 calc R U . . . C5 C 0.43791(18) 1.1736(4) 0.2646(2) 0.0120(8) Uani 1 1 d . U . . . C6 C 0.47557(18) 1.0773(4) 0.2602(2) 0.0125(8) Uani 1 1 d . U . . . C7 C 0.48297(17) 0.8788(4) 0.2720(2) 0.0114(8) Uani 1 1 d . U . . . C8 C 0.47266(18) 0.7857(4) 0.3149(2) 0.0118(8) Uani 1 1 d . U . . . C9 C 0.50332(19) 0.6843(4) 0.3273(2) 0.0154(9) Uani 1 1 d . U . . . H9 H 0.5329 0.6706 0.3079 0.018 Uiso 1 1 calc R U . . . C10 C 0.49036(19) 0.6018(4) 0.3689(2) 0.0162(9) Uani 1 1 d . U . . . H10 H 0.5104 0.5311 0.3776 0.019 Uiso 1 1 calc R U . . . C11 C 0.44763(19) 0.6262(4) 0.3969(2) 0.0179(9) Uani 1 1 d . U . . . H11 H 0.4359 0.5705 0.4227 0.021 Uiso 1 1 calc R U . . . C12 C 0.42214(19) 0.7322(4) 0.3868(2) 0.0171(9) Uani 1 1 d . U . . . H12 H 0.3951 0.7493 0.4093 0.020 Uiso 1 1 calc R U . . . C13 C 0.26080(19) 0.8930(3) 0.3809(2) 0.0138(8) Uani 1 1 d . U . . . H13A H 0.2239 0.9074 0.3899 0.017 Uiso 1 1 calc R U . . . H13B H 0.2500 0.8951 0.3288 0.017 Uiso 1 1 calc R U . . . C14 C 0.28288(18) 0.7747(4) 0.4072(2) 0.0129(8) Uani 1 1 d . U . . . C15 C 0.27577(19) 0.6896(3) 0.3584(2) 0.0137(8) Uani 1 1 d . U . . . H15 H 0.2557 0.7053 0.3092 0.016 Uiso 1 1 calc R U . . . C16 C 0.31031(18) 0.7487(4) 0.4796(2) 0.0145(8) Uani 1 1 d . U . . . H16 H 0.3143 0.8053 0.5142 0.017 Uiso 1 1 calc R U . . . C17 C 0.29733(19) 0.5813(4) 0.3796(2) 0.0143(8) Uani 1 1 d . U . . . H17 H 0.2920 0.5244 0.3448 0.017 Uiso 1 1 calc R U . . . C18 C 0.33165(19) 0.6410(4) 0.5008(2) 0.0151(8) Uani 1 1 d . U . . . H18 H 0.3501 0.6246 0.5501 0.018 Uiso 1 1 calc R U . . . C19 C 0.32661(18) 0.5555(4) 0.4512(2) 0.0140(8) Uani 1 1 d . U . . . C20 C 0.35330(18) 0.4403(4) 0.4745(2) 0.0130(8) Uani 1 1 d . U . . . H20A H 0.3923 0.4500 0.5144 0.016 Uiso 1 1 calc R U . . . H20B H 0.3614 0.4054 0.4347 0.016 Uiso 1 1 calc R 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 Mo1 0.0149(2) 0.0137(2) 0.00270(18) 0.00007(13) 0.00368(14) 0.00099(13) Mo2 0.0127(2) 0.0136(2) 0.00254(19) 0.00088(13) 0.00304(14) 0.00148(13) Ni1 0.0139(3) 0.0155(3) 0.0046(3) -0.0005(2) 0.0043(2) 0.0010(2) P1 0.0144(5) 0.0134(5) 0.0031(5) 0.0003(4) 0.0045(4) 0.0016(4) P2 0.0138(5) 0.0116(5) 0.0022(5) 0.0006(4) 0.0025(4) 0.0006(4) O1 0.0192(15) 0.0189(15) 0.0057(14) 0.0016(11) 0.0069(12) 0.0028(12) O2 0.0215(16) 0.0187(16) 0.0085(15) -0.0058(12) 0.0042(12) 0.0001(12) O3 0.0141(14) 0.0168(15) 0.0055(13) -0.0005(11) 0.0030(11) 0.0019(11) O4 0.0212(15) 0.0165(15) 0.0039(13) -0.0004(11) 0.0061(12) 0.0008(12) O5 0.0165(15) 0.0237(17) 0.0079(14) 0.0004(12) 0.0037(12) 0.0038(12) O6 0.0153(14) 0.0140(15) 0.0040(13) 0.0002(10) 0.0036(11) 0.0014(11) O7 0.0148(14) 0.0157(15) 0.0088(14) 0.0018(12) 0.0056(12) 0.0016(11) O8 0.0182(15) 0.0226(16) 0.0042(13) 0.0041(12) 0.0047(12) 0.0064(12) O9 0.0176(15) 0.0250(17) 0.0098(15) -0.0016(13) -0.0006(12) 0.0065(13) O10 0.0176(14) 0.0190(16) 0.0039(14) -0.0008(12) 0.0037(12) -0.0025(12) O11 0.0158(14) 0.0151(14) 0.0053(13) 0.0012(11) 0.0052(11) -0.0006(11) O12 0.0132(14) 0.0175(15) 0.0044(13) -0.0015(11) 0.0029(11) -0.0018(11) O13 0.0157(14) 0.0156(15) 0.0039(13) 0.0005(11) 0.0039(11) -0.0006(11) O90A 0.041(5) 0.036(11) 0.023(5) 0.007(4) 0.008(4) 0.000(5) O90B 0.034(4) 0.055(12) 0.015(4) -0.002(4) 0.011(3) -0.005(4) O91 0.033(2) 0.042(2) 0.0196(18) -0.0040(16) 0.0124(16) 0.0107(18) N1 0.0126(16) 0.0161(17) 0.0081(17) -0.0028(14) 0.0035(13) -0.0017(13) N2 0.0127(16) 0.0160(17) 0.0033(15) -0.0005(13) 0.0013(13) -0.0011(13) N3 0.0180(17) 0.0196(18) 0.0018(16) 0.0003(13) 0.0037(13) -0.0006(14) C1 0.0148(19) 0.017(2) 0.011(2) -0.0019(17) 0.0060(16) 0.0009(16) C2 0.015(2) 0.020(2) 0.017(2) -0.0005(18) 0.0050(17) 0.0022(17) C3 0.019(2) 0.016(2) 0.015(2) 0.0016(17) 0.0049(17) 0.0013(17) C4 0.015(2) 0.018(2) 0.010(2) -0.0014(16) 0.0049(16) -0.0008(16) C5 0.0114(18) 0.016(2) 0.0056(19) -0.0021(15) -0.0003(15) -0.0008(15) C6 0.017(2) 0.016(2) 0.0026(18) 0.0007(15) 0.0018(16) -0.0014(16) C7 0.0082(18) 0.016(2) 0.0058(18) -0.0007(16) -0.0019(15) -0.0022(15) C8 0.0156(19) 0.015(2) 0.0051(18) 0.0012(16) 0.0048(15) -0.0009(16) C9 0.019(2) 0.016(2) 0.013(2) -0.0019(17) 0.0081(17) -0.0012(16) C10 0.020(2) 0.019(2) 0.011(2) 0.0010(17) 0.0075(17) -0.0008(17) C11 0.021(2) 0.022(2) 0.012(2) 0.0036(18) 0.0082(18) -0.0008(18) C12 0.019(2) 0.024(2) 0.010(2) 0.0055(18) 0.0076(17) 0.0010(18) C13 0.017(2) 0.016(2) 0.0075(19) -0.0032(16) 0.0036(16) -0.0024(16) C14 0.0124(19) 0.016(2) 0.0106(19) 0.0016(16) 0.0052(16) 0.0026(16) C15 0.017(2) 0.019(2) 0.0048(18) -0.0007(15) 0.0039(16) -0.0019(16) C16 0.020(2) 0.017(2) 0.0074(19) -0.0019(16) 0.0061(16) -0.0014(17) C17 0.020(2) 0.016(2) 0.0070(19) -0.0037(16) 0.0058(16) -0.0037(16) C18 0.019(2) 0.020(2) 0.0050(19) -0.0014(16) 0.0032(16) -0.0026(17) C19 0.015(2) 0.018(2) 0.011(2) 0.0011(16) 0.0075(16) -0.0019(16) C20 0.0132(19) 0.015(2) 0.013(2) 0.0018(16) 0.0079(16) -0.0003(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.691(3) . ? Mo1 O1 1.723(3) . ? Mo1 O3 1.909(3) . ? Mo1 O7 1.999(3) 7_576 ? Mo1 O13 2.128(3) 1_565 ? Mo1 O12 2.464(3) 7_566 ? Mo2 O4 1.707(3) . ? Mo2 O5 1.710(3) . ? Mo2 O3 1.905(3) . ? Mo2 O6 1.978(3) . ? Mo2 O11 2.173(3) 1_565 ? Mo2 O12 2.310(3) 7_566 ? Ni1 O8 2.019(3) . ? Ni1 N2 2.050(3) . ? Ni1 O10 2.051(3) . ? Ni1 O9 2.106(3) . ? Ni1 N3 2.111(4) . ? Ni1 N1 2.133(4) . ? P1 O8 1.517(3) . ? P1 O6 1.542(3) . ? P1 O7 1.544(3) . ? P1 C13 1.794(4) . ? P2 O13 1.528(3) . ? P2 O11 1.528(3) . ? P2 O12 1.544(3) . ? P2 C20 1.806(4) . ? O7 Mo1 1.999(3) 7_576 ? O9 H9C 0.85(2) . ? O9 H9D 0.84(2) . ? O10 H10C 0.82(2) . ? O10 H10D 0.83(2) . ? O11 Mo2 2.173(3) 1_545 ? O12 Mo2 2.310(3) 7_566 ? O12 Mo1 2.465(3) 7_566 ? O13 Mo1 2.128(3) 1_545 ? O91 H91A 0.85(2) . ? O91 H91B 0.86(2) . ? N1 C1 1.332(5) . ? N1 C5 1.370(5) . ? N2 C6 1.342(5) . ? N2 C7 1.342(5) . ? N3 C12 1.350(5) . ? N3 C8 1.368(5) . ? C1 C2 1.398(6) . ? C1 H1 0.9500 . ? C2 C3 1.373(6) . ? C2 H2 0.9500 . ? C3 C4 1.391(6) . ? C3 H3 0.9500 . ? C4 C5 1.385(6) . ? C4 H4 0.9500 . ? C5 C6 1.481(6) . ? C6 C6 1.389(8) 2_655 ? C7 C7 1.423(8) 2_655 ? C7 C8 1.483(6) . ? C8 C9 1.383(6) . ? C9 C10 1.401(6) . ? C9 H9 0.9500 . ? C10 C11 1.382(6) . ? C10 H10 0.9500 . ? C11 C12 1.378(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.523(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.377(6) . ? C14 C16 1.399(6) . ? C15 C17 1.390(6) . ? C15 H15 0.9500 . ? C16 C18 1.382(6) . ? C16 H16 0.9500 . ? C17 C19 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.401(6) . ? C18 H18 0.9500 . ? C19 C20 1.507(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O1 104.51(14) . . ? O2 Mo1 O3 99.41(14) . . ? O1 Mo1 O3 98.07(13) . . ? O2 Mo1 O7 98.87(13) . 7_576 ? O1 Mo1 O7 89.49(13) . 7_576 ? O3 Mo1 O7 157.76(12) . 7_576 ? O2 Mo1 O13 96.08(13) . 1_565 ? O1 Mo1 O13 158.43(13) . 1_565 ? O3 Mo1 O13 84.62(12) . 1_565 ? O7 Mo1 O13 80.94(11) 7_576 1_565 ? O2 Mo1 O12 168.90(12) . 7_566 ? O1 Mo1 O12 83.96(12) . 7_566 ? O3 Mo1 O12 71.93(11) . 7_566 ? O7 Mo1 O12 88.23(11) 7_576 7_566 ? O13 Mo1 O12 76.52(10) 1_565 7_566 ? O4 Mo2 O5 102.96(14) . . ? O4 Mo2 O3 97.67(13) . . ? O5 Mo2 O3 98.48(13) . . ? O4 Mo2 O6 93.33(13) . . ? O5 Mo2 O6 95.92(13) . . ? O3 Mo2 O6 159.42(12) . . ? O4 Mo2 O11 165.47(12) . 1_565 ? O5 Mo2 O11 91.13(13) . 1_565 ? O3 Mo2 O11 83.57(12) . 1_565 ? O6 Mo2 O11 81.51(11) . 1_565 ? O4 Mo2 O12 90.23(12) . 7_566 ? O5 Mo2 O12 166.29(13) . 7_566 ? O3 Mo2 O12 75.74(11) . 7_566 ? O6 Mo2 O12 86.91(11) . 7_566 ? O11 Mo2 O12 75.98(10) 1_565 7_566 ? O8 Ni1 N2 171.20(13) . . ? O8 Ni1 O10 90.21(12) . . ? N2 Ni1 O10 98.12(12) . . ? O8 Ni1 O9 84.78(12) . . ? N2 Ni1 O9 87.31(13) . . ? O10 Ni1 O9 171.09(13) . . ? O8 Ni1 N3 99.29(13) . . ? N2 Ni1 N3 76.95(14) . . ? O10 Ni1 N3 97.18(13) . . ? O9 Ni1 N3 90.91(13) . . ? O8 Ni1 N1 106.00(13) . . ? N2 Ni1 N1 77.79(14) . . ? O10 Ni1 N1 84.52(13) . . ? O9 Ni1 N1 89.77(13) . . ? N3 Ni1 N1 154.66(13) . . ? O8 P1 O6 111.62(16) . . ? O8 P1 O7 110.30(16) . . ? O6 P1 O7 110.19(16) . . ? O8 P1 C13 113.21(19) . . ? O6 P1 C13 103.78(18) . . ? O7 P1 C13 107.49(18) . . ? O13 P2 O11 111.63(16) . . ? O13 P2 O12 112.09(16) . . ? O11 P2 O12 112.23(16) . . ? O13 P2 C20 108.35(18) . . ? O11 P2 C20 103.87(17) . . ? O12 P2 C20 108.21(18) . . ? Mo2 O3 Mo1 123.14(15) . . ? P1 O6 Mo2 144.89(18) . . ? P1 O7 Mo1 139.54(18) . 7_576 ? P1 O8 Ni1 137.19(18) . . ? Ni1 O9 H9C 119(4) . . ? Ni1 O9 H9D 123(4) . . ? H9C O9 H9D 89(5) . . ? Ni1 O10 H10C 110(4) . . ? Ni1 O10 H10D 108(4) . . ? H10C O10 H10D 110(5) . . ? P2 O11 Mo2 130.26(16) . 1_545 ? P2 O12 Mo2 137.04(17) . 7_566 ? P2 O12 Mo1 133.00(16) . 7_566 ? Mo2 O12 Mo1 89.19(9) 7_566 7_566 ? P2 O13 Mo1 130.80(17) . 1_545 ? H91A O91 H91B 102(6) . . ? C1 N1 C5 118.2(4) . . ? C1 N1 Ni1 127.3(3) . . ? C5 N1 Ni1 113.5(3) . . ? C6 N2 C7 123.3(4) . . ? C6 N2 Ni1 116.9(3) . . ? C7 N2 Ni1 118.7(3) . . ? C12 N3 C8 117.0(4) . . ? C12 N3 Ni1 126.4(3) . . ? C8 N3 Ni1 115.6(3) . . ? N1 C1 C2 122.5(4) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 119.3(4) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? N1 C5 C4 122.0(4) . . ? N1 C5 C6 114.6(4) . . ? C4 C5 C6 123.3(4) . . ? N2 C6 C6 117.4(2) . 2_655 ? N2 C6 C5 113.8(4) . . ? C6 C6 C5 128.8(2) 2_655 . ? N2 C7 C7 116.4(2) . 2_655 ? N2 C7 C8 114.2(3) . . ? C7 C7 C8 129.3(2) 2_655 . ? N3 C8 C9 122.3(4) . . ? N3 C8 C7 113.6(4) . . ? C9 C8 C7 123.8(4) . . ? C8 C9 C10 119.3(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 118.2(4) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 119.4(4) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? N3 C12 C11 123.5(4) . . ? N3 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C14 C13 P1 115.8(3) . . ? C14 C13 H13A 108.3 . . ? P1 C13 H13A 108.3 . . ? C14 C13 H13B 108.3 . . ? P1 C13 H13B 108.3 . . ? H13A C13 H13B 107.4 . . ? C15 C14 C16 118.4(4) . . ? C15 C14 C13 119.3(4) . . ? C16 C14 C13 122.3(4) . . ? C14 C15 C17 121.4(4) . . ? C14 C15 H15 119.3 . . ? C17 C15 H15 119.3 . . ? C18 C16 C14 120.3(4) . . ? C18 C16 H16 119.9 . . ? C14 C16 H16 119.9 . . ? C19 C17 C15 120.7(4) . . ? C19 C17 H17 119.6 . . ? C15 C17 H17 119.6 . . ? C16 C18 C19 121.4(4) . . ? C16 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C17 C19 C18 117.7(4) . . ? C17 C19 C20 121.1(4) . . ? C18 C19 C20 121.1(4) . . ? C19 C20 P2 116.1(3) . . ? C19 C20 H20A 108.3 . . ? P2 C20 H20A 108.3 . . ? C19 C20 H20B 108.3 . . ? P2 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? 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 O8 P1 O6 Mo2 63.2(3) . . . . ? O7 P1 O6 Mo2 -59.7(3) . . . . ? C13 P1 O6 Mo2 -174.5(3) . . . . ? O8 P1 O7 Mo1 167.6(2) . . . 7_576 ? O6 P1 O7 Mo1 -68.7(3) . . . 7_576 ? C13 P1 O7 Mo1 43.8(3) . . . 7_576 ? O6 P1 O8 Ni1 -171.4(2) . . . . ? O7 P1 O8 Ni1 -48.6(3) . . . . ? C13 P1 O8 Ni1 71.9(3) . . . . ? O13 P2 O11 Mo2 36.0(3) . . . 1_545 ? O12 P2 O11 Mo2 -90.8(2) . . . 1_545 ? C20 P2 O11 Mo2 152.5(2) . . . 1_545 ? O13 P2 O12 Mo2 20.4(3) . . . 7_566 ? O11 P2 O12 Mo2 147.0(2) . . . 7_566 ? C20 P2 O12 Mo2 -99.0(3) . . . 7_566 ? O13 P2 O12 Mo1 -146.26(19) . . . 7_566 ? O11 P2 O12 Mo1 -19.7(3) . . . 7_566 ? C20 P2 O12 Mo1 94.3(2) . . . 7_566 ? O11 P2 O13 Mo1 -36.0(3) . . . 1_545 ? O12 P2 O13 Mo1 90.9(2) . . . 1_545 ? C20 P2 O13 Mo1 -149.8(2) . . . 1_545 ? C5 N1 C1 C2 -1.1(6) . . . . ? Ni1 N1 C1 C2 -168.7(3) . . . . ? N1 C1 C2 C3 3.7(6) . . . . ? C1 C2 C3 C4 -2.3(6) . . . . ? C2 C3 C4 C5 -1.6(6) . . . . ? C1 N1 C5 C4 -3.0(6) . . . . ? Ni1 N1 C5 C4 166.3(3) . . . . ? C1 N1 C5 C6 -179.0(4) . . . . ? Ni1 N1 C5 C6 -9.7(4) . . . . ? C3 C4 C5 N1 4.3(6) . . . . ? C3 C4 C5 C6 180.0(4) . . . . ? C7 N2 C6 C6 -9.9(7) . . . 2_655 ? Ni1 N2 C6 C6 158.1(4) . . . 2_655 ? C7 N2 C6 C5 171.4(4) . . . . ? Ni1 N2 C6 C5 -20.7(4) . . . . ? N1 C5 C6 N2 19.8(5) . . . . ? C4 C5 C6 N2 -156.2(4) . . . . ? N1 C5 C6 C6 -158.8(5) . . . 2_655 ? C4 C5 C6 C6 25.3(8) . . . 2_655 ? C6 N2 C7 C7 -11.9(7) . . . 2_655 ? Ni1 N2 C7 C7 -179.7(4) . . . 2_655 ? C6 N2 C7 C8 163.9(4) . . . . ? Ni1 N2 C7 C8 -3.9(4) . . . . ? C12 N3 C8 C9 -5.4(6) . . . . ? Ni1 N3 C8 C9 163.7(3) . . . . ? C12 N3 C8 C7 -179.9(3) . . . . ? Ni1 N3 C8 C7 -10.8(4) . . . . ? N2 C7 C8 N3 9.6(5) . . . . ? C7 C7 C8 N3 -175.3(5) 2_655 . . . ? N2 C7 C8 C9 -164.8(4) . . . . ? C7 C7 C8 C9 10.3(8) 2_655 . . . ? N3 C8 C9 C10 5.8(6) . . . . ? C7 C8 C9 C10 179.7(4) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C12 -4.0(6) . . . . ? C8 N3 C12 C11 0.2(6) . . . . ? Ni1 N3 C12 C11 -167.6(3) . . . . ? C10 C11 C12 N3 4.6(7) . . . . ? O8 P1 C13 C14 51.1(4) . . . . ? O6 P1 C13 C14 -70.1(3) . . . . ? O7 P1 C13 C14 173.2(3) . . . . ? P1 C13 C14 C15 -132.1(3) . . . . ? P1 C13 C14 C16 47.9(5) . . . . ? C16 C14 C15 C17 -2.7(6) . . . . ? C13 C14 C15 C17 177.3(4) . . . . ? C15 C14 C16 C18 2.4(6) . . . . ? C13 C14 C16 C18 -177.6(4) . . . . ? C14 C15 C17 C19 0.3(6) . . . . ? C14 C16 C18 C19 0.1(6) . . . . ? C15 C17 C19 C18 2.2(6) . . . . ? C15 C17 C19 C20 -176.4(4) . . . . ? C16 C18 C19 C17 -2.4(6) . . . . ? C16 C18 C19 C20 176.2(4) . . . . ? C17 C19 C20 P2 -98.3(4) . . . . ? C18 C19 C20 P2 83.1(4) . . . . ? O13 P2 C20 C19 -65.7(3) . . . . ? O11 P2 C20 C19 175.5(3) . . . . ? O12 P2 C20 C19 56.0(3) . . . . ? _refine_diff_density_max 2.114 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.187 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957898' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound11 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 Mo5 N6 Ni2 O23 P2, 2(H2 O)' _chemical_formula_sum 'C28 H34 Mo5 N6 Ni2 O25 P2' _chemical_formula_weight 1513.67 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' Ni Ni 0.3393 1.1124 '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' _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 2/c' _space_group_name_Hall '-C 2yc' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.3753(12) _cell_length_b 11.3661(8) _cell_length_c 22.3579(15) _cell_angle_alpha 90 _cell_angle_beta 103.1180(10) _cell_angle_gamma 90 _cell_volume 4300.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 662 _cell_measurement_theta_min 2.3837 _cell_measurement_theta_max 24.4849 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_density_meas 2.36(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.338 _exptl_crystal_F_000 2960 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.209 _exptl_crystal_size_mid 0.101 _exptl_crystal_size_min 0.068 _exptl_absorpt_coefficient_mu 2.440 _shelx_estimated_absorpt_T_min 0.630 _shelx_estimated_absorpt_T_max 0.852 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.76 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33502 _diffrn_reflns_av_unetI/netI 0.0381 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.870 _diffrn_reflns_theta_max 26.369 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 4381 _reflns_number_gt 3679 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+17.3963P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4381 _refine_ls_number_parameters 317 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.39635(2) 0.42202(3) 0.70708(2) 0.00753(9) Uani 1 1 d . U . . . Mo2 Mo 0.35739(2) 0.70639(3) 0.66782(2) 0.00662(9) Uani 1 1 d . U . . . Mo3 Mo 0.5000 0.87807(4) 0.7500 0.00847(11) Uani 1 2 d S TU P . . Ni1 Ni 0.19148(3) 0.90381(5) 0.67989(2) 0.00937(12) Uani 1 1 d . U . . . P1 P 0.04754(6) 1.11857(9) 0.67987(5) 0.0067(2) Uani 1 1 d . U . . . O1 O 0.5000 0.3785(3) 0.7500 0.0090(8) Uani 1 2 d S TU P . . O2 O 0.39153(17) 0.3588(2) 0.63794(13) 0.0122(6) Uani 1 1 d . U . . . O3 O 0.33670(16) 0.3303(3) 0.73937(13) 0.0111(6) Uani 1 1 d . U . . . O4 O 0.32306(15) 0.5516(2) 0.68583(12) 0.0079(6) Uani 1 1 d . U . . . O5 O 0.33608(16) 0.7009(3) 0.58966(12) 0.0123(6) Uani 1 1 d . U . . . O6 O 0.43634(16) 0.8248(2) 0.67418(12) 0.0089(6) Uani 1 1 d . U . . . O7 O 0.56439(17) 0.9700(3) 0.72573(14) 0.0151(6) Uani 1 1 d . U . . . O8 O 0.28043(16) 0.7856(2) 0.68478(12) 0.0111(6) Uani 1 1 d . U . . . O9 O 0.27095(17) 1.0102(3) 0.73826(14) 0.0153(7) Uani 1 1 d D U . . . H9C H 0.3190(12) 0.999(4) 0.747(2) 0.018 Uiso 1 1 d D U . . . H9D H 0.259(3) 1.030(4) 0.7707(14) 0.018 Uiso 1 1 d D U . . . O10 O 0.09931(15) 1.0105(2) 0.69591(12) 0.0077(6) Uani 1 1 d . U . . . O11 O 0.07622(15) 1.2179(2) 0.72595(12) 0.0082(6) Uani 1 1 d . U . . . O12 O -0.03913(15) 1.0843(2) 0.68083(12) 0.0080(6) Uani 1 1 d . U . . . O90 O 0.3391(10) 0.0844(16) 0.3800(7) 0.306(8) Uani 1 1 d . . . . . N1 N 0.2212(2) 0.9859(3) 0.60692(15) 0.0109(7) Uani 1 1 d . U . . . N2 N 0.1796(2) 0.8239(3) 0.54005(16) 0.0130(7) Uani 1 1 d D U . . . H2' H 0.177(3) 0.805(4) 0.5018(11) 0.016 Uiso 1 1 d D U . . . N3 N 0.1159(2) 0.7933(3) 0.62235(16) 0.0126(7) Uani 1 1 d . U . . . C1 C 0.2556(2) 1.0940(4) 0.6142(2) 0.0155(9) Uani 1 1 d . U . . . H1 H 0.2567 1.1353 0.6513 0.019 Uiso 1 1 calc R U . . . C2 C 0.2886(3) 1.1464(4) 0.5712(2) 0.0190(10) Uani 1 1 d . U . . . H2 H 0.3106 1.2232 0.5778 0.023 Uiso 1 1 calc R U . . . C3 C 0.2896(3) 1.0855(4) 0.5174(2) 0.0191(10) Uani 1 1 d . U . . . H3 H 0.3137 1.1188 0.4873 0.023 Uiso 1 1 calc R U . . . C4 C 0.2552(3) 0.9773(4) 0.5086(2) 0.0158(9) Uani 1 1 d . U . . . H4 H 0.2560 0.9336 0.4726 0.019 Uiso 1 1 calc R U . . . C5 C 0.2188(2) 0.9310(4) 0.55338(19) 0.0119(8) Uani 1 1 d . U . . . C6 C 0.1230(2) 0.7695(4) 0.56482(19) 0.0118(8) Uani 1 1 d . U . . . C7 C 0.0744(3) 0.6867(4) 0.5279(2) 0.0144(9) Uani 1 1 d . U . . . H7 H 0.0814 0.6691 0.4879 0.017 Uiso 1 1 calc R U . . . C8 C 0.0166(3) 0.6313(4) 0.5502(2) 0.0176(10) Uani 1 1 d . U . . . H8 H -0.0177 0.5763 0.5254 0.021 Uiso 1 1 calc R U . . . C9 C 0.0084(3) 0.6560(4) 0.6088(2) 0.0189(10) Uani 1 1 d . U . . . H9 H -0.0314 0.6187 0.6250 0.023 Uiso 1 1 calc R U . . . C10 C 0.0593(3) 0.7358(4) 0.6431(2) 0.0161(9) Uani 1 1 d . U . . . H10 H 0.0543 0.7514 0.6838 0.019 Uiso 1 1 calc R U . . . C11 C 0.0464(2) 1.1678(4) 0.60291(17) 0.0103(8) Uani 1 1 d . U . . . H11A H 0.0100 1.2358 0.5938 0.012 Uiso 1 1 calc R U . . . H11B H 0.0999 1.1970 0.6025 0.012 Uiso 1 1 calc R U . . . C12 C 0.0224(2) 1.0793(4) 0.55058(17) 0.0114(8) Uani 1 1 d . U . . . C13 C 0.0630(2) 1.0748(4) 0.50367(18) 0.0107(8) Uani 1 1 d . U . . . H13 H 0.1066 1.1260 0.5053 0.013 Uiso 1 1 calc R U . . . C14 C 0.0415(2) 0.9975(4) 0.45441(18) 0.0118(9) Uani 1 1 d . U . . . H14 H 0.0710 0.9970 0.4235 0.014 Uiso 1 1 calc R 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 Mo1 0.00614(17) 0.00815(18) 0.00789(17) -0.00136(14) 0.00072(13) -0.00053(14) Mo2 0.00490(17) 0.00900(18) 0.00579(16) -0.00007(14) 0.00083(13) 0.00146(14) Mo3 0.0060(2) 0.0076(2) 0.0110(2) 0.000 0.00035(19) 0.000 Ni1 0.0073(3) 0.0109(3) 0.0097(3) -0.0013(2) 0.0015(2) 0.0012(2) P1 0.0053(5) 0.0095(5) 0.0051(5) -0.0001(4) 0.0012(4) 0.0011(4) O1 0.0059(19) 0.009(2) 0.012(2) 0.000 0.0011(16) 0.000 O2 0.0138(15) 0.0106(15) 0.0116(14) -0.0042(12) 0.0015(12) -0.0017(12) O3 0.0087(14) 0.0121(15) 0.0123(14) 0.0003(12) 0.0022(12) -0.0010(12) O4 0.0043(13) 0.0089(14) 0.0099(14) 0.0003(11) 0.0004(11) -0.0009(11) O5 0.0135(15) 0.0170(16) 0.0053(13) -0.0010(12) -0.0004(11) -0.0003(13) O6 0.0077(14) 0.0088(14) 0.0100(14) 0.0027(11) 0.0014(11) 0.0006(11) O7 0.0102(15) 0.0124(15) 0.0211(16) 0.0051(13) -0.0002(13) -0.0019(12) O8 0.0084(14) 0.0127(15) 0.0127(14) -0.0026(12) 0.0036(12) 0.0021(12) O9 0.0090(15) 0.0223(17) 0.0148(16) -0.0052(13) 0.0033(13) 0.0008(14) O10 0.0055(13) 0.0099(14) 0.0072(13) 0.0008(11) 0.0003(11) 0.0020(11) O11 0.0070(14) 0.0081(14) 0.0106(14) 0.0017(11) 0.0042(11) 0.0008(11) O12 0.0058(13) 0.0099(14) 0.0082(13) 0.0004(11) 0.0012(11) 0.0011(11) O90 0.296(18) 0.34(2) 0.272(17) -0.111(16) 0.050(14) -0.054(16) N1 0.0076(17) 0.0124(18) 0.0114(17) -0.0011(14) -0.0003(14) 0.0017(14) N2 0.0167(19) 0.0132(19) 0.0092(17) -0.0025(15) 0.0034(15) 0.0003(15) N3 0.0100(17) 0.0124(18) 0.0148(18) -0.0036(15) 0.0013(14) 0.0020(14) C1 0.010(2) 0.017(2) 0.017(2) -0.0015(18) -0.0021(17) 0.0002(18) C2 0.017(2) 0.019(2) 0.020(2) -0.0021(19) 0.0012(19) -0.0081(19) C3 0.016(2) 0.026(3) 0.018(2) 0.003(2) 0.0074(19) -0.002(2) C4 0.016(2) 0.020(2) 0.012(2) -0.0034(18) 0.0044(18) 0.0012(19) C5 0.007(2) 0.012(2) 0.014(2) 0.0012(17) -0.0013(16) 0.0016(16) C6 0.009(2) 0.009(2) 0.015(2) 0.0032(16) -0.0013(17) 0.0045(16) C7 0.015(2) 0.013(2) 0.015(2) -0.0001(17) 0.0043(18) 0.0029(17) C8 0.015(2) 0.009(2) 0.027(2) -0.0071(19) 0.0012(19) -0.0006(18) C9 0.013(2) 0.019(2) 0.025(2) -0.002(2) 0.0059(19) -0.0029(18) C10 0.014(2) 0.015(2) 0.020(2) -0.0008(18) 0.0034(18) -0.0009(18) C11 0.012(2) 0.013(2) 0.0067(18) 0.0034(16) 0.0025(16) 0.0019(17) C12 0.012(2) 0.016(2) 0.0057(18) 0.0018(16) 0.0005(16) 0.0052(18) C13 0.008(2) 0.013(2) 0.0105(19) 0.0030(17) -0.0008(16) 0.0003(17) C14 0.014(2) 0.016(2) 0.007(2) -0.0003(16) 0.0051(17) 0.0040(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O2 1.689(3) . ? Mo1 O3 1.738(3) . ? Mo1 O1 1.9036(11) . ? Mo1 O4 1.935(3) . ? Mo1 O12 2.303(3) 3_545 ? Mo1 O10 2.376(3) 4_546 ? Mo2 O5 1.703(3) . ? Mo2 O8 1.724(3) . ? Mo2 O6 1.904(3) . ? Mo2 O4 1.929(3) . ? Mo2 O12 2.237(3) 3_545 ? Mo2 O11 2.397(3) 4_546 ? Mo3 O7 1.707(3) . ? Mo3 O7 1.707(3) 2_656 ? Mo3 O6 1.901(3) . ? Mo3 O6 1.901(3) 2_656 ? Mo3 O11 2.383(3) 4_546 ? Mo3 O11 2.383(3) 3_545 ? Ni1 O8 2.032(3) . ? Ni1 N1 2.045(3) . ? Ni1 N3 2.048(4) . ? Ni1 O9 2.062(3) . ? Ni1 O10 2.104(3) . ? Ni1 O3 2.144(3) 4_556 ? P1 O10 1.516(3) . ? P1 O11 1.534(3) . ? P1 O12 1.560(3) . ? P1 C11 1.805(4) . ? O1 Mo1 1.9036(11) 2_656 ? O3 Ni1 2.144(3) 4_546 ? O9 H9C 0.824(19) . ? O9 H9D 0.828(19) . ? O10 Mo1 2.376(3) 4_556 ? O11 Mo3 2.383(3) 3_455 ? O11 Mo2 2.397(3) 4_556 ? O12 Mo2 2.237(3) 3_455 ? O12 Mo1 2.303(3) 3_455 ? N1 C5 1.342(5) . ? N1 C1 1.360(6) . ? N2 C6 1.380(5) . ? N2 C5 1.393(5) . ? N2 H2' 0.872(19) . ? N3 C6 1.347(5) . ? N3 C10 1.348(5) . ? C1 C2 1.364(6) . ? C1 H1 0.9500 . ? C2 C3 1.391(6) . ? C2 H2 0.9500 . ? C3 C4 1.362(6) . ? C3 H3 0.9500 . ? C4 C5 1.402(6) . ? C4 H4 0.9500 . ? C6 C7 1.402(6) . ? C7 C8 1.372(6) . ? C7 H7 0.9500 . ? C8 C9 1.378(6) . ? C8 H8 0.9500 . ? C9 C10 1.373(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.528(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.391(5) . ? C12 C14 1.397(6) 5_576 ? C13 C14 1.392(6) . ? C13 H13 0.9500 . ? C14 C12 1.397(6) 5_576 ? C14 H14 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O3 102.39(13) . . ? O2 Mo1 O1 101.28(11) . . ? O3 Mo1 O1 102.71(12) . . ? O2 Mo1 O4 101.88(13) . . ? O3 Mo1 O4 97.89(12) . . ? O1 Mo1 O4 144.70(14) . . ? O2 Mo1 O12 91.91(12) . 3_545 ? O3 Mo1 O12 163.12(11) . 3_545 ? O1 Mo1 O12 82.93(12) . 3_545 ? O4 Mo1 O12 70.05(10) . 3_545 ? O2 Mo1 O10 178.99(12) . 4_546 ? O3 Mo1 O10 76.89(11) . 4_546 ? O1 Mo1 O10 79.60(9) . 4_546 ? O4 Mo1 O10 77.56(10) . 4_546 ? O12 Mo1 O10 88.69(9) 3_545 4_546 ? O5 Mo2 O8 104.24(13) . . ? O5 Mo2 O6 95.04(13) . . ? O8 Mo2 O6 101.29(13) . . ? O5 Mo2 O4 100.09(13) . . ? O8 Mo2 O4 97.95(12) . . ? O6 Mo2 O4 151.74(11) . . ? O5 Mo2 O12 95.27(12) . 3_545 ? O8 Mo2 O12 159.36(11) . 3_545 ? O6 Mo2 O12 83.38(11) . 3_545 ? O4 Mo2 O12 71.63(10) . 3_545 ? O5 Mo2 O11 164.22(11) . 4_546 ? O8 Mo2 O11 88.64(11) . 4_546 ? O6 Mo2 O11 73.19(10) . 4_546 ? O4 Mo2 O11 86.85(10) . 4_546 ? O12 Mo2 O11 73.34(9) 3_545 4_546 ? O7 Mo3 O7 104.5(2) . 2_656 ? O7 Mo3 O6 101.67(13) . . ? O7 Mo3 O6 100.82(13) 2_656 . ? O7 Mo3 O6 100.82(13) . 2_656 ? O7 Mo3 O6 101.67(13) 2_656 2_656 ? O6 Mo3 O6 142.87(17) . 2_656 ? O7 Mo3 O11 167.75(12) . 4_546 ? O7 Mo3 O11 87.60(12) 2_656 4_546 ? O6 Mo3 O11 73.58(10) . 4_546 ? O6 Mo3 O11 78.25(11) 2_656 4_546 ? O7 Mo3 O11 87.60(12) . 3_545 ? O7 Mo3 O11 167.75(12) 2_656 3_545 ? O6 Mo3 O11 78.25(11) . 3_545 ? O6 Mo3 O11 73.58(10) 2_656 3_545 ? O11 Mo3 O11 80.41(13) 4_546 3_545 ? O8 Ni1 N1 91.01(12) . . ? O8 Ni1 N3 89.99(13) . . ? N1 Ni1 N3 91.19(14) . . ? O8 Ni1 O9 87.81(12) . . ? N1 Ni1 O9 89.04(13) . . ? N3 Ni1 O9 177.79(13) . . ? O8 Ni1 O10 166.24(11) . . ? N1 Ni1 O10 102.29(12) . . ? N3 Ni1 O10 93.22(12) . . ? O9 Ni1 O10 88.88(11) . . ? O8 Ni1 O3 90.77(11) . 4_556 ? N1 Ni1 O3 175.39(13) . 4_556 ? N3 Ni1 O3 93.06(12) . 4_556 ? O9 Ni1 O3 86.78(12) . 4_556 ? O10 Ni1 O3 75.71(10) . 4_556 ? O10 P1 O11 110.64(16) . . ? O10 P1 O12 108.49(16) . . ? O11 P1 O12 110.00(15) . . ? O10 P1 C11 110.76(17) . . ? O11 P1 C11 110.10(18) . . ? O12 P1 C11 106.76(17) . . ? Mo1 O1 Mo1 149.9(2) 2_656 . ? Mo1 O3 Ni1 112.80(14) . 4_546 ? Mo2 O4 Mo1 121.88(13) . . ? Mo3 O6 Mo2 123.73(14) . . ? Mo2 O8 Ni1 162.15(17) . . ? Ni1 O9 H9C 124(3) . . ? Ni1 O9 H9D 117(3) . . ? H9C O9 H9D 106(5) . . ? P1 O10 Ni1 149.36(17) . . ? P1 O10 Mo1 116.93(14) . 4_556 ? Ni1 O10 Mo1 92.50(10) . 4_556 ? P1 O11 Mo3 126.98(15) . 3_455 ? P1 O11 Mo2 129.44(15) . 4_556 ? Mo3 O11 Mo2 89.16(9) 3_455 4_556 ? P1 O12 Mo2 126.37(16) . 3_455 ? P1 O12 Mo1 136.94(16) . 3_455 ? Mo2 O12 Mo1 96.12(10) 3_455 3_455 ? C5 N1 C1 116.8(4) . . ? C5 N1 Ni1 122.5(3) . . ? C1 N1 Ni1 120.0(3) . . ? C6 N2 C5 131.6(4) . . ? C6 N2 H2' 113(3) . . ? C5 N2 H2' 110(3) . . ? C6 N3 C10 117.7(4) . . ? C6 N3 Ni1 122.5(3) . . ? C10 N3 Ni1 119.7(3) . . ? N1 C1 C2 123.6(4) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C1 C2 C3 118.8(4) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? N1 C5 N2 120.8(4) . . ? N1 C5 C4 122.3(4) . . ? N2 C5 C4 116.9(4) . . ? N3 C6 N2 121.4(4) . . ? N3 C6 C7 121.6(4) . . ? N2 C6 C7 117.0(4) . . ? C8 C7 C6 119.1(4) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C7 C8 C9 119.7(4) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C10 C9 C8 118.2(4) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? N3 C10 C9 123.7(4) . . ? N3 C10 H10 118.1 . . ? C9 C10 H10 118.1 . . ? C12 C11 P1 117.9(3) . . ? C12 C11 H11A 107.8 . . ? P1 C11 H11A 107.8 . . ? C12 C11 H11B 107.8 . . ? P1 C11 H11B 107.8 . . ? H11A C11 H11B 107.2 . . ? C13 C12 C14 116.5(4) . 5_576 ? C13 C12 C11 120.3(4) . . ? C14 C12 C11 123.1(3) 5_576 . ? C12 C13 C14 122.0(4) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C13 C14 C12 121.5(4) . 5_576 ? C13 C14 H14 119.2 . . ? C12 C14 H14 119.2 5_576 . ? 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 O2 Mo1 O3 Ni1 -167.65(14) . . . 4_546 ? O1 Mo1 O3 Ni1 87.59(15) . . . 4_546 ? O4 Mo1 O3 Ni1 -63.57(15) . . . 4_546 ? O12 Mo1 O3 Ni1 -20.4(5) 3_545 . . 4_546 ? O10 Mo1 O3 Ni1 11.63(12) 4_546 . . 4_546 ? O5 Mo2 O8 Ni1 -32.5(6) . . . . ? O6 Mo2 O8 Ni1 65.7(6) . . . . ? O4 Mo2 O8 Ni1 -135.1(6) . . . . ? O12 Mo2 O8 Ni1 167.1(4) 3_545 . . . ? O11 Mo2 O8 Ni1 138.3(6) 4_546 . . . ? O11 P1 O10 Ni1 -101.1(3) . . . . ? O12 P1 O10 Ni1 138.1(3) . . . . ? C11 P1 O10 Ni1 21.3(4) . . . . ? O11 P1 O10 Mo1 61.41(19) . . . 4_556 ? O12 P1 O10 Mo1 -59.34(19) . . . 4_556 ? C11 P1 O10 Mo1 -176.21(17) . . . 4_556 ? O10 P1 O11 Mo3 -156.07(16) . . . 3_455 ? O12 P1 O11 Mo3 -36.2(2) . . . 3_455 ? C11 P1 O11 Mo3 81.2(2) . . . 3_455 ? O10 P1 O11 Mo2 -29.5(2) . . . 4_556 ? O12 P1 O11 Mo2 90.3(2) . . . 4_556 ? C11 P1 O11 Mo2 -152.27(19) . . . 4_556 ? O10 P1 O12 Mo2 175.30(16) . . . 3_455 ? O11 P1 O12 Mo2 54.1(2) . . . 3_455 ? C11 P1 O12 Mo2 -65.3(2) . . . 3_455 ? O10 P1 O12 Mo1 6.1(3) . . . 3_455 ? O11 P1 O12 Mo1 -115.0(2) . . . 3_455 ? C11 P1 O12 Mo1 125.5(2) . . . 3_455 ? C5 N1 C1 C2 -1.7(6) . . . . ? Ni1 N1 C1 C2 169.1(3) . . . . ? N1 C1 C2 C3 -1.9(7) . . . . ? C1 C2 C3 C4 2.1(7) . . . . ? C2 C3 C4 C5 1.1(7) . . . . ? C1 N1 C5 N2 -175.2(4) . . . . ? Ni1 N1 C5 N2 14.3(5) . . . . ? C1 N1 C5 C4 5.0(6) . . . . ? Ni1 N1 C5 C4 -165.5(3) . . . . ? C6 N2 C5 N1 18.7(7) . . . . ? C6 N2 C5 C4 -161.5(4) . . . . ? C3 C4 C5 N1 -4.8(7) . . . . ? C3 C4 C5 N2 175.4(4) . . . . ? C10 N3 C6 N2 -179.7(4) . . . . ? Ni1 N3 C6 N2 -3.7(5) . . . . ? C10 N3 C6 C7 -1.0(6) . . . . ? Ni1 N3 C6 C7 175.0(3) . . . . ? C5 N2 C6 N3 -24.7(7) . . . . ? C5 N2 C6 C7 156.5(4) . . . . ? N3 C6 C7 C8 2.1(6) . . . . ? N2 C6 C7 C8 -179.1(4) . . . . ? C6 C7 C8 C9 -1.4(7) . . . . ? C7 C8 C9 C10 -0.2(7) . . . . ? C6 N3 C10 C9 -0.7(6) . . . . ? Ni1 N3 C10 C9 -176.9(3) . . . . ? C8 C9 C10 N3 1.3(7) . . . . ? O10 P1 C11 C12 55.0(4) . . . . ? O11 P1 C11 C12 177.7(3) . . . . ? O12 P1 C11 C12 -62.9(3) . . . . ? P1 C11 C12 C13 -138.7(3) . . . . ? P1 C11 C12 C14 43.5(5) . . . 5_576 ? C14 C12 C13 C14 -0.3(7) 5_576 . . . ? C11 C12 C13 C14 -178.3(4) . . . . ? C12 C13 C14 C12 0.4(7) . . . 5_576 ? _refine_diff_density_max 1.561 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.130 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957899' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound12 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H33 Cu2 F3 Mo2 N4 O15 P2, H2 O' _chemical_formula_sum 'C32 H35 Cu2 F3 Mo2 N4 O16 P2' _chemical_formula_weight 1169.54 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' 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' F F 0.0171 0.0103 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9305(12) _cell_length_b 12.2497(14) _cell_length_c 16.2618(18) _cell_angle_alpha 85.669(2) _cell_angle_beta 76.269(2) _cell_angle_gamma 66.823(2) _cell_volume 1944.1(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_density_meas 1.99(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 1.998 _exptl_crystal_F_000 1164 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.206 _exptl_crystal_size_mid 0.137 _exptl_crystal_size_min 0.095 _exptl_absorpt_coefficient_mu 1.885 _shelx_estimated_absorpt_T_min 0.697 _shelx_estimated_absorpt_T_max 0.841 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.84 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23327 _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.081 _diffrn_reflns_theta_max 28.078 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 9391 _reflns_number_gt 7374 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0829P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9391 _refine_ls_number_parameters 580 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.1279 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.56915(3) 1.20034(3) 0.92401(2) 0.01328(9) Uani 1 1 d . . . . . Mo2 Mo 0.81760(3) 0.78912(3) 0.52914(2) 0.01975(10) Uani 1 1 d . . . . . Cu1 Cu 0.55088(4) 1.20194(4) 0.68758(3) 0.01354(11) Uani 1 1 d . . . . . Cu2 Cu 0.83247(4) 0.79359(4) 0.79035(3) 0.01228(11) Uani 1 1 d . . . . . P1 P 0.81963(9) 1.05493(8) 0.75925(6) 0.01085(18) Uani 1 1 d . . . . . P2 P 0.57877(9) 0.93440(8) 0.70170(6) 0.01169(18) Uani 1 1 d . . . . . F1 F 0.5921(2) 1.06330(19) 1.00239(13) 0.0165(4) Uani 1 1 d . . . . . F2 F 0.3975(2) 1.2772(2) 1.00332(14) 0.0221(5) Uani 1 1 d . . . . . F3 F 0.8090(3) 0.9307(2) 0.46181(16) 0.0336(6) Uani 1 1 d . . . . . O1 O 0.4440(3) 1.1076(2) 0.89138(16) 0.0156(5) Uani 1 1 d D . . . . H1C H 0.469(4) 1.092(3) 0.8398(12) 0.019 Uiso 1 1 d D U . . . H1D H 0.455(5) 1.043(2) 0.915(2) 0.019 Uiso 1 1 d D U . . . O2 O 0.7325(3) 1.0764(2) 0.85061(16) 0.0158(5) Uani 1 1 d . . . . . O3 O 0.7393(3) 1.1199(2) 0.69391(16) 0.0149(5) Uani 1 1 d . . . . . O4 O 0.8920(3) 0.9217(2) 0.74142(16) 0.0131(5) Uani 1 1 d . . . . . O5 O 0.5010(3) 1.0668(2) 0.72511(15) 0.0133(5) Uani 1 1 d . . . . . O6 O 0.5658(4) 1.1538(3) 0.5410(2) 0.0401(8) Uani 1 1 d D . . . . H6C H 0.617(4) 1.077(2) 0.542(4) 0.048 Uiso 1 1 d D U . . . H6D H 0.488(3) 1.157(4) 0.533(4) 0.048 Uiso 1 1 d D U . . . O7 O 0.6505(3) 0.8652(2) 0.76879(16) 0.0152(5) Uani 1 1 d . . . . . O8 O 0.6741(3) 0.9203(2) 0.61336(16) 0.0171(5) Uani 1 1 d . . . . . O9 O 0.9569(3) 0.8438(3) 0.5801(2) 0.0303(7) Uani 1 1 d D . . . . H9C H 0.930(6) 0.917(2) 0.563(3) 0.036 Uiso 1 1 d D U . . . H9D H 0.934(5) 0.862(4) 0.6337(13) 0.036 Uiso 1 1 d D U . . . O10 O 0.7748(3) 0.8399(2) 0.92871(17) 0.0178(5) Uani 1 1 d D . . . . H10C H 0.742(4) 0.9121(17) 0.928(3) 0.021 Uiso 1 1 d D U . . . H10D H 0.715(3) 0.817(3) 0.954(3) 0.021 Uiso 1 1 d D U . . . O11 O 0.8313(3) 0.6869(3) 0.6155(2) 0.0341(8) Uani 1 1 d . . . . . O12 O 0.7006(3) 0.7630(3) 0.4891(2) 0.0340(7) Uani 1 1 d . . . . . O13 O 0.5264(3) 1.2878(2) 0.83976(17) 0.0215(6) Uani 1 1 d . . . . . O14 O 0.6561(3) 1.2608(3) 0.96553(18) 0.0258(6) Uani 1 1 d . . . . . O15 O 0.9746(3) 0.7043(3) 0.4560(2) 0.0365(8) Uani 1 1 d . . . . . O90 O 0.8489(5) 0.1122(4) 0.5165(2) 0.0507(10) Uani 1 1 d D . . . . H90A H 0.849(7) 0.042(3) 0.504(3) 0.061 Uiso 1 1 d D U . . . H90B H 0.830(7) 0.107(5) 0.5724(13) 0.061 Uiso 1 1 d D U . . . N1 N 0.3580(3) 1.3062(3) 0.68511(19) 0.0158(6) Uani 1 1 d . . . . . N2 N 0.5824(3) 1.3506(3) 0.64874(19) 0.0155(6) Uani 1 1 d . . . . . N3 N 1.0220(3) 0.6960(3) 0.81000(19) 0.0150(6) Uani 1 1 d . . . . . N4 N 0.8096(3) 0.6385(3) 0.8216(2) 0.0156(6) Uani 1 1 d . . . . . C1 C 0.2489(4) 1.2787(4) 0.7032(2) 0.0187(8) Uani 1 1 d . . . . . H1 H 0.2563 1.2035 0.7264 0.022 Uiso 1 1 calc R U . . . C2 C 0.1208(4) 1.3595(4) 0.6887(3) 0.0220(8) Uani 1 1 d . . . . . H2 H 0.0435 1.3386 0.7023 0.026 Uiso 1 1 calc R U . . . C3 C 0.1104(4) 1.4675(4) 0.6551(3) 0.0242(9) Uani 1 1 d . . . . . H3 H 0.0258 1.5214 0.6443 0.029 Uiso 1 1 calc R U . . . C4 C 0.2243(4) 1.4992(4) 0.6364(2) 0.0215(8) Uani 1 1 d . . . . . C5 C 0.3467(4) 1.4143(3) 0.6526(2) 0.0167(7) Uani 1 1 d . . . . . C6 C 0.2233(5) 1.6104(4) 0.6026(3) 0.0269(9) Uani 1 1 d . . . . . H6 H 0.1415 1.6681 0.5906 0.032 Uiso 1 1 calc R U . . . C7 C 0.3384(5) 1.6355(3) 0.5871(3) 0.0252(9) Uani 1 1 d . . . . . H7 H 0.3345 1.7106 0.5653 0.030 Uiso 1 1 calc R U . . . C8 C 0.4645(4) 1.5502(3) 0.6033(2) 0.0211(8) Uani 1 1 d . . . . . C9 C 0.4672(4) 1.4393(3) 0.6344(2) 0.0152(7) Uani 1 1 d . . . . . C10 C 0.5860(5) 1.5684(4) 0.5887(3) 0.0248(9) Uani 1 1 d . . . . . H10 H 0.5886 1.6423 0.5679 0.030 Uiso 1 1 calc R U . . . C11 C 0.7025(4) 1.4788(4) 0.6045(3) 0.0234(8) Uani 1 1 d . . . . . H11 H 0.7852 1.4910 0.5958 0.028 Uiso 1 1 calc R U . . . C12 C 0.6977(4) 1.3704(3) 0.6333(2) 0.0198(8) Uani 1 1 d . . . . . H12 H 0.7790 1.3084 0.6423 0.024 Uiso 1 1 calc R U . . . C13 C 1.1263(4) 0.7282(3) 0.8033(3) 0.0195(8) Uani 1 1 d . . . . . H13 H 1.1205 0.8030 0.7798 0.023 Uiso 1 1 calc R U . . . C14 C 1.2457(4) 0.6547(4) 0.8300(3) 0.0270(9) Uani 1 1 d . . . . . H14 H 1.3192 0.6799 0.8238 0.032 Uiso 1 1 calc R U . . . C15 C 1.2558(4) 0.5473(4) 0.8649(3) 0.0249(9) Uani 1 1 d . . . . . H15 H 1.3363 0.4973 0.8826 0.030 Uiso 1 1 calc R U . . . C16 C 1.1450(4) 0.5114(3) 0.8743(2) 0.0192(8) Uani 1 1 d . . . . . C17 C 1.0307(4) 0.5901(3) 0.8456(2) 0.0154(7) Uani 1 1 d . . . . . C18 C 1.1440(5) 0.4009(4) 0.9102(3) 0.0268(9) Uani 1 1 d . . . . . H18 H 1.2213 0.3469 0.9293 0.032 Uiso 1 1 calc R U . . . C19 C 1.0346(5) 0.3733(3) 0.9169(3) 0.0253(9) Uani 1 1 d . . . . . H19 H 1.0355 0.3005 0.9419 0.030 Uiso 1 1 calc R U . . . C20 C 0.9161(4) 0.4510(3) 0.8872(2) 0.0217(8) Uani 1 1 d . . . . . C21 C 0.9158(4) 0.5594(3) 0.8519(2) 0.0161(7) Uani 1 1 d . . . . . C22 C 0.8009(5) 0.4252(4) 0.8893(3) 0.0266(9) Uani 1 1 d . . . . . H22 H 0.7958 0.3534 0.9131 0.032 Uiso 1 1 calc R U . . . C23 C 0.6959(4) 0.5053(4) 0.8565(3) 0.0283(10) Uani 1 1 d . . . . . H23 H 0.6186 0.4880 0.8561 0.034 Uiso 1 1 calc R U . . . C24 C 0.7027(4) 0.6115(4) 0.8240(3) 0.0207(8) Uani 1 1 d . . . . . H24 H 0.6283 0.6666 0.8027 0.025 Uiso 1 1 calc R U . . . C25 C 0.4512(4) 0.8782(3) 0.6924(2) 0.0157(7) Uani 1 1 d . . . . . H25A H 0.4339 0.8946 0.6348 0.019 Uiso 1 1 calc R U . . . H25B H 0.4895 0.7909 0.6985 0.019 Uiso 1 1 calc R U . . . C26 C 0.3162(4) 0.9296(3) 0.7560(2) 0.0141(7) Uani 1 1 d . . . . . C27 C 0.3063(4) 0.9161(4) 0.8429(2) 0.0182(7) Uani 1 1 d . . . . . H27 H 0.3857 0.8711 0.8636 0.022 Uiso 1 1 calc R U . . . C28 C 0.1978(4) 0.9954(3) 0.7276(2) 0.0141(7) Uani 1 1 d . . . . . H28 H 0.2032 1.0047 0.6685 0.017 Uiso 1 1 calc R U . . . C29 C 0.1815(4) 0.9679(4) 0.8993(2) 0.0213(8) Uani 1 1 d . . . . . H29 H 0.1764 0.9580 0.9584 0.026 Uiso 1 1 calc R U . . . C30 C 0.0705(4) 1.0481(3) 0.7844(2) 0.0137(7) Uani 1 1 d . . . . . C31 C 0.0638(4) 1.0339(4) 0.8711(2) 0.0210(8) Uani 1 1 d . . . . . H31 H -0.0209 1.0693 0.9106 0.025 Uiso 1 1 calc R U . . . C32 C 0.9459(4) 1.1189(3) 0.7502(2) 0.0153(7) Uani 1 1 d . . . . . H32A H 0.9769 1.1331 0.6896 0.018 Uiso 1 1 calc R U . . . H32B H 0.9003 1.1973 0.7797 0.018 Uiso 1 1 calc R 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 Mo1 0.01154(16) 0.01372(16) 0.01369(15) 0.00074(11) 0.00036(12) -0.00588(12) Mo2 0.01504(18) 0.02022(18) 0.02060(18) -0.00129(13) -0.00327(13) -0.00342(14) Cu1 0.0080(2) 0.0141(2) 0.0162(2) 0.00527(16) -0.00181(17) -0.00325(17) Cu2 0.0087(2) 0.0127(2) 0.0153(2) 0.00317(16) -0.00298(16) -0.00440(17) P1 0.0066(4) 0.0120(4) 0.0128(4) 0.0025(3) -0.0009(3) -0.0035(3) P2 0.0071(4) 0.0146(4) 0.0115(4) -0.0004(3) -0.0008(3) -0.0029(3) F1 0.0174(11) 0.0193(11) 0.0155(10) 0.0054(8) -0.0048(9) -0.0103(9) F2 0.0191(12) 0.0226(12) 0.0191(11) -0.0042(9) 0.0044(9) -0.0067(10) F3 0.0407(16) 0.0449(16) 0.0229(13) 0.0107(11) -0.0105(12) -0.0246(13) O1 0.0175(13) 0.0191(13) 0.0111(12) 0.0016(10) -0.0022(10) -0.0090(11) O2 0.0099(12) 0.0179(13) 0.0150(12) 0.0014(10) 0.0016(10) -0.0031(10) O3 0.0080(12) 0.0199(13) 0.0140(12) 0.0042(10) -0.0013(10) -0.0039(10) O4 0.0114(12) 0.0108(11) 0.0173(12) 0.0020(9) -0.0027(10) -0.0051(10) O5 0.0099(12) 0.0162(12) 0.0114(11) -0.0006(9) -0.0016(9) -0.0030(10) O6 0.041(2) 0.0361(19) 0.0333(18) 0.0027(15) -0.0050(17) -0.0067(17) O7 0.0096(12) 0.0186(13) 0.0163(12) 0.0032(10) -0.0036(10) -0.0043(10) O8 0.0136(13) 0.0185(13) 0.0139(12) -0.0005(10) 0.0004(10) -0.0025(11) O9 0.0224(16) 0.0351(17) 0.0257(16) -0.0058(13) -0.0065(13) -0.0014(14) O10 0.0157(14) 0.0161(13) 0.0176(13) 0.0017(10) 0.0010(11) -0.0049(11) O11 0.0342(19) 0.0209(15) 0.0349(18) 0.0066(13) -0.0051(15) -0.0003(14) O12 0.0308(18) 0.0416(19) 0.0332(17) -0.0104(14) 0.0008(14) -0.0207(16) O13 0.0181(14) 0.0162(13) 0.0219(14) 0.0078(11) 0.0005(11) -0.0023(11) O14 0.0291(16) 0.0318(16) 0.0247(15) -0.0035(12) 0.0004(13) -0.0233(14) O15 0.0142(15) 0.058(2) 0.0276(16) -0.0278(15) 0.0017(13) -0.0022(15) O90 0.065(3) 0.055(2) 0.038(2) 0.0031(18) -0.002(2) -0.035(2) N1 0.0125(15) 0.0157(15) 0.0157(15) -0.0006(12) -0.0025(12) -0.0021(12) N2 0.0145(15) 0.0153(15) 0.0143(14) 0.0028(12) -0.0025(12) -0.0042(12) N3 0.0126(15) 0.0140(14) 0.0160(15) 0.0008(12) -0.0014(12) -0.0039(12) N4 0.0134(15) 0.0140(14) 0.0176(15) 0.0001(12) -0.0020(12) -0.0043(12) C1 0.0117(17) 0.0231(19) 0.0198(18) -0.0044(15) -0.0036(15) -0.0043(15) C2 0.0119(18) 0.029(2) 0.0222(19) -0.0074(16) -0.0026(15) -0.0035(16) C3 0.017(2) 0.025(2) 0.023(2) -0.0063(16) -0.0063(16) 0.0018(16) C4 0.020(2) 0.0215(19) 0.0159(18) -0.0005(14) -0.0071(15) 0.0010(16) C5 0.0157(18) 0.0157(17) 0.0139(16) -0.0008(13) -0.0027(14) -0.0012(14) C6 0.029(2) 0.020(2) 0.020(2) 0.0009(15) -0.0062(17) 0.0030(17) C7 0.029(2) 0.0132(18) 0.023(2) 0.0032(15) -0.0037(18) 0.0008(16) C8 0.026(2) 0.0139(18) 0.0159(18) -0.0010(14) -0.0011(16) -0.0023(16) C9 0.0132(17) 0.0145(17) 0.0120(16) -0.0031(13) 0.0015(13) -0.0012(14) C10 0.033(2) 0.0163(18) 0.0195(19) 0.0006(15) 0.0042(17) -0.0101(17) C11 0.025(2) 0.022(2) 0.024(2) 0.0002(16) 0.0002(17) -0.0135(17) C12 0.0177(19) 0.0205(19) 0.0175(18) -0.0004(14) -0.0001(15) -0.0057(16) C13 0.0126(18) 0.0145(17) 0.030(2) 0.0021(15) -0.0056(16) -0.0033(15) C14 0.0123(19) 0.026(2) 0.042(3) 0.0032(19) -0.0098(18) -0.0056(17) C15 0.0140(19) 0.022(2) 0.033(2) 0.0012(17) -0.0097(17) 0.0011(16) C16 0.0174(19) 0.0160(18) 0.0192(18) 0.0012(14) -0.0056(15) -0.0007(15) C17 0.0134(18) 0.0152(17) 0.0129(16) -0.0005(13) 0.0006(14) -0.0026(14) C18 0.029(2) 0.0182(19) 0.027(2) 0.0069(16) -0.0067(18) -0.0033(17) C19 0.028(2) 0.0134(18) 0.025(2) 0.0064(15) -0.0003(17) -0.0027(16) C20 0.025(2) 0.0153(18) 0.0192(18) 0.0024(14) 0.0032(16) -0.0074(16) C21 0.0171(18) 0.0143(17) 0.0133(16) -0.0012(13) 0.0002(14) -0.0041(14) C22 0.027(2) 0.0173(19) 0.032(2) 0.0011(16) 0.0042(18) -0.0108(17) C23 0.020(2) 0.029(2) 0.040(3) -0.0008(19) 0.0000(19) -0.0177(19) C24 0.0153(19) 0.025(2) 0.0230(19) -0.0005(15) -0.0016(15) -0.0105(16) C25 0.0101(16) 0.0197(18) 0.0160(17) -0.0039(14) -0.0006(14) -0.0049(14) C26 0.0110(17) 0.0158(17) 0.0173(17) 0.0007(13) -0.0031(14) -0.0073(14) C27 0.0134(18) 0.028(2) 0.0158(17) 0.0037(15) -0.0042(14) -0.0112(16) C28 0.0133(18) 0.0151(17) 0.0152(17) -0.0001(13) -0.0028(14) -0.0070(14) C29 0.0175(19) 0.036(2) 0.0127(17) 0.0025(15) -0.0026(15) -0.0133(17) C30 0.0103(16) 0.0187(17) 0.0165(17) 0.0029(13) -0.0033(14) -0.0106(14) C31 0.0147(18) 0.035(2) 0.0161(18) -0.0012(16) -0.0001(15) -0.0141(17) C32 0.0097(17) 0.0161(17) 0.0204(18) 0.0022(14) -0.0037(14) -0.0055(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 1.686(3) . ? Mo1 O13 1.712(3) . ? Mo1 F2 1.927(2) . ? Mo1 F1 2.001(2) . ? Mo1 O2 2.011(3) . ? Mo1 O1 2.259(3) . ? Mo2 O12 1.706(3) . ? Mo2 O11 1.802(3) . ? Mo2 O15 1.804(3) . ? Mo2 F3 1.962(3) . ? Mo2 O8 2.061(3) . ? Mo2 O9 2.222(3) . ? Cu1 O3 1.928(3) . ? Cu1 O5 1.951(3) . ? Cu1 N1 1.998(3) . ? Cu1 N2 2.012(3) . ? Cu1 O6 2.450(4) . ? Cu2 O7 1.939(3) . ? Cu2 O4 1.972(2) . ? Cu2 N4 2.024(3) . ? Cu2 N3 2.032(3) . ? Cu2 O10 2.241(3) . ? P1 O3 1.516(2) . ? P1 O4 1.523(3) . ? P1 O2 1.541(3) . ? P1 C32 1.810(4) . ? P2 O7 1.505(3) . ? P2 O5 1.534(3) . ? P2 O8 1.538(3) . ? P2 C25 1.820(4) . ? O1 H1C 0.830(18) . ? O1 H1D 0.827(18) . ? O6 H6C 0.885(19) . ? O6 H6D 0.870(19) . ? O9 H9C 0.874(19) . ? O9 H9D 0.868(19) . ? O10 H10C 0.814(19) . ? O10 H10D 0.820(19) . ? O90 H90A 0.897(19) . ? O90 H90B 0.886(19) . ? N1 C1 1.325(5) . ? N1 C5 1.358(5) . ? N2 C12 1.339(5) . ? N2 C9 1.359(5) . ? N3 C13 1.326(5) . ? N3 C17 1.357(5) . ? N4 C24 1.327(5) . ? N4 C21 1.358(5) . ? C1 C2 1.423(5) . ? C1 H1 0.9500 . ? C2 C3 1.365(6) . ? C2 H2 0.9500 . ? C3 C4 1.406(6) . ? C3 H3 0.9500 . ? C4 C5 1.404(5) . ? C4 C6 1.427(6) . ? C5 C9 1.426(5) . ? C6 C7 1.372(7) . ? C6 H6 0.9500 . ? C7 C8 1.434(6) . ? C7 H7 0.9500 . ? C8 C10 1.395(6) . ? C8 C9 1.405(5) . ? C10 C11 1.381(6) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.409(5) . ? C13 H13 0.9500 . ? C14 C15 1.366(6) . ? C14 H14 0.9500 . ? C15 C16 1.416(6) . ? C15 H15 0.9500 . ? C16 C17 1.403(5) . ? C16 C18 1.435(5) . ? C17 C21 1.426(5) . ? C18 C19 1.344(6) . ? C18 H18 0.9500 . ? C19 C20 1.441(6) . ? C19 H19 0.9500 . ? C20 C21 1.404(5) . ? C20 C22 1.405(6) . ? C22 C23 1.376(6) . ? C22 H22 0.9500 . ? C23 C24 1.389(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.513(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.393(5) . ? C26 C28 1.395(5) . ? C27 C29 1.385(5) . ? C27 H27 0.9500 . ? C28 C30 1.407(5) . ? C28 H28 0.9500 . ? C29 C31 1.388(6) . ? C29 H29 0.9500 . ? C30 C31 1.396(5) . ? C30 C32 1.507(5) 1_455 ? C31 H31 0.9500 . ? C32 C30 1.507(5) 1_655 ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? 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 O13 104.37(14) . . ? O14 Mo1 F2 95.29(12) . . ? O13 Mo1 F2 96.48(12) . . ? O14 Mo1 F1 96.55(12) . . ? O13 Mo1 F1 158.83(12) . . ? F2 Mo1 F1 84.62(9) . . ? O14 Mo1 O2 96.92(13) . . ? O13 Mo1 O2 93.02(12) . . ? F2 Mo1 O2 162.17(10) . . ? F1 Mo1 O2 81.13(10) . . ? O14 Mo1 O1 169.99(12) . . ? O13 Mo1 O1 84.69(12) . . ? F2 Mo1 O1 79.22(10) . . ? F1 Mo1 O1 74.72(9) . . ? O2 Mo1 O1 86.70(10) . . ? O12 Mo2 O11 99.67(17) . . ? O12 Mo2 O15 101.35(15) . . ? O11 Mo2 O15 98.62(16) . . ? O12 Mo2 F3 95.06(14) . . ? O11 Mo2 F3 161.67(14) . . ? O15 Mo2 F3 89.03(15) . . ? O12 Mo2 O8 94.86(13) . . ? O11 Mo2 O8 88.29(13) . . ? O15 Mo2 O8 160.98(14) . . ? F3 Mo2 O8 79.61(11) . . ? O12 Mo2 O9 173.86(14) . . ? O11 Mo2 O9 84.63(14) . . ? O15 Mo2 O9 82.21(13) . . ? F3 Mo2 O9 79.91(12) . . ? O8 Mo2 O9 80.82(11) . . ? O3 Cu1 O5 94.52(10) . . ? O3 Cu1 N1 172.48(12) . . ? O5 Cu1 N1 91.85(12) . . ? O3 Cu1 N2 91.24(12) . . ? O5 Cu1 N2 174.23(12) . . ? N1 Cu1 N2 82.38(13) . . ? O3 Cu1 O6 100.30(12) . . ? O5 Cu1 O6 89.34(11) . . ? N1 Cu1 O6 83.74(13) . . ? N2 Cu1 O6 89.92(12) . . ? O7 Cu2 O4 96.23(10) . . ? O7 Cu2 N4 91.22(12) . . ? O4 Cu2 N4 166.98(12) . . ? O7 Cu2 N3 171.82(12) . . ? O4 Cu2 N3 90.60(11) . . ? N4 Cu2 N3 81.25(12) . . ? O7 Cu2 O10 97.59(10) . . ? O4 Cu2 O10 101.16(10) . . ? N4 Cu2 O10 88.38(11) . . ? N3 Cu2 O10 85.44(11) . . ? O3 P1 O4 112.92(15) . . ? O3 P1 O2 113.28(14) . . ? O4 P1 O2 109.00(14) . . ? O3 P1 C32 103.91(16) . . ? O4 P1 C32 109.23(16) . . ? O2 P1 C32 108.25(16) . . ? O7 P2 O5 112.43(15) . . ? O7 P2 O8 113.55(15) . . ? O5 P2 O8 109.46(14) . . ? O7 P2 C25 108.25(16) . . ? O5 P2 C25 106.30(16) . . ? O8 P2 C25 106.40(16) . . ? Mo1 O1 H1C 109(3) . . ? Mo1 O1 H1D 114(3) . . ? H1C O1 H1D 106(3) . . ? P1 O2 Mo1 141.17(16) . . ? P1 O3 Cu1 138.20(16) . . ? P1 O4 Cu2 128.65(15) . . ? P2 O5 Cu1 130.12(15) . . ? Cu1 O6 H6C 97(4) . . ? Cu1 O6 H6D 112(4) . . ? H6C O6 H6D 106(4) . . ? P2 O7 Cu2 140.01(16) . . ? P2 O8 Mo2 140.11(16) . . ? Mo2 O9 H9C 98(4) . . ? Mo2 O9 H9D 117(4) . . ? H9C O9 H9D 95(3) . . ? Cu2 O10 H10C 102(3) . . ? Cu2 O10 H10D 111(3) . . ? H10C O10 H10D 108(4) . . ? H90A O90 H90B 98(4) . . ? C1 N1 C5 119.1(3) . . ? C1 N1 Cu1 128.5(3) . . ? C5 N1 Cu1 112.1(2) . . ? C12 N2 C9 118.4(3) . . ? C12 N2 Cu1 129.6(3) . . ? C9 N2 Cu1 112.0(2) . . ? C13 N3 C17 118.3(3) . . ? C13 N3 Cu2 128.9(3) . . ? C17 N3 Cu2 112.1(2) . . ? C24 N4 C21 118.6(3) . . ? C24 N4 Cu2 128.9(3) . . ? C21 N4 Cu2 112.1(2) . . ? N1 C1 C2 121.5(4) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C3 C2 C1 119.2(4) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120.4(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 116.8(4) . . ? C5 C4 C6 118.6(4) . . ? C3 C4 C6 124.6(4) . . ? N1 C5 C4 123.1(4) . . ? N1 C5 C9 116.8(3) . . ? C4 C5 C9 120.1(3) . . ? C7 C6 C4 121.2(4) . . ? C7 C6 H6 119.4 . . ? C4 C6 H6 119.4 . . ? C6 C7 C8 121.1(4) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C10 C8 C9 117.4(4) . . ? C10 C8 C7 124.7(4) . . ? C9 C8 C7 117.9(4) . . ? N2 C9 C8 122.7(4) . . ? N2 C9 C5 116.3(3) . . ? C8 C9 C5 120.9(3) . . ? C11 C10 C8 119.8(4) . . ? C11 C10 H10 120.1 . . ? C8 C10 H10 120.1 . . ? C10 C11 C12 119.4(4) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N2 C12 C11 122.2(4) . . ? N2 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? N3 C13 C14 121.9(4) . . ? N3 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.3(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 116.6(3) . . ? C17 C16 C18 119.2(4) . . ? C15 C16 C18 124.2(4) . . ? N3 C17 C16 123.8(3) . . ? N3 C17 C21 116.3(3) . . ? C16 C17 C21 119.8(3) . . ? C19 C18 C16 120.5(4) . . ? C19 C18 H18 119.7 . . ? C16 C18 H18 119.7 . . ? C18 C19 C20 121.9(4) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C22 117.3(4) . . ? C21 C20 C19 118.1(4) . . ? C22 C20 C19 124.6(4) . . ? N4 C21 C20 122.8(4) . . ? N4 C21 C17 116.8(3) . . ? C20 C21 C17 120.4(3) . . ? C23 C22 C20 119.0(4) . . ? C23 C22 H22 120.5 . . ? C20 C22 H22 120.5 . . ? C22 C23 C24 120.1(4) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? N4 C24 C23 122.2(4) . . ? N4 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C26 C25 P2 115.2(2) . . ? C26 C25 H25A 108.5 . . ? P2 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? P2 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C27 C26 C28 118.5(3) . . ? C27 C26 C25 122.1(3) . . ? C28 C26 C25 119.4(3) . . ? C29 C27 C26 120.4(3) . . ? C29 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C26 C28 C30 121.5(3) . . ? C26 C28 H28 119.2 . . ? C30 C28 H28 119.2 . . ? C27 C29 C31 121.1(3) . . ? C27 C29 H29 119.4 . . ? C31 C29 H29 119.4 . . ? C31 C30 C28 118.7(3) . . ? C31 C30 C32 121.9(3) . 1_455 ? C28 C30 C32 119.3(3) . 1_455 ? C29 C31 C30 119.7(4) . . ? C29 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C30 C32 P1 117.2(2) 1_655 . ? C30 C32 H32A 108.0 1_655 . ? P1 C32 H32A 108.0 . . ? C30 C32 H32B 108.0 1_655 . ? P1 C32 H32B 108.0 . . ? H32A C32 H32B 107.3 . . ? 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 O3 P1 O2 Mo1 -30.5(3) . . . . ? O4 P1 O2 Mo1 -157.1(2) . . . . ? C32 P1 O2 Mo1 84.2(3) . . . . ? O4 P1 O3 Cu1 110.7(2) . . . . ? O2 P1 O3 Cu1 -13.8(3) . . . . ? C32 P1 O3 Cu1 -131.0(2) . . . . ? O3 P1 O4 Cu2 -97.6(2) . . . . ? O2 P1 O4 Cu2 29.2(2) . . . . ? C32 P1 O4 Cu2 147.29(19) . . . . ? O7 P2 O5 Cu1 100.7(2) . . . . ? O8 P2 O5 Cu1 -26.4(2) . . . . ? C25 P2 O5 Cu1 -140.99(19) . . . . ? O5 P2 O7 Cu2 -103.8(3) . . . . ? O8 P2 O7 Cu2 21.2(3) . . . . ? C25 P2 O7 Cu2 139.1(2) . . . . ? O7 P2 O8 Mo2 51.5(3) . . . . ? O5 P2 O8 Mo2 178.1(2) . . . . ? C25 P2 O8 Mo2 -67.5(3) . . . . ? C5 N1 C1 C2 0.5(5) . . . . ? Cu1 N1 C1 C2 -172.4(3) . . . . ? N1 C1 C2 C3 0.3(6) . . . . ? C1 C2 C3 C4 -1.1(6) . . . . ? C2 C3 C4 C5 1.1(6) . . . . ? C2 C3 C4 C6 -178.8(4) . . . . ? C1 N1 C5 C4 -0.5(5) . . . . ? Cu1 N1 C5 C4 173.5(3) . . . . ? C1 N1 C5 C9 179.9(3) . . . . ? Cu1 N1 C5 C9 -6.1(4) . . . . ? C3 C4 C5 N1 -0.3(6) . . . . ? C6 C4 C5 N1 179.6(3) . . . . ? C3 C4 C5 C9 179.3(3) . . . . ? C6 C4 C5 C9 -0.8(5) . . . . ? C5 C4 C6 C7 -0.9(6) . . . . ? C3 C4 C6 C7 179.0(4) . . . . ? C4 C6 C7 C8 0.8(6) . . . . ? C6 C7 C8 C10 179.4(4) . . . . ? C6 C7 C8 C9 1.0(6) . . . . ? C12 N2 C9 C8 0.6(5) . . . . ? Cu1 N2 C9 C8 -177.2(3) . . . . ? C12 N2 C9 C5 -179.4(3) . . . . ? Cu1 N2 C9 C5 2.8(4) . . . . ? C10 C8 C9 N2 -1.2(5) . . . . ? C7 C8 C9 N2 177.4(3) . . . . ? C10 C8 C9 C5 178.8(3) . . . . ? C7 C8 C9 C5 -2.6(5) . . . . ? N1 C5 C9 N2 2.2(5) . . . . ? C4 C5 C9 N2 -177.4(3) . . . . ? N1 C5 C9 C8 -177.8(3) . . . . ? C4 C5 C9 C8 2.6(5) . . . . ? C9 C8 C10 C11 0.2(6) . . . . ? C7 C8 C10 C11 -178.3(4) . . . . ? C8 C10 C11 C12 1.3(6) . . . . ? C9 N2 C12 C11 1.0(6) . . . . ? Cu1 N2 C12 C11 178.4(3) . . . . ? C10 C11 C12 N2 -2.0(6) . . . . ? C17 N3 C13 C14 1.6(6) . . . . ? Cu2 N3 C13 C14 171.4(3) . . . . ? N3 C13 C14 C15 -0.7(7) . . . . ? C13 C14 C15 C16 -0.4(7) . . . . ? C14 C15 C16 C17 0.6(6) . . . . ? C14 C15 C16 C18 -179.8(4) . . . . ? C13 N3 C17 C16 -1.3(5) . . . . ? Cu2 N3 C17 C16 -172.8(3) . . . . ? C13 N3 C17 C21 179.7(3) . . . . ? Cu2 N3 C17 C21 8.2(4) . . . . ? C15 C16 C17 N3 0.2(6) . . . . ? C18 C16 C17 N3 -179.4(4) . . . . ? C15 C16 C17 C21 179.2(3) . . . . ? C18 C16 C17 C21 -0.4(6) . . . . ? C17 C16 C18 C19 -0.5(6) . . . . ? C15 C16 C18 C19 180.0(4) . . . . ? C16 C18 C19 C20 1.3(7) . . . . ? C18 C19 C20 C21 -1.3(6) . . . . ? C18 C19 C20 C22 177.4(4) . . . . ? C24 N4 C21 C20 -1.2(5) . . . . ? Cu2 N4 C21 C20 172.3(3) . . . . ? C24 N4 C21 C17 177.9(3) . . . . ? Cu2 N4 C21 C17 -8.6(4) . . . . ? C22 C20 C21 N4 0.8(6) . . . . ? C19 C20 C21 N4 179.6(4) . . . . ? C22 C20 C21 C17 -178.3(4) . . . . ? C19 C20 C21 C17 0.4(5) . . . . ? N3 C17 C21 N4 0.2(5) . . . . ? C16 C17 C21 N4 -178.9(3) . . . . ? N3 C17 C21 C20 179.4(3) . . . . ? C16 C17 C21 C20 0.3(5) . . . . ? C21 C20 C22 C23 0.7(6) . . . . ? C19 C20 C22 C23 -178.0(4) . . . . ? C20 C22 C23 C24 -1.8(7) . . . . ? C21 N4 C24 C23 0.1(6) . . . . ? Cu2 N4 C24 C23 -172.1(3) . . . . ? C22 C23 C24 N4 1.4(7) . . . . ? O7 P2 C25 C26 83.4(3) . . . . ? O5 P2 C25 C26 -37.6(3) . . . . ? O8 P2 C25 C26 -154.2(3) . . . . ? P2 C25 C26 C27 -61.2(4) . . . . ? P2 C25 C26 C28 117.1(3) . . . . ? C28 C26 C27 C29 -0.5(6) . . . . ? C25 C26 C27 C29 177.8(3) . . . . ? C27 C26 C28 C30 0.4(5) . . . . ? C25 C26 C28 C30 -178.0(3) . . . . ? C26 C27 C29 C31 0.1(6) . . . . ? C26 C28 C30 C31 0.1(5) . . . . ? C26 C28 C30 C32 179.6(3) . . . 1_455 ? C27 C29 C31 C30 0.4(6) . . . . ? C28 C30 C31 C29 -0.5(6) . . . . ? C32 C30 C31 C29 180.0(4) 1_455 . . . ? O3 P1 C32 C30 -160.1(3) . . . 1_655 ? O4 P1 C32 C30 -39.3(3) . . . 1_655 ? O2 P1 C32 C30 79.3(3) . . . 1_655 ? _refine_diff_density_max 1.052 _refine_diff_density_min -1.237 _refine_diff_density_rms 0.167 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957900' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound13 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H33 Cu2 F4 Mo2 N6 O11 P2, C23 H21 Cu F3 Mo2 N3 O11 P2, H2 O' _chemical_formula_sum 'C61 H56 Cu3 F7 Mo4 N9 O23 P4' _chemical_formula_weight 2114.40 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9981(6) _cell_length_b 20.6917(16) _cell_length_c 21.1555(16) _cell_angle_alpha 113.586(2) _cell_angle_beta 96.089(2) _cell_angle_gamma 95.629(2) _cell_volume 3546.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 749 _cell_measurement_theta_min 2.1035 _cell_measurement_theta_max 24.6003 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_F_000 2094 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.397 _exptl_crystal_size_mid 0.071 _exptl_crystal_size_min 0.044 _exptl_absorpt_coefficient_mu 1.760 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44596 _diffrn_reflns_av_unetI/netI 0.0579 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.064 _diffrn_reflns_theta_max 27.084 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 15373 _reflns_number_gt 11528 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+2.9620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 15373 _refine_ls_number_parameters 1019 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0633 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.76815(4) -0.05123(2) 0.33278(2) 0.01145(7) Uani 1 1 d . . . . . Mo2 Mo 0.81027(4) 0.02320(2) 0.18393(2) 0.01185(7) Uani 1 1 d . . . . . Mo3 Mo 1.04970(4) 0.42192(2) 0.30874(2) 0.01314(8) Uani 1 1 d . . . . . Mo4 Mo 0.97843(4) 0.47271(2) 0.14326(2) 0.01241(7) Uani 1 1 d . . . . . Cu1 Cu 0.71324(5) 0.24217(2) 0.47972(2) 0.01033(10) Uani 1 1 d . . . . . Cu2 Cu 1.18346(5) -0.08178(2) 0.17056(2) 0.00904(9) Uani 1 1 d . . . . . Cu3 Cu 0.52337(5) 0.37915(2) 0.12159(2) 0.00898(9) Uani 1 1 d . . . . . P1 P 0.70425(10) 0.11011(5) 0.34178(5) 0.00892(19) Uani 1 1 d . . . . . P2 P 1.09102(10) 0.02281(5) 0.30434(5) 0.00734(18) Uani 1 1 d . . . . . P3 P 0.74536(10) 0.48498(5) 0.25948(5) 0.00727(18) Uani 1 1 d . . . . . P4 P 1.18120(10) 0.57576(5) 0.30003(5) 0.00869(19) Uani 1 1 d . . . . . F1 F 0.8059(3) -0.14177(11) 0.27953(11) 0.0223(5) Uani 1 1 d . . . . . F2 F 0.7468(2) -0.04586(10) 0.23215(10) 0.0106(4) Uani 1 1 d . . . . . F3 F 0.6155(2) -0.00694(12) 0.13443(11) 0.0207(5) Uani 1 1 d . . . . . F4 F 0.8821(2) -0.05227(12) 0.12482(11) 0.0246(5) Uani 1 1 d . . . . . F5 F 0.9594(2) 0.32687(11) 0.26903(11) 0.0185(5) Uani 1 1 d . . . . . F6 F 1.0217(2) 0.40975(10) 0.20310(10) 0.0102(4) Uani 1 1 d . . . . . F7 F 0.8146(2) 0.40353(11) 0.09326(11) 0.0189(5) Uani 1 1 d . . . . . O1 O 0.7984(3) -0.05195(13) 0.41305(13) 0.0141(6) Uani 1 1 d . . . . . O2 O 0.5679(3) -0.07108(13) 0.31313(12) 0.0127(5) Uani 1 1 d . . . . . O3 O 0.9972(3) -0.02038(12) 0.33413(12) 0.0098(5) Uani 1 1 d . . . . . O4 O 0.7655(3) 0.05430(12) 0.36518(12) 0.0099(5) Uani 1 1 d . . . . . O5 O 0.7828(3) 0.18445(12) 0.39062(12) 0.0111(5) Uani 1 1 d . . . . . O6 O 0.7193(3) 0.09288(13) 0.26555(12) 0.0130(5) Uani 1 1 d . . . . . O7 O 0.8698(3) 0.08645(12) 0.15657(12) 0.0116(5) Uani 1 1 d . . . . . O8 O 0.9938(3) 0.04745(12) 0.25689(12) 0.0114(5) Uani 1 1 d . . . . . O9 O 1.2106(3) -0.01733(12) 0.26695(12) 0.0097(5) Uani 1 1 d . . . . . O10 O 1.4250(3) -0.09398(14) 0.17746(13) 0.0155(6) Uani 1 1 d D . . . . H10A H 1.468(4) -0.089(2) 0.2165(13) 0.019 Uiso 1 1 d D U . . . H10B H 1.485(4) -0.0660(17) 0.171(2) 0.019 Uiso 1 1 d D U . . . O11 O 0.9180(3) 0.30408(13) 0.53952(12) 0.0125(5) Uani 1 1 d . . . . . H11A H 0.9086 0.3221 0.5819 0.015 Uiso 1 1 calc R U . . . O12 O 1.2341(3) 0.40537(12) 0.29908(12) 0.0095(5) Uani 1 1 d . . . . . O13 O 1.0446(3) 0.43832(13) 0.39447(13) 0.0161(6) Uani 1 1 d . . . . . O14 O 0.8282(3) 0.44282(12) 0.29362(12) 0.0094(5) Uani 1 1 d . . . . . O15 O 1.1050(3) 0.52549(12) 0.32961(12) 0.0101(5) Uani 1 1 d . . . . . O16 O 0.8459(3) 0.51215(12) 0.21797(12) 0.0098(5) Uani 1 1 d . . . . . O17 O 0.9569(3) 0.52997(13) 0.10541(12) 0.0124(5) Uani 1 1 d . . . . . O18 O 1.1146(2) 0.42361(11) 0.09544(11) 0.0056(5) Uani 1 1 d . . . . . O19 O 1.1483(3) 0.54127(12) 0.21936(12) 0.0102(5) Uani 1 1 d . . . . . O20 O 1.1363(3) 0.64841(12) 0.33223(12) 0.0124(5) Uani 1 1 d . . . . . O21 O 0.5948(3) 0.44326(12) 0.21657(12) 0.0098(5) Uani 1 1 d . . . . . O22 O 0.2974(3) 0.35038(14) 0.15387(14) 0.0151(6) Uani 1 1 d D . . . . H22A H 0.230(3) 0.368(2) 0.142(2) 0.018 Uiso 1 1 d D U . . . H22B H 0.307(4) 0.365(2) 0.1968(10) 0.018 Uiso 1 1 d D U . . . O90 O 0.0579(3) 0.42052(15) 0.52114(14) 0.0200(6) Uani 1 1 d D . . . . H90A H 0.031(5) 0.4565(15) 0.5502(18) 0.024 Uiso 1 1 d D U . . . H90B H 0.056(5) 0.428(2) 0.4860(15) 0.024 Uiso 1 1 d D U . . . N1 N 0.7191(3) 0.17021(15) 0.52214(15) 0.0112(6) Uani 1 1 d . . . . . N2 N 0.5205(3) 0.24800(15) 0.51452(14) 0.0089(6) Uani 1 1 d . . . . . N3 N 0.6373(3) 0.31688(15) 0.45131(15) 0.0116(6) Uani 1 1 d . . . . . N4 N 1.1232(3) -0.17259(15) 0.18349(15) 0.0114(6) Uani 1 1 d . . . . . N5 N 1.1289(3) -0.14916(15) 0.07388(15) 0.0109(6) Uani 1 1 d . . . . . N6 N 1.2015(3) -0.01337(15) 0.12289(15) 0.0108(6) Uani 1 1 d . . . . . N7 N 0.5823(3) 0.28554(15) 0.11954(15) 0.0101(6) Uani 1 1 d . . . . . N8 N 0.4444(3) 0.31578(15) 0.02470(15) 0.0098(6) Uani 1 1 d . . . . . N9 N 0.4492(3) 0.45039(15) 0.08652(15) 0.0095(6) Uani 1 1 d . . . . . C1 C 0.8315(4) 0.13291(19) 0.52503(18) 0.0137(8) Uani 1 1 d . . . . . H1 H 0.9190 0.1401 0.5057 0.016 Uiso 1 1 calc R U . . . C2 C 0.8253(4) 0.0846(2) 0.55492(19) 0.0170(8) Uani 1 1 d . . . . . H2 H 0.9076 0.0597 0.5570 0.020 Uiso 1 1 calc R U . . . C3 C 0.6968(4) 0.0733(2) 0.58173(19) 0.0179(8) Uani 1 1 d . . . . . H3 H 0.6894 0.0400 0.6022 0.022 Uiso 1 1 calc R U . . . C4 C 0.5789(4) 0.11068(19) 0.57862(19) 0.0150(8) Uani 1 1 d . . . . . H4 H 0.4897 0.1032 0.5967 0.018 Uiso 1 1 calc R U . . . C5 C 0.5926(4) 0.15910(18) 0.54876(17) 0.0111(8) Uani 1 1 d . . . . . C6 C 0.4770(4) 0.20300(18) 0.54274(17) 0.0096(7) Uani 1 1 d . . . . . C7 C 0.3328(4) 0.19953(19) 0.56047(18) 0.0118(8) Uani 1 1 d . . . . . H7 H 0.3001 0.1675 0.5800 0.014 Uiso 1 1 calc R U . . . C8 C 0.2382(4) 0.24390(19) 0.54897(18) 0.0132(8) Uani 1 1 d . . . . . H8 H 0.1399 0.2428 0.5614 0.016 Uiso 1 1 calc R U . . . C9 C 0.2853(4) 0.29026(19) 0.51928(17) 0.0121(8) Uani 1 1 d . . . . . H9 H 0.2204 0.3205 0.5110 0.015 Uiso 1 1 calc R U . . . C10 C 0.4298(4) 0.29058(18) 0.50243(17) 0.0105(7) Uani 1 1 d . . . . . C11 C 0.5009(4) 0.33330(18) 0.46844(17) 0.0105(7) Uani 1 1 d . . . . . C12 C 0.4347(4) 0.3847(2) 0.45372(19) 0.0161(8) Uani 1 1 d . . . . . H12 H 0.3395 0.3958 0.4669 0.019 Uiso 1 1 calc R U . . . C13 C 0.5099(4) 0.4196(2) 0.4195(2) 0.0184(8) Uani 1 1 d . . . . . H13 H 0.4671 0.4549 0.4089 0.022 Uiso 1 1 calc R U . . . C14 C 0.6484(4) 0.4017(2) 0.4011(2) 0.0175(8) Uani 1 1 d . . . . . H14 H 0.7018 0.4246 0.3773 0.021 Uiso 1 1 calc R U . . . C15 C 0.7082(4) 0.35040(19) 0.41753(18) 0.0146(8) Uani 1 1 d . . . . . H15 H 0.8030 0.3383 0.4045 0.017 Uiso 1 1 calc R U . . . C16 C 1.2365(4) 0.05784(19) 0.15364(19) 0.0123(8) Uani 1 1 d . . . . . H16 H 1.2602 0.0809 0.2031 0.015 Uiso 1 1 calc R U . . . C17 C 1.2394(4) 0.0991(2) 0.11562(19) 0.0154(8) Uani 1 1 d . . . . . H17 H 1.2618 0.1497 0.1388 0.019 Uiso 1 1 calc R U . . . C18 C 1.2093(4) 0.0656(2) 0.04378(19) 0.0156(8) Uani 1 1 d . . . . . H18 H 1.2128 0.0927 0.0167 0.019 Uiso 1 1 calc R U . . . C19 C 1.1738(4) -0.0085(2) 0.01118(19) 0.0148(8) Uani 1 1 d . . . . . H19 H 1.1530 -0.0326 -0.0383 0.018 Uiso 1 1 calc R U . . . C20 C 1.1693(4) -0.04657(19) 0.05235(18) 0.0104(7) Uani 1 1 d . . . . . C21 C 1.1246(4) -0.12435(19) 0.02421(18) 0.0115(8) Uani 1 1 d . . . . . C22 C 1.0800(4) -0.1717(2) -0.04598(19) 0.0168(8) Uani 1 1 d . . . . . H22 H 1.0753 -0.1549 -0.0817 0.020 Uiso 1 1 calc R U . . . C23 C 1.0427(4) -0.2442(2) -0.0622(2) 0.0209(9) Uani 1 1 d . . . . . H23 H 1.0145 -0.2774 -0.1096 0.025 Uiso 1 1 calc R U . . . C24 C 1.0467(4) -0.2680(2) -0.0094(2) 0.0201(9) Uani 1 1 d . . . . . H24 H 1.0200 -0.3172 -0.0201 0.024 Uiso 1 1 calc R U . . . C25 C 1.0904(4) -0.21852(19) 0.05923(19) 0.0141(8) Uani 1 1 d . . . . . C26 C 1.0962(4) -0.23253(19) 0.12287(19) 0.0128(8) Uani 1 1 d . . . . . C27 C 1.0770(4) -0.3000(2) 0.1231(2) 0.0179(8) Uani 1 1 d . . . . . H27 H 1.0600 -0.3416 0.0805 0.022 Uiso 1 1 calc R U . . . C28 C 1.0833(4) -0.3053(2) 0.1866(2) 0.0215(9) Uani 1 1 d . . . . . H28 H 1.0720 -0.3509 0.1880 0.026 Uiso 1 1 calc R U . . . C29 C 1.1061(4) -0.2441(2) 0.2479(2) 0.0183(9) Uani 1 1 d . . . . . H29 H 1.1084 -0.2468 0.2918 0.022 Uiso 1 1 calc R U . . . C30 C 1.1255(4) -0.17844(19) 0.2440(2) 0.0143(8) Uani 1 1 d . . . . . H30 H 1.1411 -0.1362 0.2860 0.017 Uiso 1 1 calc R U . . . C31 C 0.6547(4) 0.27514(19) 0.17201(19) 0.0125(8) Uani 1 1 d . . . . . H31 H 0.6972 0.3155 0.2139 0.015 Uiso 1 1 calc R U . . . C32 C 0.6703(4) 0.20756(19) 0.1678(2) 0.0145(8) Uani 1 1 d . . . . . H32 H 0.7220 0.2016 0.2062 0.017 Uiso 1 1 calc R U . . . C33 C 0.6087(4) 0.14883(19) 0.1063(2) 0.0151(8) Uani 1 1 d . . . . . H33 H 0.6149 0.1019 0.1026 0.018 Uiso 1 1 calc R U . . . C34 C 0.5384(4) 0.15912(19) 0.05064(19) 0.0136(8) Uani 1 1 d . . . . . H34 H 0.4991 0.1196 0.0076 0.016 Uiso 1 1 calc R U . . . C35 C 0.5259(4) 0.22785(19) 0.05841(18) 0.0108(7) Uani 1 1 d . . . . . C36 C 0.4484(4) 0.24555(19) 0.00315(18) 0.0113(8) Uani 1 1 d . . . . . C37 C 0.3824(4) 0.1979(2) -0.06406(19) 0.0155(8) Uani 1 1 d . . . . . H37 H 0.3820 0.1481 -0.0791 0.019 Uiso 1 1 calc R U . . . C38 C 0.3171(4) 0.2250(2) -0.10859(19) 0.0186(9) Uani 1 1 d . . . . . H38 H 0.2741 0.1935 -0.1552 0.022 Uiso 1 1 calc R U . . . C39 C 0.3139(4) 0.2978(2) -0.08559(19) 0.0163(8) Uani 1 1 d . . . . . H39 H 0.2691 0.3166 -0.1160 0.020 Uiso 1 1 calc R U . . . C40 C 0.3780(4) 0.34259(19) -0.01687(18) 0.0111(8) Uani 1 1 d . . . . . C41 C 0.3784(4) 0.42071(19) 0.01911(18) 0.0102(7) Uani 1 1 d . . . . . C42 C 0.3074(4) 0.45956(19) -0.01134(19) 0.0130(8) Uani 1 1 d . . . . . H42 H 0.2599 0.4375 -0.0588 0.016 Uiso 1 1 calc R U . . . C43 C 0.3066(4) 0.5313(2) 0.02839(19) 0.0161(8) Uani 1 1 d . . . . . H43 H 0.2581 0.5592 0.0086 0.019 Uiso 1 1 calc R U . . . C44 C 0.3769(4) 0.5619(2) 0.09704(19) 0.0148(8) Uani 1 1 d . . . . . H44 H 0.3770 0.6110 0.1253 0.018 Uiso 1 1 calc R U . . . C45 C 0.4476(4) 0.51985(19) 0.12422(19) 0.0127(8) Uani 1 1 d . . . . . H45 H 0.4967 0.5412 0.1714 0.015 Uiso 1 1 calc R U . . . C46 C 0.5056(4) 0.10036(18) 0.34786(18) 0.0100(7) Uani 1 1 d . . . . . H46A H 0.4593 0.0513 0.3147 0.012 Uiso 1 1 calc R U . . . H46B H 0.4964 0.1043 0.3954 0.012 Uiso 1 1 calc R U . . . C47 C 0.4116(4) 0.15177(18) 0.33385(17) 0.0091(7) Uani 1 1 d . . . . . C48 C 0.4670(4) 0.19671(18) 0.30373(18) 0.0119(8) Uani 1 1 d . . . . . H48 H 0.5677 0.1967 0.2940 0.014 Uiso 1 1 calc R U . . . C49 C 0.3788(4) 0.24116(19) 0.28774(19) 0.0153(8) Uani 1 1 d . . . . . H49 H 0.4188 0.2707 0.2669 0.018 Uiso 1 1 calc R U . . . C50 C 0.2322(4) 0.24235(19) 0.3022(2) 0.0165(8) Uani 1 1 d . . . . . H50 H 0.1712 0.2726 0.2913 0.020 Uiso 1 1 calc R U . . . C51 C 0.1754(4) 0.19921(18) 0.33262(19) 0.0149(8) Uani 1 1 d . . . . . H51 H 0.0754 0.2006 0.3431 0.018 Uiso 1 1 calc R U . . . C52 C 0.2630(4) 0.15356(18) 0.34814(18) 0.0109(8) Uani 1 1 d . . . . . C53 C 0.1862(4) 0.10417(18) 0.37577(17) 0.0097(7) Uani 1 1 d . . . . . H53A H 0.1119 0.1282 0.4049 0.012 Uiso 1 1 calc R U . . . H53B H 0.2624 0.0928 0.4055 0.012 Uiso 1 1 calc R U . . . C54 C 0.7113(4) 0.56430(17) 0.32996(18) 0.0087(7) Uani 1 1 d . . . . . H54A H 0.6413 0.5502 0.3569 0.010 Uiso 1 1 calc R U . . . H54B H 0.8079 0.5885 0.3617 0.010 Uiso 1 1 calc R U . . . C55 C 0.6450(4) 0.61644(17) 0.30605(17) 0.0084(7) Uani 1 1 d . . . . . C56 C 0.7445(4) 0.65848(18) 0.28566(18) 0.0120(8) Uani 1 1 d . . . . . H56 H 0.8477 0.6522 0.2866 0.014 Uiso 1 1 calc R U . . . C57 C 0.6950(4) 0.70897(18) 0.26427(18) 0.0119(8) Uani 1 1 d . . . . . H57 H 0.7636 0.7366 0.2502 0.014 Uiso 1 1 calc R U . . . C58 C 0.5442(4) 0.71897(18) 0.26351(18) 0.0126(8) Uani 1 1 d . . . . . H58 H 0.5093 0.7540 0.2498 0.015 Uiso 1 1 calc R U . . . C59 C 0.4452(4) 0.67692(18) 0.28311(18) 0.0118(8) Uani 1 1 d . . . . . H59 H 0.3423 0.6838 0.2824 0.014 Uiso 1 1 calc R U . . . C60 C 0.4923(4) 0.62513(18) 0.30367(17) 0.0097(7) Uani 1 1 d . . . . . C61 C 0.3816(4) 0.57789(18) 0.32327(18) 0.0113(7) Uani 1 1 d . . . . . H61A H 0.4037 0.5935 0.3745 0.014 Uiso 1 1 calc R U . . . H61B H 0.4033 0.5284 0.3013 0.014 Uiso 1 1 calc R 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 Mo1 0.01566(17) 0.00963(16) 0.00958(16) 0.00584(13) 0.00090(13) -0.00272(13) Mo2 0.01920(18) 0.00867(16) 0.00645(16) 0.00373(13) -0.00106(13) -0.00266(13) Mo3 0.01910(18) 0.01419(17) 0.01196(17) 0.00889(14) 0.00574(13) 0.01007(13) Mo4 0.02137(18) 0.00845(16) 0.00677(16) 0.00237(13) 0.00001(13) 0.00528(13) Cu1 0.0098(2) 0.0113(2) 0.0126(2) 0.00712(19) 0.00342(18) 0.00238(17) Cu2 0.0110(2) 0.0067(2) 0.0074(2) 0.00121(18) 0.00143(17) -0.00019(17) Cu3 0.0109(2) 0.0075(2) 0.0075(2) 0.00227(18) 0.00017(17) 0.00181(17) P1 0.0101(5) 0.0089(5) 0.0091(5) 0.0043(4) 0.0031(4) 0.0029(4) P2 0.0068(4) 0.0076(4) 0.0070(4) 0.0027(4) 0.0005(3) 0.0007(3) P3 0.0070(4) 0.0065(4) 0.0088(5) 0.0033(4) 0.0019(3) 0.0019(3) P4 0.0087(5) 0.0082(5) 0.0081(5) 0.0028(4) 0.0000(4) 0.0005(4) F1 0.0303(14) 0.0124(12) 0.0233(13) 0.0074(10) 0.0014(10) 0.0031(10) F2 0.0101(10) 0.0128(11) 0.0115(11) 0.0080(9) 0.0012(8) 0.0004(8) F3 0.0190(12) 0.0248(13) 0.0182(12) 0.0103(10) -0.0007(9) 0.0014(10) F4 0.0244(13) 0.0229(13) 0.0240(13) 0.0056(11) 0.0088(10) 0.0045(10) F5 0.0162(12) 0.0137(11) 0.0265(13) 0.0105(10) -0.0013(9) 0.0016(9) F6 0.0115(10) 0.0113(11) 0.0091(10) 0.0049(9) 0.0027(8) 0.0028(8) F7 0.0156(12) 0.0197(12) 0.0189(12) 0.0058(10) 0.0018(9) 0.0021(9) O1 0.0148(14) 0.0154(14) 0.0153(14) 0.0096(11) 0.0035(11) 0.0018(11) O2 0.0066(12) 0.0226(15) 0.0131(13) 0.0134(12) -0.0007(10) -0.0035(10) O3 0.0087(13) 0.0112(13) 0.0118(13) 0.0074(11) 0.0005(10) 0.0013(10) O4 0.0120(13) 0.0105(13) 0.0088(13) 0.0046(11) 0.0020(10) 0.0053(10) O5 0.0114(13) 0.0100(13) 0.0105(13) 0.0027(11) 0.0029(10) 0.0009(10) O6 0.0180(14) 0.0140(13) 0.0099(13) 0.0059(11) 0.0051(11) 0.0079(11) O7 0.0130(13) 0.0107(13) 0.0124(13) 0.0065(11) 0.0016(10) 0.0011(10) O8 0.0112(13) 0.0110(13) 0.0130(13) 0.0073(11) -0.0014(10) -0.0013(10) O9 0.0097(13) 0.0091(13) 0.0075(12) 0.0007(10) 0.0012(10) 0.0014(10) O10 0.0095(14) 0.0210(15) 0.0125(14) 0.0043(12) -0.0007(11) 0.0007(11) O11 0.0111(13) 0.0163(14) 0.0082(13) 0.0028(11) 0.0016(10) 0.0034(10) O12 0.0063(12) 0.0098(13) 0.0135(13) 0.0063(11) -0.0010(10) 0.0025(10) O13 0.0198(15) 0.0181(14) 0.0154(14) 0.0117(12) 0.0042(11) 0.0040(11) O14 0.0072(12) 0.0110(13) 0.0144(13) 0.0092(11) 0.0031(10) 0.0025(10) O15 0.0128(13) 0.0081(12) 0.0095(13) 0.0041(10) 0.0019(10) 0.0006(10) O16 0.0103(13) 0.0111(13) 0.0109(13) 0.0071(11) 0.0027(10) 0.0029(10) O17 0.0151(13) 0.0124(13) 0.0110(13) 0.0062(11) 0.0009(10) 0.0027(10) O18 0.0053(12) 0.0047(12) 0.0047(12) -0.0001(10) 0.0015(9) -0.0007(9) O19 0.0100(13) 0.0105(13) 0.0090(13) 0.0042(10) 0.0004(10) -0.0023(10) O20 0.0118(13) 0.0117(13) 0.0129(13) 0.0038(11) 0.0036(10) 0.0025(10) O21 0.0085(13) 0.0118(13) 0.0082(13) 0.0039(10) -0.0012(10) 0.0018(10) O22 0.0100(14) 0.0211(15) 0.0162(14) 0.0089(13) 0.0020(12) 0.0061(11) O90 0.0322(17) 0.0166(15) 0.0139(15) 0.0080(13) 0.0049(13) 0.0063(13) N1 0.0106(16) 0.0111(16) 0.0125(16) 0.0052(13) 0.0026(12) 0.0011(12) N2 0.0106(15) 0.0082(15) 0.0062(15) 0.0014(12) 0.0014(12) 0.0009(12) N3 0.0141(16) 0.0115(16) 0.0086(16) 0.0040(13) 0.0002(12) 0.0018(12) N4 0.0106(16) 0.0074(15) 0.0135(16) 0.0014(13) 0.0027(12) 0.0017(12) N5 0.0082(15) 0.0086(15) 0.0120(16) 0.0002(13) 0.0016(12) 0.0021(12) N6 0.0094(16) 0.0105(16) 0.0104(16) 0.0022(13) 0.0029(12) 0.0007(12) N7 0.0099(15) 0.0082(15) 0.0110(16) 0.0026(13) 0.0021(12) 0.0013(12) N8 0.0101(16) 0.0102(16) 0.0083(15) 0.0026(13) 0.0022(12) 0.0023(12) N9 0.0069(15) 0.0131(16) 0.0096(16) 0.0060(13) 0.0009(12) 0.0009(12) C1 0.0125(19) 0.017(2) 0.0109(19) 0.0059(16) 0.0006(15) 0.0017(15) C2 0.022(2) 0.015(2) 0.014(2) 0.0057(17) -0.0023(16) 0.0083(16) C3 0.027(2) 0.014(2) 0.014(2) 0.0075(17) 0.0006(17) 0.0032(17) C4 0.017(2) 0.014(2) 0.014(2) 0.0067(16) 0.0034(16) -0.0019(15) C5 0.0142(19) 0.0099(18) 0.0060(18) 0.0005(15) 0.0015(14) -0.0005(14) C6 0.0116(18) 0.0074(18) 0.0062(18) 0.0000(14) -0.0004(14) -0.0006(14) C7 0.0130(19) 0.0117(19) 0.0094(18) 0.0032(15) 0.0038(15) -0.0011(15) C8 0.0106(19) 0.0128(19) 0.0142(19) 0.0034(16) 0.0038(15) 0.0004(15) C9 0.0139(19) 0.0101(18) 0.0063(18) -0.0021(15) -0.0006(14) 0.0013(15) C10 0.0135(19) 0.0099(18) 0.0051(17) 0.0004(15) -0.0006(14) 0.0027(14) C11 0.0134(19) 0.0073(18) 0.0065(18) -0.0003(15) -0.0020(14) 0.0006(14) C12 0.014(2) 0.017(2) 0.019(2) 0.0105(17) 0.0010(16) 0.0017(16) C13 0.024(2) 0.015(2) 0.019(2) 0.0111(17) 0.0001(17) 0.0028(17) C14 0.019(2) 0.018(2) 0.018(2) 0.0128(18) -0.0003(16) -0.0027(16) C15 0.0129(19) 0.017(2) 0.014(2) 0.0064(16) 0.0039(15) 0.0016(15) C16 0.0117(19) 0.0118(19) 0.0090(18) 0.0005(15) 0.0018(14) -0.0006(15) C17 0.016(2) 0.0111(19) 0.018(2) 0.0055(16) 0.0045(16) -0.0014(15) C18 0.0128(19) 0.021(2) 0.015(2) 0.0110(17) 0.0031(15) -0.0005(16) C19 0.0105(19) 0.021(2) 0.0107(19) 0.0048(17) 0.0006(15) -0.0008(15) C20 0.0076(18) 0.0130(19) 0.0094(18) 0.0030(15) 0.0032(14) 0.0019(14) C21 0.0058(18) 0.0133(19) 0.0123(19) 0.0018(16) 0.0020(14) 0.0023(14) C22 0.014(2) 0.022(2) 0.0107(19) 0.0031(17) 0.0025(15) 0.0020(16) C23 0.018(2) 0.018(2) 0.013(2) -0.0055(17) -0.0003(16) -0.0040(17) C24 0.021(2) 0.014(2) 0.018(2) 0.0006(17) 0.0004(17) 0.0003(16) C25 0.0107(19) 0.0109(19) 0.016(2) 0.0010(16) 0.0016(15) 0.0027(15) C26 0.0058(18) 0.0109(19) 0.018(2) 0.0027(16) 0.0001(14) 0.0011(14) C27 0.014(2) 0.011(2) 0.026(2) 0.0064(17) 0.0006(16) 0.0023(15) C28 0.018(2) 0.014(2) 0.034(3) 0.0118(19) 0.0027(18) 0.0022(16) C29 0.016(2) 0.020(2) 0.025(2) 0.0145(19) 0.0038(17) 0.0049(16) C30 0.0130(19) 0.0131(19) 0.019(2) 0.0080(17) 0.0023(15) 0.0044(15) C31 0.0096(18) 0.0131(19) 0.0135(19) 0.0040(16) 0.0016(15) 0.0026(15) C32 0.0122(19) 0.017(2) 0.019(2) 0.0112(17) 0.0053(16) 0.0060(15) C33 0.0113(19) 0.0107(19) 0.025(2) 0.0077(17) 0.0064(16) 0.0040(15) C34 0.0074(18) 0.0103(19) 0.018(2) 0.0007(16) 0.0014(15) 0.0012(14) C35 0.0056(17) 0.0131(19) 0.0151(19) 0.0067(16) 0.0030(14) 0.0024(14) C36 0.0074(18) 0.0115(19) 0.0137(19) 0.0033(16) 0.0036(14) 0.0013(14) C37 0.015(2) 0.0117(19) 0.015(2) 0.0008(16) 0.0043(16) 0.0027(15) C38 0.016(2) 0.020(2) 0.0090(19) -0.0028(17) -0.0027(15) 0.0013(16) C39 0.013(2) 0.022(2) 0.0103(19) 0.0034(17) -0.0013(15) 0.0017(16) C40 0.0084(18) 0.0136(19) 0.0107(19) 0.0042(16) 0.0033(14) 0.0006(14) C41 0.0071(18) 0.0140(19) 0.0110(19) 0.0069(16) 0.0025(14) -0.0005(14) C42 0.0116(19) 0.017(2) 0.0115(19) 0.0075(16) 0.0012(15) 0.0016(15) C43 0.015(2) 0.022(2) 0.017(2) 0.0119(18) 0.0052(16) 0.0066(16) C44 0.017(2) 0.0117(19) 0.015(2) 0.0046(16) 0.0038(16) 0.0063(15) C45 0.0145(19) 0.0099(19) 0.0129(19) 0.0037(16) 0.0032(15) 0.0020(15) C46 0.0094(18) 0.0101(18) 0.0101(18) 0.0047(15) -0.0004(14) -0.0006(14) C47 0.0114(18) 0.0048(17) 0.0068(18) -0.0011(14) -0.0036(14) 0.0019(14) C48 0.0097(18) 0.0108(19) 0.0116(19) 0.0018(15) 0.0005(14) -0.0003(14) C49 0.021(2) 0.0079(19) 0.016(2) 0.0057(16) -0.0010(16) -0.0004(15) C50 0.016(2) 0.0095(19) 0.021(2) 0.0055(17) -0.0041(16) 0.0027(15) C51 0.0118(19) 0.0086(19) 0.021(2) 0.0030(16) 0.0003(15) 0.0030(15) C52 0.0121(19) 0.0065(18) 0.0077(18) -0.0029(15) 0.0006(14) -0.0001(14) C53 0.0075(18) 0.0099(18) 0.0084(18) 0.0002(15) 0.0012(14) 0.0025(14) C54 0.0074(17) 0.0072(17) 0.0108(18) 0.0032(15) 0.0021(14) -0.0005(13) C55 0.0129(18) 0.0051(17) 0.0033(17) -0.0017(14) 0.0009(14) -0.0003(14) C56 0.0128(19) 0.0093(18) 0.0111(19) 0.0013(15) 0.0031(15) 0.0014(14) C57 0.0144(19) 0.0092(18) 0.0109(19) 0.0033(15) 0.0041(15) -0.0021(15) C58 0.020(2) 0.0054(18) 0.0110(19) 0.0020(15) 0.0001(15) 0.0032(15) C59 0.0111(19) 0.0096(18) 0.0130(19) 0.0036(15) -0.0003(14) 0.0011(14) C60 0.0112(18) 0.0072(18) 0.0073(18) 0.0002(14) 0.0002(14) 0.0001(14) C61 0.0098(18) 0.0103(19) 0.0127(19) 0.0042(15) -0.0001(14) 0.0013(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O1 1.697(2) . ? Mo1 O2 1.774(2) . ? Mo1 F1 1.847(2) . ? Mo1 O4 2.014(2) . ? Mo1 O3 2.090(2) . ? Mo1 F2 2.1652(19) . ? Mo2 O7 1.694(2) . ? Mo2 F4 1.796(2) . ? Mo2 F3 1.853(2) . ? Mo2 O8 2.009(2) . ? Mo2 O6 2.066(2) . ? Mo2 F2 2.1304(18) . ? Mo3 O13 1.713(2) . ? Mo3 O12 1.744(2) . ? Mo3 F5 1.858(2) . ? Mo3 O15 2.006(2) . ? Mo3 O14 2.099(2) . ? Mo3 F6 2.1305(19) . ? Mo4 O17 1.689(2) . ? Mo4 O18 1.800(2) . ? Mo4 F7 1.840(2) . ? Mo4 O16 2.036(2) . ? Mo4 O19 2.041(2) . ? Mo4 F6 2.1830(19) . ? Cu1 N2 1.951(3) . ? Cu1 O5 1.992(2) . ? Cu1 N3 2.020(3) . ? Cu1 N1 2.025(3) . ? Cu1 O11 2.094(2) . ? Cu2 O9 1.911(2) . ? Cu2 N5 1.934(3) . ? Cu2 N4 2.035(3) . ? Cu2 N6 2.044(3) . ? Cu2 O10 2.209(3) . ? Cu3 O21 1.907(2) . ? Cu3 N8 1.945(3) . ? Cu3 N9 2.033(3) . ? Cu3 N7 2.043(3) . ? Cu3 O22 2.311(3) . ? P1 O5 1.514(2) . ? P1 O6 1.530(2) . ? P1 O4 1.551(2) . ? P1 C46 1.803(3) . ? P2 O9 1.518(2) . ? P2 O3 1.525(2) . ? P2 O8 1.531(3) . ? P2 C53 1.805(3) 1_655 ? P3 O21 1.513(2) . ? P3 O14 1.535(2) . ? P3 O16 1.539(2) . ? P3 C54 1.802(3) . ? P4 O20 1.499(2) . ? P4 O19 1.545(2) . ? P4 O15 1.554(2) . ? P4 C61 1.809(4) 1_655 ? O10 H10A 0.835(18) . ? O10 H10B 0.811(18) . ? O11 H11A 0.8400 . ? O22 H22A 0.810(18) . ? O22 H22B 0.826(18) . ? O90 H90A 0.830(19) . ? O90 H90B 0.820(19) . ? N1 C1 1.342(4) . ? N1 C5 1.361(4) . ? N2 C10 1.336(4) . ? N2 C6 1.341(4) . ? N3 C15 1.344(4) . ? N3 C11 1.353(4) . ? N4 C30 1.331(4) . ? N4 C26 1.358(4) . ? N5 C21 1.340(4) . ? N5 C25 1.342(4) . ? N6 C16 1.339(4) . ? N6 C20 1.353(4) . ? N7 C31 1.329(5) . ? N7 C35 1.364(4) . ? N8 C40 1.335(5) . ? N8 C36 1.343(4) . ? N9 C45 1.338(4) . ? N9 C41 1.359(4) . ? C1 C2 1.380(5) . ? C1 H1 0.9500 . ? C2 C3 1.380(5) . ? C2 H2 0.9500 . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.474(5) . ? C6 C7 1.391(5) . ? C7 C8 1.383(5) . ? C7 H7 0.9500 . ? C8 C9 1.398(5) . ? C8 H8 0.9500 . ? C9 C10 1.384(5) . ? C9 H9 0.9500 . ? C10 C11 1.484(5) . ? C11 C12 1.390(5) . ? C12 C13 1.389(5) . ? C12 H12 0.9500 . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.381(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.388(5) . ? C16 H16 0.9500 . ? C17 C18 1.377(5) . ? C17 H17 0.9500 . ? C18 C19 1.392(5) . ? C18 H18 0.9500 . ? C19 C20 1.389(5) . ? C19 H19 0.9500 . ? C20 C21 1.470(5) . ? C21 C22 1.399(5) . ? C22 C23 1.394(5) . ? C22 H22 0.9500 . ? C23 C24 1.388(5) . ? C23 H23 0.9500 . ? C24 C25 1.386(5) . ? C24 H24 0.9500 . ? C25 C26 1.483(5) . ? C26 C27 1.391(5) . ? C27 C28 1.388(5) . ? C27 H27 0.9500 . ? C28 C29 1.380(5) . ? C28 H28 0.9500 . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.388(5) . ? C31 H31 0.9500 . ? C32 C33 1.388(5) . ? C32 H32 0.9500 . ? C33 C34 1.380(5) . ? C33 H33 0.9500 . ? C34 C35 1.382(5) . ? C34 H34 0.9500 . ? C35 C36 1.485(5) . ? C36 C37 1.389(5) . ? C37 C38 1.384(5) . ? C37 H37 0.9500 . ? C38 C39 1.390(5) . ? C38 H38 0.9500 . ? C39 C40 1.395(5) . ? C39 H39 0.9500 . ? C40 C41 1.485(5) . ? C41 C42 1.377(5) . ? C42 C43 1.384(5) . ? C42 H42 0.9500 . ? C43 C44 1.379(5) . ? C43 H43 0.9500 . ? C44 C45 1.387(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.520(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C52 1.403(5) . ? C47 C48 1.403(5) . ? C48 C49 1.387(5) . ? C48 H48 0.9500 . ? C49 C50 1.386(5) . ? C49 H49 0.9500 . ? C50 C51 1.383(5) . ? C50 H50 0.9500 . ? C51 C52 1.400(5) . ? C51 H51 0.9500 . ? C52 C53 1.513(5) . ? C53 P2 1.805(3) 1_455 ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.508(5) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C60 1.402(5) . ? C55 C56 1.405(5) . ? C56 C57 1.386(5) . ? C56 H56 0.9500 . ? C57 C58 1.391(5) . ? C57 H57 0.9500 . ? C58 C59 1.392(5) . ? C58 H58 0.9500 . ? C59 C60 1.393(5) . ? C59 H59 0.9500 . ? C60 C61 1.530(5) . ? C61 P4 1.809(3) 1_455 ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? 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 O1 Mo1 O2 100.88(11) . . ? O1 Mo1 F1 99.26(11) . . ? O2 Mo1 F1 96.82(11) . . ? O1 Mo1 O4 97.20(11) . . ? O2 Mo1 O4 92.38(10) . . ? F1 Mo1 O4 159.25(9) . . ? O1 Mo1 O3 93.55(10) . . ? O2 Mo1 O3 165.12(10) . . ? F1 Mo1 O3 84.29(9) . . ? O4 Mo1 O3 82.15(9) . . ? O1 Mo1 F2 175.65(10) . . ? O2 Mo1 F2 83.25(9) . . ? F1 Mo1 F2 81.47(8) . . ? O4 Mo1 F2 81.19(8) . . ? O3 Mo1 F2 82.24(8) . . ? O7 Mo2 F4 100.81(10) . . ? O7 Mo2 F3 99.82(11) . . ? F4 Mo2 F3 93.53(10) . . ? O7 Mo2 O8 94.53(11) . . ? F4 Mo2 O8 91.55(10) . . ? F3 Mo2 O8 163.59(9) . . ? O7 Mo2 O6 93.93(10) . . ? F4 Mo2 O6 164.89(10) . . ? F3 Mo2 O6 87.14(10) . . ? O8 Mo2 O6 83.94(10) . . ? O7 Mo2 F2 172.32(10) . . ? F4 Mo2 F2 84.51(9) . . ? F3 Mo2 F2 85.27(8) . . ? O8 Mo2 F2 79.69(8) . . ? O6 Mo2 F2 80.50(8) . . ? O13 Mo3 O12 102.83(11) . . ? O13 Mo3 F5 97.98(11) . . ? O12 Mo3 F5 96.31(10) . . ? O13 Mo3 O15 93.51(11) . . ? O12 Mo3 O15 92.65(10) . . ? F5 Mo3 O15 163.47(10) . . ? O13 Mo3 O14 92.58(10) . . ? O12 Mo3 O14 164.27(10) . . ? F5 Mo3 O14 84.46(9) . . ? O15 Mo3 O14 83.18(9) . . ? O13 Mo3 F6 170.16(10) . . ? O12 Mo3 F6 86.63(9) . . ? F5 Mo3 F6 83.47(8) . . ? O15 Mo3 F6 83.22(8) . . ? O14 Mo3 F6 77.84(8) . . ? O17 Mo4 O18 100.52(10) . . ? O17 Mo4 F7 99.69(11) . . ? O18 Mo4 F7 94.96(9) . . ? O17 Mo4 O16 97.86(10) . . ? O18 Mo4 O16 161.04(10) . . ? F7 Mo4 O16 86.45(9) . . ? O17 Mo4 O19 93.34(11) . . ? O18 Mo4 O19 90.50(10) . . ? F7 Mo4 O19 164.68(9) . . ? O16 Mo4 O19 83.80(9) . . ? O17 Mo4 F6 173.07(10) . . ? O18 Mo4 F6 81.51(8) . . ? F7 Mo4 F6 86.68(8) . . ? O16 Mo4 F6 79.70(8) . . ? O19 Mo4 F6 79.98(8) . . ? N2 Cu1 O5 135.71(11) . . ? N2 Cu1 N3 79.52(12) . . ? O5 Cu1 N3 97.63(11) . . ? N2 Cu1 N1 79.90(12) . . ? O5 Cu1 N1 97.50(11) . . ? N3 Cu1 N1 159.41(11) . . ? N2 Cu1 O11 123.67(11) . . ? O5 Cu1 O11 100.61(9) . . ? N3 Cu1 O11 96.77(11) . . ? N1 Cu1 O11 94.08(11) . . ? O9 Cu2 N5 172.66(11) . . ? O9 Cu2 N4 96.90(11) . . ? N5 Cu2 N4 80.15(12) . . ? O9 Cu2 N6 101.97(11) . . ? N5 Cu2 N6 80.12(12) . . ? N4 Cu2 N6 159.38(12) . . ? O9 Cu2 O10 91.79(10) . . ? N5 Cu2 O10 95.04(11) . . ? N4 Cu2 O10 92.49(11) . . ? N6 Cu2 O10 95.14(11) . . ? O21 Cu3 N8 177.87(11) . . ? O21 Cu3 N9 98.44(11) . . ? N8 Cu3 N9 79.84(12) . . ? O21 Cu3 N7 101.73(11) . . ? N8 Cu3 N7 80.07(12) . . ? N9 Cu3 N7 159.55(11) . . ? O21 Cu3 O22 88.94(10) . . ? N8 Cu3 O22 89.97(11) . . ? N9 Cu3 O22 95.66(10) . . ? N7 Cu3 O22 88.06(10) . . ? O5 P1 O6 112.01(14) . . ? O5 P1 O4 109.99(14) . . ? O6 P1 O4 111.36(13) . . ? O5 P1 C46 110.75(15) . . ? O6 P1 C46 108.09(15) . . ? O4 P1 C46 104.37(15) . . ? O9 P2 O3 111.71(13) . . ? O9 P2 O8 110.86(13) . . ? O3 P2 O8 112.75(13) . . ? O9 P2 C53 107.98(14) . 1_655 ? O3 P2 C53 108.35(14) . 1_655 ? O8 P2 C53 104.82(15) . 1_655 ? O21 P3 O14 111.66(13) . . ? O21 P3 O16 112.78(13) . . ? O14 P3 O16 111.95(13) . . ? O21 P3 C54 108.53(15) . . ? O14 P3 C54 106.33(15) . . ? O16 P3 C54 105.12(14) . . ? O20 P4 O19 113.71(14) . . ? O20 P4 O15 110.53(13) . . ? O19 P4 O15 110.39(13) . . ? O20 P4 C61 111.85(15) . 1_655 ? O19 P4 C61 105.88(15) . 1_655 ? O15 P4 C61 103.96(15) . 1_655 ? Mo2 F2 Mo1 141.54(10) . . ? Mo3 F6 Mo4 139.43(9) . . ? P2 O3 Mo1 137.38(15) . . ? P1 O4 Mo1 142.27(15) . . ? P1 O5 Cu1 122.64(13) . . ? P1 O6 Mo2 140.65(15) . . ? P2 O8 Mo2 146.73(15) . . ? P2 O9 Cu2 125.67(15) . . ? Cu2 O10 H10A 116(3) . . ? Cu2 O10 H10B 119(3) . . ? H10A O10 H10B 98(4) . . ? Cu1 O11 H11A 109.5 . . ? P3 O14 Mo3 136.95(13) . . ? P4 O15 Mo3 141.90(14) . . ? P3 O16 Mo4 138.48(14) . . ? P4 O19 Mo4 137.09(13) . . ? P3 O21 Cu3 136.22(14) . . ? Cu3 O22 H22A 112(3) . . ? Cu3 O22 H22B 110(3) . . ? H22A O22 H22B 108(4) . . ? H90A O90 H90B 104(4) . . ? C1 N1 C5 118.7(3) . . ? C1 N1 Cu1 126.7(2) . . ? C5 N1 Cu1 114.6(2) . . ? C10 N2 C6 122.3(3) . . ? C10 N2 Cu1 119.0(2) . . ? C6 N2 Cu1 118.3(2) . . ? C15 N3 C11 118.4(3) . . ? C15 N3 Cu1 126.5(2) . . ? C11 N3 Cu1 115.1(2) . . ? C30 N4 C26 119.4(3) . . ? C30 N4 Cu2 126.5(2) . . ? C26 N4 Cu2 113.6(2) . . ? C21 N5 C25 122.5(3) . . ? C21 N5 Cu2 118.7(2) . . ? C25 N5 Cu2 118.8(2) . . ? C16 N6 C20 119.2(3) . . ? C16 N6 Cu2 127.4(2) . . ? C20 N6 Cu2 113.4(2) . . ? C31 N7 C35 118.9(3) . . ? C31 N7 Cu3 127.3(2) . . ? C35 N7 Cu3 113.5(2) . . ? C40 N8 C36 122.0(3) . . ? C40 N8 Cu3 119.0(2) . . ? C36 N8 Cu3 118.8(2) . . ? C45 N9 C41 118.0(3) . . ? C45 N9 Cu3 127.2(2) . . ? C41 N9 Cu3 114.3(2) . . ? N1 C1 C2 122.7(3) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.5(3) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C4 C5 119.1(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 113.9(3) . . ? C4 C5 C6 124.8(3) . . ? N2 C6 C7 120.0(3) . . ? N2 C6 C5 113.2(3) . . ? C7 C6 C5 126.8(3) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C7 C8 C9 120.9(3) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C10 C9 C8 117.7(3) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? N2 C10 C9 120.7(3) . . ? N2 C10 C11 112.4(3) . . ? C9 C10 C11 126.9(3) . . ? N3 C11 C12 122.1(3) . . ? N3 C11 C10 113.8(3) . . ? C12 C11 C10 124.2(3) . . ? C13 C12 C11 119.0(3) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 118.7(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? N3 C15 C14 122.4(3) . . ? N3 C15 H15 118.8 . . ? C14 C15 H15 118.8 . . ? N6 C16 C17 122.2(3) . . ? N6 C16 H16 118.9 . . ? C17 C16 H16 118.9 . . ? C18 C17 C16 118.9(3) . . ? C18 C17 H17 120.5 . . ? C16 C17 H17 120.5 . . ? C17 C18 C19 119.4(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C20 C19 C18 118.8(3) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? N6 C20 C19 121.5(3) . . ? N6 C20 C21 114.7(3) . . ? C19 C20 C21 123.8(3) . . ? N5 C21 C22 119.8(3) . . ? N5 C21 C20 113.1(3) . . ? C22 C21 C20 127.1(3) . . ? C23 C22 C21 118.4(4) . . ? C23 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C24 C23 C22 120.3(3) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 118.7(4) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? N5 C25 C24 120.3(3) . . ? N5 C25 C26 112.7(3) . . ? C24 C25 C26 127.0(3) . . ? N4 C26 C27 121.1(3) . . ? N4 C26 C25 114.0(3) . . ? C27 C26 C25 124.9(3) . . ? C28 C27 C26 118.8(4) . . ? C28 C27 H27 120.6 . . ? C26 C27 H27 120.6 . . ? C29 C28 C27 119.7(4) . . ? C29 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C28 C29 C30 118.5(4) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? N4 C30 C29 122.4(3) . . ? N4 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N7 C31 C32 122.4(3) . . ? N7 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C31 C32 C33 118.6(4) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 119.5(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.0(3) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N7 C35 C34 121.6(3) . . ? N7 C35 C36 114.4(3) . . ? C34 C35 C36 124.0(3) . . ? N8 C36 C37 120.5(3) . . ? N8 C36 C35 112.6(3) . . ? C37 C36 C35 126.9(3) . . ? C38 C37 C36 118.3(3) . . ? C38 C37 H37 120.8 . . ? C36 C37 H37 120.8 . . ? C37 C38 C39 120.5(3) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C40 118.4(4) . . ? C38 C39 H39 120.8 . . ? C40 C39 H39 120.8 . . ? N8 C40 C39 120.2(3) . . ? N8 C40 C41 112.8(3) . . ? C39 C40 C41 127.0(3) . . ? N9 C41 C42 122.4(3) . . ? N9 C41 C40 113.9(3) . . ? C42 C41 C40 123.6(3) . . ? C41 C42 C43 118.8(3) . . ? C41 C42 H42 120.6 . . ? C43 C42 H42 120.6 . . ? C44 C43 C42 119.3(4) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 118.9(3) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? N9 C45 C44 122.5(3) . . ? N9 C45 H45 118.7 . . ? C44 C45 H45 118.7 . . ? C47 C46 P1 118.4(2) . . ? C47 C46 H46A 107.7 . . ? P1 C46 H46A 107.7 . . ? C47 C46 H46B 107.7 . . ? P1 C46 H46B 107.7 . . ? H46A C46 H46B 107.1 . . ? C52 C47 C48 117.7(3) . . ? C52 C47 C46 120.6(3) . . ? C48 C47 C46 121.7(3) . . ? C49 C48 C47 121.9(3) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C50 C49 C48 119.8(3) . . ? C50 C49 H49 120.1 . . ? C48 C49 H49 120.1 . . ? C51 C50 C49 119.5(3) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 121.0(3) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C51 C52 C47 120.1(3) . . ? C51 C52 C53 116.9(3) . . ? C47 C52 C53 122.9(3) . . ? C52 C53 P2 110.3(2) . 1_455 ? C52 C53 H53A 109.6 . . ? P2 C53 H53A 109.6 1_455 . ? C52 C53 H53B 109.6 . . ? P2 C53 H53B 109.6 1_455 . ? H53A C53 H53B 108.1 . . ? C55 C54 P3 113.7(2) . . ? C55 C54 H54A 108.8 . . ? P3 C54 H54A 108.8 . . ? C55 C54 H54B 108.8 . . ? P3 C54 H54B 108.8 . . ? H54A C54 H54B 107.7 . . ? C60 C55 C56 119.2(3) . . ? C60 C55 C54 123.8(3) . . ? C56 C55 C54 117.0(3) . . ? C57 C56 C55 121.3(3) . . ? C57 C56 H56 119.3 . . ? C55 C56 H56 119.3 . . ? C56 C57 C58 119.7(3) . . ? C56 C57 H57 120.2 . . ? C58 C57 H57 120.2 . . ? C57 C58 C59 119.1(3) . . ? C57 C58 H58 120.4 . . ? C59 C58 H58 120.4 . . ? C58 C59 C60 122.1(3) . . ? C58 C59 H59 119.0 . . ? C60 C59 H59 119.0 . . ? C59 C60 C55 118.6(3) . . ? C59 C60 C61 121.6(3) . . ? C55 C60 C61 119.7(3) . . ? C60 C61 P4 118.0(3) . 1_455 ? C60 C61 H61A 107.8 . . ? P4 C61 H61A 107.8 1_455 . ? C60 C61 H61B 107.8 . . ? P4 C61 H61B 107.8 1_455 . ? H61A C61 H61B 107.1 . . ? _refine_diff_density_max 0.801 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.121 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 957901' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound14 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Cu3 F2 Mo2 N4 O18 P4' _chemical_formula_sum 'C36 H36 Cu3 F2 Mo2 N4 O18 P4' _chemical_formula_weight 1357.07 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' F F 0.0171 0.0103 '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' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.562(2) _cell_length_b 19.809(5) _cell_length_c 13.219(3) _cell_angle_alpha 90 _cell_angle_beta 103.447(3) _cell_angle_gamma 90 _cell_volume 2180.5(9) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 1189 _cell_measurement_theta_min 2.0121 _cell_measurement_theta_max 27.7623 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_density_meas 2.00(2) _exptl_crystal_density_method flotation _exptl_crystal_density_diffrn 2.067 _exptl_crystal_F_000 1346 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.191 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_min 0.104 _exptl_absorpt_coefficient_mu 2.236 _shelx_estimated_absorpt_T_min 0.675 _shelx_estimated_absorpt_T_max 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.80 _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15384 _diffrn_reflns_av_unetI/netI 0.0514 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.056 _diffrn_reflns_theta_max 26.021 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 4293 _reflns_number_gt 3616 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2 (Bruker, 2011)' _computing_cell_refinement 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.30C (Bruker AXS Inc., 2013)' _computing_structure_solution 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalMaker (Palmer, 2010)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2011)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+16.0284P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4293 _refine_ls_number_parameters 320 _refine_ls_number_restraints 101 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1262 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 0.59126(6) 0.08461(3) 0.85379(4) 0.01533(15) Uani 1 1 d . U . . . Cu1 Cu 0.5000 0.5000 0.5000 0.0095(2) Uani 1 2 d S U P . . Cu2 Cu 0.25524(8) 0.47869(3) 0.80027(5) 0.01162(17) Uani 1 1 d . U . . . P1 P 0.31133(16) 0.39203(7) 0.60006(10) 0.0105(3) Uani 1 1 d . U . . . P2 P 0.19712(16) 0.08524(7) 0.86128(10) 0.0100(3) Uani 1 1 d . U . . . F1 F 0.7890(4) 0.04757(18) 0.8549(2) 0.0200(7) Uani 1 1 d . U . . . O1 O 0.2739(4) 0.4099(2) 0.7026(3) 0.0133(8) Uani 1 1 d . U . . . O2 O 0.1626(4) 0.4092(2) 0.5124(3) 0.0132(8) Uani 1 1 d . U . . . O3 O 0.4635(4) 0.42138(19) 0.5799(3) 0.0123(8) Uani 1 1 d . U . . . O4 O 0.3779(4) 0.1025(2) 0.8844(3) 0.0149(8) Uani 1 1 d . U . . . O5 O 0.1693(4) 0.04957(19) 0.9566(3) 0.0114(8) Uani 1 1 d . U . . . O6 O 0.1425(4) 0.04842(19) 0.7593(3) 0.0127(8) Uani 1 1 d . U . . . O7 O 0.5590(5) -0.0252(2) 0.8987(3) 0.0148(8) Uani 1 1 d D U . . . H7C H 0.482(4) -0.039(3) 0.923(4) 0.018 Uiso 1 1 d D U . . . H7D H 0.646(4) -0.037(3) 0.939(4) 0.018 Uiso 1 1 d D U . . . O8 O 0.4907(4) 0.05269(19) 0.7286(3) 0.0105(8) Uani 1 1 d . U . . . O9 O 0.6335(5) 0.1644(2) 0.8264(3) 0.0189(9) Uani 1 1 d . U . . . N1 N 0.1289(5) 0.4164(2) 0.8675(3) 0.0133(9) Uani 1 1 d . U . . . N2 N 0.2983(5) 0.5213(2) 0.9412(3) 0.0134(9) Uani 1 1 d . U . . . C1 C 0.0342(7) 0.3675(3) 0.8180(5) 0.0193(12) Uani 1 1 d . U . . . H1 H 0.0311 0.3587 0.7469 0.023 Uiso 1 1 calc R U . . . C2 C -0.0603(8) 0.3290(3) 0.8689(5) 0.0218(13) Uani 1 1 d . U . . . H2 H -0.1297 0.2950 0.8328 0.026 Uiso 1 1 calc R U . . . C3 C -0.0510(8) 0.3412(3) 0.9722(5) 0.0232(13) Uani 1 1 d . U . . . H3 H -0.1133 0.3152 1.0087 0.028 Uiso 1 1 calc R U . . . C4 C 0.0490(7) 0.3915(3) 1.0235(5) 0.0194(12) Uani 1 1 d . U . . . H4 H 0.0572 0.4001 1.0952 0.023 Uiso 1 1 calc R U . . . C5 C 0.1362(7) 0.4287(3) 0.9683(4) 0.0148(11) Uani 1 1 d . U . . . C6 C 0.2403(6) 0.4860(3) 1.0119(4) 0.0151(11) Uani 1 1 d . U . . . C7 C 0.2754(7) 0.5045(3) 1.1158(4) 0.0184(12) Uani 1 1 d . U . . . H7 H 0.2343 0.4790 1.1647 0.022 Uiso 1 1 calc R U . . . C8 C 0.3702(7) 0.5601(3) 1.1475(4) 0.0214(13) Uani 1 1 d . U . . . H8 H 0.3967 0.5732 1.2186 0.026 Uiso 1 1 calc R U . . . C9 C 0.4261(7) 0.5965(3) 1.0749(5) 0.0198(12) Uani 1 1 d . U . . . H9 H 0.4901 0.6356 1.0950 0.024 Uiso 1 1 calc R U . . . C10 C 0.3883(7) 0.5756(3) 0.9716(4) 0.0164(12) Uani 1 1 d . U . . . H10 H 0.4276 0.6008 0.9216 0.020 Uiso 1 1 calc R U . . . C11 C 0.3306(7) 0.3015(3) 0.5984(5) 0.0164(11) Uani 1 1 d . U . . . H11A H 0.3425 0.2875 0.5287 0.020 Uiso 1 1 calc R U . . . H11B H 0.4302 0.2884 0.6494 0.020 Uiso 1 1 calc R U . . . C12 C 0.1925(7) 0.2634(3) 0.6231(4) 0.0143(11) Uani 1 1 d . U . . . C13 C 0.0455(7) 0.2600(3) 0.5505(5) 0.0203(13) Uani 1 1 d . U . . . H13 H 0.0334 0.2807 0.4843 0.024 Uiso 1 1 calc R U . . . C14 C -0.0833(7) 0.2265(3) 0.5752(5) 0.0235(14) Uani 1 1 d . U . . . H14 H -0.1829 0.2241 0.5254 0.028 Uiso 1 1 calc R U . . . C15 C 0.2052(6) 0.2315(3) 0.7191(4) 0.0127(11) Uani 1 1 d . U . . . H15 H 0.3051 0.2328 0.7688 0.015 Uiso 1 1 calc R U . . . C16 C 0.0783(7) 0.1985(3) 0.7440(4) 0.0136(11) Uani 1 1 d . U . . . C17 C -0.0683(7) 0.1967(3) 0.6711(5) 0.0186(12) Uani 1 1 d . U . . . H17 H -0.1580 0.1748 0.6876 0.022 Uiso 1 1 calc R U . . . C18 C 0.0906(7) 0.1645(3) 0.8479(4) 0.0141(11) Uani 1 1 d . U . . . H18A H -0.0191 0.1566 0.8578 0.017 Uiso 1 1 calc R U . . . H18B H 0.1459 0.1955 0.9037 0.017 Uiso 1 1 calc R 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 Mo1 0.0201(3) 0.0162(3) 0.0103(3) 0.00119(19) 0.00481(19) 0.0009(2) Cu1 0.0079(4) 0.0123(5) 0.0071(4) 0.0002(3) -0.0006(3) -0.0003(3) Cu2 0.0125(3) 0.0152(4) 0.0058(3) 0.0003(3) -0.0007(2) -0.0011(3) P1 0.0096(6) 0.0131(7) 0.0070(6) 0.0004(5) -0.0018(5) -0.0009(5) P2 0.0091(6) 0.0130(7) 0.0063(6) 0.0007(5) -0.0015(5) -0.0001(5) F1 0.0153(16) 0.0290(19) 0.0131(16) -0.0009(14) -0.0023(13) 0.0002(14) O1 0.0137(19) 0.017(2) 0.0077(17) -0.0016(15) -0.0011(14) -0.0025(16) O2 0.0109(18) 0.019(2) 0.0077(18) 0.0015(15) -0.0022(14) 0.0002(15) O3 0.0117(18) 0.0139(19) 0.0095(18) 0.0034(15) -0.0010(14) 0.0005(15) O4 0.0100(18) 0.020(2) 0.0128(19) 0.0018(16) -0.0015(14) -0.0003(15) O5 0.0101(18) 0.015(2) 0.0074(17) 0.0012(15) -0.0015(14) -0.0022(15) O6 0.0123(18) 0.0146(19) 0.0088(17) -0.0014(15) -0.0023(14) 0.0025(15) O7 0.0097(18) 0.020(2) 0.0123(19) 0.0035(16) -0.0024(15) 0.0004(16) O8 0.0075(17) 0.0167(19) 0.0048(16) -0.0002(14) -0.0035(13) 0.0009(15) O9 0.017(2) 0.020(2) 0.018(2) 0.0019(17) 0.0000(16) -0.0026(16) N1 0.014(2) 0.017(2) 0.008(2) 0.0017(18) 0.0018(17) 0.0034(18) N2 0.011(2) 0.018(2) 0.008(2) 0.0013(18) -0.0036(17) 0.0041(18) C1 0.021(3) 0.019(3) 0.018(3) -0.004(2) 0.005(2) -0.001(2) C2 0.025(3) 0.013(3) 0.029(3) -0.003(2) 0.009(3) 0.000(2) C3 0.029(3) 0.017(3) 0.027(3) 0.007(3) 0.015(3) 0.003(2) C4 0.026(3) 0.021(3) 0.014(3) 0.004(2) 0.008(2) 0.008(2) C5 0.017(3) 0.018(3) 0.009(2) 0.003(2) 0.002(2) 0.008(2) C6 0.011(3) 0.022(3) 0.011(2) 0.002(2) 0.000(2) 0.008(2) C7 0.017(3) 0.030(3) 0.007(2) 0.003(2) 0.001(2) 0.005(2) C8 0.014(3) 0.036(4) 0.011(3) -0.004(2) -0.003(2) 0.007(3) C9 0.012(3) 0.030(3) 0.016(3) -0.008(2) -0.001(2) 0.001(2) C10 0.013(3) 0.021(3) 0.013(3) -0.002(2) -0.002(2) 0.002(2) C11 0.018(3) 0.013(3) 0.017(3) 0.001(2) 0.001(2) 0.003(2) C12 0.018(3) 0.008(3) 0.015(3) -0.002(2) 0.002(2) 0.000(2) C13 0.027(3) 0.019(3) 0.011(3) 0.006(2) -0.003(2) -0.002(2) C14 0.019(3) 0.023(3) 0.021(3) 0.006(3) -0.010(2) -0.004(3) C15 0.012(3) 0.015(3) 0.010(2) -0.001(2) 0.001(2) 0.003(2) C16 0.015(3) 0.013(3) 0.011(3) -0.001(2) -0.001(2) 0.003(2) C17 0.013(3) 0.018(3) 0.021(3) 0.006(2) -0.004(2) -0.003(2) C18 0.013(3) 0.017(3) 0.011(3) -0.002(2) 0.000(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 O9 1.680(4) . ? Mo1 O8 1.794(3) . ? Mo1 F1 1.842(3) . ? Mo1 O4 1.992(4) . ? Mo1 O2 2.047(4) 4_666 ? Mo1 O7 2.289(4) . ? Cu1 O5 1.944(4) 4_665 ? Cu1 O5 1.944(4) 2_556 ? Cu1 O3 1.947(4) 3_666 ? Cu1 O3 1.947(4) . ? Cu2 O6 1.902(4) 2_556 ? Cu2 O1 1.909(4) . ? Cu2 N1 1.983(5) . ? Cu2 N2 1.999(5) . ? P1 O3 1.506(4) . ? P1 O1 1.506(4) . ? P1 O2 1.547(4) . ? P1 C11 1.802(6) . ? P2 O6 1.508(4) . ? P2 O5 1.511(4) . ? P2 O4 1.545(4) . ? P2 C18 1.804(6) . ? O2 Mo1 2.047(4) 4_565 ? O5 Cu1 1.944(4) 2_546 ? O6 Cu2 1.902(4) 2_546 ? O7 H7C 0.84(2) . ? O7 H7D 0.84(2) . ? N1 C1 1.334(8) . ? N1 C5 1.341(7) . ? N2 C10 1.330(7) . ? N2 C6 1.351(7) . ? C1 C2 1.393(9) . ? C1 H1 0.9500 . ? C2 C3 1.372(9) . ? C2 H2 0.9500 . ? C3 C4 1.384(9) . ? C3 H3 0.9500 . ? C4 C5 1.373(8) . ? C4 H4 0.9500 . ? C5 C6 1.475(8) . ? C6 C7 1.386(8) . ? C7 C8 1.374(9) . ? C7 H7 0.9500 . ? C8 C9 1.372(9) . ? C8 H8 0.9500 . ? C9 C10 1.391(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.501(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.395(8) . ? C12 C15 1.399(8) . ? C13 C14 1.389(9) . ? C13 H13 0.9500 . ? C14 C17 1.377(8) . ? C14 H14 0.9500 . ? C15 C16 1.372(8) . ? C15 H15 0.9500 . ? C16 C17 1.394(8) . ? C16 C18 1.510(8) . ? C17 H17 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? 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 O9 Mo1 O8 102.35(18) . . ? O9 Mo1 F1 97.65(18) . . ? O8 Mo1 F1 96.31(15) . . ? O9 Mo1 O4 97.45(18) . . ? O8 Mo1 O4 89.09(16) . . ? F1 Mo1 O4 162.47(16) . . ? O9 Mo1 O2 97.85(18) . 4_666 ? O8 Mo1 O2 158.63(16) . 4_666 ? F1 Mo1 O2 87.79(15) . 4_666 ? O4 Mo1 O2 81.39(15) . 4_666 ? O9 Mo1 O7 174.57(17) . . ? O8 Mo1 O7 80.98(16) . . ? F1 Mo1 O7 77.61(15) . . ? O4 Mo1 O7 86.84(15) . . ? O2 Mo1 O7 79.44(15) 4_666 . ? O5 Cu1 O5 180.0 4_665 2_556 ? O5 Cu1 O3 91.10(16) 4_665 3_666 ? O5 Cu1 O3 88.90(16) 2_556 3_666 ? O5 Cu1 O3 88.90(16) 4_665 . ? O5 Cu1 O3 91.10(16) 2_556 . ? O3 Cu1 O3 180.0(2) 3_666 . ? O6 Cu2 O1 96.87(17) 2_556 . ? O6 Cu2 N1 171.76(18) 2_556 . ? O1 Cu2 N1 89.95(18) . . ? O6 Cu2 N2 94.38(18) 2_556 . ? O1 Cu2 N2 154.79(17) . . ? N1 Cu2 N2 81.17(19) . . ? O3 P1 O1 116.3(2) . . ? O3 P1 O2 112.2(2) . . ? O1 P1 O2 108.2(2) . . ? O3 P1 C11 107.3(2) . . ? O1 P1 C11 106.5(3) . . ? O2 P1 C11 105.7(2) . . ? O6 P2 O5 116.3(2) . . ? O6 P2 O4 111.9(2) . . ? O5 P2 O4 106.5(2) . . ? O6 P2 C18 106.8(2) . . ? O5 P2 C18 108.3(2) . . ? O4 P2 C18 106.7(2) . . ? P1 O1 Cu2 147.7(3) . . ? P1 O2 Mo1 141.1(2) . 4_565 ? P1 O3 Cu1 131.2(2) . . ? P2 O4 Mo1 147.6(3) . . ? P2 O5 Cu1 139.0(2) . 2_546 ? P2 O6 Cu2 130.1(2) . 2_546 ? Mo1 O7 H7C 124(4) . . ? Mo1 O7 H7D 107(4) . . ? H7C O7 H7D 109(4) . . ? C1 N1 C5 120.2(5) . . ? C1 N1 Cu2 124.4(4) . . ? C5 N1 Cu2 115.3(4) . . ? C10 N2 C6 119.3(5) . . ? C10 N2 Cu2 126.3(4) . . ? C6 N2 Cu2 114.1(4) . . ? N1 C1 C2 121.0(6) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C3 C2 C1 118.6(6) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 120.1(6) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 118.5(6) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 121.6(6) . . ? N1 C5 C6 114.3(5) . . ? C4 C5 C6 124.0(5) . . ? N2 C6 C7 121.3(6) . . ? N2 C6 C5 114.5(5) . . ? C7 C6 C5 124.2(5) . . ? C8 C7 C6 119.4(6) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 119.0(5) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C8 C9 C10 119.4(6) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 121.6(6) . . ? N2 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C12 C11 P1 114.8(4) . . ? C12 C11 H11A 108.6 . . ? P1 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? P1 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? C13 C12 C15 118.0(5) . . ? C13 C12 C11 120.3(5) . . ? C15 C12 C11 121.7(5) . . ? C14 C13 C12 120.0(5) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C17 C14 C13 120.8(5) . . ? C17 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C16 C15 C12 122.3(5) . . ? C16 C15 H15 118.9 . . ? C12 C15 H15 118.9 . . ? C15 C16 C17 118.8(5) . . ? C15 C16 C18 122.6(5) . . ? C17 C16 C18 118.6(5) . . ? C14 C17 C16 120.1(6) . . ? C14 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C16 C18 P2 113.8(4) . . ? C16 C18 H18A 108.8 . . ? P2 C18 H18A 108.8 . . ? C16 C18 H18B 108.8 . . ? P2 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? _refine_diff_density_max 0.840 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.162 _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 957902'