# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C # 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_SP4Mo8.CH3CN _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H98 Mo8 N10 O30' _chemical_formula_weight 2495.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_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 16.176(4) _cell_length_b 17.079(4) _cell_length_c 35.499(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.157(5) _cell_angle_gamma 90.00 _cell_volume 9654(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 12341 _cell_measurement_theta_min 1.17 _cell_measurement_theta_max 25 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4992 _exptl_absorpt_coefficient_mu 1.086 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8121 _exptl_absorpt_correction_T_max 0.9786 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25496 _diffrn_reflns_av_R_equivalents 0.0995 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8478 _reflns_number_gt 5404 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1041P)^2^+184.7061P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8478 _refine_ls_number_parameters 600 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1365 _refine_ls_R_factor_gt 0.0901 _refine_ls_wR_factor_ref 0.2512 _refine_ls_wR_factor_gt 0.2299 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.015 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.69429(6) 0.33968(5) -0.00158(3) 0.0345(3) Uani 1 1 d . . . Mo2 Mo 0.53738(6) 0.21201(6) 0.01451(3) 0.0435(3) Uani 1 1 d . . . Mo3 Mo 0.78316(7) 0.29998(7) -0.07358(3) 0.0439(3) Uani 1 1 d . . . Mo4 Mo 0.87067(6) 0.32848(6) 0.05734(3) 0.0393(3) Uani 1 1 d . . . O1 O 0.7446(5) 0.3277(5) 0.0516(2) 0.044(2) Uani 1 1 d . . . O2 O 0.8804(5) 0.4251(5) 0.0491(2) 0.048(2) Uani 1 1 d . . . O3 O 0.7089(5) 0.4357(4) -0.0072(2) 0.048(2) Uani 1 1 d . . . O4 O 0.8975(6) 0.3191(6) 0.1052(3) 0.060(2) Uani 1 1 d . . . O5 O 0.5897(5) 0.3342(4) 0.0054(2) 0.045(2) Uani 1 1 d . . . O6 O 0.6749(5) 0.3021(4) -0.0543(2) 0.0413(19) Uani 1 1 d . . . O7 O 0.7930(6) 0.3998(5) -0.0786(2) 0.057(2) Uani 1 1 d . . . O8 O 0.8159(4) 0.2972(4) -0.0067(2) 0.0372(18) Uani 1 1 d . . . O9 O 0.9651(5) 0.2862(5) 0.0397(2) 0.048(2) Uani 1 1 d . . . O10 O 0.6030(5) 0.2345(5) 0.0639(2) 0.048(2) Uani 1 1 d . . . O11 O 0.5270(5) 0.1145(5) 0.0223(3) 0.061(2) Uani 1 1 d . . . O12 O 0.7529(6) 0.2642(6) -0.1189(3) 0.069(3) Uani 1 1 d . . . O13 O 0.4405(5) 0.2488(6) 0.0178(3) 0.070(3) Uani 1 1 d . . . O1A O 0.7747(5) 0.6279(5) 0.1151(2) 0.051(2) Uani 1 1 d . . . N1A N 0.6120(6) 0.4818(6) 0.0886(3) 0.050(3) Uani 1 1 d . . . N2A N 0.9193(6) 0.6122(6) 0.1337(3) 0.047(2) Uani 1 1 d . . . C1A C 0.8401(7) 0.5865(8) 0.1425(4) 0.051(3) Uani 1 1 d . . . C2A C 0.8296(8) 0.4984(8) 0.1363(4) 0.056(3) Uani 1 1 d . . . H2A H 0.8761 0.4667 0.1444 0.068 Uiso 1 1 calc R . . C3A C 0.7600(8) 0.4648(8) 0.1203(4) 0.054(3) Uani 1 1 d . . . H3A H 0.7554 0.4105 0.1199 0.064 Uiso 1 1 calc R . . C4A C 0.6896(7) 0.5129(8) 0.1032(3) 0.047(3) Uani 1 1 d . . . C5A C 0.7007(7) 0.5928(7) 0.1004(3) 0.041(3) Uani 1 1 d . . . C6A C 0.6382(8) 0.6391(8) 0.0798(4) 0.056(4) Uani 1 1 d . . . H6A H 0.6463 0.6925 0.0769 0.068 Uiso 1 1 calc R . . C7A C 0.5622(9) 0.6029(11) 0.0634(5) 0.077(5) Uani 1 1 d . . . H7A H 0.5199 0.6320 0.0485 0.092 Uiso 1 1 calc R . . C8A C 0.5504(9) 0.5233(10) 0.0694(5) 0.073(5) Uani 1 1 d . . . C9A C 0.4699(11) 0.4841(12) 0.0518(7) 0.123(9) Uani 1 1 d . . . H9A1 H 0.4409 0.5159 0.0313 0.185 Uiso 1 1 calc R . . H9A2 H 0.4352 0.4773 0.0709 0.185 Uiso 1 1 calc R . . H9A3 H 0.4820 0.4339 0.0418 0.185 Uiso 1 1 calc R . . C10A C 0.5971(10) 0.3977(8) 0.0956(5) 0.072(4) Uani 1 1 d . . . H10A H 0.6057 0.3675 0.0738 0.107 Uiso 1 1 calc R . . H10B H 0.5406 0.3907 0.0998 0.107 Uiso 1 1 calc R . . H10C H 0.6356 0.3805 0.1178 0.107 Uiso 1 1 calc R . . C11A C 0.8395(8) 0.6175(9) 0.1829(4) 0.057(3) Uani 1 1 d . . . C12A C 0.8899(10) 0.6902(9) 0.1827(4) 0.066(4) Uani 1 1 d . . . C13A C 0.8927(13) 0.7573(12) 0.2056(5) 0.097(6) Uani 1 1 d . . . H13A H 0.8590 0.7623 0.2241 0.116 Uiso 1 1 calc R . . C14A C 0.9477(15) 0.8154(13) 0.1994(5) 0.112(8) Uani 1 1 d . . . H14A H 0.9514 0.8604 0.2143 0.134 Uiso 1 1 calc R . . C15A C 0.9986(14) 0.8087(14) 0.1711(6) 0.122(9) Uani 1 1 d . . . H15A H 1.0367 0.8480 0.1681 0.147 Uiso 1 1 calc R . . C16A C 0.9913(9) 0.7432(9) 0.1480(5) 0.068(4) Uani 1 1 d . . . H16A H 1.0231 0.7393 0.1286 0.081 Uiso 1 1 calc R . . C17A C 0.9370(8) 0.6835(9) 0.1534(4) 0.059(4) Uani 1 1 d . . . C18A C 0.7493(11) 0.6295(11) 0.1906(5) 0.091(6) Uani 1 1 d . . . H18A H 0.7515 0.6537 0.2152 0.137 Uiso 1 1 calc R . . H18B H 0.7216 0.5798 0.1903 0.137 Uiso 1 1 calc R . . H18C H 0.7187 0.6626 0.1711 0.137 Uiso 1 1 calc R . . C19A C 0.8874(11) 0.5599(12) 0.2129(4) 0.095(6) Uani 1 1 d . . . H19A H 0.9389 0.5444 0.2051 0.142 Uiso 1 1 calc R . . H19B H 0.8533 0.5146 0.2147 0.142 Uiso 1 1 calc R . . H19C H 0.8997 0.5853 0.2374 0.142 Uiso 1 1 calc R . . C20A C 0.9378(9) 0.6033(8) 0.0954(4) 0.057(3) Uani 1 1 d . . . H20A H 0.9225 0.5515 0.0861 0.086 Uiso 1 1 calc R . . H20B H 0.9968 0.6113 0.0959 0.086 Uiso 1 1 calc R . . H20C H 0.9064 0.6412 0.0787 0.086 Uiso 1 1 calc R . . O1B O 1.1993(6) 0.3563(6) 0.1475(3) 0.070(3) Uani 1 1 d . . . N1B N 1.1852(6) 0.4093(6) 0.0484(3) 0.046(3) Uani 1 1 d . . . N2B N 1.1071(9) 0.3776(12) 0.1901(4) 0.106(6) Uani 1 1 d . . . C1B C 1.1457(9) 0.4179(12) 0.1620(5) 0.077(5) Uani 1 1 d . . . C2B C 1.0874(10) 0.4506(10) 0.1288(5) 0.078(5) Uani 1 1 d . . . H2B H 1.0395 0.4749 0.1343 0.094 Uiso 1 1 calc R . . C3B C 1.0946(9) 0.4496(10) 0.0940(5) 0.069(4) Uani 1 1 d . . . H3B H 1.0555 0.4747 0.0756 0.083 Uiso 1 1 calc R . . C4B C 1.1670(8) 0.4075(8) 0.0832(4) 0.052(3) Uani 1 1 d . . . C5B C 1.2160(9) 0.3629(8) 0.1116(4) 0.055(3) Uani 1 1 d . . . C6B C 1.2836(10) 0.3200(9) 0.1033(4) 0.064(4) Uani 1 1 d . . . H6B H 1.3174 0.2904 0.1219 0.076 Uiso 1 1 calc R . . C7B C 1.2982(9) 0.3231(7) 0.0665(4) 0.054(3) Uani 1 1 d . . . H7B H 1.3424 0.2939 0.0602 0.064 Uiso 1 1 calc R . . C8B C 1.2503(8) 0.3675(7) 0.0386(4) 0.047(3) Uani 1 1 d . . . C9B C 1.2649(11) 0.3694(9) -0.0010(4) 0.069(4) Uani 1 1 d . . . H9B1 H 1.2124 0.3631 -0.0182 0.103 Uiso 1 1 calc R . . H9B2 H 1.3022 0.3277 -0.0049 0.103 Uiso 1 1 calc R . . H9B3 H 1.2894 0.4187 -0.0058 0.103 Uiso 1 1 calc R . . C10B C 1.1358(8) 0.4597(8) 0.0194(4) 0.055(3) Uani 1 1 d . . . H10D H 1.0774 0.4555 0.0211 0.083 Uiso 1 1 calc R . . H10E H 1.1440 0.4436 -0.0056 0.083 Uiso 1 1 calc R . . H10F H 1.1537 0.5130 0.0238 0.083 Uiso 1 1 calc R . . C11B C 1.2032(11) 0.4756(13) 0.1845(6) 0.092(6) Uani 1 1 d . . . C12B C 1.2280(14) 0.4397(16) 0.2203(6) 0.111(5) Uani 1 1 d . . . C13B C 1.2919(13) 0.4512(15) 0.2523(6) 0.118(8) Uani 1 1 d . . . H13B H 1.3320 0.4903 0.2526 0.141 Uiso 1 1 calc R . . C14B C 1.2927(17) 0.402(2) 0.2832(6) 0.130(11) Uani 1 1 d . . . H14B H 1.3364 0.4108 0.3035 0.156 Uiso 1 1 calc R . . C15B C 1.240(2) 0.343(2) 0.2886(7) 0.147(12) Uani 1 1 d . . . H15B H 1.2466 0.3144 0.3111 0.176 Uiso 1 1 calc R . . C16B C 1.1716(15) 0.3284(18) 0.2562(7) 0.141(10) Uani 1 1 d . . . H16B H 1.1319 0.2890 0.2560 0.169 Uiso 1 1 calc R . . C17B C 1.1723(15) 0.3805(19) 0.2251(5) 0.132(10) Uani 1 1 d . . . C18B C 1.2755(15) 0.4997(13) 0.1653(6) 0.122(8) Uani 1 1 d . . . H18D H 1.2549 0.5109 0.1388 0.183 Uiso 1 1 calc R . . H18E H 1.3157 0.4579 0.1672 0.183 Uiso 1 1 calc R . . H18F H 1.3019 0.5456 0.1776 0.183 Uiso 1 1 calc R . . C19B C 1.1601(18) 0.5584(17) 0.1869(8) 0.161(11) Uani 1 1 d . . . H19D H 1.1486 0.5815 0.1619 0.241 Uiso 1 1 calc R . . H19E H 1.1971 0.5918 0.2039 0.241 Uiso 1 1 calc R . . H19F H 1.1085 0.5518 0.1964 0.241 Uiso 1 1 calc R . . C20B C 1.0563(13) 0.3116(14) 0.1794(6) 0.111(5) Uani 1 1 d . . . H20D H 1.0025 0.3283 0.1658 0.167 Uiso 1 1 calc R . . H20E H 1.0489 0.2831 0.2018 0.167 Uiso 1 1 calc R . . H20F H 1.0828 0.2785 0.1631 0.167 Uiso 1 1 calc R . . N1 N 0.4662(14) 0.4733(15) -0.1630(7) 0.161(10) Uani 1 1 d . . . C1 C 0.5734(16) 0.3624(17) -0.1378(9) 0.176(13) Uani 1 1 d . . . H1A H 0.5450 0.3191 -0.1284 0.264 Uiso 1 1 calc R . . H1B H 0.6157 0.3821 -0.1177 0.264 Uiso 1 1 calc R . . H1C H 0.5991 0.3452 -0.1588 0.264 Uiso 1 1 calc R . . C2 C 0.5121(15) 0.4250(16) -0.1511(7) 0.121(8) 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 0.0280(5) 0.0252(5) 0.0472(6) 0.0002(4) -0.0017(4) 0.0005(4) Mo2 0.0279(5) 0.0343(6) 0.0681(7) -0.0003(5) 0.0079(5) -0.0020(4) Mo3 0.0421(6) 0.0436(7) 0.0439(6) 0.0048(5) 0.0020(5) -0.0064(5) Mo4 0.0333(5) 0.0335(6) 0.0465(6) -0.0039(4) -0.0054(4) -0.0045(4) O1 0.037(4) 0.039(5) 0.054(5) -0.011(4) 0.000(4) -0.001(3) O2 0.043(5) 0.038(5) 0.061(5) -0.013(4) 0.001(4) -0.005(4) O3 0.042(4) 0.024(4) 0.074(6) 0.003(4) 0.002(4) 0.002(3) O4 0.054(6) 0.061(6) 0.062(6) -0.006(5) -0.001(5) -0.007(5) O5 0.041(4) 0.029(4) 0.066(5) -0.005(4) 0.009(4) -0.002(3) O6 0.042(4) 0.037(5) 0.040(4) 0.006(3) -0.005(4) -0.002(4) O7 0.063(6) 0.043(5) 0.062(6) 0.031(4) 0.006(5) -0.009(4) O8 0.036(4) 0.025(4) 0.047(4) 0.004(3) -0.002(3) -0.005(3) O9 0.027(4) 0.049(5) 0.064(5) -0.002(4) 0.000(4) -0.002(4) O10 0.042(5) 0.045(5) 0.057(5) -0.002(4) 0.011(4) -0.006(4) O11 0.051(5) 0.048(6) 0.083(7) 0.000(5) 0.004(5) -0.012(4) O12 0.067(6) 0.080(8) 0.062(6) 0.008(5) 0.016(5) 0.002(5) O13 0.033(5) 0.061(6) 0.117(8) -0.001(6) 0.020(5) 0.011(4) O1A 0.040(5) 0.038(5) 0.070(6) 0.007(4) -0.007(4) -0.008(4) N1A 0.042(6) 0.041(6) 0.062(7) -0.002(5) -0.002(5) -0.004(5) N2A 0.048(6) 0.040(6) 0.050(6) 0.003(5) 0.001(5) -0.005(5) C1A 0.038(7) 0.054(8) 0.054(8) 0.012(6) -0.009(6) -0.008(6) C2A 0.042(7) 0.065(9) 0.062(8) 0.009(7) 0.006(6) 0.004(7) C3A 0.059(8) 0.033(7) 0.065(9) 0.005(6) 0.001(7) 0.003(6) C4A 0.038(7) 0.053(8) 0.049(7) -0.003(6) 0.005(6) -0.008(6) C5A 0.039(6) 0.037(7) 0.044(7) 0.001(5) -0.003(5) 0.010(5) C6A 0.049(8) 0.044(8) 0.073(9) 0.014(7) 0.001(7) -0.004(6) C7A 0.053(9) 0.088(13) 0.080(11) 0.017(9) -0.012(8) -0.009(8) C8A 0.047(8) 0.068(11) 0.091(12) -0.009(9) -0.025(8) -0.008(7) C9A 0.063(11) 0.091(15) 0.19(2) 0.000(14) -0.055(13) -0.024(10) C10A 0.073(10) 0.045(9) 0.097(12) 0.000(8) 0.014(9) -0.020(7) C11A 0.051(8) 0.066(10) 0.052(8) 0.005(7) 0.006(6) -0.009(7) C12A 0.071(10) 0.071(10) 0.052(8) -0.008(7) -0.001(7) -0.024(8) C13A 0.121(16) 0.100(15) 0.061(10) 0.002(10) -0.008(10) -0.036(13) C14A 0.15(2) 0.106(17) 0.071(12) -0.031(11) 0.005(13) -0.063(15) C15A 0.119(17) 0.14(2) 0.100(15) -0.039(14) 0.006(13) -0.091(16) C16A 0.055(9) 0.069(11) 0.079(10) 0.002(8) 0.012(8) -0.015(8) C17A 0.033(7) 0.084(11) 0.056(8) 0.008(8) -0.002(6) -0.005(7) C18A 0.093(13) 0.094(14) 0.099(13) -0.014(11) 0.053(11) -0.020(11) C19A 0.084(12) 0.139(18) 0.057(9) 0.045(11) 0.001(9) -0.030(12) C20A 0.054(8) 0.053(9) 0.065(9) -0.001(7) 0.012(7) 0.005(7) O1B 0.078(7) 0.075(7) 0.062(6) 0.007(5) 0.023(5) 0.024(6) N1B 0.035(5) 0.039(6) 0.060(7) 0.006(5) -0.001(5) -0.011(4) N2B 0.064(9) 0.173(18) 0.073(10) 0.006(11) -0.011(8) -0.001(10) C1B 0.050(9) 0.121(15) 0.065(10) -0.016(10) 0.026(8) 0.002(9) C2B 0.058(9) 0.089(13) 0.087(12) 0.002(10) 0.012(9) 0.035(9) C3B 0.047(8) 0.083(12) 0.077(11) 0.019(9) 0.012(8) 0.008(8) C4B 0.045(7) 0.044(8) 0.065(9) 0.002(6) 0.007(7) 0.003(6) C5B 0.056(8) 0.053(9) 0.057(8) -0.007(7) 0.009(7) 0.015(7) C6B 0.074(10) 0.062(10) 0.055(9) 0.012(7) 0.011(7) 0.010(8) C7B 0.059(8) 0.039(7) 0.065(9) 0.000(6) 0.017(7) 0.015(6) C8B 0.052(8) 0.034(7) 0.052(8) -0.011(6) -0.002(6) -0.003(6) C9B 0.094(12) 0.056(9) 0.056(9) 0.005(7) 0.009(8) 0.013(8) C10B 0.045(7) 0.052(8) 0.063(8) 0.000(7) -0.004(6) -0.004(6) C11B 0.067(11) 0.112(16) 0.091(13) -0.029(12) -0.003(10) 0.040(11) C12B 0.088(10) 0.154(16) 0.088(10) 0.010(10) 0.004(8) -0.020(10) C13B 0.091(14) 0.14(2) 0.105(16) -0.034(15) -0.024(12) 0.035(14) C14B 0.12(2) 0.20(3) 0.064(13) 0.023(17) -0.002(13) 0.09(2) C15B 0.18(3) 0.19(3) 0.068(15) -0.001(17) 0.014(18) 0.01(2) C16B 0.098(17) 0.22(3) 0.114(19) 0.01(2) 0.036(16) 0.021(18) C17B 0.119(18) 0.25(3) 0.039(10) -0.003(14) 0.028(11) 0.05(2) C18B 0.14(2) 0.100(18) 0.115(17) -0.022(13) -0.001(16) -0.008(15) C19B 0.15(2) 0.16(3) 0.17(3) 0.02(2) 0.02(2) -0.02(2) C20B 0.088(10) 0.154(16) 0.088(10) 0.010(10) 0.004(8) -0.020(10) N1 0.132(18) 0.17(2) 0.17(2) 0.058(17) -0.008(15) 0.052(16) C1 0.13(2) 0.16(3) 0.22(3) 0.07(2) -0.01(2) 0.07(2) C2 0.089(16) 0.13(2) 0.14(2) 0.012(17) -0.003(14) -0.005(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.674(8) . ? Mo1 O5 1.754(8) . ? Mo1 O1 1.932(8) . ? Mo1 O6 1.949(8) . ? Mo1 O8 2.134(7) . ? Mo1 O8 2.365(7) 7_655 ? Mo1 Mo3 3.2180(16) . ? Mo2 O11 1.701(9) . ? Mo2 O13 1.711(8) . ? Mo2 O9 1.918(9) 7_655 ? Mo2 O10 1.922(8) . ? Mo2 O5 2.297(8) . ? Mo2 O8 2.443(7) 7_655 ? Mo3 O12 1.710(10) . ? Mo3 O7 1.725(8) . ? Mo3 O10 1.906(8) 7_655 ? Mo3 O6 1.991(8) . ? Mo3 O8 2.341(7) . ? Mo3 O1 2.385(8) 7_655 ? Mo4 O4 1.684(9) . ? Mo4 O2 1.687(8) . ? Mo4 O9 1.893(8) . ? Mo4 O1 2.013(8) . ? Mo4 O6 2.346(8) 7_655 ? Mo4 O8 2.350(7) . ? O1 Mo3 2.385(8) 7_655 ? O6 Mo4 2.346(8) 7_655 ? O8 Mo1 2.365(7) 7_655 ? O8 Mo2 2.443(7) 7_655 ? O9 Mo2 1.918(9) 7_655 ? O10 Mo3 1.906(8) 7_655 ? O1A C5A 1.358(13) . ? O1A C1A 1.484(14) . ? N1A C8A 1.312(17) . ? N1A C4A 1.377(15) . ? N1A C10A 1.485(16) . ? N2A C17A 1.408(18) . ? N2A C1A 1.441(15) . ? N2A C20A 1.453(16) . ? C1A C2A 1.526(19) . ? C1A C11A 1.530(19) . ? C2A C3A 1.303(18) . ? C2A H2A 0.9300 . ? C3A C4A 1.448(17) . ? C3A H3A 0.9300 . ? C4A C5A 1.382(17) . ? C5A C6A 1.386(16) . ? C6A C7A 1.409(19) . ? C6A H6A 0.9300 . ? C7A C8A 1.39(2) . ? C7A H7A 0.9300 . ? C8A C9A 1.501(19) . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C11A C12A 1.49(2) . ? C11A C18A 1.54(2) . ? C11A C19A 1.55(2) . ? C12A C17A 1.40(2) . ? C12A C13A 1.40(2) . ? C13A C14A 1.38(3) . ? C13A H13A 0.9300 . ? C14A C15A 1.41(3) . ? C14A H14A 0.9300 . ? C15A C16A 1.38(2) . ? C15A H15A 0.9300 . ? C16A C17A 1.38(2) . ? C16A H16A 0.9300 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? O1B C5B 1.352(16) . ? O1B C1B 1.511(18) . ? N1B C4B 1.320(16) . ? N1B C8B 1.368(16) . ? N1B C10B 1.465(15) . ? N2B C20B 1.41(3) . ? N2B C1B 1.44(2) . ? N2B C17B 1.48(2) . ? C1B C2B 1.48(2) . ? C1B C11B 1.49(2) . ? C2B C3B 1.26(2) . ? C2B H2B 0.9300 . ? C3B C4B 1.482(19) . ? C3B H3B 0.9300 . ? C4B C5B 1.395(18) . ? C5B C6B 1.391(19) . ? C6B C7B 1.368(18) . ? C6B H6B 0.9300 . ? C7B C8B 1.373(17) . ? C7B H7B 0.9300 . ? C8B C9B 1.467(18) . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? C11B C12B 1.40(3) . ? C11B C18B 1.51(3) . ? C11B C19B 1.59(3) . ? C12B C17B 1.38(3) . ? C12B C13B 1.41(3) . ? C13B C14B 1.38(3) . ? C13B H13B 0.9300 . ? C14B C15B 1.35(4) . ? C14B H14B 0.9300 . ? C15B C16B 1.47(3) . ? C15B H15B 0.9300 . ? C16B C17B 1.42(3) . ? C16B H16B 0.9300 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? N1 C2 1.14(3) . ? C1 C2 1.48(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? 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 O5 103.2(4) . . ? O3 Mo1 O1 100.2(4) . . ? O5 Mo1 O1 96.2(4) . . ? O3 Mo1 O6 102.1(4) . . ? O5 Mo1 O6 97.0(4) . . ? O1 Mo1 O6 150.7(3) . . ? O3 Mo1 O8 99.9(3) . . ? O5 Mo1 O8 156.9(3) . . ? O1 Mo1 O8 79.1(3) . . ? O6 Mo1 O8 78.6(3) . . ? O3 Mo1 O8 175.9(3) . 7_655 ? O5 Mo1 O8 80.8(3) . 7_655 ? O1 Mo1 O8 78.5(3) . 7_655 ? O6 Mo1 O8 77.9(3) . 7_655 ? O8 Mo1 O8 76.1(3) . 7_655 ? O3 Mo1 Mo3 91.1(3) . . ? O5 Mo1 Mo3 132.6(3) . . ? O1 Mo1 Mo3 125.8(2) . . ? O6 Mo1 Mo3 35.7(2) . . ? O8 Mo1 Mo3 46.7(2) . . ? O8 Mo1 Mo3 86.59(19) 7_655 . ? O11 Mo2 O13 103.4(5) . . ? O11 Mo2 O9 101.1(4) . 7_655 ? O13 Mo2 O9 101.9(4) . 7_655 ? O11 Mo2 O10 95.9(4) . . ? O13 Mo2 O10 103.2(4) . . ? O9 Mo2 O10 145.4(3) 7_655 . ? O11 Mo2 O5 164.1(4) . . ? O13 Mo2 O5 92.3(4) . . ? O9 Mo2 O5 77.7(3) 7_655 . ? O10 Mo2 O5 77.8(3) . . ? O11 Mo2 O8 94.7(3) . 7_655 ? O13 Mo2 O8 162.0(4) . 7_655 ? O9 Mo2 O8 74.6(3) 7_655 7_655 ? O10 Mo2 O8 74.1(3) . 7_655 ? O5 Mo2 O8 69.7(3) . 7_655 ? O12 Mo3 O7 105.8(5) . . ? O12 Mo3 O10 99.6(4) . 7_655 ? O7 Mo3 O10 102.7(4) . 7_655 ? O12 Mo3 O6 102.0(4) . . ? O7 Mo3 O6 96.9(4) . . ? O10 Mo3 O6 145.5(3) 7_655 . ? O12 Mo3 O8 157.4(4) . . ? O7 Mo3 O8 96.7(3) . . ? O10 Mo3 O8 76.9(3) 7_655 . ? O6 Mo3 O8 72.9(3) . . ? O12 Mo3 O1 86.6(4) . 7_655 ? O7 Mo3 O1 164.6(4) . 7_655 ? O10 Mo3 O1 83.7(3) 7_655 7_655 ? O6 Mo3 O1 71.1(3) . 7_655 ? O8 Mo3 O1 70.9(3) . 7_655 ? O12 Mo3 Mo1 136.8(3) . . ? O7 Mo3 Mo1 86.3(3) . . ? O10 Mo3 Mo1 118.4(3) 7_655 . ? O6 Mo3 Mo1 34.8(2) . . ? O8 Mo3 Mo1 41.51(18) . . ? O1 Mo3 Mo1 78.29(19) 7_655 . ? O4 Mo4 O2 104.6(4) . . ? O4 Mo4 O9 102.6(4) . . ? O2 Mo4 O9 102.2(4) . . ? O4 Mo4 O1 100.2(4) . . ? O2 Mo4 O1 96.5(4) . . ? O9 Mo4 O1 145.7(3) . . ? O4 Mo4 O6 88.8(4) . 7_655 ? O2 Mo4 O6 163.7(3) . 7_655 ? O9 Mo4 O6 83.5(3) . 7_655 ? O1 Mo4 O6 71.6(3) . 7_655 ? O4 Mo4 O8 159.9(4) . . ? O2 Mo4 O8 94.9(3) . . ? O9 Mo4 O8 77.4(3) . . ? O1 Mo4 O8 72.5(3) . . ? O6 Mo4 O8 71.1(3) 7_655 . ? Mo1 O1 Mo4 110.0(4) . . ? Mo1 O1 Mo3 110.2(3) . 7_655 ? Mo4 O1 Mo3 102.7(3) . 7_655 ? Mo1 O5 Mo2 117.2(4) . . ? Mo1 O6 Mo3 109.5(3) . . ? Mo1 O6 Mo4 110.7(3) . 7_655 ? Mo3 O6 Mo4 104.7(3) . 7_655 ? Mo1 O8 Mo3 91.8(3) . . ? Mo1 O8 Mo4 92.1(3) . . ? Mo3 O8 Mo4 162.8(3) . . ? Mo1 O8 Mo1 103.9(3) . 7_655 ? Mo3 O8 Mo1 97.9(3) . 7_655 ? Mo4 O8 Mo1 97.3(3) . 7_655 ? Mo1 O8 Mo2 163.7(4) . 7_655 ? Mo3 O8 Mo2 86.3(3) . 7_655 ? Mo4 O8 Mo2 85.2(2) . 7_655 ? Mo1 O8 Mo2 92.3(3) 7_655 7_655 ? Mo4 O9 Mo2 116.8(4) . 7_655 ? Mo3 O10 Mo2 117.6(4) 7_655 . ? C5A O1A C1A 121.3(9) . . ? C8A N1A C4A 123.0(12) . . ? C8A N1A C10A 118.7(12) . . ? C4A N1A C10A 118.3(11) . . ? C17A N2A C1A 105.4(11) . . ? C17A N2A C20A 119.9(11) . . ? C1A N2A C20A 120.7(10) . . ? N2A C1A O1A 105.7(9) . . ? N2A C1A C2A 110.4(11) . . ? O1A C1A C2A 109.1(9) . . ? N2A C1A C11A 104.5(10) . . ? O1A C1A C11A 109.2(11) . . ? C2A C1A C11A 117.3(11) . . ? C3A C2A C1A 124.3(12) . . ? C3A C2A H2A 117.9 . . ? C1A C2A H2A 117.9 . . ? C2A C3A C4A 119.2(13) . . ? C2A C3A H3A 120.4 . . ? C4A C3A H3A 120.4 . . ? N1A C4A C5A 118.4(11) . . ? N1A C4A C3A 122.4(12) . . ? C5A C4A C3A 119.2(11) . . ? O1A C5A C4A 121.7(10) . . ? O1A C5A C6A 117.5(11) . . ? C4A C5A C6A 120.6(11) . . ? C5A C6A C7A 118.0(13) . . ? C5A C6A H6A 121.0 . . ? C7A C6A H6A 121.0 . . ? C8A C7A C6A 119.9(14) . . ? C8A C7A H7A 120.1 . . ? C6A C7A H7A 120.1 . . ? N1A C8A C7A 119.7(13) . . ? N1A C8A C9A 119.9(15) . . ? C7A C8A C9A 120.3(14) . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? N1A C10A H10A 109.5 . . ? N1A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? N1A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C12A C11A C1A 100.9(11) . . ? C12A C11A C18A 115.3(14) . . ? C1A C11A C18A 111.9(12) . . ? C12A C11A C19A 109.0(12) . . ? C1A C11A C19A 109.8(13) . . ? C18A C11A C19A 109.6(13) . . ? C17A C12A C13A 122.2(15) . . ? C17A C12A C11A 108.0(13) . . ? C13A C12A C11A 129.9(15) . . ? C14A C13A C12A 117(2) . . ? C14A C13A H13A 121.5 . . ? C12A C13A H13A 121.5 . . ? C13A C14A C15A 122(2) . . ? C13A C14A H14A 119.0 . . ? C15A C14A H14A 119.0 . . ? C16A C15A C14A 119.3(17) . . ? C16A C15A H15A 120.3 . . ? C14A C15A H15A 120.3 . . ? C17A C16A C15A 120.3(16) . . ? C17A C16A H16A 119.9 . . ? C15A C16A H16A 119.9 . . ? C16A C17A C12A 119.2(15) . . ? C16A C17A N2A 130.3(14) . . ? C12A C17A N2A 110.5(12) . . ? C11A C18A H18A 109.5 . . ? C11A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C11A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C11A C19A H19A 109.5 . . ? C11A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C11A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? N2A C20A H20A 109.5 . . ? N2A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? N2A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C5B O1B C1B 119.1(11) . . ? C4B N1B C8B 122.2(11) . . ? C4B N1B C10B 119.2(11) . . ? C8B N1B C10B 118.6(11) . . ? C20B N2B C1B 119.9(16) . . ? C20B N2B C17B 123(2) . . ? C1B N2B C17B 103.5(17) . . ? N2B C1B C2B 116.0(13) . . ? N2B C1B C11B 104.6(15) . . ? C2B C1B C11B 115.3(17) . . ? N2B C1B O1B 104.4(16) . . ? C2B C1B O1B 108.2(12) . . ? C11B C1B O1B 107.6(12) . . ? C3B C2B C1B 128.3(15) . . ? C3B C2B H2B 115.9 . . ? C1B C2B H2B 115.9 . . ? C2B C3B C4B 118.3(14) . . ? C2B C3B H3B 120.9 . . ? C4B C3B H3B 120.9 . . ? N1B C4B C5B 119.9(12) . . ? N1B C4B C3B 123.2(12) . . ? C5B C4B C3B 116.9(13) . . ? O1B C5B C6B 116.9(12) . . ? O1B C5B C4B 123.0(12) . . ? C6B C5B C4B 120.0(13) . . ? C7B C6B C5B 117.3(13) . . ? C7B C6B H6B 121.3 . . ? C5B C6B H6B 121.3 . . ? C6B C7B C8B 122.5(13) . . ? C6B C7B H7B 118.7 . . ? C8B C7B H7B 118.7 . . ? N1B C8B C7B 117.9(12) . . ? N1B C8B C9B 119.5(12) . . ? C7B C8B C9B 122.6(12) . . ? C8B C9B H9B1 109.5 . . ? C8B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C8B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? N1B C10B H10D 109.5 . . ? N1B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? N1B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C12B C11B C1B 104(2) . . ? C12B C11B C18B 114.0(17) . . ? C1B C11B C18B 113.5(16) . . ? C12B C11B C19B 113.5(19) . . ? C1B C11B C19B 112.4(16) . . ? C18B C11B C19B 99(2) . . ? C17B C12B C11B 110(2) . . ? C17B C12B C13B 114(2) . . ? C11B C12B C13B 136(2) . . ? C14B C13B C12B 117(3) . . ? C14B C13B H13B 121.4 . . ? C12B C13B H13B 121.4 . . ? C15B C14B C13B 130(3) . . ? C15B C14B H14B 114.8 . . ? C13B C14B H14B 114.8 . . ? C14B C15B C16B 115(3) . . ? C14B C15B H15B 122.5 . . ? C16B C15B H15B 122.5 . . ? C17B C16B C15B 113(3) . . ? C17B C16B H16B 123.5 . . ? C15B C16B H16B 123.5 . . ? C12B C17B C16B 130(2) . . ? C12B C17B N2B 108(2) . . ? C16B C17B N2B 122(3) . . ? C11B C18B H18D 109.5 . . ? C11B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C11B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C11B C19B H19D 109.5 . . ? C11B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C11B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N2B C20B H20D 109.5 . . ? N2B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? N2B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 177(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.372 _refine_diff_density_min -1.624 _refine_diff_density_rms 0.442 _database_code_depnum_ccdc_archive 'CCDC 962072' ####################################################################### # # 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_SP4Mo8.DMF _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H106 Mo8 N10 O32' _chemical_formula_weight 2559.32 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' 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 11.5703(4) _cell_length_b 11.8955(4) _cell_length_c 18.1788(6) _cell_angle_alpha 71.980(2) _cell_angle_beta 84.391(2) _cell_angle_gamma 88.1410(10) _cell_volume 2367.90(14) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 9586 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 26.32 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_F_000 1284 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 1.110 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.916 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_reflns_number 65055 _diffrn_reflns_av_unetI/netI 0.0697 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.769 _diffrn_reflns_theta_max 30.025 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 13800 _reflns_number_gt 8346 _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' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0270P)^2^+1.3687P] 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_number_reflns 13800 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 0.00796(3) 0.27846(2) 0.12152(2) 0.02509(8) Uani 1 1 d . . . . . Mo2 Mo 0.17322(2) 0.25417(3) -0.02747(2) 0.02711(8) Uani 1 1 d . . . . . Mo3 Mo -0.01166(3) 0.55502(3) 0.14406(2) 0.02664(8) Uani 1 1 d . . . . . Mo4 Mo -0.14939(2) 0.46688(2) 0.00549(2) 0.02113(7) Uani 1 1 d . . . . . O1 O 0.0196(2) 0.2396(2) 0.21848(14) 0.0415(7) Uani 1 1 d . . . . . O2 O -0.0812(2) 0.1752(2) 0.11099(14) 0.0320(6) Uani 1 1 d . . . . . O3 O 0.15337(19) 0.23185(19) 0.08248(14) 0.0290(5) Uani 1 1 d . . . . . O4 O -0.10950(19) 0.40882(18) 0.11220(12) 0.0245(5) Uani 1 1 d . . . . . O5 O 0.01661(17) 0.38899(17) -0.00923(12) 0.0204(5) Uani 1 1 d . . . . . O6 O 0.10648(18) 0.45575(18) 0.10441(13) 0.0247(5) Uani 1 1 d . . . . . O7 O 0.0801(2) 0.1485(2) -0.03014(15) 0.0344(6) Uani 1 1 d . . . . . O8 O 0.3075(2) 0.1951(2) -0.03839(17) 0.0447(7) Uani 1 1 d . . . . . O9 O 0.1551(2) 0.3624(2) -0.12860(14) 0.0309(6) Uani 1 1 d . . . . . O10 O 0.24790(18) 0.42477(19) -0.01939(14) 0.0284(5) Uani 1 1 d . . . . . O11 O -0.0359(2) 0.4746(2) 0.23890(14) 0.0448(7) Uani 1 1 d . . . . . O12 O 0.0803(2) 0.6642(2) 0.14256(14) 0.0348(6) Uani 1 1 d . . . . . O13 O -0.23540(19) 0.35644(19) 0.00268(14) 0.0314(6) Uani 1 1 d . . . . . N1A N 0.0925(3) 0.9111(3) 0.37246(18) 0.0372(8) Uani 1 1 d . . . . . C2A C 0.1136(3) 0.8266(4) 0.4431(2) 0.0393(9) Uani 1 1 d . . . . . C3A C 0.1255(4) 0.8434(4) 0.5143(3) 0.0555(12) Uani 1 1 d . . . . . H3A H 0.1230 0.9204 0.5198 0.067 Uiso 1 1 calc R U . . . C4A C 0.1410(5) 0.7441(5) 0.5773(3) 0.0744(16) Uani 1 1 d . . . . . H4A H 0.1488 0.7538 0.6265 0.089 Uiso 1 1 calc R U . . . C5A C 0.1453(5) 0.6330(5) 0.5704(3) 0.0733(16) Uani 1 1 d . . . . . H5A H 0.1569 0.5667 0.6143 0.088 Uiso 1 1 calc R U . . . C6A C 0.1327(4) 0.6168(4) 0.4984(2) 0.0575(13) Uani 1 1 d . . . . . H6A H 0.1360 0.5397 0.4931 0.069 Uiso 1 1 calc R U . . . C7A C 0.1154(3) 0.7138(3) 0.4357(2) 0.0395(9) Uani 1 1 d . . . . . C8A C 0.0932(3) 0.7230(3) 0.3540(2) 0.0344(9) Uani 1 1 d . . . . . C9A C 0.1177(3) 0.8560(3) 0.3114(2) 0.0289(8) Uani 1 1 d . . . . . O10A O 0.24332(19) 0.8716(2) 0.28829(13) 0.0314(6) Uani 1 1 d . . . . . C11A C 0.2847(3) 0.8660(3) 0.2166(2) 0.0270(8) Uani 1 1 d . . . . . C12A C 0.4009(3) 0.8413(3) 0.2052(2) 0.0350(9) Uani 1 1 d . . . . . H12A H 0.4494 0.8262 0.2465 0.042 Uiso 1 1 calc R U . . . C13A C 0.4454(3) 0.8392(3) 0.1325(2) 0.0342(9) Uani 1 1 d . . . . . H13A H 0.5257 0.8230 0.1237 0.041 Uiso 1 1 calc R U . . . C14A C 0.3756(3) 0.8601(3) 0.0720(2) 0.0278(8) Uani 1 1 d . . . . . N15A N 0.2614(2) 0.8839(2) 0.08568(16) 0.0234(6) Uani 1 1 d . . . . . C16A C 0.2142(3) 0.8907(3) 0.15596(19) 0.0241(7) Uani 1 1 d . . . . . C17A C 0.0957(3) 0.9253(3) 0.1694(2) 0.0308(8) Uani 1 1 d . . . . . H17A H 0.0494 0.9571 0.1274 0.037 Uiso 1 1 calc R U . . . C18A C 0.0523(3) 0.9117(3) 0.2425(2) 0.0356(9) Uani 1 1 d . . . . . H18A H -0.0244 0.9390 0.2510 0.043 Uiso 1 1 calc R U . . . C19A C 0.1252(4) 1.0329(3) 0.3573(3) 0.0555(12) Uani 1 1 d . . . . . H19A H 0.0799 1.0659 0.3942 0.083 Uiso 1 1 calc R U . . . H19B H 0.1098 1.0784 0.3042 0.083 Uiso 1 1 calc R U . . . H19C H 0.2081 1.0370 0.3631 0.083 Uiso 1 1 calc R U . . . C20A C -0.0370(4) 0.6979(4) 0.3507(3) 0.0679(14) Uani 1 1 d . . . . . H20A H -0.0569 0.6185 0.3854 0.102 Uiso 1 1 calc R U . . . H20B H -0.0506 0.7029 0.2974 0.102 Uiso 1 1 calc R U . . . H20C H -0.0855 0.7564 0.3672 0.102 Uiso 1 1 calc R U . . . C21A C 0.1631(4) 0.6383(3) 0.3202(2) 0.0554(13) Uani 1 1 d . . . . . H21A H 0.2457 0.6465 0.3252 0.083 Uiso 1 1 calc R U . . . H21B H 0.1506 0.6562 0.2652 0.083 Uiso 1 1 calc R U . . . H21C H 0.1383 0.5571 0.3484 0.083 Uiso 1 1 calc R U . . . C22A C 0.4231(3) 0.8578(3) -0.0066(2) 0.0368(9) Uani 1 1 d . . . . . H22A H 0.3856 0.7944 -0.0195 0.055 Uiso 1 1 calc R U . . . H22B H 0.5070 0.8436 -0.0071 0.055 Uiso 1 1 calc R U . . . H22C H 0.4079 0.9339 -0.0451 0.055 Uiso 1 1 calc R U . . . C23A C 0.1850(3) 0.8992(3) 0.02211(19) 0.0269(7) Uani 1 1 d . . . . . H23A H 0.1887 0.9814 -0.0116 0.040 Uiso 1 1 calc R U . . . H23B H 0.1048 0.8798 0.0444 0.040 Uiso 1 1 calc R U . . . H23C H 0.2111 0.8465 -0.0084 0.040 Uiso 1 1 calc R U . . . N1B N 0.7133(3) -0.0913(3) 0.26646(17) 0.0324(7) Uani 1 1 d . . . . . C2B C 0.6470(3) -0.1907(3) 0.3108(2) 0.0329(8) Uani 1 1 d . . . . . C3B C 0.6518(3) -0.3026(3) 0.3033(2) 0.0405(10) Uani 1 1 d . . . . . H3B H 0.7044 -0.3216 0.2654 0.049 Uiso 1 1 calc R U . . . C4B C 0.5758(4) -0.3869(4) 0.3540(3) 0.0516(11) Uani 1 1 d . . . . . H4B H 0.5774 -0.4652 0.3510 0.062 Uiso 1 1 calc R U . . . C5B C 0.4991(4) -0.3589(4) 0.4080(3) 0.0539(12) Uani 1 1 d . . . . . H5B H 0.4478 -0.4177 0.4413 0.065 Uiso 1 1 calc R U . . . C6B C 0.4953(4) -0.2454(4) 0.4146(2) 0.0502(11) Uani 1 1 d . . . . . H6B H 0.4413 -0.2256 0.4515 0.060 Uiso 1 1 calc R U . . . C7B C 0.5718(3) -0.1623(3) 0.3662(2) 0.0362(9) Uani 1 1 d . . . . . C8B C 0.5909(4) -0.0354(3) 0.3620(2) 0.0393(9) Uani 1 1 d . . . . . C9B C 0.6577(3) 0.0126(3) 0.2793(2) 0.0324(8) Uani 1 1 d . . . . . O10B O 0.5710(2) 0.0519(2) 0.22159(14) 0.0326(6) Uani 1 1 d . . . . . C11B C 0.5374(3) 0.1676(3) 0.1975(2) 0.0295(8) Uani 1 1 d . . . . . C12B C 0.4359(3) 0.1957(3) 0.1614(2) 0.0390(9) Uani 1 1 d . . . . . H12B H 0.3894 0.1359 0.1547 0.047 Uiso 1 1 calc R U . . . C13B C 0.4044(4) 0.3125(4) 0.1354(3) 0.0505(11) Uani 1 1 d . . . . . H13B H 0.3361 0.3335 0.1092 0.061 Uiso 1 1 calc R U . . . C14B C 0.4687(4) 0.3997(4) 0.1463(3) 0.0490(11) Uani 1 1 d . . . . . N15B N 0.5677(3) 0.3702(3) 0.18205(17) 0.0330(7) Uani 1 1 d . . . . . C16B C 0.6051(3) 0.2556(3) 0.2065(2) 0.0298(8) Uani 1 1 d . . . . . C17B C 0.7152(3) 0.2238(3) 0.2383(2) 0.0328(8) Uani 1 1 d . . . . . H17B H 0.7686 0.2834 0.2372 0.039 Uiso 1 1 calc R U . . . C18B C 0.7412(3) 0.1107(3) 0.2689(2) 0.0354(9) Uani 1 1 d . . . . . H18B H 0.8169 0.0910 0.2851 0.042 Uiso 1 1 calc R U . . . C19B C 0.7652(3) -0.0840(3) 0.1885(2) 0.0361(9) Uani 1 1 d . . . . . H19D H 0.8218 -0.1480 0.1917 0.054 Uiso 1 1 calc R U . . . H19E H 0.8042 -0.0077 0.1650 0.054 Uiso 1 1 calc R U . . . H19F H 0.7042 -0.0914 0.1564 0.054 Uiso 1 1 calc R U . . . C20B C 0.6745(5) -0.0345(4) 0.4230(2) 0.0637(14) Uani 1 1 d . . . . . H20D H 0.6394 -0.0778 0.4750 0.096 Uiso 1 1 calc R U . . . H20E H 0.6893 0.0473 0.4205 0.096 Uiso 1 1 calc R U . . . H20F H 0.7479 -0.0724 0.4123 0.096 Uiso 1 1 calc R U . . . C21B C 0.4803(4) 0.0316(4) 0.3727(3) 0.0642(14) Uani 1 1 d . . . . . H21D H 0.4267 0.0257 0.3355 0.096 Uiso 1 1 calc R U . . . H21E H 0.4987 0.1149 0.3638 0.096 Uiso 1 1 calc R U . . . H21F H 0.4439 -0.0023 0.4257 0.096 Uiso 1 1 calc R U . . . C22B C 0.4341(5) 0.5285(4) 0.1202(4) 0.094(2) Uani 1 1 d . . . . . H22D H 0.4261 0.5584 0.1650 0.141 Uiso 1 1 calc R U . . . H22E H 0.3599 0.5368 0.0973 0.141 Uiso 1 1 calc R U . . . H22F H 0.4939 0.5738 0.0814 0.141 Uiso 1 1 calc R U . . . C23B C 0.6332(3) 0.4622(3) 0.1991(2) 0.0411(10) Uani 1 1 d . . . . . H23D H 0.5845 0.5328 0.1936 0.062 Uiso 1 1 calc R U . . . H23E H 0.7032 0.4825 0.1627 0.062 Uiso 1 1 calc R U . . . H23F H 0.6555 0.4324 0.2524 0.062 Uiso 1 1 calc R U . . . N1C N 0.2576(3) 0.3276(3) 0.3829(2) 0.0503(9) Uani 1 1 d . . . . . C2C C 0.2174(5) 0.3358(5) 0.3092(3) 0.0788(16) Uani 1 1 d . . . . . H2C1 H 0.2427 0.4110 0.2711 0.118 Uiso 1 1 calc R U . . . H2C2 H 0.1324 0.3318 0.3146 0.118 Uiso 1 1 calc R U . . . H2C3 H 0.2496 0.2702 0.2917 0.118 Uiso 1 1 calc R U . . . C3C C 0.1770(5) 0.3001(5) 0.4506(3) 0.095(2) Uani 1 1 d . . . . . H3C1 H 0.1552 0.2165 0.4656 0.142 Uiso 1 1 calc R U . . . H3C2 H 0.1074 0.3495 0.4396 0.142 Uiso 1 1 calc R U . . . H3C3 H 0.2129 0.3154 0.4932 0.142 Uiso 1 1 calc R U . . . C4C C 0.3683(5) 0.3445(4) 0.3863(3) 0.0662(14) Uani 1 1 d . . . . . H4C H 0.3928 0.3403 0.4354 0.079 Uiso 1 1 calc R U . . . O5C O 0.4424(3) 0.3653(4) 0.3308(2) 0.0888(12) 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 0.03054(17) 0.01916(15) 0.02356(17) -0.00301(12) -0.00441(13) -0.00070(12) Mo2 0.02019(15) 0.02348(16) 0.0409(2) -0.01500(14) -0.00246(14) 0.00278(12) Mo3 0.03667(18) 0.02506(16) 0.02018(16) -0.00951(13) -0.00332(13) -0.00148(13) Mo4 0.01905(14) 0.01988(14) 0.02518(17) -0.00760(12) -0.00281(12) -0.00129(11) O1 0.0620(18) 0.0307(14) 0.0294(15) -0.0029(12) -0.0145(13) 0.0019(13) O2 0.0373(14) 0.0239(12) 0.0340(15) -0.0084(11) -0.0005(11) -0.0038(11) O3 0.0263(12) 0.0225(12) 0.0368(15) -0.0053(11) -0.0099(11) 0.0049(10) O4 0.0298(12) 0.0223(12) 0.0199(12) -0.0055(10) 0.0016(10) -0.0014(10) O5 0.0219(11) 0.0193(11) 0.0204(12) -0.0064(9) -0.0023(9) 0.0004(9) O6 0.0290(12) 0.0224(12) 0.0234(13) -0.0066(10) -0.0083(10) 0.0013(10) O7 0.0298(13) 0.0240(13) 0.0519(17) -0.0145(12) -0.0063(12) 0.0003(10) O8 0.0246(13) 0.0503(17) 0.069(2) -0.0334(15) -0.0066(13) 0.0113(12) O9 0.0344(14) 0.0312(13) 0.0309(14) -0.0175(11) 0.0063(11) -0.0024(11) O10 0.0220(12) 0.0279(13) 0.0370(15) -0.0126(11) -0.0028(10) 0.0003(10) O11 0.073(2) 0.0376(15) 0.0242(15) -0.0098(12) -0.0021(13) -0.0030(14) O12 0.0422(15) 0.0328(14) 0.0337(15) -0.0144(12) -0.0099(12) -0.0028(12) O13 0.0264(13) 0.0256(13) 0.0444(16) -0.0125(11) -0.0070(11) -0.0024(10) N1A 0.050(2) 0.0366(18) 0.0272(18) -0.0141(14) -0.0035(15) 0.0017(15) C2A 0.046(2) 0.048(2) 0.027(2) -0.0150(18) -0.0033(18) -0.0050(19) C3A 0.076(3) 0.059(3) 0.040(3) -0.026(2) -0.004(2) -0.019(3) C4A 0.114(5) 0.081(4) 0.030(3) -0.013(3) -0.020(3) -0.024(3) C5A 0.120(5) 0.063(3) 0.031(3) 0.000(2) -0.022(3) -0.013(3) C6A 0.093(4) 0.047(3) 0.031(2) -0.006(2) -0.012(2) -0.012(3) C7A 0.052(2) 0.041(2) 0.025(2) -0.0089(17) -0.0032(18) -0.0107(19) C8A 0.044(2) 0.037(2) 0.0220(19) -0.0075(16) -0.0042(17) -0.0055(17) C9A 0.0298(19) 0.0338(19) 0.0245(19) -0.0116(16) -0.0009(15) -0.0004(15) O10A 0.0270(13) 0.0445(15) 0.0237(14) -0.0114(11) -0.0052(10) 0.0011(11) C11A 0.0265(18) 0.0281(18) 0.0259(19) -0.0066(15) -0.0048(15) -0.0009(14) C12A 0.0277(19) 0.047(2) 0.033(2) -0.0152(18) -0.0096(17) -0.0009(17) C13A 0.0223(18) 0.044(2) 0.038(2) -0.0172(18) 0.0011(16) -0.0011(16) C14A 0.0234(17) 0.0329(19) 0.027(2) -0.0096(15) -0.0003(15) -0.0055(15) N15A 0.0217(14) 0.0226(14) 0.0247(16) -0.0047(12) -0.0047(12) -0.0024(11) C16A 0.0258(17) 0.0242(17) 0.0214(18) -0.0055(14) -0.0026(14) -0.0009(14) C17A 0.0264(18) 0.042(2) 0.028(2) -0.0150(17) -0.0077(15) 0.0056(16) C18A 0.0278(19) 0.048(2) 0.033(2) -0.0153(18) -0.0082(17) 0.0084(17) C19A 0.085(3) 0.036(2) 0.049(3) -0.019(2) -0.004(2) 0.003(2) C20A 0.078(4) 0.074(3) 0.051(3) -0.015(3) -0.006(3) -0.030(3) C21A 0.105(4) 0.029(2) 0.033(2) -0.0097(18) -0.012(2) 0.002(2) C22A 0.030(2) 0.050(2) 0.033(2) -0.0166(19) 0.0001(17) -0.0037(17) C23A 0.0281(18) 0.0294(18) 0.0255(19) -0.0101(15) -0.0082(15) 0.0015(15) N1B 0.0343(17) 0.0288(16) 0.0350(18) -0.0111(14) -0.0032(14) -0.0017(13) C2B 0.032(2) 0.034(2) 0.033(2) -0.0082(17) -0.0115(17) -0.0013(16) C3B 0.042(2) 0.037(2) 0.044(3) -0.0124(19) -0.0088(19) -0.0023(18) C4B 0.069(3) 0.034(2) 0.052(3) -0.010(2) -0.012(2) -0.009(2) C5B 0.070(3) 0.045(3) 0.039(3) 0.001(2) -0.002(2) -0.026(2) C6B 0.064(3) 0.053(3) 0.030(2) -0.008(2) 0.000(2) -0.008(2) C7B 0.046(2) 0.037(2) 0.022(2) -0.0020(16) -0.0096(17) -0.0052(18) C8B 0.055(3) 0.040(2) 0.025(2) -0.0131(17) -0.0015(18) -0.0049(19) C9B 0.035(2) 0.035(2) 0.030(2) -0.0125(17) -0.0063(16) -0.0034(16) O10B 0.0348(14) 0.0310(13) 0.0343(15) -0.0115(11) -0.0087(11) -0.0019(11) C11B 0.033(2) 0.0302(19) 0.026(2) -0.0121(16) 0.0018(16) 0.0012(16) C12B 0.042(2) 0.040(2) 0.041(2) -0.0181(19) -0.0101(19) 0.0017(18) C13B 0.056(3) 0.044(2) 0.054(3) -0.012(2) -0.033(2) 0.009(2) C14B 0.056(3) 0.035(2) 0.054(3) -0.006(2) -0.021(2) 0.006(2) N15B 0.0378(18) 0.0313(16) 0.0294(18) -0.0096(14) 0.0006(14) -0.0021(14) C16B 0.035(2) 0.0310(19) 0.0224(19) -0.0075(15) 0.0039(15) -0.0048(16) C17B 0.031(2) 0.034(2) 0.034(2) -0.0122(17) 0.0013(17) -0.0054(16) C18B 0.035(2) 0.037(2) 0.037(2) -0.0145(18) -0.0045(17) -0.0016(17) C19B 0.035(2) 0.040(2) 0.035(2) -0.0141(18) 0.0004(17) -0.0033(17) C20B 0.107(4) 0.056(3) 0.033(3) -0.016(2) -0.010(3) -0.021(3) C21B 0.080(4) 0.058(3) 0.047(3) -0.016(2) 0.027(3) 0.000(3) C22B 0.110(5) 0.034(3) 0.138(6) -0.006(3) -0.079(4) 0.011(3) C23B 0.043(2) 0.032(2) 0.049(3) -0.0168(19) 0.0062(19) -0.0100(18) N1C 0.048(2) 0.046(2) 0.056(3) -0.0168(19) 0.0021(19) -0.0052(17) C2C 0.093(4) 0.066(4) 0.085(4) -0.030(3) -0.022(3) -0.002(3) C3C 0.099(5) 0.062(3) 0.101(5) -0.011(3) 0.048(4) 0.000(3) C4C 0.069(4) 0.061(3) 0.068(4) -0.019(3) -0.004(3) -0.012(3) O5C 0.077(3) 0.104(3) 0.085(3) -0.036(2) 0.031(2) -0.034(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 O1 1.696(2) . ? Mo1 O2 1.696(2) . ? Mo1 O3 1.895(2) . ? Mo1 O4 2.006(2) . ? Mo1 O5 2.327(2) . ? Mo1 O6 2.350(2) . ? Mo1 Mo4 3.2169(4) . ? Mo2 O7 1.697(2) . ? Mo2 O8 1.704(2) . ? Mo2 O9 1.917(2) . ? Mo2 O3 1.925(2) . ? Mo2 O10 2.282(2) . ? Mo2 O5 2.447(2) . ? Mo3 O11 1.694(2) . ? Mo3 O12 1.698(2) . ? Mo3 O9 1.901(2) 2_565 ? Mo3 O6 2.003(2) . ? Mo3 O5 2.339(2) 2_565 ? Mo3 O4 2.350(2) . ? Mo3 Mo4 3.2167(4) 2_565 ? Mo4 O13 1.690(2) . ? Mo4 O10 1.753(2) 2_565 ? Mo4 O4 1.944(2) . ? Mo4 O6 1.945(2) 2_565 ? Mo4 O5 2.135(2) . ? Mo4 O5 2.360(2) 2_565 ? Mo4 Mo3 3.2167(4) 2_565 ? O5 Mo3 2.339(2) 2_565 ? O5 Mo4 2.360(2) 2_565 ? O6 Mo4 1.945(2) 2_565 ? O9 Mo3 1.901(2) 2_565 ? O10 Mo4 1.753(2) 2_565 ? N1A C2A 1.402(5) . ? N1A C19A 1.444(5) . ? N1A C9A 1.456(4) . ? C2A C7A 1.389(5) . ? C2A C3A 1.390(5) . ? C3A C4A 1.389(6) . ? C3A H3A 0.9500 . ? C4A C5A 1.365(7) . ? C4A H4A 0.9500 . ? C5A C6A 1.403(6) . ? C5A H5A 0.9500 . ? C6A C7A 1.374(5) . ? C6A H6A 0.9500 . ? C7A C8A 1.502(5) . ? C8A C21A 1.509(5) . ? C8A C9A 1.553(5) . ? C8A C20A 1.556(6) . ? C9A O10A 1.474(4) . ? C9A C18A 1.490(5) . ? O10A C11A 1.365(4) . ? C11A C12A 1.376(5) . ? C11A C16A 1.388(4) . ? C12A C13A 1.378(5) . ? C12A H12A 0.9500 . ? C13A C14A 1.384(5) . ? C13A H13A 0.9500 . ? C14A N15A 1.358(4) . ? C14A C22A 1.488(5) . ? N15A C16A 1.365(4) . ? N15A C23A 1.486(4) . ? C16A C17A 1.439(4) . ? C17A C18A 1.336(5) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19A H19A 0.9800 . ? C19A H19B 0.9800 . ? C19A H19C 0.9800 . ? C20A H20A 0.9800 . ? C20A H20B 0.9800 . ? C20A H20C 0.9800 . ? C21A H21A 0.9800 . ? C21A H21B 0.9800 . ? C21A H21C 0.9800 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? N1B C2B 1.409(4) . ? N1B C9B 1.447(4) . ? N1B C19B 1.462(4) . ? C2B C3B 1.379(5) . ? C2B C7B 1.380(5) . ? C3B C4B 1.399(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.369(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.391(6) . ? C5B H5B 0.9500 . ? C6B C7B 1.379(5) . ? C6B H6B 0.9500 . ? C7B C8B 1.510(5) . ? C8B C21B 1.514(6) . ? C8B C20B 1.545(6) . ? C8B C9B 1.566(5) . ? C9B O10B 1.482(4) . ? C9B C18B 1.495(5) . ? O10B C11B 1.365(4) . ? C11B C12B 1.382(5) . ? C11B C16B 1.387(5) . ? C12B C13B 1.371(5) . ? C12B H12B 0.9500 . ? C13B C14B 1.368(6) . ? C13B H13B 0.9500 . ? C14B N15B 1.355(5) . ? C14B C22B 1.510(6) . ? N15B C16B 1.366(4) . ? N15B C23B 1.477(4) . ? C16B C17B 1.440(5) . ? C17B C18B 1.324(5) . ? C17B H17B 0.9500 . ? C18B H18B 0.9500 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21B H21D 0.9800 . ? C21B H21E 0.9800 . ? C21B H21F 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? N1C C4C 1.314(6) . ? N1C C3C 1.429(6) . ? N1C C2C 1.433(6) . ? C2C H2C1 0.9800 . ? C2C H2C2 0.9800 . ? C2C H2C3 0.9800 . ? C3C H3C1 0.9800 . ? C3C H3C2 0.9800 . ? C3C H3C3 0.9800 . ? C4C O5C 1.226(6) . ? C4C H4C 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 104.51(12) . . ? O1 Mo1 O3 102.89(11) . . ? O2 Mo1 O3 101.22(10) . . ? O1 Mo1 O4 99.08(11) . . ? O2 Mo1 O4 97.64(10) . . ? O3 Mo1 O4 146.26(9) . . ? O1 Mo1 O5 161.20(10) . . ? O2 Mo1 O5 93.60(10) . . ? O3 Mo1 O5 77.99(8) . . ? O4 Mo1 O5 73.10(8) . . ? O1 Mo1 O6 89.87(10) . . ? O2 Mo1 O6 163.37(10) . . ? O3 Mo1 O6 83.24(8) . . ? O4 Mo1 O6 71.44(8) . . ? O5 Mo1 O6 71.49(7) . . ? O1 Mo1 Mo4 133.84(9) . . ? O2 Mo1 Mo4 85.34(8) . . ? O3 Mo1 Mo4 119.53(7) . . ? O4 Mo1 Mo4 34.84(6) . . ? O5 Mo1 Mo4 41.54(5) . . ? O6 Mo1 Mo4 78.60(5) . . ? O7 Mo2 O8 104.42(12) . . ? O7 Mo2 O9 97.95(11) . . ? O8 Mo2 O9 103.28(12) . . ? O7 Mo2 O3 98.45(11) . . ? O8 Mo2 O3 102.06(12) . . ? O9 Mo2 O3 145.17(9) . . ? O7 Mo2 O10 162.93(9) . . ? O8 Mo2 O10 92.65(10) . . ? O9 Mo2 O10 77.72(9) . . ? O3 Mo2 O10 77.61(9) . . ? O7 Mo2 O5 93.33(9) . . ? O8 Mo2 O5 162.25(10) . . ? O9 Mo2 O5 74.07(8) . . ? O3 Mo2 O5 74.48(8) . . ? O10 Mo2 O5 69.61(7) . . ? O11 Mo3 O12 105.16(12) . . ? O11 Mo3 O9 100.42(12) . 2_565 ? O12 Mo3 O9 101.88(11) . 2_565 ? O11 Mo3 O6 101.79(11) . . ? O12 Mo3 O6 96.78(10) . . ? O9 Mo3 O6 145.98(9) 2_565 . ? O11 Mo3 O5 159.62(10) . 2_565 ? O12 Mo3 O5 95.11(10) . 2_565 ? O9 Mo3 O5 77.04(8) 2_565 2_565 ? O6 Mo3 O5 73.16(8) . 2_565 ? O11 Mo3 O4 88.52(10) . . ? O12 Mo3 O4 163.81(10) . . ? O9 Mo3 O4 83.68(9) 2_565 . ? O6 Mo3 O4 71.52(8) . . ? O5 Mo3 O4 71.12(7) 2_565 . ? O11 Mo3 Mo4 136.63(9) . 2_565 ? O12 Mo3 Mo4 85.70(8) . 2_565 ? O9 Mo3 Mo4 118.58(7) 2_565 2_565 ? O6 Mo3 Mo4 34.84(6) . 2_565 ? O5 Mo3 Mo4 41.55(5) 2_565 2_565 ? O4 Mo3 Mo4 78.34(5) . 2_565 ? O13 Mo4 O10 103.80(10) . 2_565 ? O13 Mo4 O4 100.82(10) . . ? O10 Mo4 O4 96.17(10) 2_565 . ? O13 Mo4 O6 101.64(11) . 2_565 ? O10 Mo4 O6 96.53(10) 2_565 2_565 ? O4 Mo4 O6 150.67(9) . 2_565 ? O13 Mo4 O5 99.46(9) . . ? O10 Mo4 O5 156.73(9) 2_565 . ? O4 Mo4 O5 78.83(8) . . ? O6 Mo4 O5 79.09(8) 2_565 . ? O13 Mo4 O5 175.46(9) . 2_565 ? O10 Mo4 O5 80.70(9) 2_565 2_565 ? O4 Mo4 O5 77.96(8) . 2_565 ? O6 Mo4 O5 78.16(8) 2_565 2_565 ? O5 Mo4 O5 76.03(8) . 2_565 ? O13 Mo4 Mo3 90.85(8) . 2_565 ? O10 Mo4 Mo3 132.56(8) 2_565 2_565 ? O4 Mo4 Mo3 125.42(6) . 2_565 ? O6 Mo4 Mo3 36.04(6) 2_565 2_565 ? O5 Mo4 Mo3 46.61(6) . 2_565 ? O5 Mo4 Mo3 86.38(5) 2_565 2_565 ? O13 Mo4 Mo1 90.17(8) . . ? O10 Mo4 Mo1 132.30(8) 2_565 . ? O4 Mo4 Mo1 36.13(6) . . ? O6 Mo4 Mo1 125.37(6) 2_565 . ? O5 Mo4 Mo1 46.30(6) . . ? O5 Mo4 Mo1 86.32(5) 2_565 . ? Mo3 Mo4 Mo1 91.626(11) 2_565 . ? Mo1 O3 Mo2 116.16(11) . . ? Mo4 O4 Mo1 109.03(10) . . ? Mo4 O4 Mo3 110.59(9) . . ? Mo1 O4 Mo3 103.89(9) . . ? Mo4 O5 Mo1 92.16(8) . . ? Mo4 O5 Mo3 91.84(8) . 2_565 ? Mo1 O5 Mo3 162.75(10) . 2_565 ? Mo4 O5 Mo4 103.97(8) . 2_565 ? Mo1 O5 Mo4 97.62(8) . 2_565 ? Mo3 O5 Mo4 97.68(8) 2_565 2_565 ? Mo4 O5 Mo2 163.90(10) . . ? Mo1 O5 Mo2 85.50(7) . . ? Mo3 O5 Mo2 86.01(7) 2_565 . ? Mo4 O5 Mo2 92.13(7) 2_565 . ? Mo4 O6 Mo3 109.12(10) 2_565 . ? Mo4 O6 Mo1 110.05(9) 2_565 . ? Mo3 O6 Mo1 103.97(9) . . ? Mo3 O9 Mo2 117.57(11) 2_565 . ? Mo4 O10 Mo2 117.55(11) 2_565 . ? C2A N1A C19A 120.1(3) . . ? C2A N1A C9A 107.6(3) . . ? C19A N1A C9A 118.9(3) . . ? C7A C2A C3A 120.9(4) . . ? C7A C2A N1A 110.3(3) . . ? C3A C2A N1A 128.7(4) . . ? C4A C3A C2A 117.9(4) . . ? C4A C3A H3A 121.1 . . ? C2A C3A H3A 121.1 . . ? C5A C4A C3A 121.8(4) . . ? C5A C4A H4A 119.1 . . ? C3A C4A H4A 119.1 . . ? C4A C5A C6A 120.0(4) . . ? C4A C5A H5A 120.0 . . ? C6A C5A H5A 120.0 . . ? C7A C6A C5A 119.1(4) . . ? C7A C6A H6A 120.5 . . ? C5A C6A H6A 120.5 . . ? C6A C7A C2A 120.4(4) . . ? C6A C7A C8A 130.8(4) . . ? C2A C7A C8A 108.8(3) . . ? C7A C8A C21A 114.6(3) . . ? C7A C8A C9A 101.4(3) . . ? C21A C8A C9A 115.2(3) . . ? C7A C8A C20A 109.9(3) . . ? C21A C8A C20A 106.8(4) . . ? C9A C8A C20A 108.8(3) . . ? N1A C9A O10A 106.0(3) . . ? N1A C9A C18A 112.5(3) . . ? O10A C9A C18A 109.4(3) . . ? N1A C9A C8A 103.4(3) . . ? O10A C9A C8A 108.7(3) . . ? C18A C9A C8A 116.2(3) . . ? C11A O10A C9A 118.5(3) . . ? O10A C11A C12A 117.5(3) . . ? O10A C11A C16A 121.4(3) . . ? C12A C11A C16A 120.9(3) . . ? C11A C12A C13A 118.5(3) . . ? C11A C12A H12A 120.7 . . ? C13A C12A H12A 120.7 . . ? C12A C13A C14A 121.3(3) . . ? C12A C13A H13A 119.3 . . ? C14A C13A H13A 119.3 . . ? N15A C14A C13A 118.3(3) . . ? N15A C14A C22A 120.1(3) . . ? C13A C14A C22A 121.6(3) . . ? C14A N15A C16A 122.5(3) . . ? C14A N15A C23A 118.3(3) . . ? C16A N15A C23A 119.2(3) . . ? N15A C16A C11A 118.4(3) . . ? N15A C16A C17A 123.0(3) . . ? C11A C16A C17A 118.6(3) . . ? C18A C17A C16A 118.4(3) . . ? C18A C17A H17A 120.8 . . ? C16A C17A H17A 120.8 . . ? C17A C18A C9A 123.5(3) . . ? C17A C18A H18A 118.2 . . ? C9A C18A H18A 118.2 . . ? N1A C19A H19A 109.5 . . ? N1A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? N1A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C8A C20A H20A 109.5 . . ? C8A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? C8A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C8A C21A H21A 109.5 . . ? C8A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C8A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C14A C22A H22A 109.5 . . ? C14A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? C14A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? N15A C23A H23A 109.5 . . ? N15A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? N15A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? C2B N1B C9B 108.0(3) . . ? C2B N1B C19B 120.2(3) . . ? C9B N1B C19B 118.8(3) . . ? C3B C2B C7B 122.1(4) . . ? C3B C2B N1B 127.6(4) . . ? C7B C2B N1B 110.3(3) . . ? C2B C3B C4B 117.0(4) . . ? C2B C3B H3B 121.5 . . ? C4B C3B H3B 121.5 . . ? C5B C4B C3B 121.4(4) . . ? C5B C4B H4B 119.3 . . ? C3B C4B H4B 119.3 . . ? C4B C5B C6B 120.8(4) . . ? C4B C5B H5B 119.6 . . ? C6B C5B H5B 119.6 . . ? C7B C6B C5B 118.4(4) . . ? C7B C6B H6B 120.8 . . ? C5B C6B H6B 120.8 . . ? C6B C7B C2B 120.3(4) . . ? C6B C7B C8B 130.3(4) . . ? C2B C7B C8B 109.4(3) . . ? C7B C8B C21B 114.1(3) . . ? C7B C8B C20B 108.2(3) . . ? C21B C8B C20B 110.9(4) . . ? C7B C8B C9B 100.6(3) . . ? C21B C8B C9B 114.0(3) . . ? C20B C8B C9B 108.4(3) . . ? N1B C9B O10B 106.4(3) . . ? N1B C9B C18B 112.8(3) . . ? O10B C9B C18B 109.4(3) . . ? N1B C9B C8B 103.9(3) . . ? O10B C9B C8B 108.3(3) . . ? C18B C9B C8B 115.6(3) . . ? C11B O10B C9B 120.1(3) . . ? O10B C11B C12B 118.5(3) . . ? O10B C11B C16B 121.0(3) . . ? C12B C11B C16B 120.5(3) . . ? C13B C12B C11B 118.1(4) . . ? C13B C12B H12B 121.0 . . ? C11B C12B H12B 121.0 . . ? C14B C13B C12B 121.8(4) . . ? C14B C13B H13B 119.1 . . ? C12B C13B H13B 119.1 . . ? N15B C14B C13B 119.2(4) . . ? N15B C14B C22B 118.0(4) . . ? C13B C14B C22B 122.8(4) . . ? C14B N15B C16B 121.3(3) . . ? C14B N15B C23B 119.6(3) . . ? C16B N15B C23B 119.0(3) . . ? N15B C16B C11B 119.0(3) . . ? N15B C16B C17B 122.1(3) . . ? C11B C16B C17B 118.8(3) . . ? C18B C17B C16B 119.4(3) . . ? C18B C17B H17B 120.3 . . ? C16B C17B H17B 120.3 . . ? C17B C18B C9B 123.3(3) . . ? C17B C18B H18B 118.3 . . ? C9B C18B H18B 118.3 . . ? N1B C19B H19D 109.5 . . ? N1B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? N1B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C8B C20B H20D 109.5 . . ? C8B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C8B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? C8B C21B H21D 109.5 . . ? C8B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? C8B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C14B C22B H22D 109.5 . . ? C14B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? C14B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N15B C23B H23D 109.5 . . ? N15B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? N15B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C4C N1C C3C 121.7(5) . . ? C4C N1C C2C 118.9(4) . . ? C3C N1C C2C 119.4(5) . . ? N1C C2C H2C1 109.5 . . ? N1C C2C H2C2 109.5 . . ? H2C1 C2C H2C2 109.5 . . ? N1C C2C H2C3 109.5 . . ? H2C1 C2C H2C3 109.5 . . ? H2C2 C2C H2C3 109.5 . . ? N1C C3C H3C1 109.5 . . ? N1C C3C H3C2 109.5 . . ? H3C1 C3C H3C2 109.5 . . ? N1C C3C H3C3 109.5 . . ? H3C1 C3C H3C3 109.5 . . ? H3C2 C3C H3C3 109.5 . . ? O5C C4C N1C 125.0(5) . . ? O5C C4C H4C 117.5 . . ? N1C C4C H4C 117.5 . . ? _refine_diff_density_max 0.597 _refine_diff_density_min -0.583 _refine_diff_density_rms 0.109 _shelxl_version_number 2013-4 _database_code_depnum_ccdc_archive 'CCDC 962073' ####################################################################### # # 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_SP4Mo8.DMSO _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H104 Mo8 N8 O32 S2' _chemical_formula_weight 2569.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.547(4) _cell_length_b 12.049(4) _cell_length_c 18.237(6) _cell_angle_alpha 108.644(7) _cell_angle_beta 96.689(8) _cell_angle_gamma 90.338(7) _cell_volume 2385.1(14) _cell_formula_units_Z 1 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 5734 _cell_measurement_theta_min 1.19 _cell_measurement_theta_max 30.41 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8035 _exptl_absorpt_correction_T_max 0.8942 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18363 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 30.41 _reflns_number_total 13288 _reflns_number_gt 7448 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13288 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1266 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1991 _refine_ls_wR_factor_gt 0.1636 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.50004(5) 0.22059(5) 0.12096(3) 0.02960(15) Uani 1 1 d . . . Mo2 Mo 0.65085(4) 0.03677(4) 0.00511(3) 0.02440(14) Uani 1 1 d . . . Mo3 Mo 0.51796(5) -0.05295(5) 0.14311(3) 0.03179(15) Uani 1 1 d . . . Mo4 Mo 0.32577(5) 0.23869(5) -0.02717(4) 0.03267(16) Uani 1 1 d . . . O1 O 0.7366(4) 0.1475(4) 0.0014(3) 0.0390(11) Uani 1 1 d . . . O2 O 0.4174(4) 0.3476(4) -0.0305(3) 0.0437(12) Uani 1 1 d . . . O3 O 0.5889(4) 0.3242(4) 0.1100(3) 0.0373(11) Uani 1 1 d . . . O4 O 0.4248(4) -0.1620(5) 0.1430(3) 0.0462(13) Uani 1 1 d . . . O5 O 0.6165(4) 0.0953(4) 0.1113(2) 0.0300(10) Uani 1 1 d . . . O6 O 0.5497(5) 0.0280(5) 0.2372(3) 0.0552(15) Uani 1 1 d . . . O7 O 0.3528(4) 0.2612(4) 0.0819(3) 0.0353(11) Uani 1 1 d . . . O8 O 0.3407(4) 0.1309(4) -0.1275(3) 0.0367(11) Uani 1 1 d . . . O9 O 0.4840(3) 0.1086(3) -0.0096(2) 0.0245(9) Uani 1 1 d . . . O10 O 0.6000(4) -0.0419(4) -0.1042(2) 0.0306(10) Uani 1 1 d . . . O11 O 0.4938(5) 0.2589(5) 0.2176(3) 0.0498(14) Uani 1 1 d . . . O12 O 0.7486(4) -0.0680(4) 0.0182(3) 0.0325(10) Uani 1 1 d . . . O13 O 0.1905(4) 0.2899(5) -0.0378(3) 0.0561(15) Uani 1 1 d . . . N1A N 0.9360(5) 0.1421(5) 0.1839(3) 0.0376(13) Uani 1 1 d . . . N2A N 0.8020(5) 0.5959(5) 0.2662(3) 0.0360(13) Uani 1 1 d . . . O1A O 0.9417(4) 0.4576(4) 0.2260(3) 0.0401(11) Uani 1 1 d . . . C1A C 0.8547(6) 0.4975(6) 0.2817(4) 0.0347(15) Uani 1 1 d . . . C2A C 0.7716(6) 0.3975(7) 0.2711(4) 0.0433(18) Uani 1 1 d . . . H2A H 0.6977 0.4150 0.2860 0.052 Uiso 1 1 calc R . . C3A C 0.7945(6) 0.2847(6) 0.2421(4) 0.0395(16) Uani 1 1 d . . . H3A H 0.7423 0.2261 0.2427 0.047 Uiso 1 1 calc R . . C4A C 0.9019(6) 0.2565(6) 0.2099(4) 0.0350(15) Uani 1 1 d . . . C5A C 0.9707(6) 0.3439(6) 0.2009(4) 0.0353(15) Uani 1 1 d . . . C6A C 1.0680(6) 0.3166(7) 0.1623(4) 0.0425(17) Uani 1 1 d . . . H6A H 1.1141 0.3753 0.1556 0.051 Uiso 1 1 calc R . . C7A C 1.0953(7) 0.2022(8) 0.1342(5) 0.054(2) Uani 1 1 d . . . H7A H 1.1600 0.1831 0.1074 0.064 Uiso 1 1 calc R . . C8A C 1.0295(7) 0.1144(7) 0.1447(5) 0.050(2) Uani 1 1 d . . . C9A C 1.0576(9) -0.0123(8) 0.1143(7) 0.086(3) Uani 1 1 d . . . H9A1 H 1.0515 -0.0481 0.1538 0.129 Uiso 1 1 calc R . . H9A2 H 1.1357 -0.0181 0.1006 0.129 Uiso 1 1 calc R . . H9A3 H 1.0037 -0.0518 0.0690 0.129 Uiso 1 1 calc R . . C10A C 0.8715(7) 0.0514(6) 0.2028(5) 0.0463(18) Uani 1 1 d . . . H10A H 0.9131 -0.0196 0.1900 0.070 Uiso 1 1 calc R . . H10B H 0.7954 0.0371 0.1733 0.070 Uiso 1 1 calc R . . H10C H 0.8639 0.0775 0.2575 0.070 Uiso 1 1 calc R . . C11A C 0.9225(7) 0.5526(7) 0.3663(4) 0.0478(19) Uani 1 1 d . . . C12A C 0.9429(7) 0.6760(7) 0.3684(4) 0.0410(17) Uani 1 1 d . . . C13A C 1.0166(9) 0.7617(9) 0.4179(5) 0.068(3) Uani 1 1 d . . . H13A H 1.0671 0.7463 0.4568 0.082 Uiso 1 1 calc R . . C14A C 1.0167(10) 0.8717(8) 0.4106(6) 0.079(3) Uani 1 1 d . . . H14A H 1.0670 0.9314 0.4446 0.094 Uiso 1 1 calc R . . C15A C 0.9429(10) 0.8926(8) 0.3533(6) 0.073(3) Uani 1 1 d . . . H15A H 0.9441 0.9673 0.3487 0.088 Uiso 1 1 calc R . . C16A C 0.8673(7) 0.8087(7) 0.3026(5) 0.050(2) Uani 1 1 d . . . H16A H 0.8170 0.8252 0.2641 0.061 Uiso 1 1 calc R . . C17A C 0.8673(6) 0.6965(6) 0.3098(4) 0.0360(15) Uani 1 1 d . . . C18A C 1.0333(8) 0.4866(9) 0.3790(5) 0.077(3) Uani 1 1 d . . . H18A H 1.0815 0.4828 0.3389 0.116 Uiso 1 1 calc R . . H18B H 1.0114 0.4086 0.3770 0.116 Uiso 1 1 calc R . . H18C H 1.0758 0.5274 0.4290 0.116 Uiso 1 1 calc R . . C19A C 0.8412(9) 0.5479(8) 0.4240(5) 0.067(3) Uani 1 1 d . . . H19A H 0.8767 0.5906 0.4758 0.100 Uiso 1 1 calc R . . H19B H 0.8258 0.4677 0.4202 0.100 Uiso 1 1 calc R . . H19C H 0.7693 0.5823 0.4129 0.100 Uiso 1 1 calc R . . C20A C 0.7479(7) 0.5843(7) 0.1882(4) 0.0457(18) Uani 1 1 d . . . H20A H 0.6960 0.6469 0.1904 0.069 Uiso 1 1 calc R . . H20B H 0.7046 0.5104 0.1664 0.069 Uiso 1 1 calc R . . H20C H 0.8071 0.5878 0.1561 0.069 Uiso 1 1 calc R . . N1B N 0.2417(4) -0.3838(4) 0.0856(3) 0.0273(11) Uani 1 1 d . . . N2B N 0.4178(5) -0.4234(5) 0.3673(3) 0.0448(15) Uani 1 1 d . . . O1B O 0.2720(4) -0.3674(4) 0.2883(3) 0.0390(11) Uani 1 1 d . . . C1B C 0.3981(6) -0.3599(6) 0.3103(4) 0.0346(15) Uani 1 1 d . . . C2B C 0.4574(6) -0.4146(7) 0.2400(4) 0.0449(19) Uani 1 1 d . . . H2B H 0.5318 -0.4418 0.2469 0.054 Uiso 1 1 calc R . . C3B C 0.4083(6) -0.4266(7) 0.1668(4) 0.0435(18) Uani 1 1 d . . . H3B H 0.4491 -0.4593 0.1245 0.052 Uiso 1 1 calc R . . C4B C 0.2930(5) -0.3882(6) 0.1555(4) 0.0315(14) Uani 1 1 d . . . C5B C 0.2279(5) -0.3610(6) 0.2180(4) 0.0324(14) Uani 1 1 d . . . C6B C 0.1127(6) -0.3297(7) 0.2086(4) 0.0420(17) Uani 1 1 d . . . H6B H 0.0686 -0.3099 0.2501 0.050 Uiso 1 1 calc R . . C7B C 0.0666(6) -0.3290(7) 0.1362(4) 0.0423(17) Uani 1 1 d . . . H7B H -0.0109 -0.3098 0.1288 0.051 Uiso 1 1 calc R . . C8B C 0.1297(6) -0.3555(6) 0.0738(4) 0.0327(14) Uani 1 1 d . . . C9B C 0.0759(6) -0.3569(7) -0.0040(4) 0.0449(18) Uani 1 1 d . . . H9B1 H 0.1176 -0.3014 -0.0202 0.067 Uiso 1 1 calc R . . H9B2 H -0.0040 -0.3363 -0.0017 0.067 Uiso 1 1 calc R . . H9B3 H 0.0793 -0.4340 -0.0408 0.067 Uiso 1 1 calc R . . C10B C 0.3133(6) -0.4041(6) 0.0211(4) 0.0351(15) Uani 1 1 d . . . H10D H 0.3046 -0.4851 -0.0107 0.053 Uiso 1 1 calc R . . H10E H 0.3938 -0.3847 0.0420 0.053 Uiso 1 1 calc R . . H10F H 0.2880 -0.3557 -0.0100 0.053 Uiso 1 1 calc R . . C11B C 0.4368(6) -0.2335(6) 0.3573(4) 0.0386(16) Uani 1 1 d . . . C12B C 0.4145(6) -0.2268(7) 0.4368(4) 0.0407(17) Uani 1 1 d . . . C13B C 0.4039(8) -0.1321(8) 0.5014(4) 0.059(2) Uani 1 1 d . . . H13B H 0.4090 -0.0565 0.4987 0.071 Uiso 1 1 calc R . . C14B C 0.3857(9) -0.1499(10) 0.5701(5) 0.078(3) Uani 1 1 d . . . H14B H 0.3768 -0.0864 0.6140 0.093 Uiso 1 1 calc R . . C15B C 0.3805(10) -0.2629(11) 0.5735(5) 0.086(3) Uani 1 1 d . . . H15B H 0.3724 -0.2741 0.6208 0.103 Uiso 1 1 calc R . . C16B C 0.3872(8) -0.3588(9) 0.5089(5) 0.069(3) Uani 1 1 d . . . H16B H 0.3809 -0.4342 0.5118 0.083 Uiso 1 1 calc R . . C17B C 0.4035(6) -0.3413(7) 0.4391(4) 0.0438(18) Uani 1 1 d . . . C18B C 0.3783(8) -0.1420(7) 0.3268(5) 0.056(2) Uani 1 1 d . . . H18D H 0.2983 -0.1380 0.3366 0.084 Uiso 1 1 calc R . . H18E H 0.3816 -0.1630 0.2717 0.084 Uiso 1 1 calc R . . H18F H 0.4179 -0.0670 0.3528 0.084 Uiso 1 1 calc R . . C19B C 0.5715(8) -0.2164(10) 0.3567(6) 0.083(3) Uani 1 1 d . . . H19D H 0.5959 -0.1360 0.3841 0.124 Uiso 1 1 calc R . . H19E H 0.5884 -0.2367 0.3038 0.124 Uiso 1 1 calc R . . H19F H 0.6127 -0.2661 0.3818 0.124 Uiso 1 1 calc R . . C20B C 0.3737(8) -0.5433(7) 0.3469(5) 0.062(2) Uani 1 1 d . . . H20D H 0.4061 -0.5764 0.3858 0.094 Uiso 1 1 calc R . . H20E H 0.3956 -0.5880 0.2971 0.094 Uiso 1 1 calc R . . H20F H 0.2902 -0.5450 0.3443 0.094 Uiso 1 1 calc R . . S1A S 0.2005(3) 0.2102(3) 0.3665(2) 0.0682(9) Uani 0.75 1 d P . . S1B S 0.1935(11) 0.1076(12) 0.3439(8) 0.087(3) Uani 0.25 1 d P . . C21 C 0.2976(9) 0.1366(10) 0.2950(6) 0.084(3) Uani 1 1 d . . . C22 C 0.2491(11) 0.1523(13) 0.4403(7) 0.111(5) Uani 1 1 d . . . O14 O 0.0822(6) 0.1599(8) 0.3321(5) 0.106(3) 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 0.0349(3) 0.0221(3) 0.0297(3) 0.0038(2) 0.0087(2) 0.0004(2) Mo2 0.0232(3) 0.0223(3) 0.0290(3) 0.0088(2) 0.0069(2) -0.0001(2) Mo3 0.0426(3) 0.0308(3) 0.0255(3) 0.0131(2) 0.0071(2) 0.0009(3) Mo4 0.0252(3) 0.0268(3) 0.0507(4) 0.0180(3) 0.0074(2) 0.0057(2) O1 0.031(2) 0.032(3) 0.057(3) 0.015(2) 0.013(2) -0.004(2) O2 0.039(3) 0.031(3) 0.068(3) 0.022(3) 0.015(2) 0.001(2) O3 0.042(3) 0.028(2) 0.041(3) 0.009(2) 0.007(2) -0.007(2) O4 0.053(3) 0.049(3) 0.049(3) 0.028(3) 0.017(2) -0.003(3) O5 0.037(2) 0.023(2) 0.027(2) 0.0041(18) 0.0012(18) -0.0045(19) O6 0.084(4) 0.051(3) 0.028(3) 0.011(2) 0.005(3) 0.001(3) O7 0.029(2) 0.026(2) 0.052(3) 0.010(2) 0.015(2) 0.0024(19) O8 0.045(3) 0.035(3) 0.032(2) 0.015(2) -0.001(2) 0.004(2) O9 0.027(2) 0.021(2) 0.028(2) 0.0106(18) 0.0070(17) 0.0034(17) O10 0.037(2) 0.031(2) 0.031(2) 0.014(2) 0.0164(19) 0.009(2) O11 0.071(4) 0.046(3) 0.031(3) 0.007(2) 0.017(2) 0.005(3) O12 0.028(2) 0.024(2) 0.043(3) 0.007(2) 0.0063(19) 0.0006(18) O13 0.030(3) 0.062(4) 0.088(4) 0.038(3) 0.010(3) 0.022(3) N1A 0.041(3) 0.032(3) 0.040(3) 0.013(3) 0.001(3) 0.002(3) N2A 0.047(3) 0.028(3) 0.034(3) 0.009(2) 0.014(3) 0.004(3) O1A 0.049(3) 0.031(3) 0.044(3) 0.013(2) 0.016(2) 0.003(2) C1A 0.041(4) 0.036(4) 0.029(3) 0.010(3) 0.010(3) 0.006(3) C2A 0.040(4) 0.047(5) 0.046(4) 0.019(4) 0.011(3) 0.006(3) C3A 0.037(4) 0.041(4) 0.045(4) 0.022(3) 0.003(3) -0.002(3) C4A 0.039(4) 0.037(4) 0.026(3) 0.008(3) -0.002(3) 0.000(3) C5A 0.041(4) 0.031(4) 0.038(4) 0.014(3) 0.010(3) 0.007(3) C6A 0.045(4) 0.045(4) 0.047(4) 0.025(4) 0.017(3) 0.010(3) C7A 0.059(5) 0.059(5) 0.052(5) 0.025(4) 0.025(4) 0.017(4) C8A 0.056(5) 0.038(4) 0.055(5) 0.012(4) 0.017(4) 0.014(4) C9A 0.092(8) 0.048(6) 0.119(9) 0.012(6) 0.060(7) 0.023(6) C10A 0.048(4) 0.035(4) 0.060(5) 0.023(4) 0.005(4) -0.003(3) C11A 0.059(5) 0.057(5) 0.031(4) 0.021(4) 0.006(3) 0.008(4) C12A 0.050(4) 0.040(4) 0.034(4) 0.010(3) 0.012(3) -0.002(3) C13A 0.092(7) 0.065(6) 0.037(5) 0.009(4) -0.011(4) -0.007(5) C14A 0.098(8) 0.049(6) 0.072(7) 0.002(5) -0.006(6) -0.029(5) C15A 0.099(8) 0.036(5) 0.086(7) 0.018(5) 0.021(6) -0.001(5) C16A 0.058(5) 0.048(5) 0.052(5) 0.022(4) 0.018(4) 0.006(4) C17A 0.045(4) 0.029(4) 0.033(4) 0.007(3) 0.013(3) 0.000(3) C18A 0.084(7) 0.084(7) 0.058(6) 0.025(5) -0.023(5) 0.020(6) C19A 0.102(8) 0.061(6) 0.038(5) 0.016(4) 0.016(5) -0.006(5) C20A 0.050(4) 0.049(5) 0.041(4) 0.020(4) 0.003(3) 0.003(4) N1B 0.025(3) 0.027(3) 0.033(3) 0.011(2) 0.012(2) 0.003(2) N2B 0.055(4) 0.039(4) 0.042(3) 0.014(3) 0.007(3) 0.002(3) O1B 0.032(2) 0.057(3) 0.032(2) 0.016(2) 0.013(2) 0.009(2) C1B 0.030(3) 0.045(4) 0.032(3) 0.016(3) 0.007(3) 0.008(3) C2B 0.029(4) 0.064(5) 0.040(4) 0.014(4) 0.005(3) 0.012(3) C3B 0.028(3) 0.061(5) 0.039(4) 0.008(4) 0.015(3) 0.011(3) C4B 0.029(3) 0.032(4) 0.037(4) 0.014(3) 0.009(3) 0.005(3) C5B 0.029(3) 0.035(4) 0.037(4) 0.015(3) 0.010(3) 0.000(3) C6B 0.032(4) 0.052(5) 0.047(4) 0.018(4) 0.016(3) 0.006(3) C7B 0.030(3) 0.054(5) 0.048(4) 0.021(4) 0.011(3) 0.007(3) C8B 0.031(3) 0.034(4) 0.034(3) 0.010(3) 0.007(3) -0.002(3) C9B 0.038(4) 0.060(5) 0.041(4) 0.023(4) 0.001(3) -0.002(4) C10B 0.036(4) 0.033(4) 0.035(4) 0.008(3) 0.012(3) 0.005(3) C11B 0.043(4) 0.045(4) 0.029(3) 0.014(3) 0.007(3) 0.004(3) C12B 0.050(4) 0.045(4) 0.030(4) 0.014(3) 0.009(3) 0.000(3) C13B 0.075(6) 0.052(5) 0.039(4) -0.003(4) 0.011(4) -0.004(4) C14B 0.111(9) 0.078(8) 0.034(5) 0.001(5) 0.017(5) 0.001(7) C15B 0.109(9) 0.120(10) 0.036(5) 0.034(6) 0.017(5) -0.002(8) C16B 0.085(7) 0.086(7) 0.049(5) 0.041(5) 0.003(5) -0.005(6) C17B 0.048(4) 0.055(5) 0.033(4) 0.021(4) 0.007(3) 0.005(4) C18B 0.091(7) 0.031(4) 0.050(5) 0.014(4) 0.016(4) 0.009(4) C19B 0.065(6) 0.112(9) 0.070(7) 0.022(6) 0.026(5) -0.019(6) C20B 0.087(7) 0.040(5) 0.066(6) 0.025(4) 0.010(5) 0.009(5) S1A 0.0558(19) 0.0465(18) 0.107(3) 0.0323(19) 0.0057(18) 0.0028(15) S1B 0.079(8) 0.080(9) 0.104(9) 0.035(7) 0.008(7) 0.005(7) C21 0.078(7) 0.097(9) 0.095(8) 0.047(7) 0.031(6) 0.025(7) C22 0.103(9) 0.150(13) 0.079(8) 0.041(8) -0.002(7) 0.043(9) O14 0.058(4) 0.162(9) 0.107(6) 0.060(6) -0.004(4) -0.002(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O11 1.683(5) . ? Mo1 O3 1.686(5) . ? Mo1 O7 1.894(4) . ? Mo1 O5 2.006(4) . ? Mo1 O9 2.315(4) . ? Mo1 O10 2.352(5) 2_655 ? Mo1 Mo2 3.2112(10) . ? Mo2 O1 1.680(5) . ? Mo2 O12 1.752(4) . ? Mo2 O5 1.928(4) . ? Mo2 O10 1.931(4) . ? Mo2 O9 2.140(4) . ? Mo2 O9 2.364(4) 2_655 ? Mo2 Mo3 3.2028(11) 2_655 ? Mo3 O6 1.677(5) . ? Mo3 O4 1.692(5) . ? Mo3 O8 1.893(4) 2_655 ? Mo3 O10 1.994(4) 2_655 ? Mo3 O9 2.308(4) 2_655 ? Mo3 O5 2.370(4) . ? Mo3 Mo2 3.2028(11) 2_655 ? Mo4 O13 1.695(4) . ? Mo4 O2 1.701(5) . ? Mo4 O8 1.903(4) . ? Mo4 O7 1.906(5) . ? Mo4 O12 2.285(4) 2_655 ? Mo4 O9 2.473(4) . ? O8 Mo3 1.893(4) 2_655 ? O9 Mo3 2.308(4) 2_655 ? O9 Mo2 2.364(4) 2_655 ? O10 Mo3 1.994(4) 2_655 ? O10 Mo1 2.352(5) 2_655 ? O12 Mo4 2.285(4) 2_655 ? N1A C8A 1.349(9) . ? N1A C4A 1.383(8) . ? N1A C10A 1.468(9) . ? N2A C17A 1.381(8) . ? N2A C1A 1.427(8) . ? N2A C20A 1.448(9) . ? O1A C5A 1.356(7) . ? O1A C1A 1.485(7) . ? C1A C2A 1.486(10) . ? C1A C11A 1.578(10) . ? C2A C3A 1.332(10) . ? C2A H2A 0.9300 . ? C3A C4A 1.429(9) . ? C3A H3A 0.9300 . ? C4A C5A 1.377(9) . ? C5A C6A 1.381(9) . ? C6A C7A 1.361(10) . ? C6A H6A 0.9300 . ? C7A C8A 1.374(11) . ? C7A H7A 0.9300 . ? C8A C9A 1.500(11) . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A H10A 0.9600 . ? C10A H10B 0.9600 . ? C10A H10C 0.9600 . ? C11A C12A 1.491(11) . ? C11A C19A 1.503(10) . ? C11A C18A 1.544(11) . ? C12A C13A 1.349(11) . ? C12A C17A 1.385(10) . ? C13A C14A 1.374(13) . ? C13A H13A 0.9300 . ? C14A C15A 1.359(13) . ? C14A H14A 0.9300 . ? C15A C16A 1.358(12) . ? C15A H15A 0.9300 . ? C16A C17A 1.400(10) . ? C16A H16A 0.9300 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? C20A H20C 0.9600 . ? N1B C8B 1.350(8) . ? N1B C4B 1.358(8) . ? N1B C10B 1.474(7) . ? N2B C17B 1.394(9) . ? N2B C20B 1.444(10) . ? N2B C1B 1.474(9) . ? O1B C5B 1.350(8) . ? O1B C1B 1.459(7) . ? C1B C2B 1.488(9) . ? C1B C11B 1.524(10) . ? C2B C3B 1.350(10) . ? C2B H2B 0.9300 . ? C3B C4B 1.427(8) . ? C3B H3B 0.9300 . ? C4B C5B 1.390(8) . ? C5B C6B 1.391(9) . ? C6B C7B 1.368(10) . ? C6B H6B 0.9300 . ? C7B C8B 1.375(9) . ? C7B H7B 0.9300 . ? C8B C9B 1.477(9) . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10B H10D 0.9600 . ? C10B H10E 0.9600 . ? C10B H10F 0.9600 . ? C11B C12B 1.480(9) . ? C11B C18B 1.515(10) . ? C11B C19B 1.569(11) . ? C12B C13B 1.371(10) . ? C12B C17B 1.399(10) . ? C13B C14B 1.377(12) . ? C13B H13B 0.9300 . ? C14B C15B 1.384(14) . ? C14B H14B 0.9300 . ? C15B C16B 1.371(13) . ? C15B H15B 0.9300 . ? C16B C17B 1.388(10) . ? C16B H16B 0.9300 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? S1A S1B 1.171(13) . ? S1A O14 1.475(8) . ? S1A C22 1.745(12) . ? S1A C21 1.832(11) . ? S1B O14 1.459(13) . ? S1B C21 1.675(16) . ? S1B C22 1.710(17) . ? 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 O11 Mo1 O3 105.1(3) . . ? O11 Mo1 O7 103.2(2) . . ? O3 Mo1 O7 101.2(2) . . ? O11 Mo1 O5 98.7(2) . . ? O3 Mo1 O5 97.5(2) . . ? O7 Mo1 O5 146.18(18) . . ? O11 Mo1 O9 160.5(2) . . ? O3 Mo1 O9 93.58(19) . . ? O7 Mo1 O9 77.94(16) . . ? O5 Mo1 O9 72.98(15) . . ? O11 Mo1 O10 89.3(2) . 2_655 ? O3 Mo1 O10 163.18(18) . 2_655 ? O7 Mo1 O10 83.41(17) . 2_655 ? O5 Mo1 O10 71.31(16) . 2_655 ? O9 Mo1 O10 71.39(14) . 2_655 ? O11 Mo1 Mo2 133.10(18) . . ? O3 Mo1 Mo2 85.33(15) . . ? O7 Mo1 Mo2 119.69(14) . . ? O5 Mo1 Mo2 34.48(12) . . ? O9 Mo1 Mo2 41.75(9) . . ? O10 Mo1 Mo2 78.41(10) 2_655 . ? O1 Mo2 O12 104.4(2) . . ? O1 Mo2 O5 101.0(2) . . ? O12 Mo2 O5 96.77(19) . . ? O1 Mo2 O10 101.5(2) . . ? O12 Mo2 O10 96.71(19) . . ? O5 Mo2 O10 149.89(18) . . ? O1 Mo2 O9 99.21(19) . . ? O12 Mo2 O9 156.39(18) . . ? O5 Mo2 O9 78.63(16) . . ? O10 Mo2 O9 78.26(16) . . ? O1 Mo2 O9 174.92(18) . 2_655 ? O12 Mo2 O9 80.66(17) . 2_655 ? O5 Mo2 O9 77.81(16) . 2_655 ? O10 Mo2 O9 77.99(16) . 2_655 ? O9 Mo2 O9 75.73(16) . 2_655 ? O1 Mo2 Mo3 90.22(17) . 2_655 ? O12 Mo2 Mo3 132.68(15) . 2_655 ? O5 Mo2 Mo3 124.68(13) . 2_655 ? O10 Mo2 Mo3 35.97(12) . 2_655 ? O9 Mo2 Mo3 46.06(10) . 2_655 ? O9 Mo2 Mo3 86.47(10) 2_655 2_655 ? O1 Mo2 Mo1 90.22(16) . . ? O12 Mo2 Mo1 132.87(15) . . ? O5 Mo2 Mo1 36.11(12) . . ? O10 Mo2 Mo1 124.34(12) . . ? O9 Mo2 Mo1 46.10(10) . . ? O9 Mo2 Mo1 85.98(9) 2_655 . ? Mo3 Mo2 Mo1 90.80(3) 2_655 . ? O6 Mo3 O4 105.0(3) . . ? O6 Mo3 O8 99.5(2) . 2_655 ? O4 Mo3 O8 102.1(2) . 2_655 ? O6 Mo3 O10 102.1(2) . 2_655 ? O4 Mo3 O10 97.2(2) . 2_655 ? O8 Mo3 O10 146.09(18) 2_655 2_655 ? O6 Mo3 O9 158.7(2) . 2_655 ? O4 Mo3 O9 96.2(2) . 2_655 ? O8 Mo3 O9 77.28(16) 2_655 2_655 ? O10 Mo3 O9 73.10(15) 2_655 2_655 ? O6 Mo3 O5 87.8(2) . . ? O4 Mo3 O5 164.5(2) . . ? O8 Mo3 O5 84.00(18) 2_655 . ? O10 Mo3 O5 71.12(16) 2_655 . ? O9 Mo3 O5 71.00(14) 2_655 . ? O6 Mo3 Mo2 136.76(19) . 2_655 ? O4 Mo3 Mo2 86.21(17) . 2_655 ? O8 Mo3 Mo2 119.15(13) 2_655 2_655 ? O10 Mo3 Mo2 34.67(12) 2_655 2_655 ? O9 Mo3 Mo2 41.89(9) 2_655 2_655 ? O5 Mo3 Mo2 78.42(10) . 2_655 ? O13 Mo4 O2 104.4(3) . . ? O13 Mo4 O8 103.9(2) . . ? O2 Mo4 O8 97.7(2) . . ? O13 Mo4 O7 102.7(2) . . ? O2 Mo4 O7 99.1(2) . . ? O8 Mo4 O7 143.71(18) . . ? O13 Mo4 O12 91.8(2) . 2_655 ? O2 Mo4 O12 163.77(18) . 2_655 ? O8 Mo4 O12 78.08(18) . 2_655 ? O7 Mo4 O12 76.87(17) . 2_655 ? O13 Mo4 O9 161.0(2) . . ? O2 Mo4 O9 94.61(18) . . ? O8 Mo4 O9 72.98(16) . . ? O7 Mo4 O9 73.77(15) . . ? O12 Mo4 O9 69.15(14) 2_655 . ? Mo2 O5 Mo1 109.4(2) . . ? Mo2 O5 Mo3 110.14(18) . . ? Mo1 O5 Mo3 103.79(18) . . ? Mo1 O7 Mo4 117.1(2) . . ? Mo3 O8 Mo4 118.6(2) 2_655 . ? Mo2 O9 Mo3 92.06(14) . 2_655 ? Mo2 O9 Mo1 92.15(14) . . ? Mo3 O9 Mo1 162.2(2) 2_655 . ? Mo2 O9 Mo2 104.27(16) . 2_655 ? Mo3 O9 Mo2 98.23(15) 2_655 2_655 ? Mo1 O9 Mo2 97.51(14) . 2_655 ? Mo2 O9 Mo4 163.8(2) . . ? Mo3 O9 Mo4 86.00(13) 2_655 . ? Mo1 O9 Mo4 85.15(12) . . ? Mo2 O9 Mo4 91.87(13) 2_655 . ? Mo2 O10 Mo3 109.36(19) . 2_655 ? Mo2 O10 Mo1 110.10(18) . 2_655 ? Mo3 O10 Mo1 104.82(19) 2_655 2_655 ? Mo2 O12 Mo4 118.3(2) . 2_655 ? C8A N1A C4A 121.0(6) . . ? C8A N1A C10A 120.3(6) . . ? C4A N1A C10A 118.7(6) . . ? C17A N2A C1A 108.9(6) . . ? C17A N2A C20A 120.0(6) . . ? C1A N2A C20A 119.8(6) . . ? C5A O1A C1A 121.4(5) . . ? N2A C1A C2A 114.2(6) . . ? N2A C1A O1A 106.4(5) . . ? C2A C1A O1A 108.4(5) . . ? N2A C1A C11A 103.3(6) . . ? C2A C1A C11A 115.7(6) . . ? O1A C1A C11A 108.4(5) . . ? C3A C2A C1A 125.1(7) . . ? C3A C2A H2A 117.4 . . ? C1A C2A H2A 117.4 . . ? C2A C3A C4A 118.0(7) . . ? C2A C3A H3A 121.0 . . ? C4A C3A H3A 121.0 . . ? C5A C4A N1A 118.8(6) . . ? C5A C4A C3A 119.7(6) . . ? N1A C4A C3A 121.4(7) . . ? O1A C5A C4A 121.1(6) . . ? O1A C5A C6A 118.4(6) . . ? C4A C5A C6A 120.4(6) . . ? C7A C6A C5A 118.9(7) . . ? C7A C6A H6A 120.6 . . ? C5A C6A H6A 120.6 . . ? C6A C7A C8A 121.4(7) . . ? C6A C7A H7A 119.3 . . ? C8A C7A H7A 119.3 . . ? N1A C8A C7A 119.3(7) . . ? N1A C8A C9A 118.2(8) . . ? C7A C8A C9A 122.5(7) . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? N1A C10A H10A 109.5 . . ? N1A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? N1A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C12A C11A C19A 110.4(7) . . ? C12A C11A C18A 115.6(7) . . ? C19A C11A C18A 109.5(7) . . ? C12A C11A C1A 100.7(6) . . ? C19A C11A C1A 108.0(7) . . ? C18A C11A C1A 112.2(6) . . ? C13A C12A C17A 121.3(8) . . ? C13A C12A C11A 129.9(8) . . ? C17A C12A C11A 108.8(6) . . ? C12A C13A C14A 119.7(9) . . ? C12A C13A H13A 120.2 . . ? C14A C13A H13A 120.2 . . ? C15A C14A C13A 119.5(9) . . ? C15A C14A H14A 120.2 . . ? C13A C14A H14A 120.2 . . ? C14A C15A C16A 122.5(9) . . ? C14A C15A H15A 118.8 . . ? C16A C15A H15A 118.8 . . ? C15A C16A C17A 118.0(8) . . ? C15A C16A H16A 121.0 . . ? C17A C16A H16A 121.0 . . ? N2A C17A C12A 110.8(6) . . ? N2A C17A C16A 130.2(7) . . ? C12A C17A C16A 119.1(7) . . ? C11A C18A H18A 109.5 . . ? C11A C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C11A C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C11A C19A H19A 109.5 . . ? C11A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C11A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? N2A C20A H20A 109.5 . . ? N2A C20A H20B 109.5 . . ? H20A C20A H20B 109.5 . . ? N2A C20A H20C 109.5 . . ? H20A C20A H20C 109.5 . . ? H20B C20A H20C 109.5 . . ? C8B N1B C4B 122.9(5) . . ? C8B N1B C10B 118.4(5) . . ? C4B N1B C10B 118.6(5) . . ? C17B N2B C20B 121.0(7) . . ? C17B N2B C1B 105.3(6) . . ? C20B N2B C1B 119.9(6) . . ? C5B O1B C1B 119.9(5) . . ? O1B C1B N2B 105.3(5) . . ? O1B C1B C2B 109.8(5) . . ? N2B C1B C2B 111.7(6) . . ? O1B C1B C11B 109.2(5) . . ? N2B C1B C11B 104.1(5) . . ? C2B C1B C11B 116.1(6) . . ? C3B C2B C1B 123.1(6) . . ? C3B C2B H2B 118.4 . . ? C1B C2B H2B 118.4 . . ? C2B C3B C4B 118.9(6) . . ? C2B C3B H3B 120.6 . . ? C4B C3B H3B 120.6 . . ? N1B C4B C5B 118.7(5) . . ? N1B C4B C3B 123.1(6) . . ? C5B C4B C3B 118.1(6) . . ? O1B C5B C6B 117.9(6) . . ? O1B C5B C4B 121.8(6) . . ? C6B C5B C4B 120.3(6) . . ? C7B C6B C5B 117.7(6) . . ? C7B C6B H6B 121.2 . . ? C5B C6B H6B 121.2 . . ? C6B C7B C8B 122.8(6) . . ? C6B C7B H7B 118.6 . . ? C8B C7B H7B 118.6 . . ? N1B C8B C7B 117.7(6) . . ? N1B C8B C9B 121.0(6) . . ? C7B C8B C9B 121.3(6) . . ? C8B C9B H9B1 109.5 . . ? C8B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C8B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? N1B C10B H10D 109.5 . . ? N1B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? N1B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C12B C11B C18B 114.8(6) . . ? C12B C11B C1B 102.1(6) . . ? C18B C11B C1B 114.8(6) . . ? C12B C11B C19B 109.0(6) . . ? C18B C11B C19B 106.8(7) . . ? C1B C11B C19B 109.0(6) . . ? C13B C12B C17B 121.0(7) . . ? C13B C12B C11B 131.0(7) . . ? C17B C12B C11B 108.1(6) . . ? C12B C13B C14B 119.5(9) . . ? C12B C13B H13B 120.3 . . ? C14B C13B H13B 120.3 . . ? C13B C14B C15B 119.6(9) . . ? C13B C14B H14B 120.2 . . ? C15B C14B H14B 120.2 . . ? C16B C15B C14B 121.7(9) . . ? C16B C15B H15B 119.1 . . ? C14B C15B H15B 119.1 . . ? C15B C16B C17B 118.9(9) . . ? C15B C16B H16B 120.6 . . ? C17B C16B H16B 120.6 . . ? C16B C17B N2B 129.4(8) . . ? C16B C17B C12B 119.3(8) . . ? N2B C17B C12B 111.2(6) . . ? C11B C18B H18D 109.5 . . ? C11B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C11B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C11B C19B H19D 109.5 . . ? C11B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C11B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N2B C20B H20D 109.5 . . ? N2B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? N2B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? S1B S1A O14 65.7(7) . . ? S1B S1A C22 68.6(8) . . ? O14 S1A C22 108.4(6) . . ? S1B S1A C21 63.4(7) . . ? O14 S1A C21 105.8(5) . . ? C22 S1A C21 99.0(5) . . ? S1A S1B O14 67.2(7) . . ? S1A S1B C21 77.9(8) . . ? O14 S1B C21 115.0(9) . . ? S1A S1B C22 71.8(9) . . ? O14 S1B C22 111.1(9) . . ? C21 S1B C22 107.0(9) . . ? S1B C21 S1A 38.7(5) . . ? S1B C22 S1A 39.6(5) . . ? S1B O14 S1A 47.0(6) . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.462 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.170 _database_code_depnum_ccdc_archive 'CCDC 962074' ####################################################################### # # 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_(HDMA)3FeMo6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H32 Fe Mo6 N3 O25' _chemical_formula_weight 1177.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 11.157(4) _cell_length_b 11.733(4) _cell_length_c 22.906(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2998.6(17) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6428 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 30.42 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.609 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2268 _exptl_absorpt_coefficient_mu 2.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5857 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18033 _diffrn_reflns_av_R_equivalents 0.1420 _diffrn_reflns_av_sigmaI/netI 0.1412 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.42 _reflns_number_total 4565 _reflns_number_gt 2575 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0837P)^2^+0.4120P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4565 _refine_ls_number_parameters 253 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1494 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1915 _refine_ls_wR_factor_gt 0.1581 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.24038(7) 0.09289(7) 0.07287(3) 0.0188(2) Uani 1 1 d . . . Mo2 Mo 0.0000 0.0000 0.14550(5) 0.0199(3) Uani 1 2 d S . . Fe1 Fe 0.0000 0.0000 0.0000 0.0151(5) Uani 1 4 d S . . O1 O 0.3070(7) 0.0357(8) 0.0000 0.022(2) Uani 1 2 d S . . O2 O 0.1091(7) 0.1344(7) 0.0000 0.0152(17) Uani 1 2 d SD . . O3 O 0.3243(6) 0.0123(6) 0.1190(3) 0.0324(17) Uani 1 1 d . . . O4 O -0.1057(5) 0.0551(5) 0.0644(2) 0.0155(12) Uani 1 1 d D . . O5 O 0.3022(7) 0.2272(6) 0.0754(3) 0.0329(17) Uani 1 1 d . . . O6 O 0.1037(6) 0.1237(6) 0.1220(3) 0.0239(14) Uani 1 1 d . . . O7 O -0.0927(6) 0.0734(6) 0.1899(3) 0.0314(16) Uani 1 1 d . . . Mo4 Mo 0.28570(11) 0.19949(12) 0.5000 0.0432(4) Uani 1 2 d S . . Mo5 Mo 0.39548(11) 0.10259(9) 0.37326(4) 0.0460(3) Uani 1 1 d . . . Fe2 Fe 0.5000 0.0000 0.5000 0.0147(5) Uani 1 4 d S . . O8 O 0.1425(9) 0.1888(11) 0.5000 0.061(3) Uani 1 2 d S . . O9 O 0.4399(10) 0.2124(12) 0.3363(5) 0.099(5) Uani 1 1 d . . . O10 O 0.2742(10) 0.1115(12) 0.4204(6) 0.025(3) Uani 0.50 1 d P . . O11 O 0.5601(10) 0.0659(11) 0.4244(5) 0.020(3) Uani 0.50 1 d P . . O12 O 0.4747(10) 0.1517(10) 0.4605(5) 0.016(3) Uani 0.50 1 d P . . O13 O 0.3333(11) 0.0248(11) 0.4676(5) 0.024(3) Uani 0.50 1 d P . . O14 O 0.2351(14) 0.1003(16) 0.3545(11) 0.061(3) Uani 0.50 1 d P . . O15 O 0.3389(12) 0.0261(16) 0.3149(6) 0.041(4) Uani 0.50 1 d P . . O16 O 0.5706(12) 0.0458(13) 0.3580(6) 0.030(3) Uani 0.50 1 d P . . O17 O 0.3681(12) 0.2223(11) 0.4376(6) 0.029(3) Uani 0.50 1 d P . . O18 O 0.2927(16) 0.3338(14) 0.4628(10) 0.063(6) Uani 0.50 1 d P . . N1 N 0.1517(9) 0.3174(9) 0.1959(5) 0.054(3) Uani 1 1 d . . . H1A H 0.1933 0.3819 0.1895 0.064 Uiso 1 1 calc R . . H1B H 0.1634 0.2720 0.1648 0.064 Uiso 1 1 calc R . . C1 C 0.0293(12) 0.3461(13) 0.1976(7) 0.062(4) Uani 1 1 d . . . H1C H -0.0165 0.2810 0.2096 0.092 Uiso 1 1 calc R . . H1D H 0.0037 0.3697 0.1594 0.092 Uiso 1 1 calc R . . H1E H 0.0171 0.4073 0.2248 0.092 Uiso 1 1 calc R . . C2 C 0.2038(12) 0.2612(15) 0.2463(6) 0.063(4) Uani 1 1 d . . . H2A H 0.2455 0.3163 0.2697 0.095 Uiso 1 1 calc R . . H2B H 0.2590 0.2037 0.2335 0.095 Uiso 1 1 calc R . . H2C H 0.1413 0.2265 0.2690 0.095 Uiso 1 1 calc R . . N2 N 0.456(4) 0.473(2) 0.3772(10) 0.106(14) Uani 0.50 1 d P . . C3 C 0.483(3) 0.460(3) 0.4177(13) 0.064(10) Uani 0.50 1 d P . . C4 C 0.462(2) 0.506(3) 0.3163(9) 0.054(7) Uani 0.50 1 d P . . O1W O 0.0441(10) 0.3450(10) 0.0000 0.069(5) Uani 1 2 d S . . H2 H 0.078(18) 0.205(7) 0.0000 0.083 Uiso 1 2 d SD . . H4 H -0.110(13) 0.126(5) 0.050(6) 0.083 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 0.0157(4) 0.0193(4) 0.0213(4) -0.0004(3) -0.0043(3) -0.0021(3) Mo2 0.0219(6) 0.0236(6) 0.0141(5) 0.000 0.000 -0.0005(5) Fe1 0.0098(11) 0.0205(14) 0.0151(11) 0.000 0.000 -0.0003(10) O1 0.011(4) 0.018(5) 0.036(5) 0.000 0.000 0.001(4) O2 0.006(4) 0.017(5) 0.023(4) 0.000 0.000 0.001(3) O3 0.023(3) 0.040(5) 0.034(4) 0.006(3) -0.011(3) 0.002(3) O4 0.016(3) 0.015(3) 0.016(3) 0.001(2) 0.004(2) 0.000(2) O5 0.040(4) 0.022(4) 0.037(4) 0.000(3) -0.004(3) -0.013(3) O6 0.025(3) 0.026(4) 0.021(3) -0.003(3) -0.003(3) 0.001(3) O7 0.036(4) 0.037(4) 0.022(3) -0.003(3) 0.008(3) -0.004(3) Mo4 0.0160(6) 0.0155(7) 0.0982(13) 0.000 0.000 0.0062(5) Mo5 0.0628(7) 0.0393(6) 0.0357(6) 0.0183(5) -0.0276(5) -0.0180(6) Fe2 0.0107(11) 0.0179(13) 0.0154(11) 0.000 0.000 0.0019(10) O8 0.021(4) 0.044(7) 0.118(10) 0.000 0.000 0.006(4) O9 0.071(7) 0.137(11) 0.090(8) 0.089(8) -0.038(6) -0.050(7) O10 0.013(6) 0.026(8) 0.035(8) 0.010(6) -0.006(5) -0.007(5) O11 0.016(6) 0.030(7) 0.015(6) -0.012(5) -0.001(5) 0.003(5) O12 0.019(6) 0.012(6) 0.018(6) 0.000(5) 0.005(5) 0.002(5) O13 0.021(6) 0.023(7) 0.028(7) 0.007(6) 0.005(5) 0.005(5) O14 0.021(4) 0.044(7) 0.118(10) 0.000 0.000 0.006(4) O15 0.020(7) 0.080(13) 0.023(7) 0.003(8) -0.006(6) 0.002(7) O16 0.025(7) 0.044(9) 0.021(7) -0.003(6) 0.005(6) -0.010(6) O17 0.029(7) 0.017(7) 0.042(8) 0.018(6) 0.009(6) 0.010(6) O18 0.045(10) 0.027(10) 0.119(17) 0.012(10) -0.014(10) 0.004(8) N1 0.045(6) 0.048(7) 0.068(7) 0.024(6) 0.008(6) -0.003(5) C1 0.044(8) 0.078(11) 0.064(9) 0.007(8) 0.002(7) 0.014(7) C2 0.050(8) 0.095(12) 0.045(8) 0.023(8) -0.016(6) -0.011(8) N2 0.21(4) 0.07(2) 0.038(13) -0.013(13) 0.020(18) -0.11(2) C3 0.039(18) 0.09(3) 0.058(16) 0.035(17) 0.004(14) 0.012(19) C4 0.047(17) 0.09(2) 0.027(11) 0.002(14) 0.001(9) 0.02(2) O1W 0.020(6) 0.033(7) 0.154(15) 0.000 0.000 0.001(5) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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(7) . ? Mo1 O5 1.722(7) . ? Mo1 O6 1.930(6) . ? Mo1 O1 1.946(5) . ? Mo1 O2 2.274(5) . ? Mo1 O4 2.304(6) 2 ? Mo2 O7 1.688(7) . ? Mo2 O7 1.688(7) 2 ? Mo2 O6 1.932(7) 2 ? Mo2 O6 1.932(7) . ? Mo2 O4 2.293(6) . ? Mo2 O4 2.293(6) 2 ? Fe1 O2 1.992(8) . ? Fe1 O2 1.992(8) 5 ? Fe1 O4 1.996(6) 6 ? Fe1 O4 1.996(6) 5 ? Fe1 O4 1.996(6) . ? Fe1 O4 1.996(6) 2 ? O1 Mo1 1.946(5) 6 ? O2 Mo1 2.274(5) 6 ? O2 H2 0.90(2) . ? O4 Mo1 2.304(6) 2 ? O4 H4 0.89(2) . ? Mo4 O8 1.603(11) . ? Mo4 O17 1.722(13) 6_556 ? Mo4 O17 1.722(13) . ? Mo4 O18 1.793(17) . ? Mo4 O18 1.793(17) 6_556 ? Mo4 O10 2.099(14) . ? Mo4 O10 2.099(14) 6_556 ? Mo4 O13 2.244(13) . ? Mo4 O13 2.244(13) 6_556 ? Mo4 O12 2.362(11) 6_556 ? Mo4 O12 2.362(11) . ? Mo5 O9 1.619(10) . ? Mo5 O15 1.730(15) . ? Mo5 O10 1.734(13) . ? Mo5 O16 1.815(16) 2_655 ? Mo5 O14 1.840(16) . ? Mo5 O17 2.058(14) . ? Mo5 O16 2.094(14) . ? Mo5 O11 2.220(12) . ? Mo5 O12 2.261(12) . ? Mo5 O11 2.350(12) 2_655 ? Mo5 O13 2.447(12) . ? Fe2 O11 2.012(12) 6_556 ? Fe2 O11 2.012(12) 2_655 ? Fe2 O11 2.012(12) . ? Fe2 O11 2.012(12) 5_656 ? Fe2 O12 2.016(11) 2_655 ? Fe2 O12 2.016(11) 5_656 ? Fe2 O12 2.016(11) 6_556 ? Fe2 O12 2.016(11) . ? Fe2 O13 2.023(12) 5_656 ? Fe2 O13 2.023(12) 2_655 ? Fe2 O13 2.023(12) . ? Fe2 O13 2.023(12) 6_556 ? O10 O14 1.58(3) . ? O10 O13 1.625(17) . ? O10 O17 1.715(19) . ? O11 O16 1.542(16) . ? O11 O12 1.614(16) . ? O11 Mo5 2.350(12) 2_655 ? O12 O17 1.542(17) . ? O12 O12 1.81(2) 6_556 ? O13 O13 1.48(2) 6_556 ? O14 O15 1.71(2) . ? O15 O16 1.65(2) 2_655 ? O16 O15 1.65(2) 2_655 ? O16 Mo5 1.815(16) 2_655 ? O17 O18 1.66(2) . ? O18 O18 1.70(4) 6_556 ? N1 C1 1.407(16) . ? N1 C2 1.450(15) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N2 C3 0.99(3) . ? N2 N2 1.18(5) 2_665 ? N2 C3 1.40(3) 2_665 ? N2 C4 1.45(3) . ? N2 C4 1.69(3) 2_665 ? C3 C3 1.02(6) 2_665 ? C3 N2 1.40(3) 2_665 ? C4 C4 0.86(4) 2_665 ? C4 N2 1.69(3) 2_665 ? 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 O5 105.5(3) . . ? O3 Mo1 O6 100.2(3) . . ? O5 Mo1 O6 97.2(3) . . ? O3 Mo1 O1 97.5(3) . . ? O5 Mo1 O1 101.0(4) . . ? O6 Mo1 O1 150.1(3) . . ? O3 Mo1 O2 158.6(3) . . ? O5 Mo1 O2 95.0(3) . . ? O6 Mo1 O2 83.0(2) . . ? O1 Mo1 O2 72.0(3) . . ? O3 Mo1 O4 89.6(3) . 2 ? O5 Mo1 O4 162.6(3) . 2 ? O6 Mo1 O4 71.0(2) . 2 ? O1 Mo1 O4 85.3(3) . 2 ? O2 Mo1 O4 71.3(3) . 2 ? O7 Mo2 O7 105.8(5) . 2 ? O7 Mo2 O6 100.6(3) . 2 ? O7 Mo2 O6 98.7(3) 2 2 ? O7 Mo2 O6 98.7(3) . . ? O7 Mo2 O6 100.6(3) 2 . ? O6 Mo2 O6 147.7(4) 2 . ? O7 Mo2 O4 91.7(3) . . ? O7 Mo2 O4 161.4(3) 2 . ? O6 Mo2 O4 71.3(2) 2 . ? O6 Mo2 O4 82.6(2) . . ? O7 Mo2 O4 161.4(3) . 2 ? O7 Mo2 O4 91.7(3) 2 2 ? O6 Mo2 O4 82.6(2) 2 2 ? O6 Mo2 O4 71.3(2) . 2 ? O4 Mo2 O4 71.8(3) . 2 ? O2 Fe1 O2 180.0(3) . 5 ? O2 Fe1 O4 96.0(2) . 6 ? O2 Fe1 O4 84.0(2) 5 6 ? O2 Fe1 O4 84.0(2) . 5 ? O2 Fe1 O4 96.0(2) 5 5 ? O4 Fe1 O4 84.7(3) 6 5 ? O2 Fe1 O4 96.0(2) . . ? O2 Fe1 O4 84.0(2) 5 . ? O4 Fe1 O4 95.3(3) 6 . ? O4 Fe1 O4 180.0(3) 5 . ? O2 Fe1 O4 84.0(2) . 2 ? O2 Fe1 O4 96.0(2) 5 2 ? O4 Fe1 O4 180.0(4) 6 2 ? O4 Fe1 O4 95.3(3) 5 2 ? O4 Fe1 O4 84.7(3) . 2 ? Mo1 O1 Mo1 118.1(4) 6 . ? Fe1 O2 Mo1 102.9(3) . 6 ? Fe1 O2 Mo1 102.9(3) . . ? Mo1 O2 Mo1 94.5(3) 6 . ? Fe1 O2 H2 120(10) . . ? Mo1 O2 H2 116(8) 6 . ? Mo1 O2 H2 116(8) . . ? Fe1 O4 Mo2 101.7(2) . . ? Fe1 O4 Mo1 101.7(2) . 2 ? Mo2 O4 Mo1 93.1(2) . 2 ? Fe1 O4 H4 93(10) . . ? Mo2 O4 H4 126(10) . . ? Mo1 O4 H4 134(10) 2 . ? Mo1 O6 Mo2 119.6(3) . . ? O8 Mo4 O17 123.0(5) . 6_556 ? O8 Mo4 O17 123.0(5) . . ? O17 Mo4 O17 112.4(10) 6_556 . ? O8 Mo4 O18 96.4(7) . . ? O17 Mo4 O18 103.6(8) 6_556 . ? O17 Mo4 O18 56.3(8) . . ? O8 Mo4 O18 96.4(7) . 6_556 ? O17 Mo4 O18 56.3(8) 6_556 6_556 ? O17 Mo4 O18 103.6(8) . 6_556 ? O18 Mo4 O18 56.7(14) . 6_556 ? O8 Mo4 O10 84.3(4) . . ? O17 Mo4 O10 146.2(5) 6_556 . ? O17 Mo4 O10 52.2(6) . . ? O18 Mo4 O10 91.3(8) . . ? O18 Mo4 O10 147.9(8) 6_556 . ? O8 Mo4 O10 84.3(4) . 6_556 ? O17 Mo4 O10 52.2(6) 6_556 6_556 ? O17 Mo4 O10 146.2(5) . 6_556 ? O18 Mo4 O10 147.9(8) . 6_556 ? O18 Mo4 O10 91.3(8) 6_556 6_556 ? O10 Mo4 O10 120.6(7) . 6_556 ? O8 Mo4 O13 99.5(5) . . ? O17 Mo4 O13 106.9(5) 6_556 . ? O17 Mo4 O13 75.0(5) . . ? O18 Mo4 O13 129.5(8) . . ? O18 Mo4 O13 161.7(7) 6_556 . ? O10 Mo4 O13 43.8(5) . . ? O10 Mo4 O13 81.5(5) 6_556 . ? O8 Mo4 O13 99.5(5) . 6_556 ? O17 Mo4 O13 75.0(5) 6_556 6_556 ? O17 Mo4 O13 106.9(5) . 6_556 ? O18 Mo4 O13 161.7(7) . 6_556 ? O18 Mo4 O13 129.5(8) 6_556 6_556 ? O10 Mo4 O13 81.5(5) . 6_556 ? O10 Mo4 O13 43.8(5) 6_556 6_556 ? O13 Mo4 O13 38.6(6) . 6_556 ? O8 Mo4 O12 150.6(4) . 6_556 ? O17 Mo4 O12 40.7(5) 6_556 6_556 ? O17 Mo4 O12 83.0(5) . 6_556 ? O18 Mo4 O12 110.6(6) . 6_556 ? O18 Mo4 O12 89.3(7) 6_556 6_556 ? O10 Mo4 O12 105.7(4) . 6_556 ? O10 Mo4 O12 66.8(4) 6_556 6_556 ? O13 Mo4 O12 72.4(4) . 6_556 ? O13 Mo4 O12 56.3(4) 6_556 6_556 ? O8 Mo4 O12 150.6(4) . . ? O17 Mo4 O12 83.0(5) 6_556 . ? O17 Mo4 O12 40.7(5) . . ? O18 Mo4 O12 89.3(7) . . ? O18 Mo4 O12 110.6(6) 6_556 . ? O10 Mo4 O12 66.8(4) . . ? O10 Mo4 O12 105.7(4) 6_556 . ? O13 Mo4 O12 56.3(4) . . ? O13 Mo4 O12 72.4(4) 6_556 . ? O12 Mo4 O12 45.0(6) 6_556 . ? O9 Mo5 O15 96.9(7) . . ? O9 Mo5 O10 121.1(7) . . ? O15 Mo5 O10 103.2(6) . . ? O9 Mo5 O16 126.8(7) . 2_655 ? O15 Mo5 O16 55.3(7) . 2_655 ? O10 Mo5 O16 109.9(6) . 2_655 ? O9 Mo5 O14 100.8(7) . . ? O15 Mo5 O14 57.1(8) . . ? O10 Mo5 O14 52.3(8) . . ? O16 Mo5 O14 98.3(7) 2_655 . ? O9 Mo5 O17 82.9(7) . . ? O15 Mo5 O17 148.6(6) . . ? O10 Mo5 O17 52.9(6) . . ? O16 Mo5 O17 145.4(5) 2_655 . ? O14 Mo5 O17 91.9(8) . . ? O9 Mo5 O16 83.2(6) . . ? O15 Mo5 O16 92.7(6) . . ? O10 Mo5 O16 148.3(6) . . ? O16 Mo5 O16 57.9(7) 2_655 . ? O14 Mo5 O16 149.7(8) . . ? O17 Mo5 O16 118.3(5) . . ? O9 Mo5 O11 100.2(5) . . ? O15 Mo5 O11 127.5(6) . . ? O10 Mo5 O11 109.2(5) . . ? O16 Mo5 O11 75.1(5) 2_655 . ? O14 Mo5 O11 157.6(8) . . ? O17 Mo5 O11 83.0(5) . . ? O16 Mo5 O11 41.8(4) . . ? O9 Mo5 O12 98.0(5) . . ? O15 Mo5 O12 163.5(6) . . ? O10 Mo5 O12 74.9(5) . . ? O16 Mo5 O12 109.4(5) 2_655 . ? O14 Mo5 O12 126.2(8) . . ? O17 Mo5 O12 41.5(5) . . ? O16 Mo5 O12 82.1(5) . . ? O11 Mo5 O12 42.2(4) . . ? O9 Mo5 O11 149.9(5) . 2_655 ? O15 Mo5 O11 91.5(7) . 2_655 ? O10 Mo5 O11 84.6(5) . 2_655 ? O16 Mo5 O11 41.0(5) 2_655 2_655 ? O14 Mo5 O11 108.0(7) . 2_655 ? O17 Mo5 O11 104.4(4) . 2_655 ? O16 Mo5 O11 67.6(5) . 2_655 ? O11 Mo5 O11 53.1(6) . 2_655 ? O12 Mo5 O11 72.0(4) . 2_655 ? O9 Mo5 O13 147.7(6) . . ? O15 Mo5 O13 112.7(6) . . ? O10 Mo5 O13 41.5(5) . . ? O16 Mo5 O13 82.6(5) 2_655 . ? O14 Mo5 O13 85.7(8) . . ? O17 Mo5 O13 65.2(5) . . ? O16 Mo5 O13 107.0(5) . . ? O11 Mo5 O13 72.3(4) . . ? O12 Mo5 O13 54.9(4) . . ? O11 Mo5 O13 46.0(4) 2_655 . ? O11 Fe2 O11 180.000(2) 6_556 2_655 ? O11 Fe2 O11 118.9(7) 6_556 . ? O11 Fe2 O11 61.1(7) 2_655 . ? O11 Fe2 O11 61.1(7) 6_556 5_656 ? O11 Fe2 O11 118.9(7) 2_655 5_656 ? O11 Fe2 O11 180.000(2) . 5_656 ? O11 Fe2 O12 132.7(5) 6_556 2_655 ? O11 Fe2 O12 47.3(5) 2_655 2_655 ? O11 Fe2 O12 84.6(5) . 2_655 ? O11 Fe2 O12 95.4(5) 5_656 2_655 ? O11 Fe2 O12 84.6(5) 6_556 5_656 ? O11 Fe2 O12 95.4(5) 2_655 5_656 ? O11 Fe2 O12 132.7(5) . 5_656 ? O11 Fe2 O12 47.3(5) 5_656 5_656 ? O12 Fe2 O12 53.3(6) 2_655 5_656 ? O11 Fe2 O12 47.3(5) 6_556 6_556 ? O11 Fe2 O12 132.7(5) 2_655 6_556 ? O11 Fe2 O12 95.4(5) . 6_556 ? O11 Fe2 O12 84.6(5) 5_656 6_556 ? O12 Fe2 O12 180.0(6) 2_655 6_556 ? O12 Fe2 O12 126.7(6) 5_656 6_556 ? O11 Fe2 O12 95.4(5) 6_556 . ? O11 Fe2 O12 84.6(5) 2_655 . ? O11 Fe2 O12 47.3(5) . . ? O11 Fe2 O12 132.7(5) 5_656 . ? O12 Fe2 O12 126.7(6) 2_655 . ? O12 Fe2 O12 180.0(6) 5_656 . ? O12 Fe2 O12 53.3(6) 6_556 . ? O11 Fe2 O13 55.5(5) 6_556 5_656 ? O11 Fe2 O13 124.5(5) 2_655 5_656 ? O11 Fe2 O13 93.7(5) . 5_656 ? O11 Fe2 O13 86.3(5) 5_656 5_656 ? O12 Fe2 O13 84.8(5) 2_655 5_656 ? O12 Fe2 O13 65.2(5) 5_656 5_656 ? O12 Fe2 O13 95.2(5) 6_556 5_656 ? O12 Fe2 O13 114.8(5) . 5_656 ? O11 Fe2 O13 93.7(5) 6_556 2_655 ? O11 Fe2 O13 86.3(5) 2_655 2_655 ? O11 Fe2 O13 55.5(5) . 2_655 ? O11 Fe2 O13 124.5(5) 5_656 2_655 ? O12 Fe2 O13 65.2(5) 2_655 2_655 ? O12 Fe2 O13 84.8(5) 5_656 2_655 ? O12 Fe2 O13 114.8(5) 6_556 2_655 ? O12 Fe2 O13 95.2(5) . 2_655 ? O13 Fe2 O13 43.0(7) 5_656 2_655 ? O11 Fe2 O13 124.5(5) 6_556 . ? O11 Fe2 O13 55.5(5) 2_655 . ? O11 Fe2 O13 86.3(5) . . ? O11 Fe2 O13 93.7(5) 5_656 . ? O12 Fe2 O13 95.2(5) 2_655 . ? O12 Fe2 O13 114.8(5) 5_656 . ? O12 Fe2 O13 84.8(5) 6_556 . ? O12 Fe2 O13 65.2(5) . . ? O13 Fe2 O13 180.000(2) 5_656 . ? O13 Fe2 O13 137.0(7) 2_655 . ? O11 Fe2 O13 86.3(5) 6_556 6_556 ? O11 Fe2 O13 93.7(5) 2_655 6_556 ? O11 Fe2 O13 124.5(5) . 6_556 ? O11 Fe2 O13 55.5(5) 5_656 6_556 ? O12 Fe2 O13 114.8(5) 2_655 6_556 ? O12 Fe2 O13 95.2(5) 5_656 6_556 ? O12 Fe2 O13 65.2(5) 6_556 6_556 ? O12 Fe2 O13 84.8(5) . 6_556 ? O13 Fe2 O13 137.0(7) 5_656 6_556 ? O13 Fe2 O13 180.000(2) 2_655 6_556 ? O13 Fe2 O13 43.0(7) . 6_556 ? O14 O10 O13 134.2(12) . . ? O14 O10 O17 116.8(11) . . ? O13 O10 O17 94.3(9) . . ? O14 O10 Mo5 67.3(8) . . ? O13 O10 Mo5 93.4(7) . . ? O17 O10 Mo5 73.3(6) . . ? O14 O10 Mo4 152.8(11) . . ? O13 O10 Mo4 72.8(7) . . ? O17 O10 Mo4 52.5(6) . . ? Mo5 O10 Mo4 121.5(6) . . ? O16 O11 O12 130.3(11) . . ? O16 O11 Fe2 144.6(10) . . ? O12 O11 Fe2 66.5(6) . . ? O16 O11 Mo5 64.7(7) . . ? O12 O11 Mo5 70.2(6) . . ? Fe2 O11 Mo5 104.7(5) . . ? O16 O11 Mo5 50.5(7) . 2_655 ? O12 O11 Mo5 154.7(8) . 2_655 ? Fe2 O11 Mo5 100.1(5) . 2_655 ? Mo5 O11 Mo5 94.3(4) . 2_655 ? O17 O12 O11 127.9(10) . . ? O17 O12 O12 110.0(6) . 6_556 ? O11 O12 O12 120.9(6) . 6_556 ? O17 O12 Fe2 137.3(8) . . ? O11 O12 Fe2 66.3(6) . . ? O12 O12 Fe2 63.4(3) 6_556 . ? O17 O12 Mo5 62.2(7) . . ? O11 O12 Mo5 67.5(6) . . ? O12 O12 Mo5 152.2(3) 6_556 . ? Fe2 O12 Mo5 103.1(5) . . ? O17 O12 Mo4 46.7(6) . . ? O11 O12 Mo4 150.6(8) . . ? O12 O12 Mo4 67.5(3) 6_556 . ? Fe2 O12 Mo4 99.4(5) . . ? Mo5 O12 Mo4 92.8(4) . . ? O13 O13 O10 131.7(7) 6_556 . ? O13 O13 Fe2 68.5(3) 6_556 . ? O10 O13 Fe2 135.0(8) . . ? O13 O13 Mo4 70.7(3) 6_556 . ? O10 O13 Mo4 63.4(7) . . ? Fe2 O13 Mo4 103.2(6) . . ? O13 O13 Mo5 152.1(3) 6_556 . ? O10 O13 Mo5 45.0(5) . . ? Fe2 O13 Mo5 96.7(5) . . ? Mo4 O13 Mo5 91.0(4) . . ? O10 O14 O15 111.3(12) . . ? O10 O14 Mo5 60.4(8) . . ? O15 O14 Mo5 58.2(7) . . ? O16 O15 O14 110.9(11) 2_655 . ? O16 O15 Mo5 65.0(7) 2_655 . ? O14 O15 Mo5 64.7(9) . . ? O11 O16 O15 135.8(12) . 2_655 ? O11 O16 Mo5 88.5(9) . 2_655 ? O15 O16 Mo5 59.7(8) 2_655 2_655 ? O11 O16 Mo5 73.5(7) . . ? O15 O16 Mo5 146.7(9) 2_655 . ? Mo5 O16 Mo5 117.9(7) 2_655 . ? O12 O17 O18 134.1(12) . . ? O12 O17 O10 98.1(9) . . ? O18 O17 O10 111.5(10) . . ? O12 O17 Mo4 92.6(7) . . ? O18 O17 Mo4 64.0(8) . . ? O10 O17 Mo4 75.3(7) . . ? O12 O17 Mo5 76.3(7) . . ? O18 O17 Mo5 149.6(11) . . ? O10 O17 Mo5 53.8(6) . . ? Mo4 O17 Mo5 124.6(7) . . ? O17 O18 O18 110.4(9) . 6_556 ? O17 O18 Mo4 59.7(7) . . ? O18 O18 Mo4 61.6(7) 6_556 . ? C1 N1 C2 118.5(11) . . ? C1 N1 H1A 107.7 . . ? C2 N1 H1A 107.7 . . ? C1 N1 H1B 107.7 . . ? C2 N1 H1B 107.7 . . ? H1A N1 H1B 107.1 . . ? N1 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? N1 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 N2 N2 80(3) . 2_665 ? C3 N2 C3 47(3) . 2_665 ? N2 N2 C3 44.0(14) 2_665 2_665 ? C3 N2 C4 158(4) . . ? N2 N2 C4 79.2(15) 2_665 . ? C3 N2 C4 117(2) 2_665 . ? C3 N2 C4 129(4) . 2_665 ? N2 N2 C4 57.5(17) 2_665 2_665 ? C3 N2 C4 101(2) 2_665 2_665 ? C4 N2 C4 30.5(17) . 2_665 ? N2 C3 C3 88(3) . 2_665 ? N2 C3 N2 56(3) . 2_665 ? C3 C3 N2 44.8(17) 2_665 2_665 ? C4 C4 N2 90(2) 2_665 . ? C4 C4 N2 59(2) 2_665 2_665 ? N2 C4 N2 43(2) . 2_665 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 30.42 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.427 _refine_diff_density_min -1.616 _refine_diff_density_rms 0.305 _database_code_depnum_ccdc_archive 'CCDC 962075' ####################################################################### # # 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_SP2AlMo6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H69 Al Mo6 N4 O30' _chemical_formula_weight 1736.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8567(5) _cell_length_b 13.9952(9) _cell_length_c 14.8673(10) _cell_angle_alpha 107.733(4) _cell_angle_beta 91.033(4) _cell_angle_gamma 104.028(3) _cell_volume 1503.16(17) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13468 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 30.07 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.918 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 866 _exptl_absorpt_coefficient_mu 1.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8794 _exptl_absorpt_correction_T_max 0.9741 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19531 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0420 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 30.07 _reflns_number_total 8641 _reflns_number_gt 6660 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0840P)^2^+1.0800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8641 _refine_ls_number_parameters 391 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1527 _refine_ls_wR_factor_gt 0.1363 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.122 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.0000 0.0000 0.5000 0.0200(3) Uani 1 2 d S . . Mo1 Mo 0.25302(5) -0.12892(3) 0.36510(2) 0.02733(10) Uani 1 1 d . . . Mo2 Mo 0.02520(5) 0.24384(3) 0.50429(3) 0.02925(11) Uani 1 1 d . . . Mo3 Mo 0.26972(5) 0.10950(3) 0.36837(3) 0.03023(11) Uani 1 1 d . . . O1 O 0.2420(4) 0.0232(2) 0.48101(19) 0.0247(6) Uani 1 1 d D . . O2 O -0.0119(4) 0.0721(2) 0.4113(2) 0.0258(6) Uani 1 1 d D . . O3 O -0.0247(4) -0.1321(2) 0.4069(2) 0.0263(6) Uani 1 1 d D . . O4 O -0.2212(4) 0.1864(2) 0.5278(2) 0.0309(6) Uani 1 1 d . . . O5 O 0.2536(4) 0.2257(2) 0.4759(2) 0.0325(6) Uani 1 1 d . . . O6 O 0.2096(4) -0.0377(2) 0.3012(2) 0.0297(6) Uani 1 1 d . . . O7 O 0.4794(4) -0.0991(3) 0.3789(2) 0.0355(7) Uani 1 1 d . . . O8 O 0.1870(4) -0.2418(3) 0.2743(2) 0.0373(7) Uani 1 1 d . . . O9 O 0.2104(5) 0.1476(3) 0.2769(2) 0.0440(8) Uani 1 1 d . . . O10 O -0.0310(5) 0.2854(3) 0.4146(3) 0.0453(8) Uani 1 1 d . . . O11 O 0.0870(5) 0.3516(3) 0.6019(3) 0.0447(8) Uani 1 1 d . . . O12 O 0.4950(4) 0.1347(3) 0.3771(3) 0.0469(9) Uani 1 1 d . . . O13 O 0.3537(5) 0.6432(3) 0.8396(3) 0.0516(10) Uani 1 1 d . . . H1 H 0.306(7) 0.048(5) 0.536(2) 0.062 Uiso 1 1 d D . . H2 H -0.103(6) 0.052(5) 0.369(3) 0.062 Uiso 1 1 d D . . H3 H -0.094(7) -0.156(5) 0.353(3) 0.062 Uiso 1 1 d D . . C1 C 0.2255(7) 0.5898(4) 0.8894(3) 0.0403(11) Uani 1 1 d . A . C2 C 0.0518(8) 0.6002(4) 0.8612(5) 0.0655(19) Uani 1 1 d D . . C3 C 0.0397(8) 0.7029(5) 0.9249(4) 0.0593(17) Uani 1 1 d . . . C4 C -0.0694(9) 0.7623(6) 0.9182(6) 0.081(2) Uani 1 1 d . . . H4 H -0.1541 0.7418 0.8667 0.097 Uiso 1 1 calc R . . C5 C -0.0494(11) 0.8566(7) 0.9925(6) 0.082(2) Uani 1 1 d . . . H5 H -0.1201 0.9001 0.9888 0.099 Uiso 1 1 calc R . . C6 C 0.0703(10) 0.8856(5) 1.0692(5) 0.0634(17) Uani 1 1 d . . . H6 H 0.0780 0.9471 1.1180 0.076 Uiso 1 1 calc R . . C7 C 0.1812(10) 0.8236(5) 1.0748(4) 0.0592(16) Uani 1 1 d . . . H7 H 0.2642 0.8434 1.1268 0.071 Uiso 1 1 calc R . . C8 C 0.1664(9) 0.7321(4) 1.0020(4) 0.0525(14) Uani 1 1 d . A . C9 C 0.2343(8) 0.4801(4) 0.8700(4) 0.0483(13) Uani 1 1 d . . . H9 H 0.1716 0.4427 0.9063 0.058 Uiso 1 1 calc R . . C10 C 0.3239(7) 0.4323(4) 0.8054(4) 0.0451(12) Uani 1 1 d . . . H10 H 0.3228 0.3635 0.7968 0.054 Uiso 1 1 calc R . . C11 C 0.4234(6) 0.4874(4) 0.7483(4) 0.0369(10) Uani 1 1 d . . . C12 C 0.6074(7) 0.4951(4) 0.6228(4) 0.0472(12) Uani 1 1 d . . . C13 C 0.6118(8) 0.5987(5) 0.6419(5) 0.0600(16) Uani 1 1 d . . . H13 H 0.6758 0.6364 0.6061 0.072 Uiso 1 1 calc R . . C14 C 0.5218(8) 0.6469(4) 0.7136(5) 0.0607(17) Uani 1 1 d . . . H14 H 0.5244 0.7164 0.7255 0.073 Uiso 1 1 calc R . . C15 C 0.4288(7) 0.5919(4) 0.7672(4) 0.0422(11) Uani 1 1 d . . . C16 C -0.1160(15) 0.5156(9) 0.8550(8) 0.147(4) Uani 1 1 d D . . H16A H -0.1164 0.4548 0.8029 0.220 Uiso 1 1 calc R . . H16B H -0.2168 0.5400 0.8454 0.220 Uiso 1 1 calc R . . H16C H -0.1206 0.4986 0.9130 0.220 Uiso 1 1 calc R . . C17 C 0.0319(15) 0.5940(9) 0.7496(7) 0.147(4) Uani 1 1 d D . . H17A H 0.1340 0.6396 0.7365 0.220 Uiso 1 1 calc R . . H17B H -0.0715 0.6148 0.7370 0.220 Uiso 1 1 calc R . . H17C H 0.0214 0.5240 0.7099 0.220 Uiso 1 1 calc R . . C18A C 0.4020(17) 0.6713(10) 1.0443(9) 0.056(2) Uiso 0.50 1 d P A 1 C18B C 0.2646(17) 0.5956(10) 1.0629(9) 0.056(2) Uiso 0.50 1 d P A 2 C19 C 0.5117(9) 0.3314(4) 0.6595(4) 0.0522(14) Uani 1 1 d . . . H19A H 0.6122 0.3169 0.6278 0.078 Uiso 1 1 calc R . . H19B H 0.4057 0.2873 0.6209 0.078 Uiso 1 1 calc R . . H19C H 0.5155 0.3187 0.7194 0.078 Uiso 1 1 calc R . . C20 C 0.7107(10) 0.4434(6) 0.5474(5) 0.0709(19) Uani 1 1 d . . . H20A H 0.7908 0.4157 0.5751 0.106 Uiso 1 1 calc R . . H20B H 0.7761 0.4934 0.5203 0.106 Uiso 1 1 calc R . . H20C H 0.6312 0.3881 0.4987 0.106 Uiso 1 1 calc R . . N1 N 0.2633(12) 0.6546(4) 0.9908(4) 0.087(2) Uani 1 1 d . . . N2 N 0.5141(5) 0.4425(3) 0.6759(3) 0.0400(9) Uani 1 1 d . . . O14 O -0.2785(5) 0.0224(3) 0.2706(3) 0.0479(9) Uani 1 1 d . . . C21 C -0.2380(8) 0.0833(5) 0.2075(5) 0.0576(15) Uani 1 1 d . . . H21A H -0.1320 0.0718 0.1786 0.069 Uiso 1 1 calc R . . H21B H -0.2140 0.1563 0.2441 0.069 Uiso 1 1 calc R . . C22 C -0.3802(11) 0.0585(7) 0.1325(5) 0.082(2) Uani 1 1 d . . . H22A H -0.4072 -0.0142 0.0971 0.123 Uiso 1 1 calc R . . H22B H -0.3435 0.0986 0.0908 0.123 Uiso 1 1 calc R . . H22C H -0.4831 0.0748 0.1604 0.123 Uiso 1 1 calc R . . O1W O 1.2122(6) 0.1747(3) 0.7650(3) 0.0557(10) 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 Al1 0.0197(7) 0.0207(7) 0.0202(7) 0.0051(6) 0.0033(6) 0.0080(6) Mo1 0.02411(18) 0.03077(19) 0.02567(18) 0.00391(14) 0.00314(13) 0.01096(14) Mo2 0.02893(19) 0.02520(19) 0.0331(2) 0.00800(14) 0.00266(14) 0.00774(14) Mo3 0.02454(18) 0.0349(2) 0.0344(2) 0.01445(16) 0.00796(14) 0.00880(14) O1 0.0212(13) 0.0277(14) 0.0220(13) 0.0036(11) 0.0012(10) 0.0063(11) O2 0.0238(13) 0.0277(14) 0.0261(14) 0.0090(11) 0.0019(10) 0.0064(11) O3 0.0252(14) 0.0252(14) 0.0260(14) 0.0035(11) 0.0032(11) 0.0079(11) O4 0.0284(15) 0.0340(16) 0.0327(15) 0.0096(12) 0.0062(12) 0.0137(12) O5 0.0262(14) 0.0289(15) 0.0380(16) 0.0071(13) 0.0036(12) 0.0037(12) O6 0.0336(15) 0.0315(15) 0.0248(14) 0.0065(12) 0.0052(11) 0.0132(12) O7 0.0303(16) 0.0428(18) 0.0362(17) 0.0125(14) 0.0074(13) 0.0143(14) O8 0.0426(18) 0.0339(17) 0.0317(16) 0.0016(13) 0.0031(13) 0.0145(14) O9 0.051(2) 0.046(2) 0.0403(18) 0.0213(16) 0.0099(15) 0.0116(16) O10 0.047(2) 0.048(2) 0.050(2) 0.0243(17) 0.0086(16) 0.0199(17) O11 0.047(2) 0.0300(17) 0.049(2) 0.0012(15) 0.0038(16) 0.0086(15) O12 0.0295(17) 0.050(2) 0.059(2) 0.0157(18) 0.0145(16) 0.0095(15) O13 0.061(2) 0.0318(18) 0.066(2) 0.0169(17) 0.028(2) 0.0166(17) C1 0.048(3) 0.034(2) 0.034(2) 0.0099(19) 0.008(2) 0.003(2) C2 0.047(3) 0.035(3) 0.089(5) -0.008(3) 0.022(3) -0.001(2) C3 0.046(3) 0.048(3) 0.059(4) -0.010(3) 0.017(3) 0.000(2) C4 0.044(4) 0.085(5) 0.087(5) -0.010(4) 0.005(3) 0.014(3) C5 0.066(5) 0.076(5) 0.099(6) 0.011(4) 0.029(4) 0.029(4) C6 0.079(5) 0.049(3) 0.055(4) 0.006(3) 0.019(3) 0.016(3) C7 0.090(5) 0.053(3) 0.032(3) 0.007(2) 0.008(3) 0.021(3) C8 0.079(4) 0.042(3) 0.038(3) 0.013(2) 0.021(3) 0.017(3) C9 0.061(3) 0.038(3) 0.045(3) 0.017(2) 0.003(2) 0.007(2) C10 0.054(3) 0.031(2) 0.050(3) 0.013(2) -0.005(2) 0.009(2) C11 0.031(2) 0.031(2) 0.046(3) 0.0073(19) -0.0060(19) 0.0088(17) C12 0.037(3) 0.051(3) 0.056(3) 0.013(3) 0.008(2) 0.019(2) C13 0.054(3) 0.049(3) 0.086(5) 0.030(3) 0.033(3) 0.016(3) C14 0.057(4) 0.038(3) 0.100(5) 0.032(3) 0.038(3) 0.020(3) C15 0.038(3) 0.034(2) 0.057(3) 0.016(2) 0.007(2) 0.013(2) C16 0.127(7) 0.129(7) 0.145(7) -0.035(5) -0.062(5) 0.067(6) C17 0.127(7) 0.129(7) 0.145(7) -0.035(5) -0.062(5) 0.067(6) C19 0.067(4) 0.036(3) 0.052(3) 0.001(2) -0.008(3) 0.027(3) C20 0.065(4) 0.072(5) 0.075(5) 0.011(4) 0.017(3) 0.031(4) N1 0.174(8) 0.049(3) 0.039(3) 0.010(2) 0.012(4) 0.032(4) N2 0.034(2) 0.034(2) 0.049(2) 0.0052(17) -0.0097(17) 0.0143(16) O14 0.0384(19) 0.068(3) 0.049(2) 0.0298(19) 0.0103(16) 0.0207(18) C21 0.053(3) 0.066(4) 0.061(4) 0.031(3) 0.005(3) 0.014(3) C22 0.077(5) 0.117(7) 0.058(4) 0.038(4) -0.003(4) 0.025(5) O1W 0.063(3) 0.044(2) 0.055(2) 0.0157(18) -0.0130(19) 0.0054(18) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Al1 O1 1.891(3) 2_556 ? Al1 O1 1.891(3) . ? Al1 O2 1.902(3) . ? Al1 O2 1.902(3) 2_556 ? Al1 O3 1.905(3) . ? Al1 O3 1.905(3) 2_556 ? Mo1 O8 1.692(3) . ? Mo1 O7 1.719(3) . ? Mo1 O6 1.894(3) . ? Mo1 O4 1.986(3) 2_556 ? Mo1 O3 2.274(3) . ? Mo1 O1 2.317(3) . ? Mo2 O10 1.700(3) . ? Mo2 O11 1.704(3) . ? Mo2 O5 1.909(3) . ? Mo2 O4 1.989(3) . ? Mo2 O2 2.322(3) . ? Mo2 O3 2.333(3) 2_556 ? Mo3 O9 1.700(3) . ? Mo3 O12 1.713(3) . ? Mo3 O6 1.929(3) . ? Mo3 O5 1.934(3) . ? Mo3 O2 2.296(3) . ? Mo3 O1 2.330(3) . ? O1 H1 0.87(2) . ? O2 H2 0.88(2) . ? O3 Mo2 2.333(3) 2_556 ? O3 H3 0.89(2) . ? O4 Mo1 1.986(3) 2_556 ? O13 C15 1.334(6) . ? O13 C1 1.455(6) . ? C1 C2 1.473(9) . ? C1 N1 1.484(7) . ? C1 C9 1.492(7) . ? C2 C3 1.488(8) . ? C2 C16 1.524(13) . ? C2 C17 1.638(11) . ? C3 C4 1.353(10) . ? C3 C8 1.396(9) . ? C4 C5 1.411(10) . ? C4 H4 0.9300 . ? C5 C6 1.358(11) . ? C5 H5 0.9300 . ? C6 C7 1.388(9) . ? C6 H6 0.9300 . ? C7 C8 1.379(8) . ? C7 H7 0.9300 . ? C8 N1 1.441(9) . ? C9 C10 1.314(8) . ? C9 H9 0.9300 . ? C10 C11 1.435(7) . ? C10 H10 0.9300 . ? C11 N2 1.376(6) . ? C11 C15 1.392(6) . ? C12 N2 1.347(7) . ? C12 C13 1.381(8) . ? C12 C20 1.505(8) . ? C13 C14 1.383(8) . ? C13 H13 0.9300 . ? C14 C15 1.372(8) . ? C14 H14 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18A N1 1.268(14) . ? C18B N1 1.541(14) . ? C19 N2 1.494(6) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? O14 C21 1.440(7) . ? C21 C22 1.464(9) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? 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 Al1 O1 180.0 2_556 . ? O1 Al1 O2 95.21(12) 2_556 . ? O1 Al1 O2 84.79(12) . . ? O1 Al1 O2 84.79(12) 2_556 2_556 ? O1 Al1 O2 95.21(12) . 2_556 ? O2 Al1 O2 180.000(1) . 2_556 ? O1 Al1 O3 94.98(12) 2_556 . ? O1 Al1 O3 85.02(12) . . ? O2 Al1 O3 95.44(13) . . ? O2 Al1 O3 84.56(13) 2_556 . ? O1 Al1 O3 85.02(12) 2_556 2_556 ? O1 Al1 O3 94.98(12) . 2_556 ? O2 Al1 O3 84.56(13) . 2_556 ? O2 Al1 O3 95.44(13) 2_556 2_556 ? O3 Al1 O3 180.00(16) . 2_556 ? O8 Mo1 O7 106.19(16) . . ? O8 Mo1 O6 98.56(14) . . ? O7 Mo1 O6 102.64(15) . . ? O8 Mo1 O4 98.60(15) . 2_556 ? O7 Mo1 O4 94.76(14) . 2_556 ? O6 Mo1 O4 151.01(12) . 2_556 ? O8 Mo1 O3 93.63(14) . . ? O7 Mo1 O3 157.86(13) . . ? O6 Mo1 O3 83.61(12) . . ? O4 Mo1 O3 72.15(11) 2_556 . ? O8 Mo1 O1 160.23(13) . . ? O7 Mo1 O1 93.27(13) . . ? O6 Mo1 O1 73.19(11) . . ? O4 Mo1 O1 82.93(11) 2_556 . ? O3 Mo1 O1 67.93(10) . . ? O10 Mo2 O11 106.09(18) . . ? O10 Mo2 O5 101.46(16) . . ? O11 Mo2 O5 98.62(16) . . ? O10 Mo2 O4 95.51(16) . . ? O11 Mo2 O4 100.22(15) . . ? O5 Mo2 O4 149.98(13) . . ? O10 Mo2 O2 95.69(15) . . ? O11 Mo2 O2 157.85(15) . . ? O5 Mo2 O2 72.62(11) . . ? O4 Mo2 O2 81.27(11) . . ? O10 Mo2 O3 158.70(15) . 2_556 ? O11 Mo2 O3 92.65(15) . 2_556 ? O5 Mo2 O3 85.23(12) . 2_556 ? O4 Mo2 O3 70.79(11) . 2_556 ? O2 Mo2 O3 66.77(10) . 2_556 ? O9 Mo3 O12 106.58(19) . . ? O9 Mo3 O6 97.06(15) . . ? O12 Mo3 O6 99.52(16) . . ? O9 Mo3 O5 100.93(16) . . ? O12 Mo3 O5 97.24(16) . . ? O6 Mo3 O5 150.73(13) . . ? O9 Mo3 O2 93.81(15) . . ? O12 Mo3 O2 158.84(15) . . ? O6 Mo3 O2 83.17(12) . . ? O5 Mo3 O2 72.82(11) . . ? O9 Mo3 O1 158.75(14) . . ? O12 Mo3 O1 93.51(15) . . ? O6 Mo3 O1 72.31(11) . . ? O5 Mo3 O1 82.89(12) . . ? O2 Mo3 O1 67.12(10) . . ? Al1 O1 Mo1 102.94(12) . . ? Al1 O1 Mo3 103.58(12) . . ? Mo1 O1 Mo3 90.23(10) . . ? Al1 O1 H1 110(4) . . ? Mo1 O1 H1 123(4) . . ? Mo3 O1 H1 123(4) . . ? Al1 O2 Mo3 104.47(12) . . ? Al1 O2 Mo2 104.55(12) . . ? Mo3 O2 Mo2 91.20(10) . . ? Al1 O2 H2 120(4) . . ? Mo3 O2 H2 121(4) . . ? Mo2 O2 H2 111(4) . . ? Al1 O3 Mo1 104.10(12) . . ? Al1 O3 Mo2 104.06(12) . 2_556 ? Mo1 O3 Mo2 94.74(10) . 2_556 ? Al1 O3 H3 125(4) . . ? Mo1 O3 H3 106(4) . . ? Mo2 O3 H3 118(4) 2_556 . ? Mo1 O4 Mo2 117.01(15) 2_556 . ? Mo2 O5 Mo3 118.31(15) . . ? Mo1 O6 Mo3 118.93(15) . . ? C15 O13 C1 122.2(4) . . ? O13 C1 C2 107.0(5) . . ? O13 C1 N1 105.5(5) . . ? C2 C1 N1 103.9(5) . . ? O13 C1 C9 110.9(4) . . ? C2 C1 C9 114.0(4) . . ? N1 C1 C9 114.8(5) . . ? C1 C2 C3 105.5(5) . . ? C1 C2 C16 121.2(7) . . ? C3 C2 C16 111.4(6) . . ? C1 C2 C17 111.8(6) . . ? C3 C2 C17 111.1(7) . . ? C16 C2 C17 95.8(6) . . ? C4 C3 C8 122.1(6) . . ? C4 C3 C2 130.9(6) . . ? C8 C3 C2 107.0(6) . . ? C3 C4 C5 117.2(7) . . ? C3 C4 H4 121.4 . . ? C5 C4 H4 121.4 . . ? C6 C5 C4 121.8(8) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 120.2(6) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C8 C7 C6 119.0(6) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C7 C8 C3 119.7(6) . . ? C7 C8 N1 130.0(6) . . ? C3 C8 N1 110.2(5) . . ? C10 C9 C1 124.9(5) . . ? C10 C9 H9 117.5 . . ? C1 C9 H9 117.5 . . ? C9 C10 C11 119.3(5) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? N2 C11 C15 118.3(5) . . ? N2 C11 C10 123.4(4) . . ? C15 C11 C10 118.3(5) . . ? N2 C12 C13 118.5(5) . . ? N2 C12 C20 120.7(5) . . ? C13 C12 C20 120.8(6) . . ? C12 C13 C14 120.6(5) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 119.9(5) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? O13 C15 C14 117.9(5) . . ? O13 C15 C11 122.2(5) . . ? C14 C15 C11 119.8(5) . . ? C2 C16 H16A 109.5 . . ? C2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C17 H17A 109.5 . . ? C2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C12 C20 H20A 109.5 . . ? C12 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C12 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18A N1 C8 121.5(8) . . ? C18A N1 C1 126.4(9) . . ? C8 N1 C1 105.6(5) . . ? C18A N1 C18B 59.5(8) . . ? C8 N1 C18B 122.0(7) . . ? C1 N1 C18B 116.0(6) . . ? C12 N2 C11 122.9(4) . . ? C12 N2 C19 119.9(5) . . ? C11 N2 C19 117.2(5) . . ? O14 C21 C22 113.2(6) . . ? O14 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? O14 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.214 _refine_diff_density_min -1.279 _refine_diff_density_rms 0.259 _database_code_depnum_ccdc_archive 'CCDC 962076' ####################################################################### # # 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_SP2Mo6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H47.5 Mo6 N4.5 O21' _chemical_formula_weight 1515.0 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.0060 '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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_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 10.438(2) _cell_length_b 15.074(3) _cell_length_c 16.129(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.513(4) _cell_angle_gamma 90.00 _cell_volume 2456.8(9) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 11407 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 30.41 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1490 _exptl_absorpt_coefficient_mu 1.569 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5726 _exptl_absorpt_correction_T_max 0.7444 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18390 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.41 _reflns_number_total 7093 _reflns_number_gt 5145 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.4549P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7093 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0614 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.014 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.20628(3) 0.934644(19) 0.030525(18) 0.03670(8) Uani 1 1 d . . . Mo2 Mo 0.03906(3) 1.04733(2) 0.141383(18) 0.04173(9) Uani 1 1 d . . . Mo3 Mo -0.09070(3) 0.86896(2) 0.03558(2) 0.04168(9) Uani 1 1 d . . . O1 O 0.0000 1.0000 0.0000 0.0312(6) Uani 1 2 d S . . O2 O 0.0909(2) 0.84072(15) 0.05259(15) 0.0426(5) Uani 1 1 d . . . O3 O 0.2425(2) 1.05079(16) -0.00333(16) 0.0438(6) Uani 1 1 d . . . O4 O -0.0444(2) 0.93273(16) 0.14212(15) 0.0451(6) Uani 1 1 d . . . O5 O 0.1978(2) 0.98223(17) 0.13884(14) 0.0441(6) Uani 1 1 d . . . O6 O 0.3544(2) 0.88385(17) 0.05152(16) 0.0483(6) Uani 1 1 d . . . O7 O 0.1340(2) 0.90753(16) -0.08984(14) 0.0416(5) Uani 1 1 d . . . O8 O 0.1083(2) 1.14243(16) 0.08629(16) 0.0465(6) Uani 1 1 d . . . O9 O 0.0683(3) 1.0810(2) 0.24365(16) 0.0606(8) Uani 1 1 d . . . O10 O -0.1596(3) 0.77520(18) 0.0606(2) 0.0655(8) Uani 1 1 d . . . O11 O 0.5006(2) 1.01617(16) 0.28062(15) 0.0445(6) Uani 1 1 d . . . N1 N 0.4460(3) 1.20785(18) 0.14126(18) 0.0396(6) Uani 1 1 d . . . N2 N 0.7357(3) 1.00366(17) 0.31438(19) 0.0396(6) Uani 1 1 d . . . C1 C 0.6149(3) 0.9737(2) 0.2576(2) 0.0381(7) Uani 1 1 d . . . C2 C 0.6082(4) 0.9922(2) 0.1659(2) 0.0451(8) Uani 1 1 d . . . H2 H 0.6479 0.9524 0.1360 0.054 Uiso 1 1 calc R . . C3 C 0.5479(4) 1.0631(2) 0.1249(2) 0.0438(8) Uani 1 1 d . . . H3 H 0.5470 1.0733 0.0679 0.053 Uiso 1 1 calc R . . C4 C 0.4841(3) 1.1237(2) 0.1705(2) 0.0349(7) Uani 1 1 d . . . C5 C 0.4626(3) 1.0974(2) 0.2481(2) 0.0379(7) Uani 1 1 d . . . C6 C 0.3984(4) 1.1521(3) 0.2941(2) 0.0511(9) Uani 1 1 d . . . C7 C 0.3621(4) 1.2356(3) 0.2610(2) 0.0540(10) Uani 1 1 d . . . H7 H 0.3194 1.2737 0.2907 0.065 Uiso 1 1 calc R . . C8 C 0.3869(4) 1.2640(2) 0.1860(3) 0.0485(9) Uani 1 1 d . . . C9 C 0.3544(5) 1.3569(3) 0.1529(3) 0.0749(14) Uani 1 1 d . . . H9A H 0.4322 1.3842 0.1427 0.112 Uiso 1 1 calc R . . H9B H 0.3238 1.3909 0.1944 0.112 Uiso 1 1 calc R . . H9C H 0.2864 1.3548 0.1003 0.112 Uiso 1 1 calc R . . C10 C 0.4753(5) 1.2363(3) 0.0595(3) 0.0587(10) Uani 1 1 d . . . H10A H 0.4540 1.1890 0.0185 0.088 Uiso 1 1 calc R . . H10B H 0.5675 1.2506 0.0697 0.088 Uiso 1 1 calc R . . H10C H 0.4231 1.2875 0.0377 0.088 Uiso 1 1 calc R . . C11 C 0.6085(4) 0.8739(2) 0.2835(2) 0.0450(8) Uani 1 1 d . . . C12 C 0.6821(3) 0.8782(2) 0.3768(2) 0.0384(7) Uani 1 1 d . . . C13 C 0.6862(4) 0.8195(2) 0.4426(2) 0.0489(9) Uani 1 1 d . . . H13 H 0.6366 0.7675 0.4333 0.059 Uiso 1 1 calc R . . C14 C 0.7668(4) 0.8394(3) 0.5242(3) 0.0551(10) Uani 1 1 d . . . H14 H 0.7717 0.8002 0.5694 0.066 Uiso 1 1 calc R . . C15 C 0.8383(4) 0.9168(3) 0.5370(3) 0.0610(11) Uani 1 1 d . . . H15 H 0.8906 0.9298 0.5914 0.073 Uiso 1 1 calc R . . C16 C 0.8344(4) 0.9762(3) 0.4706(3) 0.0542(10) Uani 1 1 d . . . H16 H 0.8835 1.0284 0.4798 0.065 Uiso 1 1 calc R . . C17 C 0.7562(3) 0.9559(2) 0.3912(2) 0.0380(7) Uani 1 1 d . . . C18 C 0.4685(5) 0.8381(3) 0.2681(3) 0.0809(16) Uani 1 1 d . . . H18A H 0.4716 0.7764 0.2833 0.121 Uiso 1 1 calc R . . H18B H 0.4238 0.8449 0.2087 0.121 Uiso 1 1 calc R . . H18C H 0.4217 0.8705 0.3026 0.121 Uiso 1 1 calc R . . C19 C 0.6898(6) 0.8170(3) 0.2366(3) 0.0876(18) Uani 1 1 d . . . H19A H 0.7740 0.8447 0.2408 0.131 Uiso 1 1 calc R . . H19B H 0.6432 0.8115 0.1775 0.131 Uiso 1 1 calc R . . H19C H 0.7032 0.7592 0.2623 0.131 Uiso 1 1 calc R . . C20 C 0.7782(4) 1.0953(2) 0.3140(3) 0.0562(10) Uani 1 1 d . . . H20A H 0.7268 1.1317 0.3424 0.084 Uiso 1 1 calc R . . H20B H 0.7658 1.1151 0.2559 0.084 Uiso 1 1 calc R . . H20C H 0.8701 1.0998 0.3433 0.084 Uiso 1 1 calc R . . C21 C -0.0393(14) 0.5379(9) -0.0069(9) 0.108(4) Uiso 0.50 1 d P . . N3 N -0.097(3) 0.603(2) -0.0066(19) 0.149(10) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.03497(15) 0.04225(16) 0.03449(15) 0.00006(11) 0.01175(11) 0.00520(12) Mo2 0.04918(18) 0.05131(18) 0.02527(14) -0.00654(12) 0.01037(12) 0.00648(14) Mo3 0.04295(17) 0.03754(16) 0.04736(18) 0.00554(12) 0.01658(13) -0.00295(12) O1 0.0368(16) 0.0336(15) 0.0254(14) -0.0020(11) 0.0118(12) -0.0012(12) O2 0.0506(14) 0.0375(12) 0.0426(13) 0.0052(10) 0.0172(11) 0.0070(10) O3 0.0373(12) 0.0501(14) 0.0469(14) 0.0009(11) 0.0162(11) -0.0043(11) O4 0.0538(14) 0.0519(14) 0.0347(12) 0.0085(10) 0.0204(11) 0.0029(12) O5 0.0422(13) 0.0572(15) 0.0308(12) -0.0040(10) 0.0052(10) 0.0074(11) O6 0.0401(13) 0.0587(15) 0.0461(14) 0.0002(12) 0.0110(11) 0.0123(12) O7 0.0472(13) 0.0484(13) 0.0333(12) -0.0040(10) 0.0174(10) 0.0082(11) O8 0.0519(14) 0.0450(13) 0.0427(14) -0.0122(10) 0.0121(11) -0.0076(11) O9 0.0710(19) 0.0780(19) 0.0331(14) -0.0150(13) 0.0135(13) 0.0090(15) O10 0.0649(18) 0.0503(15) 0.085(2) 0.0166(15) 0.0255(16) -0.0109(14) O11 0.0497(14) 0.0494(14) 0.0418(13) 0.0146(11) 0.0254(11) 0.0091(11) N1 0.0403(15) 0.0395(14) 0.0399(15) 0.0060(12) 0.0118(12) -0.0001(12) N2 0.0459(16) 0.0305(13) 0.0461(16) 0.0033(12) 0.0184(13) -0.0036(12) C1 0.0480(19) 0.0309(15) 0.0390(17) 0.0004(13) 0.0179(15) 0.0027(14) C2 0.063(2) 0.0387(18) 0.0413(19) 0.0010(15) 0.0264(17) 0.0055(16) C3 0.057(2) 0.0450(19) 0.0352(18) 0.0029(14) 0.0220(16) 0.0000(16) C4 0.0364(16) 0.0353(16) 0.0345(16) 0.0023(13) 0.0118(13) -0.0012(13) C5 0.0373(17) 0.0424(17) 0.0362(17) 0.0052(14) 0.0137(14) 0.0048(14) C6 0.051(2) 0.066(2) 0.0391(19) 0.0009(17) 0.0166(16) 0.0190(19) C7 0.054(2) 0.062(2) 0.048(2) -0.0029(18) 0.0149(18) 0.0194(19) C8 0.046(2) 0.047(2) 0.051(2) -0.0035(17) 0.0096(17) 0.0075(16) C9 0.095(4) 0.049(2) 0.086(4) 0.009(2) 0.033(3) 0.025(2) C10 0.077(3) 0.053(2) 0.053(2) 0.0205(18) 0.029(2) 0.005(2) C11 0.065(2) 0.0276(15) 0.0407(19) 0.0037(13) 0.0108(17) -0.0063(15) C12 0.0420(18) 0.0329(16) 0.0420(18) 0.0031(13) 0.0138(14) 0.0008(13) C13 0.058(2) 0.0391(18) 0.051(2) 0.0117(16) 0.0171(18) 0.0022(16) C14 0.061(2) 0.062(2) 0.045(2) 0.0150(18) 0.0180(18) 0.014(2) C15 0.059(3) 0.079(3) 0.041(2) -0.004(2) 0.0051(18) 0.005(2) C16 0.051(2) 0.054(2) 0.054(2) -0.0053(18) 0.0059(18) -0.0077(18) C17 0.0371(17) 0.0357(16) 0.0437(19) 0.0016(14) 0.0143(14) 0.0016(13) C18 0.087(3) 0.070(3) 0.068(3) 0.025(2) -0.013(3) -0.039(3) C19 0.172(6) 0.038(2) 0.059(3) -0.0024(19) 0.040(3) 0.027(3) C20 0.053(2) 0.0355(18) 0.081(3) 0.0063(19) 0.018(2) -0.0104(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O6 1.682(2) . ? Mo1 O3 1.900(2) . ? Mo1 O5 1.911(2) . ? Mo1 O7 1.942(2) . ? Mo1 O2 1.949(2) . ? Mo1 O1 2.3061(5) . ? Mo2 O9 1.679(2) . ? Mo2 O7 1.914(2) 3_575 ? Mo2 O8 1.921(3) . ? Mo2 O5 1.935(2) . ? Mo2 O4 1.936(2) . ? Mo2 O1 2.3259(5) . ? Mo3 O10 1.680(3) . ? Mo3 O2 1.894(2) . ? Mo3 O4 1.922(3) . ? Mo3 O8 1.935(2) 3_575 ? Mo3 O3 1.958(2) 3_575 ? Mo3 O1 2.3237(5) . ? O1 Mo1 2.3061(5) 3_575 ? O1 Mo3 2.3237(4) 3_575 ? O1 Mo2 2.3259(5) 3_575 ? O3 Mo3 1.958(2) 3_575 ? O7 Mo2 1.914(2) 3_575 ? O8 Mo3 1.935(2) 3_575 ? O11 C5 1.352(4) . ? O11 C1 1.480(4) . ? N1 C8 1.357(5) . ? N1 C4 1.377(4) . ? N1 C10 1.489(4) . ? N2 C17 1.403(4) . ? N2 C1 1.434(4) . ? N2 C20 1.451(4) . ? C1 C2 1.489(5) . ? C1 C11 1.568(4) . ? C2 C3 1.329(5) . ? C2 H2 0.9300 . ? C3 C4 1.436(5) . ? C3 H3 0.9300 . ? C4 C5 1.384(4) . ? C5 C6 1.389(5) . ? C6 C7 1.382(5) . ? C7 C8 1.368(6) . ? C7 H7 0.9300 . ? C8 C9 1.507(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.510(5) . ? C11 C18 1.518(6) . ? C11 C19 1.533(6) . ? C12 C13 1.375(5) . ? C12 C17 1.390(4) . ? C13 C14 1.405(5) . ? C13 H13 0.9300 . ? C14 C15 1.373(6) . ? C14 H14 0.9300 . ? C15 C16 1.388(6) . ? C15 H15 0.9300 . ? C16 C17 1.370(5) . ? C16 H16 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N3 1.16(3) . ? C21 C21 1.39(3) 3_565 ? 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 O6 Mo1 O3 103.78(12) . . ? O6 Mo1 O5 103.74(11) . . ? O3 Mo1 O5 88.57(11) . . ? O6 Mo1 O7 102.29(11) . . ? O3 Mo1 O7 87.83(11) . . ? O5 Mo1 O7 153.83(10) . . ? O6 Mo1 O2 102.21(12) . . ? O3 Mo1 O2 153.99(10) . . ? O5 Mo1 O2 86.18(11) . . ? O7 Mo1 O2 85.79(10) . . ? O6 Mo1 O1 178.14(9) . . ? O3 Mo1 O1 77.73(7) . . ? O5 Mo1 O1 77.30(7) . . ? O7 Mo1 O1 76.60(7) . . ? O2 Mo1 O1 76.26(7) . . ? O9 Mo2 O7 103.80(12) . 3_575 ? O9 Mo2 O8 103.40(13) . . ? O7 Mo2 O8 87.55(11) 3_575 . ? O9 Mo2 O5 103.20(12) . . ? O7 Mo2 O5 152.99(10) 3_575 . ? O8 Mo2 O5 86.86(11) . . ? O9 Mo2 O4 103.61(13) . . ? O7 Mo2 O4 86.71(11) 3_575 . ? O8 Mo2 O4 152.98(10) . . ? O5 Mo2 O4 86.38(11) . . ? O9 Mo2 O1 179.56(11) . . ? O7 Mo2 O1 76.63(7) 3_575 . ? O8 Mo2 O1 76.65(7) . . ? O5 Mo2 O1 76.37(7) . . ? O4 Mo2 O1 76.33(7) . . ? O10 Mo3 O2 104.41(12) . . ? O10 Mo3 O4 103.46(14) . . ? O2 Mo3 O4 87.99(11) . . ? O10 Mo3 O8 103.41(14) . 3_575 ? O2 Mo3 O8 87.94(10) . 3_575 ? O4 Mo3 O8 153.00(10) . 3_575 ? O10 Mo3 O3 102.54(13) . 3_575 ? O2 Mo3 O3 153.05(10) . 3_575 ? O4 Mo3 O3 86.20(11) . 3_575 ? O8 Mo3 O3 85.44(11) 3_575 3_575 ? O10 Mo3 O1 178.76(11) . . ? O2 Mo3 O1 76.82(7) . . ? O4 Mo3 O1 76.65(7) . . ? O8 Mo3 O1 76.43(7) 3_575 . ? O3 Mo3 O1 76.23(7) 3_575 . ? Mo1 O1 Mo1 180.0 . 3_575 ? Mo1 O1 Mo3 89.968(17) . 3_575 ? Mo1 O1 Mo3 90.032(17) 3_575 3_575 ? Mo1 O1 Mo3 90.032(17) . . ? Mo1 O1 Mo3 89.968(17) 3_575 . ? Mo3 O1 Mo3 180.000(15) 3_575 . ? Mo1 O1 Mo2 90.180(12) . 3_575 ? Mo1 O1 Mo2 89.820(12) 3_575 3_575 ? Mo3 O1 Mo2 90.045(15) 3_575 3_575 ? Mo3 O1 Mo2 89.955(15) . 3_575 ? Mo1 O1 Mo2 89.820(12) . . ? Mo1 O1 Mo2 90.180(12) 3_575 . ? Mo3 O1 Mo2 89.955(15) 3_575 . ? Mo3 O1 Mo2 90.045(15) . . ? Mo2 O1 Mo2 180.000(5) 3_575 . ? Mo3 O2 Mo1 116.88(11) . . ? Mo1 O3 Mo3 116.07(12) . 3_575 ? Mo3 O4 Mo2 116.96(12) . . ? Mo1 O5 Mo2 116.47(11) . . ? Mo2 O7 Mo1 116.58(11) 3_575 . ? Mo2 O8 Mo3 116.92(11) . 3_575 ? C5 O11 C1 118.1(2) . . ? C8 N1 C4 121.6(3) . . ? C8 N1 C10 120.9(3) . . ? C4 N1 C10 117.6(3) . . ? C17 N2 C1 108.5(3) . . ? C17 N2 C20 120.9(3) . . ? C1 N2 C20 121.2(3) . . ? N2 C1 O11 109.8(3) . . ? N2 C1 C2 113.0(3) . . ? O11 C1 C2 109.2(3) . . ? N2 C1 C11 102.8(3) . . ? O11 C1 C11 104.9(3) . . ? C2 C1 C11 116.7(3) . . ? C3 C2 C1 122.9(3) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 118.6(3) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? N1 C4 C5 118.3(3) . . ? N1 C4 C3 122.8(3) . . ? C5 C4 C3 118.9(3) . . ? O11 C5 C4 120.7(3) . . ? O11 C5 C6 117.7(3) . . ? C4 C5 C6 121.6(3) . . ? C7 C6 C5 117.1(4) . . ? C8 C7 C6 122.2(4) . . ? C8 C7 H7 118.9 . . ? C6 C7 H7 118.9 . . ? N1 C8 C7 119.1(3) . . ? N1 C8 C9 118.9(4) . . ? C7 C8 C9 122.0(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C18 114.1(3) . . ? C12 C11 C19 108.0(3) . . ? C18 C11 C19 110.5(4) . . ? C12 C11 C1 100.3(3) . . ? C18 C11 C1 113.6(3) . . ? C19 C11 C1 109.9(3) . . ? C13 C12 C17 120.3(3) . . ? C13 C12 C11 130.6(3) . . ? C17 C12 C11 109.1(3) . . ? C12 C13 C14 118.7(4) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 121.5(4) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C17 C16 C15 118.2(4) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? C16 C17 C12 121.4(3) . . ? C16 C17 N2 129.4(3) . . ? C12 C17 N2 109.2(3) . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C11 C19 H19A 109.5 . . ? C11 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C11 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C21 171(3) . 3_565 ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.731 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.105 #===END _database_code_depnum_ccdc_archive 'CCDC 962077'