# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1491 data_global #================================================================= # SUBMISSION DETAILS _publ_contact_author ; Dr. Michael Ward School of Chemistry University of Bristol Cantock's Close BS8 1TS Bristol UK ; _publ_contact_author_phone '0117 9287655' _publ_contact_author_fax '0117 9290509' _publ_contact_author_email mike.ward@bristol.ac.uk _publ_contact_letter ; This CIF file contains details of the two crystal structures in the paper 'Dinuclear oxo-molybdenum(V) complexes which show strong electrochemical interactions across bis-phenolate bridging ligands: a combined spectroelectrochemical and computational study' by N. C. Harden et al, submitted to Dalton Transactions for publication. ; #================================================================= data_mdw _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H31 B Cl Mo N6 O3 S' _chemical_formula_weight 661.84 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.581(2) _cell_length_b 17.475(3) _cell_length_c 12.663(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.7720(10) _cell_angle_gamma 90.00 _cell_volume 2905.89(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method ? _exptl_crystal_F_000 1356 _exptl_absorpt_coefficient_mu 0.655 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.891 _exptl_absorpt_correction_T_max 0.731 _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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29491 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6675 _reflns_number_observed 5801 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+4.5936P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6675 _refine_ls_number_parameters 390 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_obs 0.0459 _refine_ls_wR_factor_all 0.1043 _refine_ls_wR_factor_obs 0.1019 _refine_ls_goodness_of_fit_all 1.247 _refine_ls_goodness_of_fit_obs 1.313 _refine_ls_restrained_S_all 1.247 _refine_ls_restrained_S_obs 1.313 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.66407(2) 0.53190(2) 0.81015(2) 0.03730(10) Uani 1 d . . B B 0.6650(3) 0.6749(2) 0.6363(3) 0.0349(8) Uani 1 d . . H H 0.6656(22) 0.7216(18) 0.5811(24) 0.022(8) Uiso 1 d . . C12 C 0.8406(3) 0.7273(2) 0.7514(3) 0.0384(8) Uani 1 d . . C13 C 0.8464(3) 0.7945(2) 0.6808(4) 0.0579(11) Uani 1 d . . H13A H 0.8543(24) 0.7771(2) 0.6115(10) 0.087 Uiso 1 calc R . H13B H 0.9036(14) 0.8258(10) 0.7156(12) 0.087 Uiso 1 calc R . H13C H 0.7850(10) 0.8240(10) 0.6697(21) 0.087 Uiso 1 calc R . C14 C 0.9097(3) 0.7027(2) 0.8450(3) 0.0410(8) Uani 1 d . . H14 H 0.9709(3) 0.7261(2) 0.8795(3) 0.049 Uiso 1 calc R . C15 C 0.8701(2) 0.6362(2) 0.8778(3) 0.0321(7) Uani 1 d . . C16 C 0.9172(3) 0.5877(2) 0.9745(3) 0.0401(8) Uani 1 d . . H16A H 0.8749(10) 0.5883(12) 1.0247(10) 0.060 Uiso 1 calc R . H16B H 0.9833(8) 0.6075(9) 1.0099(12) 0.060 Uiso 1 calc R . H16C H 0.9237(18) 0.5362(4) 0.9510(4) 0.060 Uiso 1 calc R . C22 C 0.6535(2) 0.5838(2) 0.4690(3) 0.0389(8) Uani 1 d . . C23 C 0.6599(3) 0.6460(3) 0.3891(3) 0.0562(11) Uani 1 d . . H23A H 0.6020(13) 0.6793(10) 0.3799(19) 0.084 Uiso 1 calc R . H23B H 0.6605(24) 0.6236(3) 0.3200(8) 0.084 Uiso 1 calc R . H23C H 0.7212(12) 0.6750(11) 0.4162(12) 0.084 Uiso 1 calc R . C24 C 0.6407(3) 0.5065(2) 0.4542(3) 0.0420(9) Uani 1 d . . H24 H 0.6329(3) 0.4801(2) 0.3888(3) 0.050 Uiso 1 calc R . C25 C 0.6417(2) 0.4748(2) 0.5547(3) 0.0339(7) Uani 1 d . . C26 C 0.6285(3) 0.3929(2) 0.5800(3) 0.0409(8) Uani 1 d . . H26A H 0.6736(14) 0.3803(4) 0.6494(10) 0.061 Uiso 1 calc R . H26B H 0.6439(19) 0.3613(2) 0.5243(11) 0.061 Uiso 1 calc R . H26C H 0.5594(5) 0.3841(4) 0.5827(20) 0.061 Uiso 1 calc R . C32 C 0.4920(3) 0.7264(2) 0.6611(3) 0.0414(8) Uani 1 d . . C33 C 0.4842(3) 0.7897(3) 0.5813(4) 0.0640(13) Uani 1 d . . H33A H 0.5439(12) 0.8213(11) 0.6021(16) 0.096 Uiso 1 calc R . H33B H 0.4249(15) 0.8199(12) 0.5801(20) 0.096 Uiso 1 calc R . H33C H 0.4789(26) 0.7688(3) 0.5099(6) 0.096 Uiso 1 calc R . C34 C 0.4244(3) 0.7045(2) 0.7198(3) 0.0470(9) Uani 1 d . . H34 H 0.3630(3) 0.7281(2) 0.7195(3) 0.056 Uiso 1 calc R . C35 C 0.4657(2) 0.6403(2) 0.7795(3) 0.0390(8) Uani 1 d . . C36 C 0.4215(3) 0.5916(3) 0.8530(3) 0.0490(10) Uani 1 d . . H36A H 0.3996(20) 0.5437(7) 0.8178(10) 0.073 Uiso 1 calc R . H36B H 0.3643(14) 0.6174(8) 0.8684(19) 0.073 Uiso 1 calc R . H36C H 0.4722(7) 0.5826(14) 0.9200(10) 0.073 Uiso 1 calc R . C42 C 0.7950(2) 0.3864(2) 0.8715(2) 0.0256(6) Uani 1 d . . C43 C 0.7789(2) 0.3696(2) 0.9731(3) 0.0309(7) Uani 1 d . . H43 H 0.7505(2) 0.4062(2) 1.0098(3) 0.037 Uiso 1 calc R . C44 C 0.8050(2) 0.2984(2) 1.0195(2) 0.0312(7) Uani 1 d . . H44 H 0.7938(2) 0.2874(2) 1.0873(2) 0.037 Uiso 1 calc R . C45 C 0.8478(2) 0.2430(2) 0.9659(2) 0.0262(6) Uani 1 d . . C46 C 0.8647(2) 0.2604(2) 0.8644(2) 0.0292(6) Uani 1 d . . H46 H 0.8937(2) 0.2241(2) 0.8278(2) 0.035 Uiso 1 calc R . C47 C 0.8385(2) 0.3316(2) 0.8187(2) 0.0296(6) Uani 1 d . . H47 H 0.8502(2) 0.3429(2) 0.7511(2) 0.035 Uiso 1 calc R . C49 C 0.9281(2) 0.1007(2) 0.9372(2) 0.0274(6) Uani 1 d . . C50 C 0.8617(2) 0.0637(2) 0.8508(3) 0.0347(7) Uani 1 d . . H50 H 0.7918(2) 0.0670(2) 0.8430(3) 0.042 Uiso 1 calc R . C51 C 0.8982(3) 0.0222(2) 0.7766(3) 0.0366(7) Uani 1 d . . H51 H 0.8531(3) -0.0019(2) 0.7184(3) 0.044 Uiso 1 calc R . C52 C 1.0020(2) 0.0162(2) 0.7886(3) 0.0293(6) Uani 1 d . . C53 C 1.0695(2) 0.0525(2) 0.8753(3) 0.0332(7) Uani 1 d . . H53 H 1.1394(2) 0.0481(2) 0.8839(3) 0.040 Uiso 1 calc R . C54 C 1.0325(2) 0.0953(2) 0.9488(3) 0.0313(7) Uani 1 d . . H54 H 1.0775(2) 0.1204(2) 1.0059(3) 0.038 Uiso 1 calc R . N11 N 0.7625(2) 0.6772(2) 0.7297(2) 0.0320(6) Uani 1 d . . N17 N 0.7802(2) 0.62091(15) 0.8075(2) 0.0294(6) Uani 1 d . . N21 N 0.6607(2) 0.5991(2) 0.5755(2) 0.0323(6) Uani 1 d . . N27 N 0.6542(2) 0.5307(2) 0.6286(2) 0.0301(6) Uani 1 d . . N31 N 0.5715(2) 0.6782(2) 0.6850(2) 0.0337(6) Uani 1 d . . N37 N 0.5561(2) 0.6243(2) 0.7581(2) 0.0329(6) Uani 1 d . . O41 O 0.7744(2) 0.45723(12) 0.8236(2) 0.0309(5) Uani 1 d . . O55 O 1.0333(2) -0.02630(15) 0.7138(2) 0.0423(6) Uani 1 d . . H55 H 1.0945(7) -0.0198(20) 0.7213(25) 0.063 Uiso 1 calc R . S48 S 0.87988(7) 0.15332(5) 1.03261(7) 0.0338(2) Uani 1 d . . Cl1 Cl 0.6748(2) 0.55056(15) 0.9879(2) 0.0417(5) Uani 0.50 d P 1 O1 O 0.5591(10) 0.4615(7) 0.7799(12) 0.039(3) Uani 0.50 d P 1 Cl1' Cl 0.5453(4) 0.4425(3) 0.7912(5) 0.0371(7) Uani 0.50 d P 2 O1' O 0.6795(6) 0.5594(4) 0.9438(5) 0.044(2) Uani 0.50 d P 2 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 0.0347(2) 0.0451(2) 0.0356(2) 0.01585(13) 0.01538(12) 0.01472(13) B 0.028(2) 0.036(2) 0.036(2) 0.010(2) -0.0004(15) 0.0040(15) C12 0.032(2) 0.031(2) 0.049(2) 0.0037(15) 0.0048(15) -0.0009(14) C13 0.052(2) 0.044(2) 0.071(3) 0.017(2) 0.003(2) -0.014(2) C14 0.031(2) 0.037(2) 0.047(2) -0.003(2) -0.0030(15) -0.0030(14) C15 0.029(2) 0.030(2) 0.033(2) -0.0045(13) -0.0002(13) 0.0042(13) C16 0.033(2) 0.043(2) 0.035(2) -0.0042(15) -0.0079(14) 0.0074(15) C22 0.024(2) 0.062(2) 0.028(2) 0.005(2) 0.0018(13) 0.0054(15) C23 0.049(2) 0.083(3) 0.035(2) 0.017(2) 0.009(2) -0.004(2) C24 0.031(2) 0.064(3) 0.028(2) -0.005(2) 0.0027(13) 0.008(2) C25 0.0196(14) 0.050(2) 0.030(2) -0.0027(14) 0.0017(12) 0.0039(14) C26 0.029(2) 0.047(2) 0.043(2) -0.016(2) 0.0020(14) 0.0010(15) C32 0.029(2) 0.041(2) 0.048(2) -0.002(2) -0.0035(15) 0.0085(14) C33 0.044(2) 0.057(3) 0.081(3) 0.026(2) -0.002(2) 0.021(2) C34 0.029(2) 0.054(2) 0.051(2) -0.010(2) -0.002(2) 0.016(2) C35 0.027(2) 0.052(2) 0.036(2) -0.012(2) 0.0053(14) 0.0044(15) C36 0.037(2) 0.068(3) 0.046(2) -0.010(2) 0.017(2) 0.004(2) C42 0.0207(13) 0.0249(15) 0.0295(14) 0.0033(12) 0.0033(11) -0.0013(11) C43 0.032(2) 0.031(2) 0.032(2) -0.0006(13) 0.0126(13) 0.0064(13) C44 0.032(2) 0.038(2) 0.0269(15) 0.0062(13) 0.0126(13) 0.0039(13) C45 0.0242(14) 0.027(2) 0.0272(14) 0.0036(12) 0.0072(12) -0.0027(11) C46 0.031(2) 0.028(2) 0.030(2) -0.0034(12) 0.0119(13) -0.0021(12) C47 0.032(2) 0.033(2) 0.0247(14) 0.0004(12) 0.0103(12) -0.0045(13) C49 0.034(2) 0.0184(14) 0.0313(15) 0.0039(11) 0.0110(13) 0.0003(12) C50 0.025(2) 0.037(2) 0.043(2) -0.0032(14) 0.0090(14) -0.0027(13) C51 0.035(2) 0.035(2) 0.038(2) -0.0075(14) 0.0057(14) -0.0027(14) C52 0.035(2) 0.0231(15) 0.032(2) 0.0014(12) 0.0128(13) 0.0022(12) C53 0.0247(15) 0.036(2) 0.040(2) 0.0037(14) 0.0092(13) 0.0008(13) C54 0.032(2) 0.030(2) 0.030(2) 0.0002(13) 0.0049(13) -0.0011(13) N11 0.0263(13) 0.0288(14) 0.0366(14) 0.0074(11) 0.0004(11) -0.0004(11) N17 0.0266(13) 0.0277(13) 0.0301(13) 0.0048(10) 0.0003(10) 0.0039(10) N21 0.0237(13) 0.043(2) 0.0277(13) 0.0069(11) 0.0013(10) 0.0005(11) N27 0.0219(12) 0.0385(15) 0.0280(13) 0.0001(11) 0.0031(10) 0.0014(11) N31 0.0265(13) 0.0333(15) 0.0364(14) 0.0030(12) -0.0009(11) 0.0054(11) N37 0.0266(13) 0.040(2) 0.0302(13) -0.0029(12) 0.0043(11) 0.0053(11) O41 0.0315(11) 0.0296(12) 0.0320(11) 0.0043(9) 0.0090(9) 0.0020(9) O55 0.0406(13) 0.0440(14) 0.0449(14) -0.0108(11) 0.0156(11) 0.0046(12) S48 0.0448(5) 0.0286(4) 0.0327(4) 0.0049(3) 0.0182(4) 0.0033(3) Cl1 0.0478(11) 0.0433(12) 0.0344(13) -0.0025(10) 0.0112(11) 0.0055(8) O1 0.033(4) 0.045(7) 0.040(5) -0.007(4) 0.013(3) -0.012(4) Cl1' 0.0266(13) 0.038(2) 0.0454(14) 0.0081(12) 0.0077(10) -0.0070(11) O1' 0.051(3) 0.058(4) 0.024(3) 0.003(3) 0.013(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1' 1.720(6) . ? Mo1 O1 1.847(10) . ? Mo1 O41 1.962(2) . ? Mo1 N37 2.168(3) . ? Mo1 Cl1' 2.214(4) . ? Mo1 N17 2.221(3) . ? Mo1 Cl1 2.242(2) . ? Mo1 N27 2.268(3) . ? B N21 1.526(5) . ? B N11 1.535(4) . ? B N31 1.548(5) . ? C12 N11 1.349(4) . ? C12 C14 1.380(5) . ? C12 C13 1.491(5) . ? C14 C15 1.388(5) . ? C15 N17 1.341(4) . ? C15 C16 1.493(4) . ? C22 N21 1.354(4) . ? C22 C24 1.370(6) . ? C22 C23 1.503(5) . ? C24 C25 1.385(5) . ? C25 N27 1.334(4) . ? C25 C26 1.487(5) . ? C32 N31 1.341(4) . ? C32 C34 1.374(5) . ? C32 C33 1.484(5) . ? C34 C35 1.390(5) . ? C35 N37 1.352(4) . ? C35 C36 1.494(5) . ? C42 O41 1.375(3) . ? C42 C47 1.384(4) . ? C42 C43 1.390(4) . ? C43 C44 1.383(4) . ? C44 C45 1.391(4) . ? C45 C46 1.395(4) . ? C45 S48 1.781(3) . ? C46 C47 1.380(4) . ? C49 C50 1.387(4) . ? C49 C54 1.391(4) . ? C49 S48 1.771(3) . ? C50 C51 1.377(5) . ? C51 C52 1.382(4) . ? C52 O55 1.356(4) . ? C52 C53 1.391(4) . ? C53 C54 1.384(4) . ? N11 N17 1.369(3) . ? N21 N27 1.384(4) . ? N31 N37 1.374(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1' Mo1 O41 101.7(3) . . ? O1 Mo1 O41 96.2(5) . . ? O1' Mo1 N37 89.7(3) . . ? O1 Mo1 N37 90.4(5) . . ? O41 Mo1 N37 164.68(9) . . ? O1' Mo1 Cl1' 101.9(3) . . ? O41 Mo1 Cl1' 93.4(2) . . ? N37 Mo1 Cl1' 94.3(2) . . ? O1' Mo1 N17 84.8(3) . . ? O1 Mo1 N17 167.5(4) . . ? O41 Mo1 N17 86.41(9) . . ? N37 Mo1 N17 84.35(10) . . ? Cl1' Mo1 N17 173.1(2) . . ? O1 Mo1 Cl1 98.9(5) . . ? O41 Mo1 Cl1 99.04(9) . . ? N37 Mo1 Cl1 93.60(10) . . ? N17 Mo1 Cl1 92.79(10) . . ? O1' Mo1 N27 163.8(3) . . ? O1 Mo1 N27 86.6(5) . . ? O41 Mo1 N27 85.88(9) . . ? N37 Mo1 N27 80.68(10) . . ? Cl1' Mo1 N27 91.8(2) . . ? N17 Mo1 N27 81.35(9) . . ? Cl1 Mo1 N27 172.14(10) . . ? N21 B N11 109.0(3) . . ? N21 B N31 107.6(3) . . ? N11 B N31 109.0(3) . . ? N11 C12 C14 107.4(3) . . ? N11 C12 C13 123.3(3) . . ? C14 C12 C13 129.3(3) . . ? C12 C14 C15 106.7(3) . . ? N17 C15 C14 109.0(3) . . ? N17 C15 C16 123.9(3) . . ? C14 C15 C16 127.1(3) . . ? N21 C22 C24 107.8(3) . . ? N21 C22 C23 121.8(4) . . ? C24 C22 C23 130.5(3) . . ? C22 C24 C25 107.3(3) . . ? N27 C25 C24 108.7(3) . . ? N27 C25 C26 123.7(3) . . ? C24 C25 C26 127.5(3) . . ? N31 C32 C34 108.3(3) . . ? N31 C32 C33 122.3(3) . . ? C34 C32 C33 129.4(3) . . ? C32 C34 C35 106.7(3) . . ? N37 C35 C34 108.5(3) . . ? N37 C35 C36 122.5(3) . . ? C34 C35 C36 128.9(3) . . ? O41 C42 C47 118.2(3) . . ? O41 C42 C43 122.5(3) . . ? C47 C42 C43 119.2(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 120.8(3) . . ? C44 C45 C46 119.0(3) . . ? C44 C45 S48 117.6(2) . . ? C46 C45 S48 123.4(2) . . ? C47 C46 C45 119.8(3) . . ? C46 C47 C42 121.1(3) . . ? C50 C49 C54 119.5(3) . . ? C50 C49 S48 120.0(2) . . ? C54 C49 S48 120.5(2) . . ? C51 C50 C49 120.6(3) . . ? C50 C51 C52 119.9(3) . . ? O55 C52 C51 117.2(3) . . ? O55 C52 C53 122.6(3) . . ? C51 C52 C53 120.1(3) . . ? C54 C53 C52 119.8(3) . . ? C53 C54 C49 120.1(3) . . ? C12 N11 N17 109.6(3) . . ? C12 N11 B 130.7(3) . . ? N17 N11 B 119.7(3) . . ? C15 N17 N11 107.3(3) . . ? C15 N17 Mo1 131.2(2) . . ? N11 N17 Mo1 121.3(2) . . ? C22 N21 N27 108.4(3) . . ? C22 N21 B 131.1(3) . . ? N27 N21 B 120.3(3) . . ? C25 N27 N21 107.7(3) . . ? C25 N27 Mo1 132.9(2) . . ? N21 N27 Mo1 119.3(2) . . ? C32 N31 N37 109.3(3) . . ? C32 N31 B 129.0(3) . . ? N37 N31 B 121.6(3) . . ? C35 N37 N31 107.2(3) . . ? C35 N37 Mo1 132.1(2) . . ? N31 N37 Mo1 120.5(2) . . ? C42 O41 Mo1 134.5(2) . . ? C49 S48 C45 102.78(14) . . ? _refine_diff_density_max 0.571 _refine_diff_density_min -1.008 _refine_diff_density_rms 0.067 #=END data_mdw2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C46 H61 B2 Cl4 Mo2 N12 O4 S' _chemical_formula_weight 1233.43 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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' _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 10.8807(12) _cell_length_b 15.5555(13) _cell_length_c 16.969(3) _cell_angle_alpha 80.708(10) _cell_angle_beta 79.243(14) _cell_angle_gamma 76.397(7) _cell_volume 2721.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.505 _exptl_crystal_density_method ? _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.722 _exptl_absorpt_correction_T_max 0.808 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Siemens SMART Area Detector' _diffrn_measurement_method '\w rotation with narrow frames (0.3 degrees)' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28471 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12324 _reflns_number_observed 8527 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0910P)^2^+0.4300P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12321 _refine_ls_number_parameters 696 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_obs 0.0507 _refine_ls_wR_factor_all 0.1648 _refine_ls_wR_factor_obs 0.1459 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.156 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.161 _refine_ls_shift/esd_max 0.065 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Mo1 Mo 0.17591(4) 0.54798(2) -0.33934(2) 0.03623(12) Uani 1 d . . Mo2 Mo 0.31798(4) -0.16335(3) -0.06537(2) 0.03454(12) Uani 1 d . . B1 B 0.0781(5) 0.7664(3) -0.3873(3) 0.0361(12) Uani 1 d . . H1 H 0.0370(43) 0.8432(29) -0.4071(28) 0.043 Uiso 1 d . . B2 B 0.1717(5) -0.2140(3) 0.1219(3) 0.0315(10) Uani 1 d . . H2 H 0.1231(42) -0.2294(27) 0.1835(27) 0.038 Uiso 1 d . . Cl2 Cl 0.4581(4) -0.2679(3) -0.1355(2) 0.0374(8) Uani 0.595(8) d P 1 O2 O 0.2217(10) -0.1071(7) -0.1348(6) 0.040(2) Uani 0.595(8) d P 1 Cl1 Cl 0.0716(7) 0.4484(4) -0.3488(5) 0.0367(11) Uani 0.442(8) d P 1 O1 O 0.2145(19) 0.5146(11) -0.2367(10) 0.035(4) Uani 0.442(8) d P 1 O1' O 0.0681(15) 0.4793(7) -0.3497(10) 0.043(3) Uani 0.558(8) d P 2 O2' O 0.4194(14) -0.2562(10) -0.1157(10) 0.038(3) Uani 0.405(8) d P 2 Cl2' Cl 0.2154(5) -0.0910(4) -0.1653(3) 0.0433(13) Uani 0.405(8) d P 2 Cl1' Cl 0.2287(5) 0.4930(3) -0.2168(3) 0.0319(9) Uani 0.558(8) d P 2 S1 S 0.66898(11) 0.12537(7) -0.37055(7) 0.0432(3) Uani 1 d . . N111 N 0.1322(3) 0.6267(2) -0.4558(2) 0.0321(8) Uani 1 d . . C112 C 0.1272(4) 0.6017(3) -0.5273(3) 0.0379(10) Uani 1 d . . C113 C 0.1770(5) 0.5088(3) -0.5467(3) 0.0456(12) Uani 1 d . . H11A H 0.1702(30) 0.5062(5) -0.6031(7) 0.068 Uiso 1 calc R . H11B H 0.1267(21) 0.4692(5) -0.5109(14) 0.068 Uiso 1 calc R . H11C H 0.2669(10) 0.4896(9) -0.5390(20) 0.068 Uiso 1 calc R . C114 C 0.0698(5) 0.6761(3) -0.5760(3) 0.0468(12) Uani 1 d . . H114 H 0.0528(5) 0.6775(3) -0.6292(3) 0.056 Uiso 1 calc R . C115 C 0.0425(4) 0.7469(3) -0.5314(3) 0.0439(12) Uani 1 d . . C116 C -0.0177(5) 0.8426(4) -0.5541(3) 0.060(2) Uani 1 d . . H11D H 0.0469(10) 0.8790(5) -0.5615(23) 0.090 Uiso 1 calc R . H11E H -0.0871(25) 0.8628(8) -0.5110(11) 0.090 Uiso 1 calc R . H11F H -0.0522(33) 0.8486(5) -0.6045(13) 0.090 Uiso 1 calc R . N117 N 0.0809(3) 0.7167(2) -0.4594(2) 0.0331(8) Uani 1 d . . N121 N 0.2750(3) 0.6613(2) -0.3448(2) 0.0308(8) Uani 1 d . . C122 C 0.3914(4) 0.6643(3) -0.3298(3) 0.0343(10) Uani 1 d . . C123 C 0.4845(4) 0.5831(3) -0.3032(3) 0.0437(11) Uani 1 d . . H12A H 0.5685(8) 0.5976(6) -0.3072(19) 0.066 Uiso 1 calc R . H12B H 0.4913(24) 0.5369(8) -0.3378(13) 0.066 Uiso 1 calc R . H12C H 0.4551(16) 0.5611(13) -0.2470(7) 0.066 Uiso 1 calc R . C124 C 0.4050(5) 0.7522(3) -0.3427(3) 0.0409(11) Uani 1 d . . H124 H 0.4779(5) 0.7729(3) -0.3369(3) 0.049 Uiso 1 calc R . C125 C 0.2942(5) 0.8032(3) -0.3653(3) 0.0378(10) Uani 1 d . . C126 C 0.2574(6) 0.9021(3) -0.3874(3) 0.0574(15) Uani 1 d . . H12D H 0.2554(37) 0.9156(3) -0.4456(5) 0.086 Uiso 1 calc R . H12E H 0.3203(21) 0.9306(4) -0.3731(21) 0.086 Uiso 1 calc R . H12F H 0.1725(17) 0.9250(5) -0.3578(18) 0.086 Uiso 1 calc R . N127 N 0.2143(3) 0.7479(2) -0.3668(2) 0.0335(8) Uani 1 d . . N131 N 0.0064(3) 0.6413(2) -0.2893(2) 0.0318(8) Uani 1 d . . C132 C -0.0907(4) 0.6304(3) -0.2300(3) 0.0404(11) Uani 1 d . . C133 C -0.1057(5) 0.5418(3) -0.1853(3) 0.059(2) Uani 1 d . . H13A H -0.1205(36) 0.5046(10) -0.2225(6) 0.088 Uiso 1 calc R . H13B H -0.1787(23) 0.5499(4) -0.1416(15) 0.088 Uiso 1 calc R . H13C H -0.0277(15) 0.5128(11) -0.1624(19) 0.088 Uiso 1 calc R . C134 C -0.1697(4) 0.7124(3) -0.2181(3) 0.0468(12) Uani 1 d . . H134 H -0.2458(4) 0.7236(3) -0.1801(3) 0.056 Uiso 1 calc R . C135 C -0.1167(4) 0.7743(3) -0.2718(3) 0.0431(12) Uani 1 d . . C136 C -0.1596(6) 0.8735(3) -0.2840(3) 0.063(2) Uani 1 d . . H13D H -0.2216(30) 0.8932(4) -0.2372(12) 0.094 Uiso 1 calc R . H13E H -0.1997(35) 0.8914(4) -0.3329(14) 0.094 Uiso 1 calc R . H13F H -0.0855(8) 0.9010(3) -0.2898(25) 0.094 Uiso 1 calc R . N137 N -0.0099(3) 0.7313(2) -0.3149(2) 0.0324(8) Uani 1 d . . O141 O 0.3342(3) 0.4858(2) -0.3982(2) 0.0306(6) Uani 1 d . . C142 C 0.4032(4) 0.4005(2) -0.3912(2) 0.0257(8) Uani 1 d . . C143 C 0.3651(4) 0.3335(3) -0.3334(3) 0.0380(11) Uani 1 d . . H143 H 0.2859(4) 0.3460(3) -0.2983(3) 0.046 Uiso 1 calc R . C144 C 0.4426(4) 0.2487(3) -0.3268(3) 0.0391(11) Uani 1 d . . H144 H 0.4160(4) 0.2035(3) -0.2871(3) 0.047 Uiso 1 calc R . C145 C 0.5582(4) 0.2294(2) -0.3776(2) 0.0297(9) Uani 1 d . . C146 C 0.5932(4) 0.2954(2) -0.4371(2) 0.0273(8) Uani 1 d . . H146 H 0.6707(4) 0.2821(2) -0.4736(2) 0.033 Uiso 1 calc R . C147 C 0.5176(4) 0.3800(2) -0.4441(2) 0.0262(8) Uani 1 d . . H147 H 0.5434(4) 0.4244(2) -0.4850(2) 0.031 Uiso 1 calc R . N211 N 0.2011(3) -0.0762(2) 0.0238(2) 0.0284(7) Uani 1 d . . C212 C 0.1646(4) 0.0123(3) 0.0209(3) 0.0336(9) Uani 1 d . . C213 C 0.1997(5) 0.0750(3) -0.0523(3) 0.0454(12) Uani 1 d . . H21A H 0.2899(10) 0.0776(17) -0.0570(11) 0.068 Uiso 1 calc R . H21B H 0.1461(22) 0.1346(6) -0.0471(10) 0.068 Uiso 1 calc R . H21C H 0.1860(30) 0.0537(12) -0.1006(4) 0.068 Uiso 1 calc R . C214 C 0.0919(4) 0.0340(3) 0.0943(3) 0.0398(11) Uani 1 d . . H214 H 0.0549(4) 0.0923(3) 0.1084(3) 0.048 Uiso 1 calc R . C215 C 0.0839(4) -0.0445(3) 0.1421(3) 0.0367(10) Uani 1 d . . C216 C 0.0168(6) -0.0622(4) 0.2269(3) 0.0558(14) Uani 1 d . . H21D H -0.0430(27) -0.0076(8) 0.2424(9) 0.084 Uiso 1 calc R . H21E H 0.0802(6) -0.0811(24) 0.2639(4) 0.084 Uiso 1 calc R . H21F H -0.0304(29) -0.1093(18) 0.2299(6) 0.084 Uiso 1 calc R . N217 N 0.1499(3) -0.1115(2) 0.0988(2) 0.0292(7) Uani 1 d . . N221 N 0.1772(3) -0.2459(2) -0.0202(2) 0.0298(7) Uani 1 d . . C222 C 0.1146(4) -0.2857(3) -0.0606(3) 0.0387(10) Uani 1 d . . C223 C 0.1494(5) -0.2918(4) -0.1490(3) 0.0567(14) Uani 1 d . . H22A H 0.0885(21) -0.3194(22) -0.1666(5) 0.085 Uiso 1 calc R . H22B H 0.2359(14) -0.3282(20) -0.1602(4) 0.085 Uiso 1 calc R . H22C H 0.1465(34) -0.2319(4) -0.1784(3) 0.085 Uiso 1 calc R . C224 C 0.0190(4) -0.3179(3) -0.0064(3) 0.0435(11) Uani 1 d . . H224 H -0.0388(4) -0.3495(3) -0.0183(3) 0.052 Uiso 1 calc R . C225 C 0.0235(4) -0.2955(3) 0.0685(3) 0.0357(10) Uani 1 d . . C226 C -0.0602(5) -0.3099(3) 0.1474(3) 0.0473(12) Uani 1 d . . H22D H -0.1202(21) -0.3460(19) 0.1420(6) 0.071 Uiso 1 calc R . H22E H -0.1082(24) -0.2522(3) 0.1637(10) 0.071 Uiso 1 calc R . H22F H -0.0074(5) -0.3410(20) 0.1885(5) 0.071 Uiso 1 calc R . N227 N 0.1205(3) -0.2524(2) 0.0596(2) 0.0291(7) Uani 1 d . . N231 N 0.3983(3) -0.2289(2) 0.0477(2) 0.0321(8) Uani 1 d . . C232 C 0.5167(4) -0.2660(3) 0.0615(3) 0.0388(10) Uani 1 d . . C233 C 0.6338(5) -0.2568(4) 0.0011(3) 0.0552(14) Uani 1 d . . H23A H 0.6397(20) -0.2922(20) -0.0428(12) 0.083 Uiso 1 calc R . H23B H 0.7099(5) -0.2782(23) 0.0276(6) 0.083 Uiso 1 calc R . H23C H 0.6283(17) -0.1940(5) -0.0209(17) 0.083 Uiso 1 calc R . C234 C 0.5118(5) -0.3137(3) 0.1385(3) 0.0432(11) Uani 1 d . . H234 H 0.5824(5) -0.3466(3) 0.1637(3) 0.052 Uiso 1 calc R . C235 C 0.3852(4) -0.3036(3) 0.1704(3) 0.0368(10) Uani 1 d . . C236 C 0.3242(5) -0.3417(3) 0.2508(3) 0.0473(12) Uani 1 d . . H23D H 0.3908(5) -0.3756(19) 0.2821(8) 0.071 Uiso 1 calc R . H23E H 0.2708(25) -0.3814(17) 0.2427(3) 0.071 Uiso 1 calc R . H23F H 0.2709(25) -0.2932(3) 0.2801(9) 0.071 Uiso 1 calc R . N237 N 0.3169(3) -0.2518(2) 0.1162(2) 0.0300(7) Uani 1 d . . O241 O 0.4399(3) -0.0858(2) -0.0826(2) 0.0349(7) Uani 1 d . . C242 C 0.4928(4) -0.0401(3) -0.1496(3) 0.0316(9) Uani 1 d . . C243 C 0.4831(5) -0.0526(3) -0.2276(3) 0.0450(12) Uani 1 d . . H243 H 0.4414(5) -0.0971(3) -0.2355(3) 0.054 Uiso 1 calc R . C244 C 0.5341(5) -0.0006(3) -0.2931(3) 0.0420(11) Uani 1 d . . H244 H 0.5254(5) -0.0088(3) -0.3459(3) 0.050 Uiso 1 calc R . C245 C 0.5977(4) 0.0634(3) -0.2840(3) 0.0329(10) Uani 1 d . . C246 C 0.6093(4) 0.0749(3) -0.2070(3) 0.0363(10) Uani 1 d . . H246 H 0.6531(4) 0.1186(3) -0.2000(3) 0.044 Uiso 1 calc R . C247 C 0.5581(4) 0.0241(3) -0.1398(3) 0.0337(9) Uani 1 d . . H247 H 0.5673(4) 0.0327(3) -0.0872(3) 0.040 Uiso 1 calc R . Cl32 Cl 0.2516(2) 1.2744(2) -0.58876(15) 0.1102(7) Uani 1 d . . Cl31 Cl 0.3765(3) 1.1211(2) -0.4907(2) 0.1511(11) Uani 1 d . . C31 C 0.3223(9) 1.2384(5) -0.5020(5) 0.106(3) Uani 1 d . . H31A H 0.2593(9) 1.2561(5) -0.4541(5) 0.127 Uiso 1 calc R . H31B H 0.3954(9) 1.2672(5) -0.5053(5) 0.127 Uiso 1 calc R . C2 C -0.3682(8) 0.4673(6) -0.0340(7) 0.092(3) Uani 1 d U . C1 C -0.3435(12) 0.4893(7) 0.0187(9) 0.134(4) Uani 1 d U . C3 C -0.4384(14) 0.4880(15) -0.0234(23) 0.339(17) Uani 1 d U . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0354(2) 0.0243(2) 0.0345(2) 0.00366(15) 0.0124(2) 0.00332(15) Mo2 0.0397(2) 0.0490(2) 0.0187(2) -0.0022(2) 0.00031(15) -0.0218(2) B1 0.036(3) 0.026(2) 0.035(3) 0.001(2) 0.007(2) 0.003(2) B2 0.037(3) 0.033(2) 0.022(2) -0.003(2) 0.001(2) -0.006(2) Cl2 0.034(2) 0.043(2) 0.034(2) -0.0167(11) 0.0036(12) -0.0020(13) O2 0.042(4) 0.053(5) 0.022(4) 0.003(4) -0.003(4) -0.013(3) Cl1 0.036(2) 0.035(3) 0.040(2) 0.001(2) -0.0090(13) -0.011(2) O1 0.043(7) 0.030(8) 0.032(9) -0.003(5) -0.009(6) -0.003(6) O1' 0.040(4) 0.036(6) 0.047(5) 0.006(6) -0.004(3) -0.005(6) O2' 0.034(8) 0.033(5) 0.042(8) -0.021(5) 0.002(5) 0.009(5) Cl2' 0.034(2) 0.062(3) 0.028(3) 0.004(2) -0.005(2) -0.006(2) Cl1' 0.037(2) 0.028(2) 0.027(2) 0.0017(13) -0.0049(13) -0.0032(13) S1 0.0381(6) 0.0254(5) 0.0470(7) 0.0070(5) 0.0175(5) 0.0044(4) N111 0.027(2) 0.038(2) 0.023(2) 0.0002(15) 0.0021(14) 0.0016(15) C112 0.028(2) 0.054(3) 0.026(2) -0.002(2) 0.000(2) -0.003(2) C113 0.043(3) 0.060(3) 0.031(2) -0.013(2) -0.006(2) 0.000(2) C114 0.040(3) 0.067(3) 0.023(2) 0.004(2) 0.000(2) 0.000(2) C115 0.033(2) 0.055(3) 0.028(2) 0.010(2) 0.005(2) 0.003(2) C116 0.050(3) 0.062(3) 0.044(3) 0.019(3) 0.001(2) 0.011(3) N117 0.029(2) 0.034(2) 0.024(2) 0.0039(14) 0.0032(14) 0.0069(15) N121 0.031(2) 0.024(2) 0.032(2) -0.0040(14) 0.0035(15) -0.0034(14) C122 0.032(2) 0.038(2) 0.032(2) -0.007(2) 0.004(2) -0.010(2) C123 0.027(2) 0.046(3) 0.057(3) -0.007(2) -0.006(2) -0.005(2) C124 0.043(3) 0.043(3) 0.039(3) -0.012(2) 0.005(2) -0.018(2) C125 0.050(3) 0.030(2) 0.031(2) -0.005(2) 0.008(2) -0.016(2) C126 0.081(4) 0.029(2) 0.058(3) -0.007(2) 0.007(3) -0.016(3) N127 0.043(2) 0.020(2) 0.031(2) -0.0015(14) 0.002(2) -0.0007(15) N131 0.029(2) 0.030(2) 0.029(2) 0.0001(14) 0.0032(15) 0.0007(14) C132 0.031(2) 0.047(3) 0.034(2) -0.003(2) 0.010(2) -0.004(2) C133 0.049(3) 0.049(3) 0.059(3) 0.006(3) 0.024(3) -0.006(2) C134 0.037(3) 0.048(3) 0.039(3) -0.005(2) 0.014(2) 0.007(2) C135 0.039(3) 0.042(3) 0.036(2) -0.008(2) 0.005(2) 0.011(2) C136 0.064(4) 0.039(3) 0.059(3) -0.007(2) 0.015(3) 0.021(3) N137 0.035(2) 0.026(2) 0.027(2) -0.0022(14) 0.0032(15) 0.0055(14) O141 0.0308(15) 0.0227(13) 0.0291(15) 0.0006(11) 0.0029(12) 0.0042(11) C142 0.025(2) 0.025(2) 0.023(2) -0.001(2) 0.000(2) -0.001(2) C143 0.035(2) 0.031(2) 0.035(2) 0.003(2) 0.012(2) 0.000(2) C144 0.037(2) 0.028(2) 0.038(2) 0.006(2) 0.014(2) -0.001(2) C145 0.032(2) 0.021(2) 0.027(2) 0.001(2) 0.005(2) 0.000(2) C146 0.025(2) 0.028(2) 0.024(2) -0.002(2) 0.005(2) -0.004(2) C147 0.027(2) 0.024(2) 0.023(2) 0.002(2) 0.002(2) -0.004(2) N211 0.034(2) 0.027(2) 0.023(2) -0.0002(13) -0.0014(14) -0.0071(14) C212 0.035(2) 0.033(2) 0.033(2) -0.001(2) -0.007(2) -0.006(2) C213 0.049(3) 0.030(2) 0.048(3) 0.006(2) -0.002(2) -0.004(2) C214 0.042(3) 0.033(2) 0.043(3) -0.012(2) -0.002(2) -0.004(2) C215 0.040(2) 0.042(2) 0.025(2) -0.010(2) -0.002(2) -0.001(2) C216 0.073(4) 0.053(3) 0.032(3) -0.016(2) 0.013(2) -0.006(3) N217 0.035(2) 0.029(2) 0.022(2) -0.0022(13) -0.0006(14) -0.0046(14) N221 0.031(2) 0.036(2) 0.022(2) -0.0064(14) 0.0015(14) -0.0082(15) C222 0.036(2) 0.044(2) 0.040(3) -0.016(2) -0.002(2) -0.012(2) C223 0.054(3) 0.081(4) 0.046(3) -0.033(3) 0.003(2) -0.027(3) C224 0.036(2) 0.037(2) 0.060(3) -0.013(2) -0.003(2) -0.012(2) C225 0.032(2) 0.026(2) 0.044(3) 0.001(2) 0.002(2) -0.006(2) C226 0.039(3) 0.039(2) 0.055(3) 0.011(2) 0.006(2) -0.012(2) N227 0.031(2) 0.028(2) 0.025(2) -0.0003(14) 0.0014(14) -0.0062(14) N231 0.033(2) 0.037(2) 0.025(2) -0.0002(15) -0.0022(15) -0.009(2) C232 0.033(2) 0.049(3) 0.031(2) -0.004(2) -0.007(2) -0.003(2) C233 0.036(3) 0.080(4) 0.044(3) 0.002(3) -0.002(2) -0.012(3) C234 0.036(3) 0.059(3) 0.029(2) -0.002(2) -0.010(2) 0.002(2) C235 0.046(3) 0.037(2) 0.025(2) -0.002(2) -0.010(2) -0.003(2) C236 0.058(3) 0.050(3) 0.026(2) 0.010(2) -0.006(2) -0.007(2) N237 0.035(2) 0.034(2) 0.019(2) 0.0012(14) -0.0026(14) -0.0071(15) O241 0.037(2) 0.044(2) 0.0253(15) 0.0013(13) -0.0023(13) -0.0175(14) C242 0.032(2) 0.031(2) 0.029(2) 0.000(2) 0.000(2) -0.008(2) C243 0.063(3) 0.052(3) 0.027(2) 0.000(2) -0.004(2) -0.032(3) C244 0.054(3) 0.049(3) 0.026(2) -0.001(2) -0.001(2) -0.022(2) C245 0.028(2) 0.024(2) 0.035(2) 0.004(2) 0.005(2) 0.003(2) C246 0.039(2) 0.025(2) 0.043(3) 0.000(2) -0.001(2) -0.010(2) C247 0.035(2) 0.035(2) 0.030(2) -0.002(2) -0.005(2) -0.008(2) Cl32 0.0906(15) 0.143(2) 0.104(2) -0.0098(14) -0.0191(12) -0.0398(14) Cl31 0.134(2) 0.142(2) 0.178(3) 0.016(2) -0.046(2) -0.037(2) C31 0.135(8) 0.109(6) 0.096(6) 0.000(5) -0.049(6) -0.052(6) C2 0.054(5) 0.071(5) 0.134(9) -0.026(5) 0.041(5) -0.014(4) C1 0.125(9) 0.070(6) 0.186(13) -0.005(7) -0.009(8) 0.002(6) C3 0.107(10) 0.245(20) 0.712(54) -0.195(25) -0.112(23) 0.002(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1' 1.810(14) . ? Mo1 O1 1.83(2) . ? Mo1 O141 1.945(3) . ? Mo1 Cl1 2.165(6) . ? Mo1 N131 2.187(3) . ? Mo1 N111 2.220(3) . ? Mo1 Cl1' 2.242(5) . ? Mo1 N121 2.254(3) . ? Mo2 O2 1.716(10) . ? Mo2 O2' 1.825(13) . ? Mo2 O241 1.947(3) . ? Mo2 N221 2.180(3) . ? Mo2 N211 2.209(3) . ? Mo2 Cl2' 2.211(5) . ? Mo2 N231 2.250(3) . ? Mo2 Cl2 2.273(4) . ? B1 N137 1.521(6) . ? B1 N127 1.536(7) . ? B1 N117 1.542(6) . ? B2 N227 1.538(6) . ? B2 N237 1.541(6) . ? B2 N217 1.551(6) . ? S1 C245 1.777(4) . ? S1 C145 1.778(4) . ? N111 C112 1.346(5) . ? N111 N117 1.376(5) . ? C112 C114 1.398(6) . ? C112 C113 1.487(6) . ? C114 C115 1.381(7) . ? C115 N117 1.342(6) . ? C115 C116 1.498(6) . ? N121 C122 1.351(5) . ? N121 N127 1.380(4) . ? C122 C124 1.388(6) . ? C122 C123 1.487(6) . ? C124 C125 1.362(7) . ? C125 N127 1.364(6) . ? C125 C126 1.500(6) . ? N131 C132 1.338(5) . ? N131 N137 1.376(4) . ? C132 C134 1.381(6) . ? C132 C133 1.491(7) . ? C134 C135 1.368(7) . ? C135 N137 1.345(5) . ? C135 C136 1.496(6) . ? O141 C142 1.361(4) . ? C142 C143 1.394(5) . ? C142 C147 1.394(5) . ? C143 C144 1.389(6) . ? C144 C145 1.383(5) . ? C145 C146 1.388(5) . ? C146 C147 1.379(5) . ? N211 C212 1.336(5) . ? N211 N217 1.373(4) . ? C212 C214 1.390(6) . ? C212 C213 1.498(6) . ? C214 C215 1.364(6) . ? C215 N217 1.356(5) . ? C215 C216 1.502(6) . ? N221 C222 1.353(5) . ? N221 N227 1.377(4) . ? C222 C224 1.386(6) . ? C222 C223 1.490(6) . ? C224 C225 1.383(7) . ? C225 N227 1.351(5) . ? C225 C226 1.489(6) . ? N231 C232 1.329(5) . ? N231 N237 1.375(4) . ? C232 C234 1.392(6) . ? C232 C233 1.498(6) . ? C234 C235 1.365(6) . ? C235 N237 1.335(5) . ? C235 C236 1.497(6) . ? O241 C242 1.348(5) . ? C242 C243 1.395(6) . ? C242 C247 1.401(6) . ? C243 C244 1.374(6) . ? C244 C245 1.380(6) . ? C245 C246 1.380(6) . ? C246 C247 1.383(6) . ? Cl32 C31 1.740(8) . ? Cl31 C31 1.772(9) . ? C2 C3 0.76(2) . ? C2 C1 1.10(2) . ? C1 C3 1.37(3) . ? C3 C3 1.43(5) 2_465 ? 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 O141 100.1(5) . . ? O1 Mo1 O141 98.5(6) . . ? O1 Mo1 Cl1 101.2(6) . . ? O141 Mo1 Cl1 93.1(2) . . ? O1' Mo1 N131 86.9(5) . . ? O1 Mo1 N131 88.2(6) . . ? O141 Mo1 N131 168.55(12) . . ? Cl1 Mo1 N131 94.6(2) . . ? O1' Mo1 N111 88.1(5) . . ? O1 Mo1 N111 163.4(6) . . ? O141 Mo1 N111 88.16(12) . . ? Cl1 Mo1 N111 93.6(2) . . ? N131 Mo1 N111 83.01(12) . . ? O1' Mo1 Cl1' 102.0(5) . . ? O141 Mo1 Cl1' 94.8(2) . . ? N131 Mo1 Cl1' 92.6(2) . . ? N111 Mo1 Cl1' 168.8(2) . . ? O1' Mo1 N121 164.8(4) . . ? O1 Mo1 N121 86.3(6) . . ? O141 Mo1 N121 87.21(12) . . ? Cl1 Mo1 N121 172.4(2) . . ? N131 Mo1 N121 83.95(12) . . ? N111 Mo1 N121 78.81(13) . . ? Cl1' Mo1 N121 90.5(2) . . ? O2 Mo2 O241 98.9(4) . . ? O2' Mo2 O241 98.7(5) . . ? O2 Mo2 N221 88.2(4) . . ? O2' Mo2 N221 88.6(5) . . ? O241 Mo2 N221 168.25(12) . . ? O2 Mo2 N211 88.8(3) . . ? O2' Mo2 N211 165.1(5) . . ? O241 Mo2 N211 86.78(12) . . ? N221 Mo2 N211 84.01(12) . . ? O2' Mo2 Cl2' 99.5(5) . . ? O241 Mo2 Cl2' 94.4(2) . . ? N221 Mo2 Cl2' 93.4(2) . . ? N211 Mo2 Cl2' 93.8(2) . . ? O2 Mo2 N231 165.5(3) . . ? O2' Mo2 N231 87.4(5) . . ? O241 Mo2 N231 88.08(12) . . ? N221 Mo2 N231 83.01(13) . . ? N211 Mo2 N231 78.90(12) . . ? Cl2' Mo2 N231 172.1(2) . . ? O2 Mo2 Cl2 102.8(3) . . ? O241 Mo2 Cl2 92.56(14) . . ? N221 Mo2 Cl2 94.98(14) . . ? N211 Mo2 Cl2 168.33(14) . . ? N231 Mo2 Cl2 89.43(14) . . ? N137 B1 N127 109.3(4) . . ? N137 B1 N117 108.9(4) . . ? N127 B1 N117 108.5(3) . . ? N227 B2 N237 108.7(3) . . ? N227 B2 N217 107.8(3) . . ? N237 B2 N217 108.2(4) . . ? C245 S1 C145 103.4(2) . . ? C112 N111 N117 107.3(3) . . ? C112 N111 Mo1 131.7(3) . . ? N117 N111 Mo1 120.2(2) . . ? N111 C112 C114 108.7(4) . . ? N111 C112 C113 122.9(4) . . ? C114 C112 C113 128.4(4) . . ? C115 C114 C112 106.4(4) . . ? N117 C115 C114 108.1(4) . . ? N117 C115 C116 122.5(5) . . ? C114 C115 C116 129.4(5) . . ? C115 N117 N111 109.6(4) . . ? C115 N117 B1 130.6(4) . . ? N111 N117 B1 119.8(3) . . ? C122 N121 N127 106.9(3) . . ? C122 N121 Mo1 132.7(3) . . ? N127 N121 Mo1 120.5(3) . . ? N121 C122 C124 109.1(4) . . ? N121 C122 C123 122.6(4) . . ? C124 C122 C123 128.3(4) . . ? C125 C124 C122 107.2(4) . . ? C124 C125 N127 108.0(4) . . ? C124 C125 C126 129.7(4) . . ? N127 C125 C126 122.2(4) . . ? C125 N127 N121 108.8(4) . . ? C125 N127 B1 132.0(4) . . ? N121 N127 B1 119.2(3) . . ? C132 N131 N137 106.9(3) . . ? C132 N131 Mo1 132.3(3) . . ? N137 N131 Mo1 120.6(2) . . ? N131 C132 C134 109.3(4) . . ? N131 C132 C133 123.2(4) . . ? C134 C132 C133 127.4(4) . . ? C135 C134 C132 106.6(4) . . ? N137 C135 C134 108.1(4) . . ? N137 C135 C136 122.1(4) . . ? C134 C135 C136 129.7(4) . . ? C135 N137 N131 109.0(3) . . ? C135 N137 B1 130.0(4) . . ? N131 N137 B1 120.7(3) . . ? C142 O141 Mo1 134.2(2) . . ? O141 C142 C143 122.9(3) . . ? O141 C142 C147 118.2(3) . . ? C143 C142 C147 118.9(3) . . ? C144 C143 C142 120.2(4) . . ? C145 C144 C143 120.6(4) . . ? C144 C145 C146 118.8(4) . . ? C144 C145 S1 124.4(3) . . ? C146 C145 S1 116.8(3) . . ? C147 C146 C145 121.1(3) . . ? C146 C147 C142 120.1(3) . . ? C212 N211 N217 106.7(3) . . ? C212 N211 Mo2 132.3(3) . . ? N217 N211 Mo2 121.0(2) . . ? N211 C212 C214 109.5(4) . . ? N211 C212 C213 122.9(4) . . ? C214 C212 C213 127.6(4) . . ? C215 C214 C212 106.7(4) . . ? N217 C215 C214 107.6(4) . . ? N217 C215 C216 122.0(4) . . ? C214 C215 C216 130.4(4) . . ? C215 N217 N211 109.4(3) . . ? C215 N217 B2 130.3(3) . . ? N211 N217 B2 120.3(3) . . ? C222 N221 N227 107.4(3) . . ? C222 N221 Mo2 130.3(3) . . ? N227 N221 Mo2 121.5(2) . . ? N221 C222 C224 108.6(4) . . ? N221 C222 C223 122.9(4) . . ? C224 C222 C223 128.5(4) . . ? C225 C224 C222 107.1(4) . . ? N227 C225 C224 107.6(4) . . ? N227 C225 C226 122.3(4) . . ? C224 C225 C226 130.1(4) . . ? C225 N227 N221 109.2(3) . . ? C225 N227 B2 130.8(4) . . ? N221 N227 B2 120.0(3) . . ? C232 N231 N237 106.9(3) . . ? C232 N231 Mo2 132.4(3) . . ? N237 N231 Mo2 119.6(3) . . ? N231 C232 C234 109.2(4) . . ? N231 C232 C233 123.5(4) . . ? C234 C232 C233 127.2(4) . . ? C235 C234 C232 106.2(4) . . ? N237 C235 C234 108.3(4) . . ? N237 C235 C236 122.4(4) . . ? C234 C235 C236 129.2(4) . . ? C235 N237 N231 109.3(3) . . ? C235 N237 B2 130.6(4) . . ? N231 N237 B2 119.9(3) . . ? C242 O241 Mo2 132.5(3) . . ? O241 C242 C243 123.0(4) . . ? O241 C242 C247 118.0(4) . . ? C243 C242 C247 119.0(4) . . ? C244 C243 C242 119.9(4) . . ? C243 C244 C245 121.6(4) . . ? C244 C245 C246 118.6(4) . . ? C244 C245 S1 120.1(3) . . ? C246 C245 S1 121.2(3) . . ? C245 C246 C247 121.2(4) . . ? C246 C247 C242 119.7(4) . . ? Cl32 C31 Cl31 110.7(4) . . ? C3 C2 C1 92.5(28) . . ? C2 C1 C3 33.6(12) . . ? C2 C3 C1 53.9(19) . . ? C2 C3 C3 160.0(59) . 2_465 ? C1 C3 C3 111.2(38) . 2_465 ? _refine_diff_density_max 0.784 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.104 #=END