# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 1999 # CCDC Number: 440/130 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 'Spectroscopic studies and molecular orbital calculations....' by R. Kowallick, et al, submitted to New J. Chem. for publication. ; #=============================================================== data_sader _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28.50 H34 B Cl4 Mo N8 O2' _chemical_formula_weight 769.19 _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' '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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 24.826(2) _cell_length_b 39.023(3) _cell_length_c 14.233(4) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(8) _cell_angle_gamma 90.000(12) _cell_volume 13789.3(36) _cell_formula_units_Z 16 _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 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method ? _exptl_crystal_F_000 6272 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.87 _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 21987 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -45 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.58 _reflns_number_total 7756 _reflns_number_observed 6038 _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 1 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^)+(0.0547P)^2^+3.2212P] 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 SHELXL _refine_ls_extinction_coef 0.00003(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(4) _refine_ls_number_reflns 7755 _refine_ls_number_parameters 430 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_obs 0.0511 _refine_ls_wR_factor_all 0.1185 _refine_ls_wR_factor_obs 0.1031 _refine_ls_goodness_of_fit_all 1.059 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.070 _refine_ls_shift/esd_max 0.002 _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 0.29868(2) 0.063848(10) 0.56981(3) 0.02459(11) Uani 1 d . . Cl1 Cl 0.28655(6) 0.07590(4) 0.73466(12) 0.0477(4) Uani 1 d . . O1 O 0.2683(2) -0.00714(13) 0.5981(3) 0.0525(12) Uani 1 d . . O2 O 0.0361(2) 0.05709(13) 0.6444(4) 0.0704(15) Uani 1 d . . N1 N 0.2812(2) 0.01670(15) 0.5870(3) 0.0365(11) Uani 1 d . . N11 N 0.3127(2) 0.05916(11) 0.4195(3) 0.0298(10) Uani 1 d . . N12 N 0.3564(2) 0.07573(11) 0.3824(3) 0.0326(10) Uani 1 d . . N21 N 0.3857(2) 0.05860(9) 0.5836(3) 0.0287(10) Uani 1 d . . N22 N 0.4186(2) 0.07635(11) 0.5219(3) 0.0298(10) Uani 1 d . . N31 N 0.3165(2) 0.11991(10) 0.5433(3) 0.0264(9) Uani 1 d . . N32 N 0.3604(2) 0.12706(10) 0.4878(3) 0.0285(9) Uani 1 d . . N41 N 0.2139(2) 0.07660(10) 0.5484(3) 0.0278(10) Uani 1 d . . C13 C 0.3601(2) 0.0678(2) 0.2896(4) 0.047(2) Uani 1 d . . C14 C 0.4055(3) 0.0804(2) 0.2278(5) 0.079(3) Uani 1 d . . H17A H 0.4294(3) 0.0952(2) 0.2647(5) 0.118 Uiso 1 calc R . H17B H 0.3906(3) 0.0935(2) 0.1751(5) 0.118 Uiso 1 calc R . H17C H 0.4259(3) 0.0608(2) 0.2037(5) 0.118 Uiso 1 calc R . C15 C 0.3178(2) 0.0468(2) 0.2682(4) 0.051(2) Uani 1 d . . H3A H 0.3097(2) 0.0375(2) 0.2081(4) 0.061 Uiso 1 calc R . C16 C 0.2895(2) 0.04164(14) 0.3490(4) 0.0360(13) Uani 1 d . . C17 C 0.2390(2) 0.01990(15) 0.3667(4) 0.047(2) Uani 1 d . . H6A H 0.2287(2) 0.02169(15) 0.4330(4) 0.070 Uiso 1 calc R . H6B H 0.2467(2) -0.00409(15) 0.3514(4) 0.070 Uiso 1 calc R . H6C H 0.2095(2) 0.02821(15) 0.3271(4) 0.070 Uiso 1 calc R . C23 C 0.4707(2) 0.07236(15) 0.5483(4) 0.0371(14) Uani 1 d . . C24 C 0.5168(2) 0.0897(2) 0.4989(5) 0.058(2) Uani 1 d . . H10A H 0.5030(2) 0.1029(2) 0.4455(5) 0.086 Uiso 1 calc R . H10B H 0.5422(2) 0.0724(2) 0.4763(5) 0.086 Uiso 1 calc R . H10C H 0.5351(2) 0.1051(2) 0.5427(5) 0.086 Uiso 1 calc R . C25 C 0.4711(2) 0.0513(2) 0.6266(5) 0.046(2) Uani 1 d . . H11A H 0.5020(2) 0.0437(2) 0.6602(5) 0.055 Uiso 1 calc R . C26 C 0.4180(2) 0.04336(13) 0.6466(4) 0.0363(13) Uani 1 d . . C27 C 0.3965(3) 0.0224(2) 0.7250(5) 0.060(2) Uani 1 d . . H1A H 0.3571(3) 0.0214(2) 0.7206(5) 0.090 Uiso 1 calc R . H1B H 0.4068(3) 0.0329(2) 0.7850(5) 0.090 Uiso 1 calc R . H1C H 0.4113(3) -0.0008(2) 0.7213(5) 0.090 Uiso 1 calc R . C33 C 0.3690(2) 0.16126(13) 0.4858(4) 0.0410(14) Uani 1 d . . C34 C 0.4151(3) 0.1768(2) 0.4334(6) 0.062(2) Uani 1 d . . H2A H 0.4348(3) 0.1588(2) 0.4001(6) 0.094 Uiso 1 calc R . H2B H 0.4392(3) 0.1883(2) 0.4778(6) 0.094 Uiso 1 calc R . H2C H 0.4013(3) 0.1935(2) 0.3880(6) 0.094 Uiso 1 calc R . C35 C 0.3298(2) 0.17636(13) 0.5428(4) 0.0417(15) Uani 1 d . . H4A H 0.3259(2) 0.20006(13) 0.5564(4) 0.050 Uiso 1 calc R . C36 C 0.2980(2) 0.15006(10) 0.5753(5) 0.0314(10) Uani 1 d . . C37 C 0.2489(2) 0.15388(14) 0.6361(4) 0.0419(14) Uani 1 d . . H5A H 0.2337(2) 0.13121(14) 0.6493(4) 0.063 Uiso 1 calc R . H5B H 0.2220(2) 0.16792(14) 0.6034(4) 0.063 Uiso 1 calc R . H5C H 0.2589(2) 0.16501(14) 0.6953(4) 0.063 Uiso 1 calc R . C42 C 0.1768(2) 0.06445(13) 0.6083(4) 0.0331(12) Uani 1 d . . H24A H 0.1875(2) 0.04728(13) 0.6518(4) 0.040 Uiso 1 calc R . C43 C 0.1239(2) 0.07554(14) 0.6102(4) 0.0357(13) Uani 1 d . . C44 C 0.1079(2) 0.10039(14) 0.5459(4) 0.0423(15) Uani 1 d . . H16A H 0.0719(2) 0.10849(14) 0.5447(4) 0.051 Uiso 1 calc R . C45 C 0.1459(2) 0.11304(13) 0.4836(4) 0.0361(12) Uani 1 d . . H22A H 0.1363(2) 0.13031(13) 0.4396(4) 0.043 Uiso 1 calc R . C46 C 0.1977(2) 0.10046(12) 0.4857(4) 0.0332(11) Uani 1 d . . H25A H 0.2231(2) 0.10888(12) 0.4414(4) 0.040 Uiso 1 calc R . C47 C 0.0824(2) 0.0595(2) 0.6737(5) 0.049(2) Uani 1 d . . C51 C 0.0979(2) 0.04655(15) 0.7677(5) 0.046(2) Uani 1 d . . C52 C 0.0691(3) 0.0192(2) 0.8048(6) 0.068(2) Uani 1 d . . H18A H 0.0414(3) 0.0088(2) 0.7687(6) 0.082 Uiso 1 calc R . C53 C 0.0806(3) 0.0068(2) 0.8950(7) 0.080(3) Uani 1 d . . H28A H 0.0601(3) -0.0114(2) 0.9212(7) 0.096 Uiso 1 calc R . C54 C 0.1211(3) 0.0213(2) 0.9443(6) 0.080(3) Uani 1 d . . H27A H 0.1292(3) 0.0126(2) 1.0050(6) 0.096 Uiso 1 calc R . C55 C 0.1516(3) 0.0485(2) 0.9096(5) 0.059(2) Uani 1 d . . H19A H 0.1796(3) 0.0583(2) 0.9461(5) 0.071 Uiso 1 calc R . C56 C 0.1400(2) 0.06094(14) 0.8201(5) 0.051(2) Uani 1 d . . H26A H 0.1606(2) 0.07921(14) 0.7946(5) 0.061 Uiso 1 calc R . B1 B 0.3931(2) 0.0985(2) 0.4420(4) 0.0322(13) Uani 1 d . . H1 H 0.4221(2) 0.1086(2) 0.4019(4) 0.039 Uiso 1 calc R . C1 C 0.5575(3) 0.1820(3) 0.2312(6) 0.094(3) Uani 1 d DU . Cl2 Cl 0.5194(3) 0.1404(2) 0.2570(7) 0.130(3) Uani 0.50 d PDU 1 Cl3 Cl 0.6265(2) 0.16071(15) 0.2249(4) 0.100(2) Uani 0.50 d PDU 1 Cl2' Cl 0.5546(4) 0.1452(2) 0.2738(6) 0.125(3) Uani 0.50 d PDU 2 Cl3' Cl 0.6183(2) 0.2048(2) 0.2374(3) 0.120(2) Uani 0.50 d PDU 2 C2 C 0.7109(6) 0.2408(5) 0.2675(13) 0.099(6) Uani 0.50 d PDU . Cl4 Cl 0.6458(2) 0.25192(12) 0.2411(4) 0.0917(14) Uani 0.50 d PDU . Cl5 Cl 0.7500 0.2500 0.1754(3) 0.0999(11) Uani 1 d SDU . 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 0.0235(2) 0.0210(2) 0.0292(2) 0.0048(2) -0.0056(2) -0.0023(2) Cl1 0.0444(9) 0.0434(8) 0.0554(10) 0.0033(8) -0.0064(7) -0.0085(7) O1 0.049(3) 0.065(3) 0.043(3) 0.004(2) -0.004(2) 0.014(2) O2 0.026(2) 0.096(4) 0.090(4) 0.019(3) -0.008(2) -0.011(2) N1 0.022(2) 0.065(3) 0.022(3) -0.018(2) -0.007(2) 0.007(2) N11 0.030(2) 0.028(2) 0.031(2) 0.003(2) -0.003(2) 0.001(2) N12 0.031(2) 0.041(3) 0.026(2) -0.001(2) 0.001(2) -0.002(2) N21 0.026(2) 0.020(2) 0.040(3) 0.000(2) -0.003(2) 0.000(2) N22 0.024(2) 0.033(2) 0.032(2) -0.003(2) 0.001(2) -0.002(2) N31 0.023(2) 0.025(2) 0.031(2) 0.005(2) -0.003(2) -0.004(2) N32 0.029(2) 0.026(2) 0.030(2) 0.006(2) 0.001(2) -0.004(2) N41 0.027(2) 0.022(2) 0.035(3) 0.003(2) -0.009(2) -0.004(2) C13 0.043(3) 0.072(4) 0.027(3) -0.007(3) -0.002(2) -0.004(3) C14 0.066(5) 0.133(7) 0.038(4) -0.021(4) 0.016(4) -0.035(5) C15 0.049(4) 0.078(5) 0.025(3) -0.011(3) -0.004(3) -0.006(3) C16 0.041(3) 0.038(3) 0.028(3) -0.007(2) -0.009(2) -0.004(2) C17 0.050(4) 0.049(4) 0.042(3) -0.008(3) -0.015(3) -0.016(3) C23 0.025(3) 0.043(3) 0.044(4) -0.007(3) -0.001(2) 0.003(2) C24 0.030(3) 0.073(5) 0.070(5) 0.009(4) -0.004(3) -0.003(3) C25 0.034(3) 0.041(3) 0.063(4) -0.003(3) -0.018(3) 0.009(3) C26 0.038(3) 0.023(3) 0.048(3) 0.002(2) -0.018(3) 0.001(2) C27 0.055(4) 0.053(4) 0.072(5) 0.030(4) -0.027(4) -0.012(3) C33 0.049(4) 0.029(3) 0.045(3) 0.015(3) -0.008(3) -0.018(3) C34 0.060(4) 0.040(3) 0.088(6) 0.021(4) 0.017(4) -0.017(3) C35 0.044(3) 0.023(3) 0.058(4) 0.007(2) -0.006(3) -0.001(2) C36 0.035(2) 0.020(2) 0.038(3) -0.001(3) -0.011(2) 0.000(2) C37 0.039(3) 0.028(3) 0.059(4) -0.012(3) 0.001(3) 0.005(2) C42 0.029(3) 0.028(3) 0.042(3) 0.008(2) -0.010(2) -0.004(2) C43 0.027(3) 0.030(3) 0.050(3) 0.007(2) -0.006(2) -0.003(2) C44 0.029(3) 0.045(3) 0.054(4) 0.007(3) -0.011(3) 0.007(2) C45 0.037(3) 0.030(3) 0.041(3) 0.007(2) -0.015(3) 0.004(2) C46 0.038(3) 0.028(3) 0.033(3) 0.006(2) -0.013(2) -0.007(2) C47 0.024(3) 0.054(4) 0.069(4) 0.015(3) 0.002(3) -0.004(3) C51 0.022(3) 0.047(3) 0.068(4) 0.023(3) 0.001(3) -0.002(2) C52 0.037(3) 0.070(4) 0.099(6) 0.043(5) 0.014(4) -0.001(3) C53 0.052(5) 0.077(5) 0.112(7) 0.058(5) 0.027(5) 0.004(4) C54 0.056(5) 0.098(6) 0.086(6) 0.061(5) 0.031(5) 0.034(4) C55 0.037(4) 0.087(5) 0.054(4) 0.018(4) 0.008(3) 0.015(3) C56 0.039(3) 0.051(3) 0.062(4) 0.026(4) 0.015(3) 0.007(3) B1 0.028(3) 0.035(3) 0.033(3) 0.006(3) -0.002(3) -0.007(3) C1 0.065(6) 0.147(10) 0.070(6) -0.006(6) 0.008(4) -0.002(5) Cl2 0.114(6) 0.094(4) 0.183(9) 0.047(5) 0.054(6) 0.005(4) Cl3 0.066(3) 0.121(4) 0.112(4) -0.038(3) 0.007(3) 0.001(3) Cl2' 0.190(9) 0.089(4) 0.096(4) -0.012(3) 0.000(6) 0.018(5) Cl3' 0.079(3) 0.209(6) 0.073(3) 0.059(4) -0.002(2) -0.012(4) C2 0.075(12) 0.136(16) 0.086(13) -0.004(12) -0.001(10) 0.056(11) Cl4 0.082(3) 0.095(3) 0.098(3) -0.019(3) -0.005(3) 0.025(2) Cl5 0.123(3) 0.064(2) 0.113(3) 0.000 0.000 -0.003(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 N1 1.906(6) . ? Mo1 N11 2.175(5) . ? Mo1 N21 2.179(4) . ? Mo1 N41 2.185(4) . ? Mo1 N31 2.263(4) . ? Mo1 Cl1 2.412(2) . ? O1 N1 0.996(6) . ? O2 C47 1.226(7) . ? N11 C16 1.345(6) . ? N11 N12 1.370(6) . ? N12 C13 1.360(7) . ? N12 B1 1.530(7) . ? N21 C26 1.341(6) . ? N21 N22 1.386(6) . ? N22 C23 1.355(6) . ? N22 B1 1.563(7) . ? N31 C36 1.342(6) . ? N31 N32 1.374(5) . ? N32 C33 1.352(6) . ? N32 B1 1.525(7) . ? N41 C42 1.340(7) . ? N41 C46 1.351(6) . ? C13 C15 1.366(8) . ? C13 C14 1.512(9) . ? C15 C16 1.363(8) . ? C16 C17 1.534(8) . ? C23 C25 1.385(8) . ? C23 C24 1.503(8) . ? C25 C26 1.385(8) . ? C26 C27 1.483(9) . ? C33 C35 1.399(8) . ? C33 C34 1.493(8) . ? C35 C36 1.374(7) . ? C36 C37 1.504(8) . ? C42 C43 1.384(7) . ? C43 C44 1.391(7) . ? C43 C47 1.507(8) . ? C44 C45 1.386(8) . ? C45 C46 1.376(7) . ? C47 C51 1.481(9) . ? C51 C52 1.391(8) . ? C51 C56 1.401(9) . ? C52 C53 1.401(12) . ? C53 C54 1.351(12) . ? C54 C55 1.393(10) . ? C55 C56 1.394(9) . ? C1 Cl2' 1.560(12) . ? C1 Cl3' 1.755(10) . ? C1 Cl3 1.906(10) . ? C1 Cl2 1.912(11) . ? Cl3' Cl4 1.963(8) . ? C2 Cl5 1.67(2) . ? C2 Cl4 1.715(14) . ? Cl5 C2 1.67(2) 14_655 ? 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 N1 Mo1 N11 94.7(2) . . ? N1 Mo1 N21 97.1(2) . . ? N11 Mo1 N21 85.5(2) . . ? N1 Mo1 N41 91.1(2) . . ? N11 Mo1 N41 92.1(2) . . ? N21 Mo1 N41 171.66(15) . . ? N1 Mo1 N31 177.1(2) . . ? N11 Mo1 N31 83.44(15) . . ? N21 Mo1 N31 84.97(14) . . ? N41 Mo1 N31 86.83(14) . . ? N1 Mo1 Cl1 92.02(13) . . ? N11 Mo1 Cl1 173.30(12) . . ? N21 Mo1 Cl1 93.12(13) . . ? N41 Mo1 Cl1 88.34(11) . . ? N31 Mo1 Cl1 89.90(11) . . ? O1 N1 Mo1 174.1(5) . . ? C16 N11 N12 107.0(4) . . ? C16 N11 Mo1 135.1(4) . . ? N12 N11 Mo1 117.8(3) . . ? C13 N12 N11 108.6(5) . . ? C13 N12 B1 129.2(5) . . ? N11 N12 B1 122.1(4) . . ? C26 N21 N22 107.1(4) . . ? C26 N21 Mo1 133.9(4) . . ? N22 N21 Mo1 118.7(3) . . ? C23 N22 N21 109.2(4) . . ? C23 N22 B1 130.7(5) . . ? N21 N22 B1 119.9(4) . . ? C36 N31 N32 106.7(4) . . ? C36 N31 Mo1 136.4(3) . . ? N32 N31 Mo1 116.6(3) . . ? C33 N32 N31 109.8(4) . . ? C33 N32 B1 128.8(4) . . ? N31 N32 B1 121.3(4) . . ? C42 N41 C46 117.4(4) . . ? C42 N41 Mo1 119.5(3) . . ? C46 N41 Mo1 122.4(3) . . ? N12 C13 C15 107.6(5) . . ? N12 C13 C14 122.6(6) . . ? C15 C13 C14 129.7(5) . . ? C16 C15 C13 107.3(5) . . ? N11 C16 C15 109.5(5) . . ? N11 C16 C17 120.5(5) . . ? C15 C16 C17 129.9(5) . . ? N22 C23 C25 107.4(5) . . ? N22 C23 C24 123.0(5) . . ? C25 C23 C24 129.6(5) . . ? C26 C25 C23 106.9(5) . . ? N21 C26 C25 109.4(5) . . ? N21 C26 C27 122.2(5) . . ? C25 C26 C27 128.3(5) . . ? N32 C33 C35 107.0(4) . . ? N32 C33 C34 122.2(6) . . ? C35 C33 C34 130.7(5) . . ? C36 C35 C33 106.3(5) . . ? N31 C36 C35 110.2(5) . . ? N31 C36 C37 124.0(4) . . ? C35 C36 C37 125.8(5) . . ? N41 C42 C43 123.6(5) . . ? C42 C43 C44 118.4(5) . . ? C42 C43 C47 122.1(5) . . ? C44 C43 C47 119.4(5) . . ? C45 C44 C43 118.4(5) . . ? C46 C45 C44 119.6(5) . . ? N41 C46 C45 122.5(5) . . ? O2 C47 C51 121.7(6) . . ? O2 C47 C43 117.9(6) . . ? C51 C47 C43 120.4(5) . . ? C52 C51 C56 119.4(6) . . ? C52 C51 C47 118.1(6) . . ? C56 C51 C47 122.6(5) . . ? C51 C52 C53 120.5(8) . . ? C54 C53 C52 118.9(7) . . ? C53 C54 C55 122.6(7) . . ? C54 C55 C56 118.6(7) . . ? C55 C56 C51 120.0(6) . . ? N32 B1 N12 110.2(4) . . ? N32 B1 N22 108.1(4) . . ? N12 B1 N22 108.8(4) . . ? Cl2' C1 Cl3' 119.1(7) . . ? Cl3 C1 Cl2 94.9(5) . . ? C1 Cl3' Cl4 141.0(5) . . ? Cl5 C2 Cl4 108.7(10) . . ? C2 Cl4 Cl3' 95.6(8) . . ? C2 Cl5 C2 76.6(13) . 14_655 ? _refine_diff_density_max 0.632 _refine_diff_density_min -0.573 _refine_diff_density_rms 0.091 #=END data_fun _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C22.50 H29.50 B Cl Mo N9 O' _chemical_formula_weight 584.25 _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' '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 8.3816(13) _cell_length_b 12.774(3) _cell_length_c 13.902(3) _cell_angle_alpha 108.66(2) _cell_angle_beta 93.351(14) _cell_angle_gamma 91.54(2) _cell_volume 1406.2(5) _cell_formula_units_Z 2 _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 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method ? _exptl_crystal_F_000 599 _exptl_absorpt_coefficient_mu 0.593 _exptl_absorpt_correction_type 'Empirical, pseudo-azimuthal scan (SADABS)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.92 _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 12252 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4933 _reflns_number_observed 4504 _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 2 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^)+(0.0577P)^2^+2.1664P] 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 4931 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_obs 0.0357 _refine_ls_wR_factor_all 0.1042 _refine_ls_wR_factor_obs 0.1010 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.078 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.078 _refine_ls_shift/esd_max -0.011 _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 0.96196(3) 0.78960(2) 0.71914(2) 0.02022(11) Uani 1 d . . Cl1 Cl 0.81223(12) 0.67708(9) 0.56486(8) 0.0475(2) Uani 1 d . . O52 O 0.7568(4) 0.7063(3) 0.8389(2) 0.0520(8) Uani 1 d . . N11 N 0.9274(3) 1.0339(2) 0.7350(2) 0.0235(6) Uani 1 d . . N12 N 0.8387(3) 0.9380(2) 0.7244(2) 0.0228(5) Uani 1 d . . N21 N 1.1731(3) 1.0007(2) 0.8308(2) 0.0232(6) Uani 1 d . . N22 N 1.1140(3) 0.9040(2) 0.8436(2) 0.0233(5) Uani 1 d . . N31 N 1.1622(3) 0.9494(2) 0.6391(2) 0.0227(5) Uani 1 d . . N32 N 1.1355(3) 0.8373(2) 0.6220(2) 0.0228(5) Uani 1 d . . N41 N 1.1207(3) 0.6542(2) 0.7177(2) 0.0230(5) Uani 1 d . . C47 C 1.4224(5) 0.3929(3) 0.7100(3) 0.0449(10) Uani 1 d . . N51 N 0.8257(4) 0.7415(3) 0.8027(3) 0.0391(8) Uani 1 d . . C13 C 0.6842(4) 0.9638(3) 0.7267(2) 0.0253(7) Uani 1 d . . C14 C 0.6743(4) 1.0757(3) 0.7387(3) 0.0287(7) Uani 1 d . . H11A H 0.5814(4) 1.1146(3) 0.7423(3) 0.034 Uiso 1 calc R . C15 C 0.8286(4) 1.1177(3) 0.7442(2) 0.0261(7) Uani 1 d . . C16 C 0.5534(4) 0.8793(3) 0.7181(3) 0.0342(8) Uani 1 d . . H21A H 0.5985(4) 0.8090(3) 0.7104(3) 0.051 Uiso 1 calc R . H21B H 0.4819(4) 0.8734(3) 0.6598(3) 0.051 Uiso 1 calc R . H21C H 0.4954(4) 0.9010(3) 0.7784(3) 0.051 Uiso 1 calc R . C17 C 0.8894(4) 1.2326(3) 0.7568(3) 0.0370(8) Uani 1 d . . H2A H 1.0041(4) 1.2349(3) 0.7578(3) 0.055 Uiso 1 calc R . H2B H 0.8569(4) 1.2823(3) 0.8196(3) 0.055 Uiso 1 calc R . H2C H 0.8464(4) 1.2546(3) 0.7010(3) 0.055 Uiso 1 calc R . C23 C 1.1702(4) 0.9040(3) 0.9357(2) 0.0301(7) Uani 1 d . . C24 C 1.2671(4) 0.9997(3) 0.9822(3) 0.0355(8) Uani 1 d . . H7A H 1.3215(4) 1.0198(3) 1.0461(3) 0.043 Uiso 1 calc R . C25 C 1.2664(4) 1.0581(3) 0.9147(2) 0.0306(7) Uani 1 d . . C26 C 1.1281(5) 0.8139(3) 0.9778(3) 0.0431(9) Uani 1 d . . H20A H 1.0592(5) 0.7587(3) 0.9287(3) 0.065 Uiso 1 calc R . H20B H 1.0740(5) 0.8441(3) 1.0390(3) 0.065 Uiso 1 calc R . H20C H 1.2240(5) 0.7810(3) 0.9929(3) 0.065 Uiso 1 calc R . C27 C 1.3484(5) 1.1679(3) 0.9272(3) 0.0431(9) Uani 1 d . . H1A H 1.3258(5) 1.1877(3) 0.8669(3) 0.065 Uiso 1 calc R . H1B H 1.4618(5) 1.1631(3) 0.9379(3) 0.065 Uiso 1 calc R . H1C H 1.3102(5) 1.2231(3) 0.9847(3) 0.065 Uiso 1 calc R . C33 C 1.2035(4) 0.7844(3) 0.5352(2) 0.0270(7) Uani 1 d . . C34 C 1.2697(4) 0.8619(3) 0.4959(2) 0.0314(7) Uani 1 d . . H13A H 1.3232(4) 0.8472(3) 0.4366(2) 0.038 Uiso 1 calc R . C35 C 1.2403(4) 0.9647(3) 0.5621(2) 0.0277(7) Uani 1 d . . C36 C 1.2073(5) 0.6616(3) 0.4924(3) 0.0365(8) Uani 1 d . . H5A H 1.1524(5) 0.6285(3) 0.5350(3) 0.055 Uiso 1 calc R . H5B H 1.3164(5) 0.6404(3) 0.4898(3) 0.055 Uiso 1 calc R . H5C H 1.1556(5) 0.6369(3) 0.4250(3) 0.055 Uiso 1 calc R . C37 C 1.2779(5) 1.0770(3) 0.5541(3) 0.0413(9) Uani 1 d . . H18A H 1.2426(5) 1.1328(3) 0.6124(3) 0.062 Uiso 1 calc R . H18B H 1.2239(5) 1.0829(3) 0.4934(3) 0.062 Uiso 1 calc R . H18C H 1.3913(5) 1.0871(3) 0.5514(3) 0.062 Uiso 1 calc R . C42 C 1.2797(4) 0.6725(3) 0.7379(3) 0.0300(7) Uani 1 d . . H8A H 1.3220(4) 0.7446(3) 0.7538(3) 0.036 Uiso 1 calc R . C43 C 1.3830(4) 0.5902(3) 0.7363(3) 0.0346(8) Uani 1 d . . H3A H 1.4924(4) 0.6062(3) 0.7510(3) 0.041 Uiso 1 calc R . C44 C 1.3197(4) 0.4825(3) 0.7121(3) 0.0315(7) Uani 1 d . . C45 C 1.1562(4) 0.4623(3) 0.6910(3) 0.0339(8) Uani 1 d . . H15A H 1.1114(4) 0.3908(3) 0.6742(3) 0.041 Uiso 1 calc R . C46 C 1.0604(4) 0.5498(3) 0.6953(3) 0.0286(7) Uani 1 d . . H17A H 0.9504(4) 0.5361(3) 0.6822(3) 0.034 Uiso 1 calc R . N48 N 1.5034(5) 0.3224(3) 0.7100(4) 0.0652(12) Uani 1 d . . B1 B 1.1120(4) 1.0336(3) 0.7377(3) 0.0240(7) Uani 1 d . . H1 H 1.1561(4) 1.1075(3) 0.7441(3) 0.029 Uiso 1 calc R . C1 C 1.4310(42) 1.4761(13) 0.9993(14) 0.183(16) Uani 0.50 d P . H1D H 1.4395(42) 1.4499(13) 1.0576(14) 0.219 Uiso 0.50 calc PR . H1E H 1.4282(42) 1.4103(13) 0.9400(14) 0.219 Uiso 0.50 calc PR . C2 C 1.2623(50) 1.5168(23) 0.9988(19) 0.214(18) Uani 0.50 d P . H30A H 1.2580(50) 1.5348(23) 0.9361(19) 0.257 Uiso 0.50 calc PR . H30B H 1.2776(50) 1.5880(23) 1.0519(19) 0.257 Uiso 0.50 calc PR . C3 C 1.0839(31) 1.4922(18) 1.0054(21) 0.177(14) Uani 0.50 d P . H31A H 1.0810(31) 1.4137(18) 0.9682(21) 0.212 Uiso 0.50 calc PR . H31B H 1.0893(31) 1.4952(18) 1.0762(21) 0.212 Uiso 0.50 calc PR . 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 0.0150(2) 0.0221(2) 0.0247(2) 0.00931(11) 0.00054(10) 0.00148(10) Cl1 0.0412(5) 0.0498(6) 0.0510(6) 0.0158(5) 0.0024(4) 0.0040(4) O52 0.053(2) 0.065(2) 0.036(2) 0.0116(15) -0.0004(14) 0.017(2) N11 0.0205(13) 0.0213(13) 0.0293(14) 0.0089(11) 0.0020(11) 0.0028(10) N12 0.0172(13) 0.0251(13) 0.0268(13) 0.0098(11) -0.0005(10) 0.0008(10) N21 0.0172(12) 0.0235(13) 0.0256(13) 0.0033(11) 0.0016(10) 0.0012(10) N22 0.0194(13) 0.0245(13) 0.0254(13) 0.0074(11) -0.0004(10) 0.0017(10) N31 0.0196(13) 0.0236(13) 0.0264(13) 0.0103(11) 0.0013(10) 0.0005(10) N32 0.0213(13) 0.0223(13) 0.0252(13) 0.0080(11) 0.0030(10) 0.0015(10) N41 0.0201(13) 0.0220(13) 0.0276(13) 0.0091(11) 0.0018(11) 0.0013(10) C47 0.037(2) 0.033(2) 0.062(3) 0.012(2) -0.003(2) 0.007(2) N51 0.027(2) 0.022(2) 0.054(2) -0.0043(15) -0.022(2) 0.0085(13) C13 0.018(2) 0.033(2) 0.027(2) 0.0133(14) 0.0016(12) 0.0052(13) C14 0.020(2) 0.036(2) 0.033(2) 0.0157(15) 0.0020(13) 0.0108(14) C15 0.027(2) 0.026(2) 0.026(2) 0.0100(13) 0.0007(13) 0.0074(13) C16 0.017(2) 0.043(2) 0.047(2) 0.021(2) 0.0007(14) 0.0019(14) C17 0.034(2) 0.025(2) 0.053(2) 0.014(2) -0.002(2) 0.0063(14) C23 0.026(2) 0.037(2) 0.026(2) 0.0092(14) -0.0008(13) 0.0025(14) C24 0.030(2) 0.047(2) 0.024(2) 0.005(2) -0.0052(14) -0.002(2) C25 0.021(2) 0.036(2) 0.028(2) 0.0000(14) 0.0019(13) -0.0005(14) C26 0.048(2) 0.053(2) 0.032(2) 0.021(2) -0.006(2) -0.004(2) C27 0.040(2) 0.042(2) 0.036(2) -0.001(2) 0.000(2) -0.013(2) C33 0.024(2) 0.032(2) 0.023(2) 0.0067(13) 0.0012(13) 0.0012(13) C34 0.031(2) 0.040(2) 0.024(2) 0.0114(15) 0.0067(14) 0.0000(15) C35 0.023(2) 0.034(2) 0.029(2) 0.0136(14) 0.0010(13) -0.0015(13) C36 0.042(2) 0.033(2) 0.031(2) 0.0038(15) 0.010(2) 0.004(2) C37 0.052(2) 0.037(2) 0.040(2) 0.019(2) 0.012(2) -0.005(2) C42 0.022(2) 0.027(2) 0.042(2) 0.0129(15) 0.0005(14) -0.0001(13) C43 0.021(2) 0.033(2) 0.050(2) 0.014(2) -0.0006(15) 0.0034(14) C44 0.029(2) 0.028(2) 0.036(2) 0.0093(15) 0.0016(14) 0.0085(14) C45 0.033(2) 0.022(2) 0.046(2) 0.0096(15) 0.000(2) -0.0005(14) C46 0.022(2) 0.026(2) 0.037(2) 0.0078(14) 0.0005(14) -0.0002(13) N48 0.049(2) 0.039(2) 0.102(3) 0.015(2) -0.008(2) 0.019(2) B1 0.019(2) 0.022(2) 0.031(2) 0.0079(15) 0.0017(14) 0.0005(13) C1 0.431(53) 0.042(10) 0.076(9) 0.015(8) 0.052(20) -0.011(15) C2 0.428(59) 0.125(22) 0.096(15) 0.037(14) 0.038(28) 0.083(32) C3 0.264(40) 0.075(11) 0.138(17) -0.028(11) -0.061(27) 0.009(21) _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 N51 1.899(5) . ? Mo1 N12 2.166(3) . ? Mo1 N22 2.186(3) . ? Mo1 N41 2.207(3) . ? Mo1 N32 2.241(3) . ? Mo1 Cl1 2.4200(12) . ? O52 N51 0.977(4) . ? N11 C15 1.349(4) . ? N11 N12 1.378(4) . ? N11 B1 1.546(4) . ? N12 C13 1.345(4) . ? N21 C25 1.351(4) . ? N21 N22 1.385(4) . ? N21 B1 1.548(4) . ? N22 C23 1.338(4) . ? N31 C35 1.349(4) . ? N31 N32 1.384(4) . ? N31 B1 1.536(4) . ? N32 C33 1.348(4) . ? N41 C42 1.344(4) . ? N41 C46 1.345(4) . ? C47 N48 1.142(5) . ? C47 C44 1.445(5) . ? C13 C14 1.390(5) . ? C13 C16 1.491(5) . ? C14 C15 1.376(5) . ? C15 C17 1.493(5) . ? C23 C24 1.397(5) . ? C23 C26 1.492(5) . ? C24 C25 1.373(5) . ? C25 C27 1.499(5) . ? C33 C34 1.392(5) . ? C33 C36 1.491(5) . ? C34 C35 1.380(5) . ? C35 C37 1.501(5) . ? C42 C43 1.376(5) . ? C43 C44 1.390(5) . ? C44 C45 1.384(5) . ? C45 C46 1.382(5) . ? C1 C1 1.29(6) 2_887 ? C1 C2 1.52(4) . ? C2 C3 1.53(4) . ? C3 C3 1.43(5) 2_787 ? 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 N51 Mo1 N12 96.64(11) . . ? N51 Mo1 N22 96.26(11) . . ? N12 Mo1 N22 83.07(10) . . ? N51 Mo1 N41 89.48(11) . . ? N12 Mo1 N41 171.42(9) . . ? N22 Mo1 N41 90.31(10) . . ? N51 Mo1 N32 175.78(11) . . ? N12 Mo1 N32 87.46(10) . . ? N22 Mo1 N32 83.22(10) . . ? N41 Mo1 N32 86.34(9) . . ? N51 Mo1 Cl1 92.32(9) . . ? N12 Mo1 Cl1 93.83(7) . . ? N22 Mo1 Cl1 171.16(7) . . ? N41 Mo1 Cl1 91.92(7) . . ? N32 Mo1 Cl1 88.39(7) . . ? C15 N11 N12 109.6(2) . . ? C15 N11 B1 130.3(3) . . ? N12 N11 B1 120.2(2) . . ? C13 N12 N11 106.8(2) . . ? C13 N12 Mo1 133.9(2) . . ? N11 N12 Mo1 119.1(2) . . ? C25 N21 N22 108.9(3) . . ? C25 N21 B1 130.5(3) . . ? N22 N21 B1 120.1(2) . . ? C23 N22 N21 107.2(3) . . ? C23 N22 Mo1 134.6(2) . . ? N21 N22 Mo1 118.2(2) . . ? C35 N31 N32 109.5(3) . . ? C35 N31 B1 130.5(3) . . ? N32 N31 B1 119.9(2) . . ? C33 N32 N31 106.7(2) . . ? C33 N32 Mo1 135.5(2) . . ? N31 N32 Mo1 116.6(2) . . ? C42 N41 C46 117.9(3) . . ? C42 N41 Mo1 121.6(2) . . ? C46 N41 Mo1 120.5(2) . . ? N48 C47 C44 178.8(5) . . ? O52 N51 Mo1 171.9(4) . . ? N12 C13 C14 109.2(3) . . ? N12 C13 C16 121.6(3) . . ? C14 C13 C16 129.2(3) . . ? C15 C14 C13 106.7(3) . . ? N11 C15 C14 107.7(3) . . ? N11 C15 C17 122.2(3) . . ? C14 C15 C17 130.0(3) . . ? N22 C23 C24 109.2(3) . . ? N22 C23 C26 122.8(3) . . ? C24 C23 C26 128.0(3) . . ? C25 C24 C23 106.4(3) . . ? N21 C25 C24 108.3(3) . . ? N21 C25 C27 123.1(3) . . ? C24 C25 C27 128.6(3) . . ? N32 C33 C34 109.4(3) . . ? N32 C33 C36 123.5(3) . . ? C34 C33 C36 127.2(3) . . ? C35 C34 C33 106.6(3) . . ? N31 C35 C34 107.9(3) . . ? N31 C35 C37 122.9(3) . . ? C34 C35 C37 129.2(3) . . ? N41 C42 C43 123.4(3) . . ? C42 C43 C44 118.2(3) . . ? C45 C44 C43 119.0(3) . . ? C45 C44 C47 120.4(3) . . ? C43 C44 C47 120.6(3) . . ? C46 C45 C44 119.2(3) . . ? N41 C46 C45 122.3(3) . . ? N31 B1 N11 109.2(3) . . ? N31 B1 N21 110.1(3) . . ? N11 B1 N21 108.2(3) . . ? C1 C1 C2 132.0(28) 2_887 . ? C1 C2 C3 146.8(26) . . ? C3 C3 C2 155.4(39) 2_787 . ? _refine_diff_density_max 0.995 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.083