#------------------------------------------------------------------------------ #$Date: 2011-03-31 14:48:06 +0300 (Thu, 31 Mar 2011) $ #$Revision: 17004 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/4316795.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4316795 loop_ _publ_author_name 'Victor W. L. Ng' 'Michelle K. Taylor' 'Jonathan M. White' 'Charles G. Young' _publ_section_title ; cis-Dioxo- and cis-(Hydroxo)oxo-Mo(V) Complexes Stabilized by Intramolecular Hydrogen-Bonding ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9460 _journal_page_last 9469 _journal_volume 49 _journal_year 2010 _chemical_formula_sum 'C32 H40 B Mo N7 O4' _chemical_formula_weight 693.46 _chemical_name_common Tp(iPr)MoO2(OAr-2-CON(Me)Ph) _chemical_name_systematic ; ? ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 92.468(6) _cell_angle_beta 97.569(7) _cell_angle_gamma 103.852(8) _cell_formula_units_Z 2 _cell_length_a 8.7355(8) _cell_length_b 11.2816(9) _cell_length_c 17.2653(12) _cell_measurement_reflns_used 7185 _cell_measurement_temperature 130(2) _cell_measurement_theta_max 73.1679 _cell_measurement_theta_min 4.9526 _cell_volume 1632.7(2) _computing_cell_refinement ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _diffrn_ambient_temperature 130(2) _diffrn_measured_fraction_theta_full 0.942 _diffrn_measured_fraction_theta_max 0.942 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10520 _diffrn_reflns_theta_full 74.05 _diffrn_reflns_theta_max 74.05 _diffrn_reflns_theta_min 4.97 _exptl_absorpt_coefficient_mu 3.671 _exptl_absorpt_correction_T_max 0.7831 _exptl_absorpt_correction_T_min 0.3862 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.411 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.3249 _exptl_crystal_size_mid 0.1024 _exptl_crystal_size_min 0.0660 _refine_diff_density_max 1.307 _refine_diff_density_min -1.144 _refine_diff_density_rms 0.110 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 406 _refine_ls_number_reflns 6243 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.118 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0466 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0921P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1294 _refine_ls_wR_factor_ref 0.1369 _reflns_number_gt 5507 _reflns_number_total 6243 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ic1011428_si_002_4.cif _[local]_cod_data_source_block jmwng20 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_database_code 4316795 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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 C1 C 0.1814(4) 0.2983(3) 0.14540(19) 0.0216(7) Uani 1 1 d . . . C2 C 0.1514(4) 0.3935(3) 0.1007(2) 0.0226(7) Uani 1 1 d . . . C3 C 0.2389(5) 0.4245(4) 0.0385(2) 0.0267(8) Uani 1 1 d . . . H3 H 0.2230 0.4906 0.0088 0.032 Uiso 1 1 calc R . . C4 C 0.3476(5) 0.3609(4) 0.0198(2) 0.0283(8) Uani 1 1 d . . . H4 H 0.4027 0.3811 -0.0236 0.034 Uiso 1 1 calc R . . C5 C 0.3755(5) 0.2674(4) 0.0646(2) 0.0273(8) Uani 1 1 d . . . H5 H 0.4511 0.2242 0.0523 0.033 Uiso 1 1 calc R . . C6 C 0.2939(4) 0.2364(3) 0.1276(2) 0.0226(7) Uani 1 1 d . . . H6 H 0.3150 0.1729 0.1585 0.027 Uiso 1 1 calc R . . C7 C 0.0452(5) 0.4749(3) 0.1198(2) 0.0255(8) Uani 1 1 d . . . C8 C -0.1902(6) 0.5085(4) 0.1653(3) 0.0377(10) Uani 1 1 d . . . H8A H -0.2969 0.4619 0.1724 0.057 Uiso 1 1 calc R . . H8B H -0.1995 0.5715 0.1289 0.057 Uiso 1 1 calc R . . H8C H -0.1319 0.5475 0.2160 0.057 Uiso 1 1 calc R . . C11 C 0.3627(5) 0.1294(4) 0.5202(2) 0.0317(9) Uani 1 1 d . . . H11 H 0.4520 0.1044 0.5453 0.038 Uiso 1 1 calc R . . C12 C 0.2385(6) 0.1476(4) 0.5561(2) 0.0339(9) Uani 1 1 d . . . H12 H 0.2247 0.1372 0.6092 0.041 Uiso 1 1 calc R . . C13 C 0.1369(5) 0.1843(3) 0.4984(2) 0.0244(7) Uani 1 1 d . . . C14 C -0.0175(5) 0.2185(4) 0.5060(2) 0.0266(8) Uani 1 1 d . . . H14 H -0.0869 0.1989 0.4540 0.032 Uiso 1 1 calc R . . C15 C -0.1051(6) 0.1444(4) 0.5659(3) 0.0393(10) Uani 1 1 d . . . H15A H -0.2046 0.1684 0.5698 0.059 Uiso 1 1 calc R . . H15B H -0.0377 0.1601 0.6171 0.059 Uiso 1 1 calc R . . H15C H -0.1293 0.0569 0.5492 0.059 Uiso 1 1 calc R . . C16 C 0.0098(6) 0.3545(4) 0.5282(3) 0.0418(11) Uani 1 1 d . . . H16A H -0.0925 0.3735 0.5327 0.063 Uiso 1 1 calc R . . H16B H 0.0595 0.4014 0.4876 0.063 Uiso 1 1 calc R . . H16C H 0.0801 0.3762 0.5785 0.063 Uiso 1 1 calc R . . C21 C 0.6372(5) 0.3466(4) 0.3598(2) 0.0276(8) Uani 1 1 d . . . H21 H 0.7355 0.3290 0.3795 0.033 Uiso 1 1 calc R . . C22 C 0.6180(5) 0.4570(4) 0.3355(2) 0.0308(8) Uani 1 1 d . . . H22 H 0.6997 0.5293 0.3341 0.037 Uiso 1 1 calc R . . C23 C 0.4550(5) 0.4420(3) 0.3135(2) 0.0248(8) Uani 1 1 d . . . C24 C 0.3706(5) 0.5367(3) 0.2857(2) 0.0268(8) Uani 1 1 d . . . H24 H 0.2612 0.4937 0.2594 0.032 Uiso 1 1 calc R . . C25 C 0.4583(5) 0.6120(4) 0.2260(3) 0.0369(10) Uani 1 1 d . . . H25A H 0.4017 0.6734 0.2085 0.055 Uiso 1 1 calc R . . H25B H 0.4625 0.5576 0.1808 0.055 Uiso 1 1 calc R . . H25C H 0.5670 0.6530 0.2503 0.055 Uiso 1 1 calc R . . C26 C 0.3546(6) 0.6198(4) 0.3551(3) 0.0433(11) Uani 1 1 d . . . H26A H 0.2992 0.6811 0.3359 0.065 Uiso 1 1 calc R . . H26B H 0.4609 0.6611 0.3825 0.065 Uiso 1 1 calc R . . H26C H 0.2936 0.5704 0.3913 0.065 Uiso 1 1 calc R . . C31 C 0.3676(5) -0.0553(4) 0.2847(2) 0.0267(8) Uani 1 1 d . . . H31 H 0.4574 -0.0875 0.2992 0.032 Uiso 1 1 calc R . . C32 C 0.2397(5) -0.1076(4) 0.2294(2) 0.0278(8) Uani 1 1 d . . . H32 H 0.2236 -0.1820 0.1979 0.033 Uiso 1 1 calc R . . C33 C 0.1374(5) -0.0294(3) 0.2285(2) 0.0227(7) Uani 1 1 d . . . C34 C -0.0227(5) -0.0457(3) 0.1796(2) 0.0248(8) Uani 1 1 d . . . H34 H -0.0485 0.0359 0.1778 0.030 Uiso 1 1 calc R . . C35 C -0.1510(5) -0.1320(4) 0.2166(2) 0.0359(9) Uani 1 1 d . . . H35A H -0.2549 -0.1416 0.1843 0.054 Uiso 1 1 calc R . . H35B H -0.1542 -0.0978 0.2693 0.054 Uiso 1 1 calc R . . H35C H -0.1262 -0.2120 0.2199 0.054 Uiso 1 1 calc R . . C36 C -0.0188(6) -0.0931(4) 0.0963(2) 0.0352(9) Uani 1 1 d . . . H36A H -0.1238 -0.1031 0.0650 0.053 Uiso 1 1 calc R . . H36B H 0.0089 -0.1723 0.0970 0.053 Uiso 1 1 calc R . . H36C H 0.0611 -0.0346 0.0730 0.053 Uiso 1 1 calc R . . C41 C -0.1852(4) 0.2995(4) 0.1162(2) 0.0249(8) Uani 1 1 d . . . C42 C -0.2618(5) 0.2356(4) 0.1733(2) 0.0272(8) Uani 1 1 d . . . H42 H -0.2573 0.2754 0.2235 0.033 Uiso 1 1 calc R . . C43 C -0.3433(5) 0.1158(4) 0.1572(3) 0.0358(9) Uani 1 1 d . . . H43 H -0.3938 0.0725 0.1967 0.043 Uiso 1 1 calc R . . C44 C -0.3532(5) 0.0568(4) 0.0842(3) 0.0356(9) Uani 1 1 d . . . H44 H -0.4100 -0.0265 0.0733 0.043 Uiso 1 1 calc R . . C45 C -0.2785(5) 0.1218(4) 0.0270(3) 0.0349(9) Uani 1 1 d . . . H45 H -0.2850 0.0823 -0.0234 0.042 Uiso 1 1 calc R . . C46 C -0.1951(5) 0.2426(4) 0.0425(2) 0.0293(8) Uani 1 1 d . . . H46 H -0.1450 0.2862 0.0031 0.035 Uiso 1 1 calc R . . N1 N -0.1037(4) 0.4252(3) 0.13338(18) 0.0275(7) Uani 1 1 d . . . N11 N 0.1988(4) 0.1865(3) 0.43063(16) 0.0211(6) Uani 1 1 d . . . N12 N 0.3397(4) 0.1520(3) 0.44529(17) 0.0220(6) Uani 1 1 d . . . N21 N 0.3791(4) 0.3255(3) 0.32329(17) 0.0218(6) Uani 1 1 d . . . N22 N 0.4944(4) 0.2684(3) 0.35119(17) 0.0230(6) Uani 1 1 d . . . N31 N 0.2032(4) 0.0670(3) 0.28105(16) 0.0206(6) Uani 1 1 d . . . N32 N 0.3448(4) 0.0500(3) 0.31536(17) 0.0237(6) Uani 1 1 d . . . O1 O 0.0998(3) 0.2682(2) 0.20658(13) 0.0222(5) Uani 1 1 d . . . O2 O -0.0700(3) 0.1361(2) 0.31560(14) 0.0239(5) Uani 1 1 d . . . O3 O 0.0831(3) 0.3690(2) 0.35436(15) 0.0264(6) Uani 1 1 d . . . O4 O 0.0997(4) 0.5868(3) 0.12495(17) 0.0341(6) Uani 1 1 d . . . B1 B 0.4452(5) 0.1413(4) 0.3811(2) 0.0227(8) Uani 1 1 d . . . H1 H 0.5413 0.1136 0.4032 0.027 Uiso 1 1 calc R . . Mo1 Mo 0.10923(3) 0.23659(2) 0.314326(14) 0.01883(11) 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 C1 0.0254(18) 0.0204(18) 0.0188(15) 0.0056(13) 0.0064(13) 0.0028(14) C2 0.0255(18) 0.0200(18) 0.0232(16) 0.0042(13) 0.0067(14) 0.0052(14) C3 0.034(2) 0.027(2) 0.0212(16) 0.0117(14) 0.0066(15) 0.0084(16) C4 0.031(2) 0.031(2) 0.0252(17) 0.0089(15) 0.0112(15) 0.0067(17) C5 0.0250(18) 0.032(2) 0.0273(18) 0.0047(15) 0.0076(14) 0.0096(16) C6 0.0236(17) 0.0214(18) 0.0241(16) 0.0075(13) 0.0063(13) 0.0056(14) C7 0.037(2) 0.0229(19) 0.0197(16) 0.0085(13) 0.0048(14) 0.0120(16) C8 0.046(3) 0.038(2) 0.039(2) 0.0058(18) 0.0178(19) 0.023(2) C11 0.038(2) 0.033(2) 0.0278(19) 0.0081(16) 0.0038(16) 0.0152(18) C12 0.046(2) 0.042(2) 0.0182(16) 0.0091(15) 0.0051(16) 0.019(2) C13 0.033(2) 0.0198(18) 0.0215(16) 0.0016(13) 0.0072(14) 0.0062(15) C14 0.034(2) 0.0230(19) 0.0222(16) 0.0010(14) 0.0089(15) 0.0045(16) C15 0.047(3) 0.028(2) 0.048(2) 0.0091(18) 0.025(2) 0.0081(19) C16 0.048(3) 0.025(2) 0.059(3) 0.0088(19) 0.025(2) 0.013(2) C21 0.0228(18) 0.033(2) 0.0245(17) 0.0038(15) 0.0026(14) 0.0029(16) C22 0.032(2) 0.027(2) 0.0300(18) 0.0036(15) 0.0077(16) -0.0010(16) C23 0.033(2) 0.0176(18) 0.0244(17) 0.0020(13) 0.0108(14) 0.0044(15) C24 0.032(2) 0.0143(18) 0.0348(19) 0.0059(14) 0.0125(16) 0.0025(15) C25 0.037(2) 0.026(2) 0.053(3) 0.0208(18) 0.016(2) 0.0088(18) C26 0.055(3) 0.022(2) 0.054(3) -0.0066(19) 0.018(2) 0.009(2) C31 0.034(2) 0.025(2) 0.0288(18) 0.0104(14) 0.0086(15) 0.0175(16) C32 0.040(2) 0.0206(19) 0.0275(18) 0.0042(14) 0.0092(16) 0.0135(17) C33 0.0333(19) 0.0163(17) 0.0212(16) 0.0082(12) 0.0093(14) 0.0072(15) C34 0.0299(19) 0.0198(18) 0.0242(17) 0.0025(13) 0.0087(14) 0.0024(15) C35 0.040(2) 0.029(2) 0.034(2) 0.0074(16) 0.0080(18) -0.0022(18) C36 0.044(2) 0.040(2) 0.0248(19) 0.0006(16) 0.0042(17) 0.017(2) C41 0.0231(18) 0.026(2) 0.0321(18) 0.0101(15) 0.0084(14) 0.0148(15) C42 0.0270(19) 0.037(2) 0.0218(16) 0.0114(15) 0.0021(14) 0.0142(17) C43 0.028(2) 0.041(2) 0.041(2) 0.0194(18) 0.0078(17) 0.0086(18) C44 0.026(2) 0.032(2) 0.048(2) 0.0056(18) 0.0011(17) 0.0052(17) C45 0.029(2) 0.038(2) 0.040(2) -0.0005(18) 0.0063(17) 0.0123(18) C46 0.0255(19) 0.036(2) 0.0303(18) 0.0056(16) 0.0060(15) 0.0134(17) N1 0.0335(18) 0.0271(17) 0.0277(15) 0.0043(12) 0.0110(13) 0.0149(14) N11 0.0309(16) 0.0141(14) 0.0193(13) 0.0063(10) 0.0054(12) 0.0055(12) N12 0.0259(15) 0.0215(15) 0.0222(14) 0.0097(11) -0.0004(11) 0.0137(13) N21 0.0280(16) 0.0189(15) 0.0221(14) 0.0040(11) 0.0047(12) 0.0118(13) N22 0.0275(16) 0.0191(16) 0.0242(14) 0.0061(11) 0.0049(12) 0.0079(13) N31 0.0257(15) 0.0192(15) 0.0190(13) 0.0071(11) 0.0016(11) 0.0093(12) N32 0.0321(17) 0.0196(16) 0.0217(14) 0.0057(11) 0.0076(12) 0.0078(13) O1 0.0246(12) 0.0277(14) 0.0178(11) 0.0115(9) 0.0046(9) 0.0110(11) O2 0.0262(13) 0.0224(13) 0.0243(12) 0.0070(10) 0.0066(10) 0.0058(11) O3 0.0349(15) 0.0192(13) 0.0281(13) 0.0041(10) 0.0101(11) 0.0092(11) O4 0.0425(17) 0.0211(15) 0.0419(16) 0.0098(11) 0.0097(13) 0.0112(13) B1 0.028(2) 0.020(2) 0.0241(18) 0.0112(15) 0.0032(16) 0.0131(17) Mo1 0.02366(17) 0.01604(17) 0.01889(16) 0.00625(10) 0.00615(10) 0.00650(11) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -0.0483 2.7339 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 120.7(3) . . ? O1 C1 C2 119.0(3) . . ? C6 C1 C2 120.3(3) . . ? C1 C2 C3 118.1(3) . . ? C1 C2 C7 124.6(3) . . ? C3 C2 C7 116.9(3) . . ? C4 C3 C2 121.4(3) . . ? C3 C4 C5 119.5(3) . . ? C4 C5 C6 120.5(4) . . ? C5 C6 C1 120.1(3) . . ? O4 C7 N1 121.3(4) . . ? O4 C7 C2 118.6(4) . . ? N1 C7 C2 120.0(3) . . ? N12 C11 C12 109.8(4) . . ? C11 C12 C13 105.6(3) . . ? N11 C13 C12 108.7(3) . . ? N11 C13 C14 123.1(3) . . ? C12 C13 C14 128.1(3) . . ? C13 C14 C16 111.5(3) . . ? C13 C14 C15 111.2(3) . . ? C16 C14 C15 109.9(3) . . ? N22 C21 C22 108.2(4) . . ? C21 C22 C23 106.3(4) . . ? N21 C23 C22 108.8(3) . . ? N21 C23 C24 123.6(3) . . ? C22 C23 C24 127.6(3) . . ? C23 C24 C25 110.6(3) . . ? C23 C24 C26 110.5(3) . . ? C25 C24 C26 110.8(3) . . ? N32 C31 C32 108.4(3) . . ? C31 C32 C33 105.9(3) . . ? N31 C33 C32 109.2(3) . . ? N31 C33 C34 123.0(3) . . ? C32 C33 C34 127.8(3) . . ? C33 C34 C36 110.4(3) . . ? C33 C34 C35 110.3(3) . . ? C36 C34 C35 111.0(3) . . ? C46 C41 C42 120.0(4) . . ? C46 C41 N1 120.6(3) . . ? C42 C41 N1 119.3(3) . . ? C43 C42 C41 120.0(4) . . ? C42 C43 C44 120.9(4) . . ? C43 C44 C45 118.8(4) . . ? C46 C45 C44 121.0(4) . . ? C45 C46 C41 119.2(4) . . ? C7 N1 C41 124.8(3) . . ? C7 N1 C8 117.0(3) . . ? C41 N1 C8 118.1(3) . . ? C13 N11 N12 107.4(3) . . ? C13 N11 Mo1 130.3(3) . . ? N12 N11 Mo1 122.3(2) . . ? C11 N12 N11 108.4(3) . . ? C11 N12 B1 128.8(3) . . ? N11 N12 B1 122.8(3) . . ? C23 N21 N22 106.6(3) . . ? C23 N21 Mo1 129.6(3) . . ? N22 N21 Mo1 123.3(2) . . ? C21 N22 N21 110.2(3) . . ? C21 N22 B1 129.4(3) . . ? N21 N22 B1 119.3(3) . . ? C33 N31 N32 106.9(3) . . ? C33 N31 Mo1 130.3(2) . . ? N32 N31 Mo1 122.8(2) . . ? C31 N32 N31 109.7(3) . . ? C31 N32 B1 130.6(3) . . ? N31 N32 B1 119.6(3) . . ? C1 O1 Mo1 147.3(2) . . ? N32 B1 N22 110.4(3) . . ? N32 B1 N12 108.0(3) . . ? N22 B1 N12 106.8(3) . . ? O3 Mo1 O2 102.97(13) . . ? O3 Mo1 O1 101.15(12) . . ? O2 Mo1 O1 102.11(11) . . ? O3 Mo1 N11 91.04(12) . . ? O2 Mo1 N11 90.45(12) . . ? O1 Mo1 N11 159.92(11) . . ? O3 Mo1 N21 89.56(12) . . ? O2 Mo1 N21 163.66(11) . . ? O1 Mo1 N21 85.41(11) . . ? N11 Mo1 N21 78.72(11) . . ? O3 Mo1 N31 165.87(12) . . ? O2 Mo1 N31 86.68(12) . . ? O1 Mo1 N31 86.64(10) . . ? N11 Mo1 N31 78.43(10) . . ? N21 Mo1 N31 79.24(11) . . ? 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 C1 O1 1.361(4) . ? C1 C6 1.392(5) . ? C1 C2 1.404(5) . ? C2 C3 1.407(5) . ? C2 C7 1.509(5) . ? C3 C4 1.381(6) . ? C4 C5 1.384(5) . ? C5 C6 1.388(5) . ? C7 O4 1.232(5) . ? C7 N1 1.343(5) . ? C8 N1 1.470(5) . ? C11 N12 1.328(5) . ? C11 C12 1.369(6) . ? C12 C13 1.389(5) . ? C13 N11 1.351(4) . ? C13 C14 1.508(6) . ? C14 C16 1.519(6) . ? C14 C15 1.526(5) . ? C21 N22 1.330(5) . ? C21 C22 1.373(6) . ? C22 C23 1.392(6) . ? C23 N21 1.352(5) . ? C23 C24 1.497(5) . ? C24 C25 1.531(5) . ? C24 C26 1.531(5) . ? C31 N32 1.347(5) . ? C31 C32 1.366(6) . ? C32 C33 1.397(5) . ? C33 N31 1.347(5) . ? C33 C34 1.502(5) . ? C34 C36 1.521(5) . ? C34 C35 1.527(5) . ? C41 C46 1.383(5) . ? C41 C42 1.395(5) . ? C41 N1 1.425(5) . ? C42 C43 1.365(6) . ? C43 C44 1.382(6) . ? C44 C45 1.394(6) . ? C45 C46 1.378(6) . ? N11 N12 1.374(4) . ? N11 Mo1 2.204(3) . ? N12 B1 1.550(5) . ? N21 N22 1.368(4) . ? N21 Mo1 2.312(3) . ? N22 B1 1.528(5) . ? N31 N32 1.360(4) . ? N31 Mo1 2.334(3) . ? N32 B1 1.524(5) . ? O1 Mo1 1.904(2) . ? O2 Mo1 1.703(3) . ? O3 Mo1 1.696(3) . ?