# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. #============================================================================== # 1. SUBMISSION DETAILS _journal_coden_Cambridge 0182 #============================================================================== # 0. AUDIT DETAILS _audit_creation_date ' 2005' _audit_creation_method SHELX-97 _audit_update_record ; ? ; _publ_contact_author_name 'Prof. F. Gordon A. Stone' _publ_contact_author_address ; Department of Chemistry and Biochemistry Baylor University One Bear Place # 97348 Waco TX, 76798-7348 USA ; _publ_contact_author_email 'Gordon Stone@baylor.edu' _publ_contact_author_fax '+1 254 710 2403' _publ_contact_author_phone '+1 254 710 4427' _publ_requested_category ? _publ_requested_coeditor_name ? _publ_contact_letter # Include date of submission ; This CIF is submitted as supplementary data for the following manuscript, submitted to Chemical Communications: The bis-molybdenum(0) trianion [1,3,6-{Mo(CO)~3~}-3,6-(\m-H)~2~-1,1,1- (CO)~3~-2-Ph-closo-1,2-MoCB~9~H~7~]^3-^ and its use as a scaffold in the assembly of heteropolymetallic complexes Date of submission: 25/4/05 With thanks, Prof. F. Gordon A. Stone ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; The bis-molybdenum(0) trianion [1,3,6-{Mo(CO)~3~}-3,6-(\m-H)~2~-1,1,1- (CO)~3~-2-Ph-closo-1,2-MoCB~9~H~7~]^3-^ and its use as a scaffold in the assembly of heteropolymetallic complexes ; loop_ _publ_author_name _publ_author_address P.Lei ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; T.D.McGrath ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; F.G.A.Stone ; Department of Chemistry and Biochemistry Baylor University Waco TX, 76798-7348 USA ; #============================================================================== _publ_section_exptl_refinement ; X-ray intensity data were collected at 110(2) K on a Bruker-Nonius X8 APEX CCD area-detector diffractometer using Mo-K\a X-radiation. Several sets of narrow data 'frames' were collected at different values of \q, for various initial values of \f and \w, using 0.5\% increments of \f or \w. The data frames were integrated using SAINT (Bruker, 2003); the substantial redundancy in data allowed an empirical absorption correction (SADABS; Bruker, 2003) to be applied, based on multiple measurements of equivalent reflections. All structures were solved using conventional direct methods (Bruker, 2003) and refined by full-matrix least-squares on all F^2^ data using SHELXL-97 (Bruker, 2001). The locations of the cage-carbon atoms were verified by examination of the appropriate internuclear distances and the magnitudes of their isotropic thermal displacement parameters. All non-hydrogen atoms were assigned anisotropic displacement parameters, although in instances where data or crystal quality were not optimal, or where significant disorder was present, appropriate restraints and/or constraints were applied to several atoms' thermal parameters (ISOR, SIMU, EADP cards in SHELXL (Bruker, 2001)). All hydrogen atoms were included in calculated positions and allowed to ride on their parent atoms, and were assigned fixed isotropic thermal parameters, calculated as U~iso~(H) = 1.2 x U~iso~(parent) or U~iso~(H) = 1.5 x U~iso~(parent) for methyl hydrogens. The carborane H atoms, involved in B-H...M agostic-type interactions, were located in difference maps and were allowed free positional refinement with thermal parameters as just described. Crystals of 1a contained two independent formula units per asymmetric fraction of the unit cell. These differed primarily in the dispositions of the cations and some disorder therein, although in one of the anions there was also some disorder associated with the cage-bound phenyl ring. Disordered components were treated as separate parts with refining complementary occupancies. Crystals of 2 also showed some cation disorder, treated as above. In addition, one half molecule of CH~2~Cl~2~ as solvate occurred in the asymmetric fraction, located close to an inversion centre, which was treated as above. C-Cl bond lengths were restrained towards 1.76(2) \%A (DFIX card in SHELXL (Bruker, 2001)). Crystals of 4 contained two independent molecules per asymmetric fraction, differing primarily in the dispositions of the phosphine phenyl rings. In addition, several partial molecules of CH~2~Cl~2~ occurred in the unique portion of the unit cell. These were modelled as two whole molecules and one quarter molecule in three locations treated as follows. One molecule was disordered over two sites, with the two components assigned refining complementary occupancies. The second molecule was disordered over three sites, of which the three components' occupancies were initially allowed to refine, with their total restrained towards unity. When these occupancies had converged they were fixed at 26, 32 and 42%. The occupancy of the quarter molecule was also initially allowed to refine and then fixed at 25% - this solvate occurs close to an inversion centre. C-Cl bond lengths were restrained towards 1.76(2) \%A (DFIX card in SHELXL (Bruker, 2001)). This modelling of the solvate is not perfect and more complicated disorder is accommodated by allowing the (very) unusually large thermal parameters of several of the solvate atoms. #=== LOOK WITHIN THE data BLOCK FOR COMPOUND 3 FOR COMMENTS ON THAT STRUCTURE. ; _publ_section_references ; Bruker (2001). SHELXTL-PC. Version 6.12. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Bruker (2003). APEX 2. Version 1.0-5. Bruker Analytical X-ray Solutions, Madison, Wisconsin, USA. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #============================================================================== data_1a _database_code_depnum_ccdc_archive 'CCDC 270993' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C8 H20 N), C13 H14 B9 Mo2 O6' _chemical_formula_sum 'C37 H74 B9 Mo2 N3 O6' _chemical_formula_weight 946.16 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' 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 Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 26.518(2) _cell_length_b 17.1036(11) _cell_length_c 20.3798(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9243.4(12) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 7550 _cell_measurement_theta_min 2.187 _cell_measurement_theta_max 23.529 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.360 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3952 _exptl_absorpt_coefficient_mu 0.587 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8817 _exptl_absorpt_correction_T_max 0.9276 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 206587 _diffrn_reflns_av_R_equivalents 0.0838 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -41 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 33.76 _reflns_number_total 32248 _reflns_number_gt 22363 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.9093P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.049(18) _refine_ls_number_reflns 32248 _refine_ls_number_parameters 1064 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.282518(10) 0.477534(14) 0.329575(14) 0.01265(6) Uani 1 1 d . . . Mo2 Mo 0.392475(11) 0.450627(15) 0.279838(15) 0.01672(6) Uani 1 1 d . . . C2 C 0.21105(12) 0.47288(18) 0.26898(16) 0.0158(7) Uani 1 1 d . . . B3 B 0.33282(15) 0.5554(2) 0.26957(19) 0.0174(8) Uani 1 1 d D . . H3 H 0.3756(13) 0.568(2) 0.2861(19) 0.021 Uiso 1 1 d D . . B4 B 0.21742(15) 0.5677(2) 0.2777(2) 0.0216(8) Uani 1 1 d . . . H4 H 0.1891 0.5992 0.3087 0.026 Uiso 1 1 calc R . . B5 B 0.25076(16) 0.4406(2) 0.2168(2) 0.0197(8) Uani 1 1 d . . . H5 H 0.2474 0.3778 0.2018 0.024 Uiso 1 1 calc R . . B6 B 0.31594(15) 0.4850(2) 0.2152(2) 0.0160(8) Uani 1 1 d D . . H6 H 0.3466(11) 0.4457(18) 0.1920(17) 0.019 Uiso 1 1 d D . . B7 B 0.28114(15) 0.6148(2) 0.2751(2) 0.0207(8) Uani 1 1 d . . . H7 H 0.2851 0.6710 0.3028 0.025 Uiso 1 1 calc R . . B8 B 0.20807(16) 0.5205(2) 0.1976(2) 0.0240(9) Uani 1 1 d . . . H8 H 0.1736 0.5202 0.1658 0.029 Uiso 1 1 calc R . . B9 B 0.30859(17) 0.5886(2) 0.1950(2) 0.0235(9) Uani 1 1 d . . . H9 H 0.3320 0.6258 0.1615 0.028 Uiso 1 1 calc R . . B10 B 0.24385(16) 0.6065(2) 0.2028(2) 0.0234(9) Uani 1 1 d . . . H10 H 0.2282 0.6610 0.1802 0.028 Uiso 1 1 calc R . . B11 B 0.26742(15) 0.5182(2) 0.1596(2) 0.0209(8) Uani 1 1 d . . . H11 H 0.2698 0.5066 0.1056 0.025 Uiso 1 1 calc R . . C3 C 0.16588(13) 0.4282(2) 0.29026(17) 0.0226(8) Uani 1 1 d . . . C4 C 0.16809(15) 0.3483(2) 0.30330(18) 0.0258(8) Uani 1 1 d . . . H4' H 0.1994 0.3219 0.2988 0.031 Uiso 1 1 calc R . . C5 C 0.12568(15) 0.3060(2) 0.3227(2) 0.0327(9) Uani 1 1 d . . . H5' H 0.1284 0.2516 0.3315 0.039 Uiso 1 1 calc R . . C6 C 0.07931(15) 0.3435(3) 0.3293(2) 0.0347(10) Uani 1 1 d . . . H6' H 0.0503 0.3147 0.3421 0.042 Uiso 1 1 calc R . . C7 C 0.07571(15) 0.4231(3) 0.3170(2) 0.0384(11) Uani 1 1 d . . . H7' H 0.0444 0.4494 0.3222 0.046 Uiso 1 1 calc R . . C8 C 0.11907(15) 0.4644(2) 0.2968(2) 0.0320(9) Uani 1 1 d . . . H8' H 0.1163 0.5186 0.2873 0.038 Uiso 1 1 calc R . . C11 C 0.23424(14) 0.4899(2) 0.40403(18) 0.0207(7) Uani 1 1 d . . . O11 O 0.20569(11) 0.50202(18) 0.44568(15) 0.0393(7) Uani 1 1 d . . . C12 C 0.29242(13) 0.3665(2) 0.34692(18) 0.0209(8) Uani 1 1 d . . . O12 O 0.29701(11) 0.29861(14) 0.35655(16) 0.0409(8) Uani 1 1 d . . . C13 C 0.33190(15) 0.5055(2) 0.3985(2) 0.0269(8) Uani 1 1 d . . . O13 O 0.35744(10) 0.52483(19) 0.44228(15) 0.0445(8) Uani 1 1 d . . . C14 C 0.40663(13) 0.3403(2) 0.27484(19) 0.0220(7) Uani 1 1 d . . . O14 O 0.41647(11) 0.27286(14) 0.27082(15) 0.0353(7) Uani 1 1 d . . . C15 C 0.43575(16) 0.4531(2) 0.3558(2) 0.0346(10) Uani 1 1 d . . . O15 O 0.46378(12) 0.4570(2) 0.40052(18) 0.0572(11) Uani 1 1 d . . . C16 C 0.45448(14) 0.46719(19) 0.23315(18) 0.0212(7) Uani 1 1 d . . . O16 O 0.49389(10) 0.47730(14) 0.20691(14) 0.0278(6) Uani 1 1 d . . . Mo1A Mo -0.452210(10) -0.032676(14) 0.436899(14) 0.01367(6) Uani 1 1 d . A . Mo2A Mo -0.559081(11) -0.056930(16) 0.504698(16) 0.01815(6) Uani 1 1 d . A . C2A C -0.37834(13) -0.01681(17) 0.49140(17) 0.0169(7) Uani 1 1 d . . . B3A B -0.50247(15) 0.0539(2) 0.48948(19) 0.0158(8) Uani 1 1 d D . . H3A H -0.5480(13) 0.065(2) 0.4797(18) 0.019 Uiso 1 1 d D A . B4A B -0.38883(15) 0.0731(2) 0.4730(2) 0.0177(8) Uani 1 1 d . A . H4A H -0.3630 0.1013 0.4365 0.021 Uiso 1 1 calc R . . B5A B -0.41430(15) -0.0440(2) 0.5500(2) 0.0166(8) Uani 1 1 d . A . H5A H -0.4074 -0.1029 0.5722 0.020 Uiso 1 1 calc R . . B6A B -0.48026(15) -0.0056(2) 0.55045(19) 0.0166(8) Uani 1 1 d D A . H6A H -0.5123(14) -0.045(2) 0.5821(18) 0.020 Uiso 1 1 d D . . B7A B -0.45433(15) 0.1150(2) 0.4737(2) 0.0185(8) Uani 1 1 d . A . H7A H -0.4614 0.1652 0.4396 0.022 Uiso 1 1 calc R . . B8A B -0.37419(15) 0.0421(2) 0.5566(2) 0.0178(8) Uani 1 1 d . A . H8A H -0.3386 0.0503 0.5854 0.021 Uiso 1 1 calc R . . B9A B -0.47734(15) 0.0999(2) 0.5569(2) 0.0178(8) Uani 1 1 d . A . H9A H -0.5014 0.1401 0.5869 0.021 Uiso 1 1 calc R . . B10A B -0.41399(15) 0.1234(2) 0.5448(2) 0.0178(8) Uani 1 1 d . . . H10A H -0.4000 0.1823 0.5605 0.021 Uiso 1 1 calc R A . B11A B -0.43273(15) 0.0406(2) 0.5977(2) 0.0174(8) Uani 1 1 d . A . H11A H -0.4333 0.0379 0.6526 0.021 Uiso 1 1 calc R . . C11A C -0.40762(15) -0.05054(19) 0.35941(19) 0.0229(8) Uani 1 1 d . . . O11A O -0.38145(12) -0.06391(17) 0.31515(15) 0.0410(7) Uani 1 1 d . A . C12A C -0.46366(11) -0.14507(17) 0.43686(18) 0.0153(6) Uani 1 1 d . . . O12A O -0.46842(9) -0.21368(12) 0.43502(13) 0.0226(5) Uani 1 1 d . A . C13A C -0.50575(16) -0.01913(19) 0.37043(18) 0.0239(8) Uani 1 1 d . . . O13A O -0.53611(11) -0.01021(15) 0.32927(16) 0.0346(6) Uani 1 1 d . A . C14A C -0.56870(14) -0.1659(2) 0.52461(18) 0.0239(8) Uani 1 1 d . . . O14A O -0.57618(11) -0.23133(16) 0.53799(14) 0.0351(7) Uani 1 1 d . A . C15A C -0.61086(14) -0.0701(2) 0.4386(2) 0.0262(8) Uani 1 1 d . . . O15A O -0.64359(11) -0.07932(17) 0.40082(15) 0.0404(7) Uani 1 1 d . A . C16A C -0.61295(15) -0.0398(2) 0.5661(2) 0.0306(9) Uani 1 1 d . . . O16A O -0.64582(12) -0.0308(2) 0.60442(18) 0.0514(9) Uani 1 1 d . A . C102 C -0.32878(13) -0.0645(2) 0.4833(3) 0.0151(8) Uiso 0.491(5) 1 d PG A 1 C103 C -0.33159(14) -0.1430(2) 0.4660(3) 0.0170(8) Uiso 0.491(5) 1 d PG A 1 H1XA H -0.3635 -0.1677 0.4619 0.020 Uiso 0.491(5) 1 calc PR A 1 C104 C -0.28768(18) -0.1853(2) 0.4547(3) 0.0203(9) Uiso 0.491(5) 1 d PG A 1 H1XB H -0.2896 -0.2390 0.4428 0.024 Uiso 0.491(5) 1 calc PR A 1 C105 C -0.24098(14) -0.1491(2) 0.4607(3) 0.0223(11) Uiso 0.491(5) 1 d PG A 1 H1XC H -0.2110 -0.1781 0.4530 0.027 Uiso 0.491(5) 1 calc PR A 1 C106 C -0.23817(13) -0.0707(3) 0.4780(3) 0.0235(11) Uiso 0.491(5) 1 d PG A 1 H1XD H -0.2063 -0.0459 0.4821 0.028 Uiso 0.491(5) 1 calc PR A 1 C107 C -0.28208(16) -0.0283(2) 0.4893(3) 0.0175(10) Uiso 0.491(5) 1 d PG A 1 H1XE H -0.2802 0.0253 0.5011 0.021 Uiso 0.491(5) 1 calc PR A 1 C10A C -0.33127(11) -0.05885(17) 0.4674(2) 0.0151(8) Uiso 0.509(5) 1 d PG A 2 C10B C -0.33200(12) -0.13873(18) 0.45485(19) 0.0170(8) Uiso 0.509(5) 1 d PG A 2 H10F H -0.3627 -0.1670 0.4579 0.020 Uiso 0.509(5) 1 calc PR A 2 C10C C -0.28773(13) -0.17726(16) 0.4379(2) 0.0203(9) Uiso 0.509(5) 1 d PG A 2 H10G H -0.2882 -0.2319 0.4293 0.024 Uiso 0.509(5) 1 calc PR A 2 C10D C -0.24273(12) -0.13592(15) 0.4334(2) 0.0223(11) Uiso 0.509(5) 1 d PG A 2 H10H H -0.2125 -0.1623 0.4218 0.027 Uiso 0.509(5) 1 calc PR A 2 C10E C -0.24200(11) -0.05604(15) 0.44595(17) 0.0235(11) Uiso 0.509(5) 1 d PG A 2 H10I H -0.2113 -0.0278 0.4429 0.028 Uiso 0.509(5) 1 calc PR A 2 C10F C -0.28627(12) -0.01750(16) 0.46292(19) 0.0175(10) Uiso 0.509(5) 1 d PG A 2 H10J H -0.2858 0.0371 0.4715 0.021 Uiso 0.509(5) 1 calc PR A 2 N1 N 0.24760(8) 0.74578(12) 0.00131(11) 0.0157(5) Uani 1 1 d R . . C21 C 0.23117(9) 0.74354(14) -0.07033(11) 0.0260(8) Uani 1 1 d R . . H21A H 0.2435 0.6941 -0.0898 0.031 Uiso 1 1 calc R . . H21B H 0.1939 0.7421 -0.0716 0.031 Uiso 1 1 calc R . . C22 C 0.24858(17) 0.8094(2) -0.11252(19) 0.0304(9) Uani 1 1 d . . . H22A H 0.2355 0.8024 -0.1571 0.046 Uiso 1 1 calc R . . H22B H 0.2855 0.8102 -0.1136 0.046 Uiso 1 1 calc R . . H22C H 0.2361 0.8589 -0.0946 0.046 Uiso 1 1 calc R . . C23 C 0.23340(13) 0.6685(2) 0.03404(18) 0.0215(7) Uani 1 1 d . . . H23A H 0.2466 0.6252 0.0067 0.026 Uiso 1 1 calc R . . H23B H 0.2507 0.6657 0.0770 0.026 Uiso 1 1 calc R . . C24 C 0.17870(14) 0.6550(2) 0.0449(2) 0.0314(9) Uani 1 1 d . . . H24A H 0.1738 0.6042 0.0661 0.047 Uiso 1 1 calc R . . H24B H 0.1611 0.6556 0.0026 0.047 Uiso 1 1 calc R . . H24C H 0.1651 0.6964 0.0731 0.047 Uiso 1 1 calc R . . C25 C 0.22012(14) 0.81430(19) 0.03403(18) 0.0230(8) Uani 1 1 d . . . H25A H 0.2279 0.8627 0.0094 0.028 Uiso 1 1 calc R . . H25B H 0.1833 0.8052 0.0309 0.028 Uiso 1 1 calc R . . C26 C 0.23401(16) 0.8266(2) 0.10604(19) 0.0314(9) Uani 1 1 d . . . H26A H 0.2154 0.8716 0.1234 0.047 Uiso 1 1 calc R . . H26B H 0.2703 0.8363 0.1097 0.047 Uiso 1 1 calc R . . H26C H 0.2252 0.7798 0.1312 0.047 Uiso 1 1 calc R . . C27 C 0.30356(12) 0.75815(19) 0.00815(19) 0.0221(7) Uani 1 1 d . . . H27A H 0.3126 0.7543 0.0552 0.027 Uiso 1 1 calc R . . H27B H 0.3118 0.8118 -0.0066 0.027 Uiso 1 1 calc R . . C28 C 0.33589(14) 0.7002(2) -0.0306(2) 0.0360(10) Uani 1 1 d . . . H28A H 0.3716 0.7121 -0.0238 0.054 Uiso 1 1 calc R . . H28B H 0.3279 0.7044 -0.0775 0.054 Uiso 1 1 calc R . . H28C H 0.3288 0.6469 -0.0155 0.054 Uiso 1 1 calc R . . N2 N 0.43626(11) 0.40212(16) 0.03594(14) 0.0190(6) Uani 1 1 d . . . C31 C 0.39272(13) 0.3738(2) -0.00605(18) 0.0230(8) Uani 1 1 d . . . H31A H 0.3895 0.4089 -0.0444 0.028 Uiso 1 1 calc R . . H31B H 0.4010 0.3210 -0.0228 0.028 Uiso 1 1 calc R . . C32 C 0.34289(16) 0.3701(3) 0.0283(2) 0.0431(11) Uani 1 1 d . . . H32A H 0.3170 0.3516 -0.0024 0.065 Uiso 1 1 calc R . . H32B H 0.3338 0.4223 0.0442 0.065 Uiso 1 1 calc R . . H32C H 0.3452 0.3339 0.0655 0.065 Uiso 1 1 calc R . . C33 C 0.42846(15) 0.48581(19) 0.05746(19) 0.0250(8) Uani 1 1 d . . . H33A H 0.3967 0.4888 0.0828 0.030 Uiso 1 1 calc R . . H33B H 0.4563 0.5005 0.0874 0.030 Uiso 1 1 calc R . . C34 C 0.42614(16) 0.5450(2) 0.0027(2) 0.0327(9) Uani 1 1 d . . . H34A H 0.4208 0.5972 0.0211 0.049 Uiso 1 1 calc R . . H34B H 0.3982 0.5319 -0.0269 0.049 Uiso 1 1 calc R . . H34C H 0.4579 0.5442 -0.0219 0.049 Uiso 1 1 calc R . . C35 C 0.48412(13) 0.39403(19) -0.00645(18) 0.0225(8) Uani 1 1 d . . . H35A H 0.4882 0.3383 -0.0184 0.027 Uiso 1 1 calc R . . H35B H 0.4789 0.4236 -0.0476 0.027 Uiso 1 1 calc R . . C36 C 0.53288(15) 0.4222(3) 0.0251(2) 0.0379(11) Uani 1 1 d . . . H36A H 0.5609 0.4147 -0.0055 0.057 Uiso 1 1 calc R . . H36B H 0.5392 0.3922 0.0653 0.057 Uiso 1 1 calc R . . H36C H 0.5299 0.4778 0.0360 0.057 Uiso 1 1 calc R . . C37 C 0.44165(15) 0.35342(19) 0.09858(18) 0.0235(8) Uani 1 1 d . . . H37A H 0.4718 0.3719 0.1227 0.028 Uiso 1 1 calc R . . H37B H 0.4119 0.3634 0.1268 0.028 Uiso 1 1 calc R . . C38 C 0.44640(15) 0.2660(2) 0.0884(2) 0.0285(9) Uani 1 1 d . . . H38A H 0.4492 0.2400 0.1311 0.043 Uiso 1 1 calc R . . H38B H 0.4766 0.2549 0.0622 0.043 Uiso 1 1 calc R . . H38C H 0.4165 0.2465 0.0653 0.043 Uiso 1 1 calc R . . N3 N 0.43478(10) 0.76245(14) 0.25650(14) 0.0142(6) Uani 1 1 d . . . C41 C 0.45895(14) 0.68574(17) 0.23650(18) 0.0211(7) Uani 1 1 d . . . H41A H 0.4394 0.6423 0.2561 0.025 Uiso 1 1 calc R . . H41B H 0.4934 0.6836 0.2551 0.025 Uiso 1 1 calc R . . C42 C 0.46225(16) 0.6727(2) 0.1625(2) 0.0326(9) Uani 1 1 d . . . H42A H 0.4784 0.6222 0.1537 0.049 Uiso 1 1 calc R . . H42B H 0.4822 0.7147 0.1425 0.049 Uiso 1 1 calc R . . H42C H 0.4282 0.6728 0.1437 0.049 Uiso 1 1 calc R . . C43 C 0.46300(13) 0.83194(18) 0.22718(18) 0.0208(7) Uani 1 1 d . . . H43A H 0.4570 0.8325 0.1792 0.025 Uiso 1 1 calc R . . H43B H 0.4483 0.8805 0.2454 0.025 Uiso 1 1 calc R . . C44 C 0.51914(14) 0.8334(2) 0.2389(2) 0.0281(8) Uani 1 1 d . . . H44A H 0.5336 0.8802 0.2185 0.042 Uiso 1 1 calc R . . H44B H 0.5345 0.7866 0.2196 0.042 Uiso 1 1 calc R . . H44C H 0.5258 0.8343 0.2862 0.042 Uiso 1 1 calc R . . C45 C 0.43642(13) 0.77012(19) 0.33141(17) 0.0195(7) Uani 1 1 d . . . H45A H 0.4722 0.7728 0.3453 0.023 Uiso 1 1 calc R . . H45B H 0.4203 0.8202 0.3438 0.023 Uiso 1 1 calc R . . C46 C 0.41099(16) 0.7050(2) 0.36925(18) 0.0306(9) Uani 1 1 d . . . H46A H 0.4138 0.7153 0.4164 0.046 Uiso 1 1 calc R . . H46B H 0.4274 0.6551 0.3590 0.046 Uiso 1 1 calc R . . H46C H 0.3753 0.7023 0.3569 0.046 Uiso 1 1 calc R . . C47 C 0.38073(13) 0.7639(2) 0.23057(18) 0.0238(8) Uani 1 1 d . . . H47A H 0.3817 0.7559 0.1825 0.029 Uiso 1 1 calc R . . H47B H 0.3622 0.7192 0.2499 0.029 Uiso 1 1 calc R . . C48 C 0.35146(15) 0.8373(2) 0.2444(2) 0.0368(10) Uani 1 1 d . . . H48A H 0.3175 0.8325 0.2259 0.055 Uiso 1 1 calc R . . H48B H 0.3686 0.8820 0.2243 0.055 Uiso 1 1 calc R . . H48C H 0.3492 0.8453 0.2919 0.055 Uiso 1 1 calc R . . N4 N 0.57544(12) 0.22026(17) 0.25643(15) 0.0236(6) Uani 1 1 d . . . C51 C 0.5348(2) 0.2645(4) 0.2946(3) 0.0348(13) Uani 0.699(3) 1 d P B 1 H51A H 0.5143 0.2940 0.2625 0.042 Uiso 0.699(3) 1 calc PR B 1 H51B H 0.5123 0.2252 0.3151 0.042 Uiso 0.699(3) 1 calc PR B 1 C53 C 0.5522(2) 0.1702(4) 0.2032(3) 0.0351(13) Uani 0.699(3) 1 d P B 1 H53A H 0.5349 0.2058 0.1722 0.042 Uiso 0.699(3) 1 calc PR B 1 H53B H 0.5802 0.1453 0.1788 0.042 Uiso 0.699(3) 1 calc PR B 1 C55 C 0.6043(2) 0.1692(3) 0.3068(3) 0.0247(11) Uani 0.699(3) 1 d P B 1 H55A H 0.6200 0.2034 0.3402 0.030 Uiso 0.699(3) 1 calc PR B 1 H55B H 0.5801 0.1344 0.3295 0.030 Uiso 0.699(3) 1 calc PR B 1 C57 C 0.61330(19) 0.2771(3) 0.2272(3) 0.0215(10) Uani 0.699(3) 1 d P B 1 H57A H 0.6367 0.2476 0.1986 0.026 Uiso 0.699(3) 1 calc PR B 1 H57B H 0.6334 0.3002 0.2632 0.026 Uiso 0.699(3) 1 calc PR B 1 C52 C 0.5502(2) 0.3185(3) 0.3454(2) 0.0505(13) Uani 0.699(3) 1 d P B 1 H52A H 0.5203 0.3423 0.3653 0.076 Uiso 0.699(3) 1 calc PR B 1 H52B H 0.5714 0.3594 0.3261 0.076 Uiso 0.699(3) 1 calc PR B 1 H52C H 0.5694 0.2903 0.3790 0.076 Uiso 0.699(3) 1 calc PR B 1 C54 C 0.5167(2) 0.1088(3) 0.2203(3) 0.0696(18) Uani 0.699(3) 1 d P B 1 H54A H 0.5051 0.0826 0.1803 0.104 Uiso 0.699(3) 1 calc PR B 1 H54B H 0.4877 0.1318 0.2432 0.104 Uiso 0.699(3) 1 calc PR B 1 H54C H 0.5333 0.0707 0.2491 0.104 Uiso 0.699(3) 1 calc PR B 1 C56 C 0.64511(18) 0.1197(2) 0.2743(3) 0.0477(12) Uani 0.699(3) 1 d P B 1 H56A H 0.6623 0.0882 0.3077 0.072 Uiso 0.699(3) 1 calc PR B 1 H56B H 0.6696 0.1539 0.2526 0.072 Uiso 0.699(3) 1 calc PR B 1 H56C H 0.6297 0.0850 0.2417 0.072 Uiso 0.699(3) 1 calc PR B 1 C58 C 0.58980(16) 0.3430(2) 0.1873(2) 0.0330(9) Uani 0.699(3) 1 d P B 1 H58A H 0.6165 0.3764 0.1695 0.049 Uiso 0.699(3) 1 calc PR B 1 H58B H 0.5677 0.3741 0.2156 0.049 Uiso 0.699(3) 1 calc PR B 1 H58C H 0.5701 0.3208 0.1511 0.049 Uiso 0.699(3) 1 calc PR B 1 C51' C 0.5869(5) 0.2585(9) 0.3170(7) 0.0348(13) Uani 0.301(3) 1 d P B 2 H51C H 0.6198 0.2850 0.3115 0.042 Uiso 0.301(3) 1 calc PR B 2 H51D H 0.5917 0.2173 0.3506 0.042 Uiso 0.301(3) 1 calc PR B 2 C53' C 0.5300(5) 0.1615(8) 0.2648(6) 0.0351(13) Uani 0.301(3) 1 d P B 2 H53C H 0.5366 0.1322 0.3058 0.042 Uiso 0.301(3) 1 calc PR B 2 H53D H 0.4998 0.1939 0.2730 0.042 Uiso 0.301(3) 1 calc PR B 2 C55' C 0.6204(5) 0.1825(7) 0.2239(6) 0.0247(11) Uani 0.301(3) 1 d P B 2 H55C H 0.6456 0.2229 0.2122 0.030 Uiso 0.301(3) 1 calc PR B 2 H55D H 0.6096 0.1558 0.1831 0.030 Uiso 0.301(3) 1 calc PR B 2 C57' C 0.5515(5) 0.2829(7) 0.2051(6) 0.0215(10) Uani 0.301(3) 1 d P B 2 H57C H 0.5401 0.2553 0.1651 0.026 Uiso 0.301(3) 1 calc PR B 2 H57D H 0.5219 0.3086 0.2253 0.026 Uiso 0.301(3) 1 calc PR B 2 C52' C 0.5502(2) 0.3185(3) 0.3454(2) 0.0505(13) Uani 0.301(3) 1 d P B 2 H52D H 0.5628 0.3369 0.3879 0.076 Uiso 0.301(3) 1 calc PR B 2 H52E H 0.5171 0.2942 0.3512 0.076 Uiso 0.301(3) 1 calc PR B 2 H52F H 0.5473 0.3629 0.3152 0.076 Uiso 0.301(3) 1 calc PR B 2 C54' C 0.5167(2) 0.1088(3) 0.2203(3) 0.0696(18) Uani 0.301(3) 1 d P B 2 H54D H 0.4866 0.0809 0.2355 0.104 Uiso 0.301(3) 1 calc PR B 2 H54E H 0.5443 0.0716 0.2139 0.104 Uiso 0.301(3) 1 calc PR B 2 H54F H 0.5093 0.1351 0.1787 0.104 Uiso 0.301(3) 1 calc PR B 2 C56' C 0.64511(18) 0.1197(2) 0.2743(3) 0.0477(12) Uani 0.301(3) 1 d P B 2 H56D H 0.6738 0.0938 0.2530 0.072 Uiso 0.301(3) 1 calc PR B 2 H56E H 0.6198 0.0805 0.2863 0.072 Uiso 0.301(3) 1 calc PR B 2 H56F H 0.6567 0.1468 0.3138 0.072 Uiso 0.301(3) 1 calc PR B 2 C58' C 0.58980(16) 0.3430(2) 0.1873(2) 0.0330(9) Uani 0.301(3) 1 d P B 2 H58D H 0.5749 0.3804 0.1565 0.049 Uiso 0.301(3) 1 calc PR B 2 H58E H 0.6189 0.3175 0.1668 0.049 Uiso 0.301(3) 1 calc PR B 2 H58F H 0.6008 0.3706 0.2270 0.049 Uiso 0.301(3) 1 calc PR B 2 N5 N -0.11970(14) -0.3019(3) 0.5460(2) 0.0555(12) Uani 1 1 d . . . C61 C -0.0994(3) -0.2433(4) 0.5845(4) 0.0449(16) Uani 0.649(3) 1 d P C 1 H61A H -0.0621 -0.2441 0.5816 0.054 Uiso 0.649(3) 1 calc PR C 1 H61B H -0.1091 -0.2508 0.6310 0.054 Uiso 0.649(3) 1 calc PR C 1 C63 C -0.0861(3) -0.3825(4) 0.5691(4) 0.0404(15) Uani 0.649(3) 1 d P C 1 H63A H -0.0983 -0.4282 0.5439 0.049 Uiso 0.649(3) 1 calc PR C 1 H63B H -0.0502 -0.3743 0.5577 0.049 Uiso 0.649(3) 1 calc PR C 1 C65 C -0.1726(3) -0.3224(4) 0.5657(4) 0.0410(15) Uani 0.649(3) 1 d P C 1 H65A H -0.1721 -0.3336 0.6134 0.049 Uiso 0.649(3) 1 calc PR C 1 H65D H -0.1934 -0.2748 0.5597 0.049 Uiso 0.649(3) 1 calc PR C 1 C67 C -0.1117(3) -0.3051(4) 0.4733(4) 0.0463(17) Uani 0.649(3) 1 d P C 1 H67B H -0.1376 -0.2718 0.4520 0.056 Uiso 0.649(3) 1 calc PR C 1 H67D H -0.1174 -0.3594 0.4584 0.056 Uiso 0.649(3) 1 calc PR C 1 C62 C -0.1208(3) -0.1620(4) 0.5578(5) 0.056(2) Uani 0.649(3) 1 d P C 1 H62A H -0.1068 -0.1191 0.5839 0.083 Uiso 0.649(3) 1 calc PR C 1 H62B H -0.1576 -0.1618 0.5614 0.083 Uiso 0.649(3) 1 calc PR C 1 H62C H -0.1111 -0.1554 0.5118 0.083 Uiso 0.649(3) 1 calc PR C 1 C64 C -0.0900(3) -0.4009(5) 0.6424(4) 0.058(2) Uani 0.649(3) 1 d P C 1 H64A H -0.0700 -0.4476 0.6524 0.087 Uiso 0.649(3) 1 calc PR C 1 H64B H -0.1253 -0.4102 0.6540 0.087 Uiso 0.649(3) 1 calc PR C 1 H64C H -0.0770 -0.3565 0.6678 0.087 Uiso 0.649(3) 1 calc PR C 1 C66 C -0.1980(10) -0.3829(12) 0.5360(11) 0.050(4) Uani 0.649(3) 1 d P C 1 H66A H -0.2321 -0.3868 0.5545 0.076 Uiso 0.649(3) 1 calc PR C 1 H66B H -0.1799 -0.4320 0.5437 0.076 Uiso 0.649(3) 1 calc PR C 1 H66C H -0.2002 -0.3731 0.4887 0.076 Uiso 0.649(3) 1 calc PR C 1 C68 C -0.0606(3) -0.2792(5) 0.4499(4) 0.0548(18) Uani 0.649(3) 1 d P C 1 H68A H -0.0591 -0.2827 0.4019 0.082 Uiso 0.649(3) 1 calc PR C 1 H68B H -0.0346 -0.3130 0.4690 0.082 Uiso 0.649(3) 1 calc PR C 1 H68C H -0.0546 -0.2250 0.4635 0.082 Uiso 0.649(3) 1 calc PR C 1 C61' C -0.1552(5) -0.2162(8) 0.5731(7) 0.0449(16) Uani 0.351(3) 1 d P C 2 H61C H -0.1666 -0.1868 0.5340 0.054 Uiso 0.351(3) 1 calc PR C 2 H61D H -0.1857 -0.2341 0.5969 0.054 Uiso 0.351(3) 1 calc PR C 2 C62' C -0.1259(6) -0.1613(8) 0.6172(9) 0.056(2) Uani 0.351(3) 1 d P C 2 H62D H -0.1474 -0.1173 0.6299 0.083 Uiso 0.351(3) 1 calc PR C 2 H62E H -0.0962 -0.1418 0.5937 0.083 Uiso 0.351(3) 1 calc PR C 2 H62F H -0.1150 -0.1895 0.6567 0.083 Uiso 0.351(3) 1 calc PR C 2 C63' C -0.1104(5) -0.3365(7) 0.6119(7) 0.0404(15) Uani 0.351(3) 1 d P C 2 H63C H -0.1425 -0.3461 0.6353 0.049 Uiso 0.351(3) 1 calc PR C 2 H63D H -0.0890 -0.3017 0.6389 0.049 Uiso 0.351(3) 1 calc PR C 2 C65' C -0.1650(5) -0.3267(7) 0.5060(7) 0.0410(15) Uani 0.351(3) 1 d P C 2 H65B H -0.1535 -0.3443 0.4622 0.049 Uiso 0.351(3) 1 calc PR C 2 H65C H -0.1874 -0.2810 0.4997 0.049 Uiso 0.351(3) 1 calc PR C 2 C67' C -0.0773(5) -0.2665(8) 0.5142(7) 0.0463(17) Uani 0.351(3) 1 d P C 2 H67A H -0.0656 -0.2229 0.5422 0.056 Uiso 0.351(3) 1 calc PR C 2 H67C H -0.0894 -0.2432 0.4726 0.056 Uiso 0.351(3) 1 calc PR C 2 C64' C -0.0832(7) -0.4138(11) 0.5968(9) 0.058(2) Uani 0.351(3) 1 d P C 2 H64D H -0.0771 -0.4422 0.6378 0.087 Uiso 0.351(3) 1 calc PR C 2 H64E H -0.0509 -0.4028 0.5753 0.087 Uiso 0.351(3) 1 calc PR C 2 H64F H -0.1042 -0.4458 0.5677 0.087 Uiso 0.351(3) 1 calc PR C 2 C66' C -0.200(2) -0.404(3) 0.544(2) 0.050(4) Uani 0.351(3) 1 d P C 2 H66D H -0.2296 -0.4159 0.5171 0.076 Uiso 0.351(3) 1 calc PR C 2 H66E H -0.2109 -0.3869 0.5877 0.076 Uiso 0.351(3) 1 calc PR C 2 H66F H -0.1786 -0.4501 0.5478 0.076 Uiso 0.351(3) 1 calc PR C 2 C68' C -0.0298(6) -0.3186(9) 0.4974(8) 0.0548(18) Uani 0.351(3) 1 d P C 2 H68D H -0.0042 -0.2864 0.4756 0.082 Uiso 0.351(3) 1 calc PR C 2 H68E H -0.0400 -0.3613 0.4682 0.082 Uiso 0.351(3) 1 calc PR C 2 H68F H -0.0158 -0.3404 0.5380 0.082 Uiso 0.351(3) 1 calc PR C 2 N6 N -0.3035(3) -0.1065(4) 0.7426(4) 0.0190(11) Uani 0.503(2) 1 d P D 1 C71 C -0.2605(3) -0.0859(4) 0.7879(4) 0.0276(12) Uani 0.503(2) 1 d P D 1 H71A H -0.2283 -0.0972 0.7654 0.033 Uiso 0.503(2) 1 calc PR D 1 H71B H -0.2624 -0.1196 0.8273 0.033 Uiso 0.503(2) 1 calc PR D 1 C72 C -0.2607(4) -0.0006(5) 0.8095(5) 0.0341(18) Uani 0.503(2) 1 d P D 1 H72A H -0.2316 0.0093 0.8379 0.051 Uiso 0.503(2) 1 calc PR D 1 H72B H -0.2918 0.0105 0.8337 0.051 Uiso 0.503(2) 1 calc PR D 1 H72C H -0.2588 0.0333 0.7708 0.051 Uiso 0.503(2) 1 calc PR D 1 C73 C -0.3004(3) -0.0590(4) 0.6777(4) 0.0210(10) Uani 0.503(2) 1 d P D 1 H73A H -0.3286 -0.0755 0.6491 0.025 Uiso 0.503(2) 1 calc PR D 1 H73B H -0.3055 -0.0031 0.6882 0.025 Uiso 0.503(2) 1 calc PR D 1 C74 C -0.2526(3) -0.0667(4) 0.6401(4) 0.0284(12) Uani 0.503(2) 1 d P D 1 H74A H -0.2546 -0.0347 0.6002 0.043 Uiso 0.503(2) 1 calc PR D 1 H74B H -0.2475 -0.1215 0.6280 0.043 Uiso 0.503(2) 1 calc PR D 1 H74C H -0.2243 -0.0488 0.6671 0.043 Uiso 0.503(2) 1 calc PR D 1 C77 C -0.3566(3) -0.0907(5) 0.7722(4) 0.0233(12) Uani 0.503(2) 1 d P D 1 H77A H -0.3626 -0.0336 0.7720 0.028 Uiso 0.503(2) 1 calc PR D 1 H77B H -0.3821 -0.1150 0.7432 0.028 Uiso 0.503(2) 1 calc PR D 1 C78 C -0.3646(3) -0.1206(4) 0.8409(4) 0.0276(12) Uani 0.503(2) 1 d P D 1 H78A H -0.3990 -0.1082 0.8551 0.041 Uiso 0.503(2) 1 calc PR D 1 H78B H -0.3404 -0.0956 0.8706 0.041 Uiso 0.503(2) 1 calc PR D 1 H78C H -0.3597 -0.1774 0.8418 0.041 Uiso 0.503(2) 1 calc PR D 1 C76 C -0.3290(4) -0.2266(5) 0.6718(5) 0.0354(17) Uani 0.503(2) 1 d P D 1 H76A H -0.3227 -0.2829 0.6679 0.053 Uiso 0.503(2) 1 calc PR D 1 H76B H -0.3190 -0.2005 0.6309 0.053 Uiso 0.503(2) 1 calc PR D 1 H76C H -0.3649 -0.2175 0.6799 0.053 Uiso 0.503(2) 1 calc PR D 1 C75 C -0.2986(3) -0.1940(4) 0.7280(4) 0.0223(11) Uani 0.503(2) 1 d P D 1 H75A H -0.2626 -0.2053 0.7193 0.027 Uiso 0.503(2) 1 calc PR D 1 H75B H -0.3081 -0.2230 0.7682 0.027 Uiso 0.503(2) 1 calc PR D 1 N6' N -0.2827(3) -0.1063(4) 0.7210(3) 0.0190(11) Uani 0.497(2) 1 d P D 2 C71' C -0.2703(3) -0.0191(4) 0.7156(4) 0.0276(12) Uani 0.497(2) 1 d P D 2 H71C H -0.2399 -0.0132 0.6878 0.033 Uiso 0.497(2) 1 calc PR D 2 H71D H -0.2986 0.0073 0.6928 0.033 Uiso 0.497(2) 1 calc PR D 2 C72' C -0.2611(4) 0.0217(5) 0.7791(5) 0.0341(18) Uani 0.497(2) 1 d P D 2 H72D H -0.2544 0.0772 0.7708 0.051 Uiso 0.497(2) 1 calc PR D 2 H72E H -0.2319 -0.0017 0.8011 0.051 Uiso 0.497(2) 1 calc PR D 2 H72F H -0.2909 0.0166 0.8072 0.051 Uiso 0.497(2) 1 calc PR D 2 C73' C -0.2384(3) -0.1498(4) 0.7492(4) 0.0210(10) Uani 0.497(2) 1 d P D 2 H73C H -0.2491 -0.2043 0.7578 0.025 Uiso 0.497(2) 1 calc PR D 2 H73D H -0.2299 -0.1259 0.7921 0.025 Uiso 0.497(2) 1 calc PR D 2 C74' C -0.1900(3) -0.1521(4) 0.7071(4) 0.0284(12) Uani 0.497(2) 1 d P D 2 H74D H -0.1638 -0.1815 0.7303 0.043 Uiso 0.497(2) 1 calc PR D 2 H74E H -0.1783 -0.0987 0.6990 0.043 Uiso 0.497(2) 1 calc PR D 2 H74F H -0.1973 -0.1777 0.6651 0.043 Uiso 0.497(2) 1 calc PR D 2 C75' C -0.2946(3) -0.1341(4) 0.6525(4) 0.0223(11) Uani 0.497(2) 1 d P D 2 H75C H -0.3234 -0.1033 0.6356 0.027 Uiso 0.497(2) 1 calc PR D 2 H75D H -0.2652 -0.1228 0.6241 0.027 Uiso 0.497(2) 1 calc PR D 2 C76' C -0.3070(4) -0.2187(5) 0.6461(5) 0.0354(17) Uani 0.497(2) 1 d P D 2 H76D H -0.3147 -0.2307 0.6002 0.053 Uiso 0.497(2) 1 calc PR D 2 H76E H -0.3365 -0.2308 0.6734 0.053 Uiso 0.497(2) 1 calc PR D 2 H76F H -0.2782 -0.2501 0.6606 0.053 Uiso 0.497(2) 1 calc PR D 2 C77' C -0.3259(3) -0.1216(4) 0.7667(4) 0.0233(12) Uani 0.497(2) 1 d P D 2 H77C H -0.3158 -0.1059 0.8115 0.028 Uiso 0.497(2) 1 calc PR D 2 H77D H -0.3326 -0.1786 0.7674 0.028 Uiso 0.497(2) 1 calc PR D 2 C78' C -0.3749(3) -0.0789(5) 0.7487(5) 0.0276(12) Uani 0.497(2) 1 d P D 2 H78D H -0.4013 -0.0924 0.7805 0.041 Uiso 0.497(2) 1 calc PR D 2 H78E H -0.3857 -0.0947 0.7047 0.041 Uiso 0.497(2) 1 calc PR D 2 H78F H -0.3692 -0.0223 0.7496 0.041 Uiso 0.497(2) 1 calc PR D 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 0.01406(13) 0.01220(11) 0.01170(12) -0.00001(10) -0.00009(12) -0.00130(10) Mo2 0.01390(14) 0.01871(13) 0.01755(14) -0.00297(11) -0.00055(12) 0.00049(10) C2 0.0125(16) 0.0199(15) 0.0151(18) 0.0033(12) 0.0006(13) -0.0009(12) B3 0.0164(19) 0.0154(16) 0.020(2) -0.0005(14) 0.0041(15) -0.0042(14) B4 0.018(2) 0.0210(18) 0.026(2) 0.0086(17) -0.0016(19) 0.0006(14) B5 0.019(2) 0.0230(18) 0.017(2) 0.0013(15) 0.0028(16) -0.0074(16) B6 0.0150(19) 0.0142(16) 0.019(2) -0.0004(14) -0.0006(15) -0.0016(14) B7 0.021(2) 0.0155(16) 0.026(2) 0.0012(15) 0.0076(18) 0.0003(14) B8 0.015(2) 0.035(2) 0.022(2) 0.0119(17) 0.0017(17) 0.0016(17) B9 0.027(2) 0.0189(18) 0.025(2) 0.0079(16) 0.0052(18) -0.0028(16) B10 0.026(2) 0.0259(19) 0.018(2) 0.0105(15) 0.0046(18) 0.0085(17) B11 0.021(2) 0.0262(19) 0.016(2) 0.0045(15) -0.0031(16) 0.0002(16) C3 0.0186(18) 0.0335(18) 0.0155(19) 0.0064(14) -0.0054(15) -0.0048(14) C4 0.025(2) 0.0296(19) 0.0226(19) -0.0031(14) -0.0025(16) -0.0092(15) C5 0.035(2) 0.0347(19) 0.028(2) -0.0015(17) -0.0002(19) -0.0180(17) C6 0.023(2) 0.062(3) 0.0197(19) 0.008(2) -0.0032(18) -0.0275(18) C7 0.015(2) 0.070(3) 0.031(3) 0.016(2) -0.0032(17) -0.0082(19) C8 0.020(2) 0.046(2) 0.029(2) 0.0169(17) -0.0014(16) -0.0039(16) C11 0.0202(19) 0.0255(17) 0.0162(19) -0.0009(14) -0.0031(15) 0.0010(14) O11 0.0405(18) 0.0555(17) 0.0218(17) -0.0020(14) 0.0130(14) 0.0030(15) C12 0.0132(17) 0.0275(17) 0.022(2) 0.0062(14) 0.0013(14) 0.0003(13) O12 0.0326(17) 0.0169(13) 0.073(2) 0.0176(13) 0.0100(15) 0.0011(11) C13 0.025(2) 0.0324(19) 0.024(2) -0.0051(16) 0.0059(17) -0.0034(15) O13 0.0221(15) 0.087(2) 0.0242(16) -0.0241(16) -0.0008(13) -0.0086(15) C14 0.0155(17) 0.0278(17) 0.0227(19) 0.0009(15) -0.0014(15) -0.0023(13) O14 0.0389(17) 0.0224(13) 0.0445(19) 0.0031(12) 0.0027(14) 0.0050(11) C15 0.028(2) 0.046(2) 0.030(2) -0.0112(19) -0.0015(19) 0.0120(18) O15 0.0376(19) 0.090(3) 0.044(2) -0.0329(19) -0.0286(17) 0.0287(17) C16 0.0211(19) 0.0171(15) 0.025(2) -0.0040(13) -0.0040(16) -0.0008(13) O16 0.0186(14) 0.0303(14) 0.0346(16) -0.0068(11) 0.0070(12) -0.0056(11) Mo1A 0.01712(14) 0.01146(11) 0.01243(13) -0.00091(10) 0.00110(12) -0.00015(10) Mo2A 0.01245(14) 0.02016(13) 0.02185(15) -0.00572(12) -0.00167(13) -0.00067(11) C2A 0.0176(17) 0.0130(14) 0.0203(19) -0.0067(12) 0.0051(14) -0.0020(12) B3A 0.0160(19) 0.0145(16) 0.017(2) -0.0019(14) -0.0018(15) 0.0016(13) B4A 0.021(2) 0.0138(16) 0.019(2) -0.0041(14) 0.0044(17) -0.0045(14) B5A 0.0138(19) 0.0173(17) 0.019(2) -0.0019(14) -0.0040(16) -0.0019(14) B6A 0.019(2) 0.0161(16) 0.0146(19) -0.0015(14) -0.0010(16) -0.0015(14) B7A 0.027(2) 0.0119(15) 0.017(2) -0.0027(14) 0.0014(17) 0.0039(14) B8A 0.0146(19) 0.0156(17) 0.023(2) -0.0027(15) -0.0018(16) -0.0015(13) B9A 0.020(2) 0.0173(17) 0.016(2) -0.0026(14) -0.0011(16) 0.0013(14) B10A 0.020(2) 0.0119(15) 0.022(2) -0.0036(14) 0.0057(17) -0.0034(14) B11A 0.020(2) 0.0172(17) 0.0145(19) -0.0022(14) -0.0001(16) -0.0019(14) C11A 0.026(2) 0.0166(15) 0.026(2) -0.0016(14) 0.0013(16) -0.0055(14) O11A 0.0490(19) 0.0430(17) 0.0309(17) -0.0080(13) 0.0215(15) -0.0067(14) C12A 0.0113(15) 0.0188(14) 0.0157(16) -0.0014(14) 0.0006(15) 0.0000(11) O12A 0.0263(13) 0.0150(10) 0.0265(13) -0.0022(11) -0.0050(12) -0.0007(9) C13A 0.038(2) 0.0154(16) 0.0181(19) -0.0015(13) 0.0027(17) 0.0050(14) O13A 0.0455(17) 0.0366(14) 0.0217(14) -0.0060(12) -0.0167(14) 0.0147(13) C14A 0.0155(18) 0.0326(19) 0.024(2) -0.0024(15) -0.0049(14) -0.0057(14) O14A 0.0398(18) 0.0297(14) 0.0358(17) 0.0025(12) -0.0005(14) -0.0125(12) C15A 0.0196(19) 0.0281(17) 0.031(2) -0.0110(16) -0.0021(18) 0.0023(14) O15A 0.0282(16) 0.0483(17) 0.0447(19) -0.0190(14) -0.0162(14) 0.0071(13) C16A 0.020(2) 0.036(2) 0.037(2) -0.0103(17) 0.0081(18) -0.0067(16) O16A 0.0309(18) 0.060(2) 0.063(2) -0.0163(17) 0.0175(17) -0.0081(15) N1 0.0166(14) 0.0142(12) 0.0163(14) -0.0006(11) -0.0040(12) -0.0015(10) C21 0.035(2) 0.0277(17) 0.0151(18) 0.0036(14) -0.0077(17) -0.0081(15) C22 0.042(2) 0.0285(18) 0.021(2) 0.0080(15) -0.0091(18) -0.0057(17) C23 0.0231(19) 0.0221(16) 0.0193(18) 0.0061(13) 0.0001(15) -0.0029(13) C24 0.021(2) 0.0313(19) 0.042(3) 0.0115(18) -0.0018(18) -0.0112(15) C25 0.0232(19) 0.0167(15) 0.029(2) 0.0041(14) 0.0013(16) -0.0005(13) C26 0.042(3) 0.0258(18) 0.026(2) -0.0029(15) 0.0060(19) -0.0036(17) C27 0.0163(17) 0.0228(16) 0.027(2) 0.0022(15) 0.0046(16) -0.0052(13) C28 0.017(2) 0.034(2) 0.057(3) 0.0004(19) 0.0107(19) 0.0037(16) N2 0.0210(16) 0.0173(13) 0.0187(15) -0.0028(11) 0.0023(12) -0.0004(11) C31 0.0208(19) 0.0233(17) 0.025(2) -0.0018(14) -0.0007(15) -0.0052(13) C32 0.026(2) 0.065(3) 0.038(3) 0.016(2) 0.0011(19) -0.012(2) C33 0.030(2) 0.0172(16) 0.028(2) -0.0067(14) -0.0035(17) 0.0025(14) C34 0.043(2) 0.0195(17) 0.036(2) 0.0035(16) -0.004(2) 0.0033(15) C35 0.0213(19) 0.0216(16) 0.024(2) 0.0029(14) 0.0085(15) 0.0011(13) C36 0.026(2) 0.047(2) 0.041(3) 0.019(2) -0.0016(19) -0.0013(18) C37 0.032(2) 0.0183(16) 0.0198(19) 0.0007(13) 0.0044(16) -0.0020(14) C38 0.036(2) 0.0201(17) 0.029(2) 0.0000(15) 0.0025(18) 0.0007(15) N3 0.0155(15) 0.0147(12) 0.0123(13) 0.0012(10) 0.0003(11) -0.0033(10) C41 0.0254(19) 0.0115(14) 0.027(2) 0.0002(13) 0.0067(16) -0.0015(13) C42 0.036(2) 0.0303(19) 0.032(2) -0.0111(17) 0.0105(19) 0.0019(17) C43 0.028(2) 0.0156(15) 0.0189(18) 0.0025(13) -0.0027(15) -0.0055(13) C44 0.024(2) 0.0310(19) 0.029(2) 0.0011(16) 0.0052(17) -0.0123(16) C45 0.0229(18) 0.0238(16) 0.0119(16) -0.0048(14) -0.0010(15) 0.0011(13) C46 0.041(3) 0.035(2) 0.0159(19) -0.0006(15) 0.0038(17) -0.0139(18) C47 0.0198(19) 0.0341(19) 0.0174(19) 0.0010(15) -0.0080(15) -0.0049(15) C48 0.023(2) 0.047(2) 0.040(3) 0.002(2) -0.0028(19) 0.0049(18) N4 0.0210(16) 0.0312(16) 0.0185(16) 0.0007(13) -0.0018(13) 0.0002(13) C51 0.019(3) 0.056(3) 0.030(3) 0.003(2) 0.004(2) 0.012(2) C53 0.041(3) 0.044(3) 0.021(3) 0.006(2) -0.014(2) -0.025(2) C55 0.030(3) 0.027(2) 0.017(2) 0.0012(18) -0.003(2) 0.0007(19) C57 0.022(2) 0.023(2) 0.020(2) 0.0024(18) 0.0026(19) -0.0022(18) C52 0.060(3) 0.061(3) 0.031(3) -0.003(2) 0.012(2) 0.030(2) C54 0.062(4) 0.067(4) 0.080(5) 0.013(3) -0.014(3) -0.041(3) C56 0.047(3) 0.038(2) 0.058(3) 0.015(2) 0.011(3) 0.020(2) C58 0.034(2) 0.034(2) 0.031(2) 0.0074(17) -0.0030(19) 0.0023(17) C51' 0.019(3) 0.056(3) 0.030(3) 0.003(2) 0.004(2) 0.012(2) C53' 0.041(3) 0.044(3) 0.021(3) 0.006(2) -0.014(2) -0.025(2) C55' 0.030(3) 0.027(2) 0.017(2) 0.0012(18) -0.003(2) 0.0007(19) C57' 0.022(2) 0.023(2) 0.020(2) 0.0024(18) 0.0026(19) -0.0022(18) C52' 0.060(3) 0.061(3) 0.031(3) -0.003(2) 0.012(2) 0.030(2) C54' 0.062(4) 0.067(4) 0.080(5) 0.013(3) -0.014(3) -0.041(3) C56' 0.047(3) 0.038(2) 0.058(3) 0.015(2) 0.011(3) 0.020(2) C58' 0.034(2) 0.034(2) 0.031(2) 0.0074(17) -0.0030(19) 0.0023(17) N5 0.019(2) 0.096(3) 0.051(3) -0.035(2) -0.0013(18) -0.021(2) C61 0.028(3) 0.060(4) 0.047(4) -0.018(3) -0.012(3) 0.020(3) C63 0.043(4) 0.040(3) 0.038(4) -0.002(3) -0.009(3) 0.002(3) C65 0.042(4) 0.046(3) 0.036(3) -0.003(3) 0.007(3) -0.024(3) C67 0.051(4) 0.055(4) 0.033(4) -0.013(3) 0.021(3) -0.024(3) C62 0.055(4) 0.036(3) 0.076(5) -0.006(4) -0.003(5) -0.019(3) C64 0.067(5) 0.073(5) 0.033(4) 0.007(4) -0.001(4) -0.012(4) C66 0.036(4) 0.088(13) 0.028(6) 0.014(6) -0.003(4) -0.032(7) C68 0.055(5) 0.065(4) 0.045(5) -0.006(3) -0.004(3) 0.000(3) C61' 0.028(3) 0.060(4) 0.047(4) -0.018(3) -0.012(3) 0.020(3) C62' 0.055(4) 0.036(3) 0.076(5) -0.006(4) -0.003(5) -0.019(3) C63' 0.043(4) 0.040(3) 0.038(4) -0.002(3) -0.009(3) 0.002(3) C65' 0.042(4) 0.046(3) 0.036(3) -0.003(3) 0.007(3) -0.024(3) C67' 0.051(4) 0.055(4) 0.033(4) -0.013(3) 0.021(3) -0.024(3) C64' 0.067(5) 0.073(5) 0.033(4) 0.007(4) -0.001(4) -0.012(4) C66' 0.036(4) 0.088(13) 0.028(6) 0.014(6) -0.003(4) -0.032(7) C68' 0.055(5) 0.065(4) 0.045(5) -0.006(3) -0.004(3) 0.000(3) N6 0.025(4) 0.0142(16) 0.018(4) 0.001(2) 0.000(2) 0.003(3) C71 0.033(3) 0.025(2) 0.025(3) -0.001(2) 0.001(2) -0.004(2) C72 0.040(3) 0.021(4) 0.042(6) -0.010(3) 0.004(4) -0.009(3) C73 0.021(3) 0.019(2) 0.023(3) 0.0053(19) 0.001(2) 0.0017(19) C74 0.026(3) 0.031(3) 0.028(3) 0.006(2) 0.006(2) 0.005(2) C77 0.015(3) 0.030(3) 0.025(3) 0.009(2) -0.002(3) -0.002(2) C78 0.019(3) 0.029(3) 0.035(4) 0.001(2) 0.004(2) -0.002(2) C76 0.040(5) 0.025(3) 0.042(5) -0.003(3) -0.008(3) -0.007(3) C75 0.025(3) 0.022(2) 0.020(3) -0.0007(19) -0.007(2) 0.003(2) N6' 0.025(4) 0.0142(16) 0.018(4) 0.001(2) 0.000(2) 0.003(3) C71' 0.033(3) 0.025(2) 0.025(3) -0.001(2) 0.001(2) -0.004(2) C72' 0.040(3) 0.021(4) 0.042(6) -0.010(3) 0.004(4) -0.009(3) C73' 0.021(3) 0.019(2) 0.023(3) 0.0053(19) 0.001(2) 0.0017(19) C74' 0.026(3) 0.031(3) 0.028(3) 0.006(2) 0.006(2) 0.005(2) C75' 0.025(3) 0.022(2) 0.020(3) -0.0007(19) -0.007(2) 0.003(2) C76' 0.040(5) 0.025(3) 0.042(5) -0.003(3) -0.008(3) -0.007(3) C77' 0.015(3) 0.030(3) 0.025(3) 0.009(2) -0.002(3) -0.002(2) C78' 0.019(3) 0.029(3) 0.035(4) 0.001(2) 0.004(2) -0.002(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 C12 1.950(3) . ? Mo1 C13 1.979(4) . ? Mo1 C11 1.997(4) . ? Mo1 B3 2.247(4) . ? Mo1 C2 2.263(3) . ? Mo1 B6 2.497(4) . ? Mo1 B5 2.529(4) . ? Mo1 B4 2.545(4) . ? Mo1 B7 2.598(4) . ? Mo1 Mo2 3.1212(4) . ? Mo2 C16 1.921(4) . ? Mo2 C14 1.926(3) . ? Mo2 C15 1.928(4) . ? Mo2 H3 2.06(3) . ? Mo2 H6 2.17(4) . ? Mo2 B3 2.399(4) . ? Mo2 B6 2.490(4) . ? C2 C3 1.486(5) . ? C2 B5 1.596(5) . ? C2 B4 1.641(5) . ? C2 B8 1.669(5) . ? B3 H3 1.20(4) . ? B3 B6 1.696(5) . ? B3 B7 1.710(5) . ? B3 B9 1.746(6) . ? B4 B10 1.806(6) . ? B4 B8 1.838(7) . ? B4 B7 1.873(5) . ? B5 B8 1.817(6) . ? B5 B11 1.821(5) . ? B5 B6 1.888(6) . ? B6 H6 1.156(18) . ? B6 B11 1.807(6) . ? B6 B9 1.830(5) . ? B7 B10 1.780(6) . ? B7 B9 1.843(6) . ? B8 B10 1.753(6) . ? B8 B11 1.755(6) . ? B9 B10 1.751(6) . ? B9 B11 1.778(6) . ? B10 B11 1.856(6) . ? C3 C4 1.393(5) . ? C3 C8 1.394(5) . ? C4 C5 1.395(5) . ? C5 C6 1.394(6) . ? C6 C7 1.387(6) . ? C7 C8 1.411(5) . ? C11 O11 1.156(4) . ? C12 O12 1.184(4) . ? C13 O13 1.168(5) . ? C14 O14 1.186(4) . ? C15 O15 1.177(5) . ? C16 O16 1.187(4) . ? Mo1A C12A 1.946(3) . ? Mo1A C13A 1.976(4) . ? Mo1A C11A 1.996(4) . ? Mo1A B3A 2.262(4) . ? Mo1A C2A 2.268(3) . ? Mo1A B6A 2.474(4) . ? Mo1A B5A 2.522(4) . ? Mo1A B4A 2.576(4) . ? Mo1A B7A 2.635(3) . ? Mo1A Mo2A 3.1801(5) . ? Mo2A C16A 1.922(4) . ? Mo2A C14A 1.925(4) . ? Mo2A C15A 1.937(4) . ? Mo2A H6A 2.02(4) . ? Mo2A H3A 2.16(3) . ? Mo2A B3A 2.438(4) . ? Mo2A B6A 2.451(4) . ? C2A C10A 1.522(4) . ? C2A C102 1.556(5) . ? C2A B5A 1.597(5) . ? C2A B4A 1.607(5) . ? C2A B8A 1.671(5) . ? B3A H3A 1.24(3) . ? B3A B7A 1.680(5) . ? B3A B6A 1.711(5) . ? B3A B9A 1.717(5) . ? B4A B10A 1.824(5) . ? B4A B8A 1.825(6) . ? B4A B7A 1.879(6) . ? B5A B11A 1.811(5) . ? B5A B8A 1.821(5) . ? B5A B6A 1.868(6) . ? B6A H6A 1.26(4) . ? B6A B11A 1.773(5) . ? B6A B9A 1.811(5) . ? B7A B10A 1.807(6) . ? B7A B9A 1.820(6) . ? B8A B10A 1.762(5) . ? B8A B11A 1.765(6) . ? B9A B10A 1.745(6) . ? B9A B11A 1.766(5) . ? B10A B11A 1.848(5) . ? C11A O11A 1.161(5) . ? C12A O12A 1.181(3) . ? C13A O13A 1.173(5) . ? C14A O14A 1.168(4) . ? C15A O15A 1.171(4) . ? C16A O16A 1.180(5) . ? C102 C103 1.3900 . ? C102 C107 1.3900 . ? C103 C104 1.3900 . ? C104 C105 1.3900 . ? C105 C106 1.3900 . ? C106 C107 1.3900 . ? C10A C10B 1.3900 . ? C10A C10F 1.3900 . ? C10B C10C 1.3900 . ? C10C C10D 1.3900 . ? C10D C10E 1.3900 . ? C10E C10F 1.3900 . ? N1 C27 1.505(4) . ? N1 C21 1.5241 . ? N1 C23 1.528(4) . ? N1 C25 1.533(4) . ? C21 C22 1.491(4) . ? C23 C24 1.485(5) . ? C25 C26 1.528(5) . ? C27 C28 1.531(5) . ? N2 C33 1.511(4) . ? N2 C31 1.517(4) . ? N2 C37 1.531(4) . ? N2 C35 1.542(4) . ? C31 C32 1.497(6) . ? C33 C34 1.508(5) . ? C35 C36 1.522(5) . ? C37 C38 1.515(4) . ? N3 C41 1.516(4) . ? N3 C43 1.526(4) . ? N3 C47 1.528(4) . ? N3 C45 1.533(5) . ? C41 C42 1.528(5) . ? C43 C44 1.508(5) . ? C45 C46 1.513(5) . ? C47 C48 1.502(5) . ? N4 C51' 1.430(15) . ? N4 C55' 1.508(12) . ? N4 C53 1.514(6) . ? N4 C57 1.519(6) . ? N4 C51 1.530(6) . ? N4 C55 1.550(6) . ? N4 C53' 1.578(12) . ? N4 C57' 1.626(12) . ? C51 C52 1.446(8) . ? C53 C54 1.452(7) . ? C55 C56 1.526(7) . ? C57 C58 1.523(6) . ? N5 C61 1.382(8) . ? N5 C67' 1.434(12) . ? N5 C63' 1.487(13) . ? N5 C67 1.499(8) . ? N5 C65 1.502(7) . ? N5 C65' 1.512(13) . ? N5 C63 1.707(9) . ? N5 C61' 1.828(12) . ? C61 C62 1.597(10) . ? C63 C64 1.530(11) . ? C65 C66 1.37(2) . ? C67 C68 1.505(10) . ? C61' C62' 1.514(18) . ? C63' C64' 1.54(2) . ? C65' C66' 1.79(3) . ? C67' C68' 1.579(19) . ? N6 C71 1.506(11) . ? N6 C75 1.533(9) . ? N6 C73 1.554(10) . ? N6 C77 1.555(11) . ? C71 C72 1.524(11) . ? C73 C74 1.486(10) . ? C77 C78 1.505(11) . ? C76 C75 1.508(12) . ? N6' C77' 1.500(10) . ? N6' C73' 1.504(10) . ? N6' C75' 1.509(10) . ? N6' C71' 1.530(10) . ? C71' C72' 1.491(13) . ? C73' C74' 1.545(10) . ? C75' C76' 1.489(11) . ? C77' C78' 1.536(11) . ? 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 C12 Mo1 C13 91.03(15) . . ? C12 Mo1 C11 92.98(14) . . ? C13 Mo1 C11 81.91(15) . . ? C12 Mo1 B3 126.59(14) . . ? C13 Mo1 B3 81.37(15) . . ? C11 Mo1 B3 137.00(14) . . ? C12 Mo1 C2 100.22(13) . . ? C13 Mo1 C2 161.76(14) . . ? C11 Mo1 C2 83.20(14) . . ? B3 Mo1 C2 102.77(13) . . ? C12 Mo1 B6 99.86(14) . . ? C13 Mo1 B6 114.53(14) . . ? C11 Mo1 B6 158.69(13) . . ? B3 Mo1 B6 41.49(13) . . ? C2 Mo1 B6 77.86(12) . . ? C12 Mo1 B5 88.08(14) . . ? C13 Mo1 B5 157.82(14) . . ? C11 Mo1 B5 120.27(14) . . ? B3 Mo1 B5 81.42(13) . . ? C2 Mo1 B5 38.40(13) . . ? B6 Mo1 B5 44.12(12) . . ? C12 Mo1 B4 139.22(14) . . ? C13 Mo1 B4 126.64(15) . . ? C11 Mo1 B4 79.41(14) . . ? B3 Mo1 B4 79.48(13) . . ? C2 Mo1 B4 39.36(12) . . ? B6 Mo1 B4 79.76(14) . . ? B5 Mo1 B4 63.12(14) . . ? C12 Mo1 B7 163.74(14) . . ? C13 Mo1 B7 95.38(15) . . ? C11 Mo1 B7 102.69(13) . . ? B3 Mo1 B7 40.54(13) . . ? C2 Mo1 B7 77.69(12) . . ? B6 Mo1 B7 63.89(12) . . ? B5 Mo1 B7 80.36(13) . . ? B4 Mo1 B7 42.69(12) . . ? C12 Mo1 Mo2 77.84(10) . . ? C13 Mo1 Mo2 69.39(11) . . ? C11 Mo1 Mo2 149.48(10) . . ? B3 Mo1 Mo2 49.90(10) . . ? C2 Mo1 Mo2 126.86(8) . . ? B6 Mo1 Mo2 51.15(9) . . ? B5 Mo1 Mo2 88.80(9) . . ? B4 Mo1 Mo2 126.03(10) . . ? B7 Mo1 Mo2 90.44(9) . . ? C16 Mo2 C14 87.22(14) . . ? C16 Mo2 C15 83.41(18) . . ? C14 Mo2 C15 87.01(17) . . ? C16 Mo2 H3 94.2(10) . . ? C14 Mo2 H3 178.6(10) . . ? C15 Mo2 H3 93.3(11) . . ? C16 Mo2 H6 94.4(7) . . ? C14 Mo2 H6 91.6(7) . . ? C15 Mo2 H6 177.5(5) . . ? H3 Mo2 H6 88.1(13) . . ? C16 Mo2 B3 114.27(13) . . ? C14 Mo2 B3 148.79(13) . . ? C15 Mo2 B3 116.51(15) . . ? H3 Mo2 B3 30.1(10) . . ? H6 Mo2 B3 65.6(6) . . ? C16 Mo2 B6 113.64(14) . . ? C14 Mo2 B6 111.22(13) . . ? C15 Mo2 B6 154.82(15) . . ? H3 Mo2 B6 68.0(10) . . ? H6 Mo2 B6 27.6(5) . . ? B3 Mo2 B6 40.55(12) . . ? C16 Mo2 Mo1 159.87(10) . . ? C14 Mo2 Mo1 110.10(10) . . ? C15 Mo2 Mo1 106.97(13) . . ? H3 Mo2 Mo1 68.5(10) . . ? H6 Mo2 Mo1 75.5(6) . . ? B3 Mo2 Mo1 45.76(9) . . ? B6 Mo2 Mo1 51.35(9) . . ? C3 C2 B5 123.3(3) . . ? C3 C2 B4 124.1(3) . . ? B5 C2 B4 110.3(3) . . ? C3 C2 B8 117.9(3) . . ? B5 C2 B8 67.6(2) . . ? B4 C2 B8 67.4(3) . . ? C3 C2 Mo1 122.3(2) . . ? B5 C2 Mo1 79.8(2) . . ? B4 C2 Mo1 79.63(19) . . ? B8 C2 Mo1 119.9(2) . . ? H3 B3 B6 123.9(17) . . ? H3 B3 B7 129.2(17) . . ? B6 B3 B7 104.7(3) . . ? H3 B3 B9 122.2(18) . . ? B6 B3 B9 64.2(2) . . ? B7 B3 B9 64.5(2) . . ? H3 B3 Mo1 120.8(17) . . ? B6 B3 Mo1 77.18(19) . . ? B7 B3 Mo1 80.83(19) . . ? B9 B3 Mo1 116.6(2) . . ? H3 B3 Mo2 59.0(16) . . ? B6 B3 Mo2 72.60(18) . . ? B7 B3 Mo2 165.1(2) . . ? B9 B3 Mo2 124.2(2) . . ? Mo1 B3 Mo2 84.34(12) . . ? C2 B4 B10 108.1(3) . . ? C2 B4 B8 57.0(2) . . ? B10 B4 B8 57.5(2) . . ? C2 B4 B7 121.0(3) . . ? B10 B4 B7 57.8(2) . . ? B8 B4 B7 106.6(3) . . ? C2 B4 Mo1 61.01(16) . . ? B10 B4 Mo1 108.1(2) . . ? B8 B4 Mo1 101.2(2) . . ? B7 B4 Mo1 70.15(17) . . ? C2 B5 B8 58.1(2) . . ? C2 B5 B11 109.6(3) . . ? B8 B5 B11 57.7(2) . . ? C2 B5 B6 118.4(3) . . ? B8 B5 B6 105.3(3) . . ? B11 B5 B6 58.3(2) . . ? C2 B5 Mo1 61.76(18) . . ? B8 B5 Mo1 102.4(2) . . ? B11 B5 Mo1 108.6(2) . . ? B6 B5 Mo1 67.04(17) . . ? H6 B6 B3 119.6(18) . . ? H6 B6 B11 115.3(18) . . ? B3 B6 B11 112.0(3) . . ? H6 B6 B9 123.0(18) . . ? B3 B6 B9 59.2(2) . . ? B11 B6 B9 58.5(2) . . ? H6 B6 B5 114.7(18) . . ? B3 B6 B5 121.1(3) . . ? B11 B6 B5 59.0(2) . . ? B9 B6 B5 107.2(3) . . ? H6 B6 Mo2 60.4(18) . . ? B3 B6 Mo2 66.85(18) . . ? B11 B6 Mo2 170.7(3) . . ? B9 B6 Mo2 115.7(2) . . ? B5 B6 Mo2 130.0(2) . . ? H6 B6 Mo1 127.1(18) . . ? B3 B6 Mo1 61.33(18) . . ? B11 B6 Mo1 110.4(2) . . ? B9 B6 Mo1 102.8(2) . . ? B5 B6 Mo1 68.84(17) . . ? Mo2 B6 Mo1 77.50(12) . . ? B3 B7 B10 110.1(3) . . ? B3 B7 B9 58.7(2) . . ? B10 B7 B9 57.8(2) . . ? B3 B7 B4 118.0(3) . . ? B10 B7 B4 59.2(2) . . ? B9 B7 B4 106.1(3) . . ? B3 B7 Mo1 58.64(16) . . ? B10 B7 Mo1 106.8(2) . . ? B9 B7 Mo1 98.82(19) . . ? B4 B7 Mo1 67.16(16) . . ? C2 B8 B10 109.4(3) . . ? C2 B8 B11 109.3(3) . . ? B10 B8 B11 63.9(2) . . ? C2 B8 B5 54.3(2) . . ? B10 B8 B5 106.3(3) . . ? B11 B8 B5 61.3(2) . . ? C2 B8 B4 55.6(2) . . ? B10 B8 B4 60.3(2) . . ? B11 B8 B4 106.3(3) . . ? B5 B8 B4 93.2(3) . . ? B3 B9 B10 109.8(3) . . ? B3 B9 B11 111.0(3) . . ? B10 B9 B11 63.5(2) . . ? B3 B9 B6 56.6(2) . . ? B10 B9 B6 104.6(3) . . ? B11 B9 B6 60.1(2) . . ? B3 B9 B7 56.8(2) . . ? B10 B9 B7 59.3(2) . . ? B11 B9 B7 106.3(3) . . ? B6 B9 B7 94.5(3) . . ? B9 B10 B8 112.3(3) . . ? B9 B10 B7 62.9(2) . . ? B8 B10 B7 114.7(3) . . ? B9 B10 B4 113.2(3) . . ? B8 B10 B4 62.2(2) . . ? B7 B10 B4 63.0(2) . . ? B9 B10 B11 59.0(2) . . ? B8 B10 B11 58.1(2) . . ? B7 B10 B11 105.7(3) . . ? B4 B10 B11 103.5(3) . . ? B8 B11 B9 110.9(3) . . ? B8 B11 B6 111.6(3) . . ? B9 B11 B6 61.4(2) . . ? B8 B11 B5 61.1(2) . . ? B9 B11 B5 112.5(3) . . ? B6 B11 B5 62.7(2) . . ? B8 B11 B10 58.0(2) . . ? B9 B11 B10 57.6(2) . . ? B6 B11 B10 101.4(3) . . ? B5 B11 B10 102.0(3) . . ? C4 C3 C8 117.1(3) . . ? C4 C3 C2 121.8(3) . . ? C8 C3 C2 121.2(3) . . ? C3 C4 C5 122.0(4) . . ? C6 C5 C4 119.9(4) . . ? C7 C6 C5 119.7(3) . . ? C6 C7 C8 119.2(4) . . ? C3 C8 C7 122.1(4) . . ? O11 C11 Mo1 175.5(3) . . ? O12 C12 Mo1 177.9(3) . . ? O13 C13 Mo1 173.9(3) . . ? O14 C14 Mo2 178.2(3) . . ? O15 C15 Mo2 176.7(4) . . ? O16 C16 Mo2 177.1(3) . . ? C12A Mo1A C13A 90.19(14) . . ? C12A Mo1A C11A 86.62(14) . . ? C13A Mo1A C11A 84.33(16) . . ? C12A Mo1A B3A 123.70(13) . . ? C13A Mo1A B3A 79.90(14) . . ? C11A Mo1A B3A 145.46(14) . . ? C12A Mo1A C2A 104.67(12) . . ? C13A Mo1A C2A 160.43(14) . . ? C11A Mo1A C2A 83.93(14) . . ? B3A Mo1A C2A 101.45(12) . . ? C12A Mo1A B6A 97.95(13) . . ? C13A Mo1A B6A 113.78(14) . . ? C11A Mo1A B6A 161.17(14) . . ? B3A Mo1A B6A 42.05(13) . . ? C2A Mo1A B6A 77.25(12) . . ? C12A Mo1A B5A 89.25(13) . . ? C13A Mo1A B5A 157.21(14) . . ? C11A Mo1A B5A 118.37(15) . . ? B3A Mo1A B5A 81.50(13) . . ? C2A Mo1A B5A 38.49(12) . . ? B6A Mo1A B5A 43.90(13) . . ? C12A Mo1A B4A 142.69(13) . . ? C13A Mo1A B4A 125.61(13) . . ? C11A Mo1A B4A 86.96(13) . . ? B3A Mo1A B4A 77.85(13) . . ? C2A Mo1A B4A 38.07(11) . . ? B6A Mo1A B4A 78.33(13) . . ? B5A Mo1A B4A 62.14(12) . . ? C12A Mo1A B7A 160.65(14) . . ? C13A Mo1A B7A 93.86(13) . . ? C11A Mo1A B7A 112.60(13) . . ? B3A Mo1A B7A 39.22(13) . . ? C2A Mo1A B7A 76.38(12) . . ? B6A Mo1A B7A 63.15(12) . . ? B5A Mo1A B7A 79.75(12) . . ? B4A Mo1A B7A 42.25(12) . . ? C12A Mo1A Mo2A 74.47(9) . . ? C13A Mo1A Mo2A 70.90(11) . . ? C11A Mo1A Mo2A 148.38(11) . . ? B3A Mo1A Mo2A 49.80(10) . . ? C2A Mo1A Mo2A 124.92(8) . . ? B6A Mo1A Mo2A 49.47(9) . . ? B5A Mo1A Mo2A 87.03(9) . . ? B4A Mo1A Mo2A 123.29(9) . . ? B7A Mo1A Mo2A 88.99(9) . . ? C16A Mo2A C14A 84.95(16) . . ? C16A Mo2A C15A 86.78(17) . . ? C14A Mo2A C15A 86.54(15) . . ? C16A Mo2A H6A 86.1(11) . . ? C14A Mo2A H6A 91.1(10) . . ? C15A Mo2A H6A 172.6(11) . . ? C16A Mo2A H3A 96.2(9) . . ? C14A Mo2A H3A 178.5(10) . . ? C15A Mo2A H3A 92.6(10) . . ? H6A Mo2A H3A 89.9(14) . . ? C16A Mo2A B3A 114.95(14) . . ? C14A Mo2A B3A 149.49(14) . . ? C15A Mo2A B3A 116.03(15) . . ? H6A Mo2A B3A 68.8(10) . . ? H3A Mo2A B3A 30.4(9) . . ? C16A Mo2A B6A 109.36(15) . . ? C14A Mo2A B6A 112.31(14) . . ? C15A Mo2A B6A 155.63(15) . . ? H6A Mo2A B6A 30.8(10) . . ? H3A Mo2A B6A 68.2(10) . . ? B3A Mo2A B6A 40.97(12) . . ? C16A Mo2A Mo1A 157.74(12) . . ? C14A Mo2A Mo1A 109.64(11) . . ? C15A Mo2A Mo1A 110.17(12) . . ? H6A Mo2A Mo1A 77.2(11) . . ? H3A Mo2A Mo1A 69.5(9) . . ? B3A Mo2A Mo1A 45.13(9) . . ? B6A Mo2A Mo1A 50.11(9) . . ? C10A C2A C102 12.8(3) . . ? C10A C2A B5A 126.4(3) . . ? C102 C2A B5A 115.5(3) . . ? C10A C2A B4A 121.3(3) . . ? C102 C2A B4A 128.6(3) . . ? B5A C2A B4A 110.5(3) . . ? C10A C2A B8A 119.1(3) . . ? C102 C2A B8A 110.2(3) . . ? B5A C2A B8A 67.7(2) . . ? B4A C2A B8A 67.6(2) . . ? C10A C2A Mo1A 119.6(2) . . ? C102 C2A Mo1A 127.9(2) . . ? B5A C2A Mo1A 79.38(19) . . ? B4A C2A Mo1A 81.4(2) . . ? B8A C2A Mo1A 121.2(2) . . ? H3A B3A B7A 128.3(17) . . ? H3A B3A B6A 122.7(17) . . ? B7A B3A B6A 104.3(3) . . ? H3A B3A B9A 116.1(17) . . ? B7A B3A B9A 64.8(2) . . ? B6A B3A B9A 63.8(2) . . ? H3A B3A Mo1A 126.5(17) . . ? B7A B3A Mo1A 82.4(2) . . ? B6A B3A Mo1A 75.61(18) . . ? B9A B3A Mo1A 116.7(2) . . ? H3A B3A Mo2A 62.2(16) . . ? B7A B3A Mo2A 167.3(2) . . ? B6A B3A Mo2A 69.93(18) . . ? B9A B3A Mo2A 119.6(2) . . ? Mo1A B3A Mo2A 85.06(11) . . ? C2A B4A B10A 109.1(3) . . ? C2A B4A B8A 57.8(2) . . ? B10A B4A B8A 57.8(2) . . ? C2A B4A B7A 121.5(3) . . ? B10A B4A B7A 58.4(2) . . ? B8A B4A B7A 107.5(3) . . ? C2A B4A Mo1A 60.51(17) . . ? B10A B4A Mo1A 108.8(2) . . ? B8A B4A Mo1A 101.63(19) . . ? B7A B4A Mo1A 70.53(16) . . ? C2A B5A B11A 109.3(3) . . ? C2A B5A B8A 58.1(2) . . ? B11A B5A B8A 58.1(2) . . ? C2A B5A B6A 117.4(3) . . ? B11A B5A B6A 57.6(2) . . ? B8A B5A B6A 105.2(2) . . ? C2A B5A Mo1A 62.12(18) . . ? B11A B5A Mo1A 108.8(2) . . ? B8A B5A Mo1A 103.8(2) . . ? B6A B5A Mo1A 66.69(17) . . ? H6A B6A B3A 117.0(17) . . ? H6A B6A B11A 116.0(17) . . ? B3A B6A B11A 112.0(3) . . ? H6A B6A B9A 121.3(16) . . ? B3A B6A B9A 58.3(2) . . ? B11A B6A B9A 59.0(2) . . ? H6A B6A B5A 116.8(17) . . ? B3A B6A B5A 121.8(3) . . ? B11A B6A B5A 59.6(2) . . ? B9A B6A B5A 108.1(3) . . ? H6A B6A Mo2A 55.2(17) . . ? B3A B6A Mo2A 69.11(19) . . ? B11A B6A Mo2A 166.6(3) . . ? B9A B6A Mo2A 114.9(2) . . ? B5A B6A Mo2A 132.1(2) . . ? H6A B6A Mo1A 125.7(17) . . ? B3A B6A Mo1A 62.33(17) . . ? B11A B6A Mo1A 112.2(2) . . ? B9A B6A Mo1A 104.0(2) . . ? B5A B6A Mo1A 69.40(18) . . ? Mo2A B6A Mo1A 80.42(12) . . ? B3A B7A B10A 110.2(3) . . ? B3A B7A B9A 58.6(2) . . ? B10A B7A B9A 57.5(2) . . ? B3A B7A B4A 117.8(3) . . ? B10A B7A B4A 59.3(2) . . ? B9A B7A B4A 105.2(3) . . ? B3A B7A Mo1A 58.34(16) . . ? B10A B7A Mo1A 107.00(19) . . ? B9A B7A Mo1A 97.83(19) . . ? B4A B7A Mo1A 67.21(15) . . ? C2A B8A B10A 109.2(3) . . ? C2A B8A B11A 108.1(3) . . ? B10A B8A B11A 63.2(2) . . ? C2A B8A B5A 54.2(2) . . ? B10A B8A B5A 106.2(3) . . ? B11A B8A B5A 60.6(2) . . ? C2A B8A B4A 54.5(2) . . ? B10A B8A B4A 61.1(2) . . ? B11A B8A B4A 105.1(3) . . ? B5A B8A B4A 92.4(2) . . ? B3A B9A B10A 111.5(3) . . ? B3A B9A B11A 112.0(3) . . ? B10A B9A B11A 63.5(2) . . ? B3A B9A B6A 57.9(2) . . ? B10A B9A B6A 105.1(3) . . ? B11A B9A B6A 59.4(2) . . ? B3A B9A B7A 56.6(2) . . ? B10A B9A B7A 60.9(2) . . ? B11A B9A B7A 107.2(3) . . ? B6A B9A B7A 95.1(2) . . ? B9A B10A B8A 112.0(3) . . ? B9A B10A B7A 61.6(2) . . ? B8A B10A B7A 113.6(3) . . ? B9A B10A B4A 110.9(3) . . ? B8A B10A B4A 61.1(2) . . ? B7A B10A B4A 62.3(2) . . ? B9A B10A B11A 58.8(2) . . ? B8A B10A B11A 58.5(2) . . ? B7A B10A B11A 104.3(2) . . ? B4A B10A B11A 101.8(2) . . ? B8A B11A B9A 110.9(3) . . ? B8A B11A B6A 111.9(3) . . ? B9A B11A B6A 61.5(2) . . ? B8A B11A B5A 61.2(2) . . ? B9A B11A B5A 112.7(3) . . ? B6A B11A B5A 62.8(2) . . ? B8A B11A B10A 58.3(2) . . ? B9A B11A B10A 57.7(2) . . ? B6A B11A B10A 102.5(3) . . ? B5A B11A B10A 103.1(3) . . ? O11A C11A Mo1A 177.3(3) . . ? O12A C12A Mo1A 176.6(3) . . ? O13A C13A Mo1A 177.4(3) . . ? O14A C14A Mo2A 177.4(3) . . ? O15A C15A Mo2A 177.0(4) . . ? O16A C16A Mo2A 178.6(4) . . ? C103 C102 C107 120.0 . . ? C103 C102 C2A 119.2(3) . . ? C107 C102 C2A 120.6(3) . . ? C104 C103 C102 120.0 . . ? C103 C104 C105 120.0 . . ? C106 C105 C104 120.0 . . ? C107 C106 C105 120.0 . . ? C106 C107 C102 120.0 . . ? C10B C10A C10F 120.0 . . ? C10B C10A C2A 120.81(17) . . ? C10F C10A C2A 119.00(18) . . ? C10C C10B C10A 120.0 . . ? C10B C10C C10D 120.0 . . ? C10E C10D C10C 120.0 . . ? C10D C10E C10F 120.0 . . ? C10E C10F C10A 120.0 . . ? C27 N1 C21 111.96(19) . . ? C27 N1 C23 108.9(2) . . ? C21 N1 C23 109.03(17) . . ? C27 N1 C25 108.7(2) . . ? C21 N1 C25 107.5(2) . . ? C23 N1 C25 110.8(2) . . ? C22 C21 N1 116.43(18) . . ? C24 C23 N1 116.1(3) . . ? C26 C25 N1 114.1(3) . . ? N1 C27 C28 114.4(3) . . ? C33 N2 C31 111.2(3) . . ? C33 N2 C37 106.6(3) . . ? C31 N2 C37 111.6(3) . . ? C33 N2 C35 111.1(3) . . ? C31 N2 C35 106.4(3) . . ? C37 N2 C35 110.0(3) . . ? C32 C31 N2 115.0(3) . . ? C34 C33 N2 115.2(3) . . ? C36 C35 N2 115.7(3) . . ? C38 C37 N2 115.5(3) . . ? C41 N3 C43 111.2(2) . . ? C41 N3 C47 108.5(3) . . ? C43 N3 C47 108.2(3) . . ? C41 N3 C45 109.3(2) . . ? C43 N3 C45 108.0(2) . . ? C47 N3 C45 111.7(3) . . ? N3 C41 C42 114.6(3) . . ? C44 C43 N3 115.8(3) . . ? C46 C45 N3 115.6(3) . . ? C48 C47 N3 115.7(3) . . ? C51' N4 C55' 114.1(7) . . ? C51' N4 C53 164.7(7) . . ? C55' N4 C53 76.3(6) . . ? C51' N4 C57 84.6(6) . . ? C55' N4 C57 65.1(5) . . ? C53 N4 C57 110.5(4) . . ? C51' N4 C51 59.0(6) . . ? C55' N4 C51 172.7(6) . . ? C53 N4 C51 111.0(4) . . ? C57 N4 C51 110.4(4) . . ? C51' N4 C55 65.3(6) . . ? C55' N4 C55 70.1(5) . . ? C53 N4 C55 110.9(4) . . ? C57 N4 C55 107.1(3) . . ? C51 N4 C55 106.8(3) . . ? C51' N4 C53' 111.1(8) . . ? C55' N4 C53' 112.2(8) . . ? C53 N4 C53' 53.6(5) . . ? C57 N4 C53' 162.6(5) . . ? C51 N4 C53' 73.9(6) . . ? C55 N4 C53' 86.9(6) . . ? C51' N4 C57' 109.7(7) . . ? C55' N4 C57' 107.9(6) . . ? C53 N4 C57' 75.7(5) . . ? C57 N4 C57' 65.4(5) . . ? C51 N4 C57' 74.1(5) . . ? C55 N4 C57' 171.9(5) . . ? C53' N4 C57' 101.1(7) . . ? C52 C51 N4 118.7(4) . . ? C54 C53 N4 120.0(5) . . ? C56 C55 N4 112.1(4) . . ? N4 C57 C58 114.4(4) . . ? C61 N5 C67' 69.2(6) . . ? C61 N5 C63' 73.2(6) . . ? C67' N5 C63' 116.5(9) . . ? C61 N5 C67 122.2(5) . . ? C67' N5 C67 57.1(6) . . ? C63' N5 C67 148.8(7) . . ? C61 N5 C65 112.5(5) . . ? C67' N5 C65 162.5(8) . . ? C63' N5 C65 79.7(7) . . ? C67 N5 C65 112.8(5) . . ? C61 N5 C65' 145.0(7) . . ? C67' N5 C65' 119.9(8) . . ? C63' N5 C65' 120.4(8) . . ? C67 N5 C65' 64.5(6) . . ? C65 N5 C65' 48.4(5) . . ? C61 N5 C63 103.0(5) . . ? C67' N5 C63 93.2(7) . . ? C63' N5 C63 49.0(6) . . ? C67 N5 C63 99.8(5) . . ? C65 N5 C63 103.1(5) . . ? C65' N5 C63 109.7(6) . . ? C61 N5 C61' 56.5(5) . . ? C67' N5 C61' 101.7(8) . . ? C63' N5 C61' 97.6(7) . . ? C67 N5 C61' 113.6(6) . . ? C65 N5 C61' 68.0(6) . . ? C65' N5 C61' 88.8(7) . . ? C63 N5 C61' 146.4(6) . . ? N5 C61 C62 107.4(6) . . ? C64 C63 N5 113.6(6) . . ? C66 C65 N5 121.0(12) . . ? N5 C67 C68 115.5(6) . . ? C62' C61' N5 114.3(9) . . ? N5 C63' C64' 103.9(11) . . ? N5 C65' C66' 112.7(18) . . ? N5 C67' C68' 119.1(11) . . ? C71 N6 C75 106.4(6) . . ? C71 N6 C73 111.1(6) . . ? C75 N6 C73 109.9(6) . . ? C71 N6 C77 114.0(6) . . ? C75 N6 C77 108.7(6) . . ? C73 N6 C77 106.7(6) . . ? N6 C71 C72 113.5(7) . . ? C74 C73 N6 116.0(6) . . ? C78 C77 N6 115.5(7) . . ? C76 C75 N6 117.6(6) . . ? C77' N6' C73' 105.8(6) . . ? C77' N6' C75' 111.1(6) . . ? C73' N6' C75' 111.1(6) . . ? C77' N6' C71' 112.3(6) . . ? C73' N6' C71' 110.0(6) . . ? C75' N6' C71' 106.6(6) . . ? C72' C71' N6' 115.4(7) . . ? N6' C73' C74' 116.6(6) . . ? C76' C75' N6' 115.7(7) . . ? N6' C77' C78' 114.6(7) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.228 _refine_diff_density_min -0.843 _refine_diff_density_rms 0.121 #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 270994' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C8 H20 N), C36 H38 B9 Mo O3 P2 Pt, 0.5(C H2 Cl2) ' _chemical_formula_sum 'C44.5 H59 B9 Cl Mo N O3 P2 Pt' _chemical_formula_weight 1141.64 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting 'Monoclinic ' _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4426(9) _cell_length_b 22.8219(14) _cell_length_c 15.1963(10) _cell_angle_alpha 90.00 _cell_angle_beta 101.002(3) _cell_angle_gamma 90.00 _cell_volume 4916.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8482 _cell_measurement_theta_min 2.781 _cell_measurement_theta_max 34.000 _exptl_crystal_description needle _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2276 _exptl_absorpt_coefficient_mu 3.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5980 _exptl_absorpt_correction_T_max 0.7495 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 88217 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 35.74 _reflns_number_total 21411 _reflns_number_gt 17667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+1.7994P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21411 _refine_ls_number_parameters 599 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0607 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.818784(10) 0.299977(6) 0.606226(9) 0.01148(3) Uani 1 1 d . . . C2 C 0.87463(11) 0.37624(7) 0.68943(11) 0.0142(3) Uani 1 1 d . . . B3 B 0.68377(13) 0.27176(8) 0.65651(13) 0.0142(3) Uani 1 1 d . . . H3 H 0.6272(15) 0.2419(9) 0.6239(14) 0.017 Uiso 1 1 d . . . B4 B 0.76888(13) 0.39798(9) 0.64435(13) 0.0151(3) Uani 1 1 d . . . H4 H 0.7611 0.4341 0.5935 0.018 Uiso 1 1 calc R . . B5 B 0.86825(13) 0.32821(9) 0.76597(13) 0.0145(3) Uani 1 1 d . . . H5 H 0.9360 0.3110 0.8061 0.017 Uiso 1 1 calc R . . B6 B 0.76767(13) 0.27392(8) 0.75774(13) 0.0142(3) Uani 1 1 d . . . H6 H 0.7876(15) 0.2396(9) 0.8117(14) 0.017 Uiso 1 1 d . . . B7 B 0.66943(13) 0.34609(9) 0.63103(13) 0.0157(3) Uani 1 1 d . . . H7 H 0.6102 0.3563 0.5740 0.019 Uiso 1 1 calc R . . B8 B 0.81837(13) 0.40214(9) 0.76545(13) 0.0151(3) Uani 1 1 d . . . H8 H 0.8446 0.4412 0.8076 0.018 Uiso 1 1 calc R . . B9 B 0.66158(13) 0.31852(9) 0.74274(13) 0.0156(3) Uani 1 1 d . . . H9 H 0.5973 0.3100 0.7719 0.019 Uiso 1 1 calc R . . B10 B 0.69534(13) 0.39109(9) 0.72905(13) 0.0156(3) Uani 1 1 d . . . H10 H 0.6459 0.4269 0.7406 0.019 Uiso 1 1 calc R . . B11 B 0.76431(13) 0.34434(9) 0.81233(13) 0.0149(3) Uani 1 1 d . . . H11 H 0.7673 0.3459 0.8865 0.018 Uiso 1 1 calc R . . C3 C 0.96379(12) 0.40857(8) 0.68227(12) 0.0168(3) Uani 1 1 d . . . C4 C 1.05098(13) 0.39252(9) 0.73498(13) 0.0235(4) Uani 1 1 d . . . H4A H 1.0550 0.3586 0.7718 0.028 Uiso 1 1 calc R . . C5 C 1.13160(14) 0.42592(11) 0.73371(15) 0.0315(5) Uani 1 1 d . . . H5A H 1.1901 0.4144 0.7695 0.038 Uiso 1 1 calc R . . C6 C 1.12742(15) 0.47577(10) 0.68067(16) 0.0326(5) Uani 1 1 d . . . H6A H 1.1821 0.4991 0.6818 0.039 Uiso 1 1 calc R . . C7 C 1.04289(16) 0.49118(9) 0.62627(15) 0.0291(4) Uani 1 1 d . . . H7A H 1.0397 0.5247 0.5887 0.035 Uiso 1 1 calc R . . C8 C 0.96239(13) 0.45762(8) 0.62652(13) 0.0218(4) Uani 1 1 d . . . H8A H 0.9051 0.4682 0.5879 0.026 Uiso 1 1 calc R . . C101 C 0.84768(12) 0.34020(8) 0.49621(12) 0.0192(3) Uani 1 1 d . . . O101 O 0.86132(10) 0.36199(7) 0.43184(10) 0.0309(3) Uani 1 1 d . . . C102 C 0.94927(12) 0.26559(8) 0.62274(12) 0.0180(3) Uani 1 1 d . . . O102 O 1.02592(10) 0.24882(7) 0.63460(11) 0.0279(3) Uani 1 1 d . . . C103 C 0.75161(14) 0.24639(8) 0.50880(12) 0.0205(3) Uani 1 1 d . . . O103 O 0.71040(12) 0.21935(7) 0.44892(9) 0.0322(4) Uani 1 1 d . . . Pt1 Pt 0.781982(4) 0.191285(3) 0.662890(4) 0.01183(2) Uani 1 1 d . . . P1 P 0.87782(3) 0.119209(19) 0.63658(3) 0.01419(8) Uani 1 1 d . . . P2 P 0.70072(3) 0.119494(19) 0.71918(3) 0.01350(8) Uani 1 1 d . . . C11 C 0.66239(12) 0.12822(8) 0.82577(11) 0.0166(3) Uani 1 1 d . . . C12 C 0.60991(13) 0.17805(9) 0.83906(13) 0.0203(3) Uani 1 1 d . . . H12A H 0.5968 0.2071 0.7936 0.024 Uiso 1 1 calc R . . C13 C 0.57690(14) 0.18509(9) 0.91915(14) 0.0255(4) Uani 1 1 d . . . H13A H 0.5410 0.2187 0.9280 0.031 Uiso 1 1 calc R . . C14 C 0.59688(14) 0.14260(11) 0.98593(13) 0.0291(5) Uani 1 1 d . . . H14A H 0.5734 0.1469 1.0399 0.035 Uiso 1 1 calc R . . C15 C 0.65078(15) 0.09431(11) 0.97396(13) 0.0299(5) Uani 1 1 d . . . H15A H 0.6657 0.0661 1.0205 0.036 Uiso 1 1 calc R . . C16 C 0.68358(14) 0.08665(9) 0.89402(13) 0.0238(4) Uani 1 1 d . . . H16A H 0.7203 0.0532 0.8861 0.029 Uiso 1 1 calc R . . C21 C 0.59407(12) 0.09644(7) 0.64130(11) 0.0153(3) Uani 1 1 d . . . C22 C 0.53047(12) 0.05751(8) 0.66911(12) 0.0193(3) Uani 1 1 d . . . H22A H 0.5412 0.0443 0.7295 0.023 Uiso 1 1 calc R . . C23 C 0.45167(13) 0.03803(9) 0.60883(13) 0.0237(4) Uani 1 1 d . . . H23A H 0.4093 0.0112 0.6280 0.028 Uiso 1 1 calc R . . C24 C 0.43457(14) 0.05775(9) 0.52034(13) 0.0238(4) Uani 1 1 d . . . H24A H 0.3802 0.0447 0.4796 0.029 Uiso 1 1 calc R . . C25 C 0.49691(14) 0.09636(9) 0.49185(13) 0.0235(4) Uani 1 1 d . . . H25A H 0.4854 0.1097 0.4315 0.028 Uiso 1 1 calc R . . C26 C 0.57663(13) 0.11571(8) 0.55193(12) 0.0196(3) Uani 1 1 d . . . H26A H 0.6193 0.1421 0.5322 0.024 Uiso 1 1 calc R . . C27 C 0.77366(12) 0.05269(7) 0.73068(12) 0.0168(3) Uani 1 1 d . . . H27A H 0.8236 0.0550 0.7852 0.020 Uiso 1 1 calc R . . H27B H 0.7343 0.0177 0.7354 0.020 Uiso 1 1 calc R . . C28 C 0.81778(12) 0.04866(8) 0.64658(12) 0.0170(3) Uani 1 1 d . . . H28A H 0.7683 0.0417 0.5928 0.020 Uiso 1 1 calc R . . H28B H 0.8636 0.0160 0.6524 0.020 Uiso 1 1 calc R . . C31 C 0.92249(13) 0.11184(8) 0.53272(12) 0.0189(3) Uani 1 1 d . . . C32 C 0.86288(14) 0.09246(11) 0.45530(13) 0.0279(4) Uani 1 1 d . . . H32A H 0.7985 0.0845 0.4563 0.034 Uiso 1 1 calc R . . C33 C 0.89707(16) 0.08452(12) 0.37577(14) 0.0341(5) Uani 1 1 d . . . H33A H 0.8563 0.0703 0.3236 0.041 Uiso 1 1 calc R . . C34 C 0.99034(16) 0.09745(10) 0.37316(15) 0.0300(5) Uani 1 1 d . . . H34A H 1.0135 0.0921 0.3193 0.036 Uiso 1 1 calc R . . C35 C 1.04913(17) 0.11803(12) 0.44873(16) 0.0364(5) Uani 1 1 d . . . H35A H 1.1127 0.1275 0.4466 0.044 Uiso 1 1 calc R . . C36 C 1.01602(15) 0.12518(10) 0.52862(15) 0.0311(5) Uani 1 1 d . . . H36A H 1.0574 0.1392 0.5806 0.037 Uiso 1 1 calc R . . C41 C 0.98147(12) 0.11289(8) 0.72633(13) 0.0200(3) Uani 1 1 d . . . C42 C 1.03878(14) 0.06313(10) 0.73230(16) 0.0318(5) Uani 1 1 d . . . H42A H 1.0282 0.0346 0.6860 0.038 Uiso 1 1 calc R . . C43 C 1.11199(16) 0.05534(12) 0.80680(19) 0.0407(6) Uani 1 1 d . . . H43A H 1.1500 0.0211 0.8112 0.049 Uiso 1 1 calc R . . C44 C 1.12901(16) 0.09724(12) 0.87382(17) 0.0390(6) Uani 1 1 d . . . H44A H 1.1782 0.0916 0.9243 0.047 Uiso 1 1 calc R . . C45 C 1.07401(16) 0.14738(11) 0.86703(15) 0.0336(5) Uani 1 1 d . . . H45A H 1.0869 0.1766 0.9122 0.040 Uiso 1 1 calc R . . C46 C 0.99973(13) 0.15521(9) 0.79424(13) 0.0233(4) Uani 1 1 d . . . H46A H 0.9615 0.1893 0.7908 0.028 Uiso 1 1 calc R . . N1 N 0.83718(11) 0.24753(8) 1.13443(11) 0.0251(4) Uani 1 1 d . . . C51 C 0.74242(16) 0.23100(13) 1.15773(16) 0.0297(5) Uani 0.850(2) 1 d P A 1 H51A H 0.6939 0.2586 1.1270 0.036 Uiso 0.850(2) 1 calc PR A 1 H51B H 0.7250 0.1913 1.1339 0.036 Uiso 0.850(2) 1 calc PR A 1 C52 C 0.74038(19) 0.23151(14) 1.25740(17) 0.0319(6) Uani 0.850(2) 1 d P A 1 H52A H 0.6774 0.2203 1.2665 0.048 Uiso 0.850(2) 1 calc PR A 1 H52B H 0.7555 0.2709 1.2815 0.048 Uiso 0.850(2) 1 calc PR A 1 H52C H 0.7869 0.2036 1.2885 0.048 Uiso 0.850(2) 1 calc PR A 1 C53 C 0.8679(2) 0.30852(12) 1.1725(2) 0.0377(6) Uani 0.850(2) 1 d P A 1 H53A H 0.8890 0.3050 1.2382 0.045 Uiso 0.850(2) 1 calc PR A 1 H53B H 0.9228 0.3214 1.1472 0.045 Uiso 0.850(2) 1 calc PR A 1 C54 C 0.7918(5) 0.3562(3) 1.1538(3) 0.0607(15) Uani 0.850(2) 1 d P A 1 H54A H 0.8176 0.3932 1.1804 0.091 Uiso 0.850(2) 1 calc PR A 1 H54B H 0.7377 0.3447 1.1802 0.091 Uiso 0.850(2) 1 calc PR A 1 H54C H 0.7716 0.3611 1.0889 0.091 Uiso 0.850(2) 1 calc PR A 1 C55 C 0.91294(17) 0.20497(13) 1.17583(16) 0.0296(5) Uani 0.850(2) 1 d P A 1 H55A H 0.9737 0.2181 1.1616 0.035 Uiso 0.850(2) 1 calc PR A 1 H55B H 0.9189 0.2064 1.2418 0.035 Uiso 0.850(2) 1 calc PR A 1 C56 C 0.8965(2) 0.14232(19) 1.1458(2) 0.0410(8) Uani 0.850(2) 1 d P A 1 H56A H 0.9488 0.1179 1.1761 0.061 Uiso 0.850(2) 1 calc PR A 1 H56B H 0.8925 0.1400 1.0808 0.061 Uiso 0.850(2) 1 calc PR A 1 H56C H 0.8373 0.1283 1.1609 0.061 Uiso 0.850(2) 1 calc PR A 1 C57 C 0.82426(17) 0.24740(14) 1.03277(16) 0.0320(6) Uani 0.850(2) 1 d P A 1 H57A H 0.7852 0.2817 1.0092 0.038 Uiso 0.850(2) 1 calc PR A 1 H57B H 0.7888 0.2117 1.0096 0.038 Uiso 0.850(2) 1 calc PR A 1 C58 C 0.9152(4) 0.2492(4) 0.9962(5) 0.0315(9) Uani 0.850(2) 1 d P A 1 H58A H 0.9002 0.2492 0.9305 0.047 Uiso 0.850(2) 1 calc PR A 1 H58B H 0.9536 0.2148 1.0172 0.047 Uiso 0.850(2) 1 calc PR A 1 H58C H 0.9504 0.2849 1.0173 0.047 Uiso 0.850(2) 1 calc PR A 1 C51' C 0.8666(9) 0.2526(7) 1.2336(9) 0.0297(5) Uani 0.150(2) 1 d P A 2 H51C H 0.8890 0.2930 1.2487 0.036 Uiso 0.150(2) 1 calc PR A 2 H51D H 0.9202 0.2257 1.2540 0.036 Uiso 0.150(2) 1 calc PR A 2 C52' C 0.7879(11) 0.2384(8) 1.2842(10) 0.0319(6) Uani 0.150(2) 1 d P A 2 H52D H 0.8131 0.2390 1.3488 0.048 Uiso 0.150(2) 1 calc PR A 2 H52E H 0.7623 0.1995 1.2666 0.048 Uiso 0.150(2) 1 calc PR A 2 H52F H 0.7377 0.2677 1.2697 0.048 Uiso 0.150(2) 1 calc PR A 2 C55' C 0.8053(10) 0.1839(7) 1.1048(9) 0.0296(5) Uani 0.150(2) 1 d P A 2 H55C H 0.7459 0.1765 1.1264 0.035 Uiso 0.150(2) 1 calc PR A 2 H55D H 0.7891 0.1840 1.0385 0.035 Uiso 0.150(2) 1 calc PR A 2 C53' C 0.7592(11) 0.2859(8) 1.0898(12) 0.0377(6) Uani 0.150(2) 1 d P A 2 H53C H 0.6990 0.2732 1.1058 0.045 Uiso 0.150(2) 1 calc PR A 2 H53D H 0.7528 0.2831 1.0239 0.045 Uiso 0.150(2) 1 calc PR A 2 C54' C 0.781(4) 0.351(2) 1.121(2) 0.0607(15) Uani 0.150(2) 1 d P A 2 H54D H 0.7283 0.3757 1.0932 0.091 Uiso 0.150(2) 1 calc PR A 2 H54E H 0.8388 0.3635 1.1018 0.091 Uiso 0.150(2) 1 calc PR A 2 H54F H 0.7892 0.3528 1.1860 0.091 Uiso 0.150(2) 1 calc PR A 2 C56' C 0.8634(16) 0.1353(14) 1.1295(17) 0.0410(8) Uani 0.150(2) 1 d P A 2 H56D H 0.8305 0.0997 1.1048 0.061 Uiso 0.150(2) 1 calc PR A 2 H56E H 0.8788 0.1325 1.1950 0.061 Uiso 0.150(2) 1 calc PR A 2 H56F H 0.9217 0.1398 1.1059 0.061 Uiso 0.150(2) 1 calc PR A 2 C57' C 0.9293(10) 0.2584(8) 1.0969(9) 0.0320(6) Uani 0.150(2) 1 d P A 2 H57C H 0.9520 0.2981 1.1164 0.038 Uiso 0.150(2) 1 calc PR A 2 H57D H 0.9772 0.2304 1.1275 0.038 Uiso 0.150(2) 1 calc PR A 2 C58' C 0.929(3) 0.254(3) 1.003(3) 0.0315(9) Uani 0.150(2) 1 d P A 2 H58D H 0.9940 0.2593 0.9930 0.047 Uiso 0.150(2) 1 calc PR A 2 H58E H 0.8891 0.2852 0.9714 0.047 Uiso 0.150(2) 1 calc PR A 2 H58F H 0.9053 0.2159 0.9810 0.047 Uiso 0.150(2) 1 calc PR A 2 C1S C 0.9740(3) -0.0183(2) 0.9539(4) 0.0403(11) Uani 0.50 1 d PD . . H1S1 H 0.9843 -0.0118 0.8921 0.048 Uiso 0.50 1 calc PR . . H1S2 H 0.9339 -0.0536 0.9522 0.048 Uiso 0.50 1 calc PR . . Cl1 Cl 0.91443(6) 0.03541(5) 0.97843(7) 0.0753(3) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01175(6) 0.01174(6) 0.01133(6) 0.00039(4) 0.00316(4) -0.00076(4) C2 0.0137(7) 0.0143(7) 0.0146(7) -0.0005(6) 0.0029(6) -0.0022(6) B3 0.0129(8) 0.0149(8) 0.0149(8) -0.0002(6) 0.0032(6) 0.0001(6) B4 0.0134(8) 0.0146(8) 0.0167(8) 0.0015(6) 0.0015(6) 0.0005(6) B5 0.0135(8) 0.0142(8) 0.0154(8) -0.0009(6) 0.0017(6) 0.0010(6) B6 0.0138(8) 0.0148(8) 0.0141(8) 0.0000(6) 0.0032(6) 0.0005(6) B7 0.0147(8) 0.0144(8) 0.0176(8) 0.0011(7) 0.0020(6) 0.0009(7) B8 0.0144(8) 0.0147(8) 0.0166(8) -0.0009(7) 0.0038(6) 0.0005(6) B9 0.0139(8) 0.0156(8) 0.0180(8) 0.0001(7) 0.0046(6) 0.0010(6) B10 0.0133(8) 0.0160(8) 0.0180(8) -0.0008(7) 0.0039(6) 0.0016(6) B11 0.0137(8) 0.0171(8) 0.0144(8) 0.0000(7) 0.0038(6) -0.0002(7) C3 0.0160(7) 0.0171(8) 0.0187(8) -0.0052(6) 0.0074(6) -0.0030(6) C4 0.0160(8) 0.0300(10) 0.0245(9) -0.0037(8) 0.0035(7) -0.0045(7) C5 0.0179(9) 0.0464(14) 0.0311(11) -0.0091(10) 0.0069(8) -0.0094(9) C6 0.0272(10) 0.0376(12) 0.0382(12) -0.0180(10) 0.0197(9) -0.0175(9) C7 0.0340(11) 0.0218(9) 0.0369(11) -0.0052(8) 0.0207(9) -0.0104(8) C8 0.0215(9) 0.0189(8) 0.0272(9) -0.0005(7) 0.0103(7) -0.0040(7) C101 0.0166(8) 0.0210(8) 0.0202(8) 0.0028(7) 0.0041(6) 0.0014(6) O101 0.0271(7) 0.0419(9) 0.0256(7) 0.0135(7) 0.0097(6) 0.0002(6) C102 0.0195(8) 0.0161(8) 0.0200(8) 0.0018(6) 0.0078(6) -0.0018(6) O102 0.0172(6) 0.0281(8) 0.0400(8) 0.0030(6) 0.0092(6) 0.0037(5) C103 0.0260(9) 0.0212(9) 0.0158(8) 0.0014(6) 0.0077(7) -0.0050(7) O103 0.0482(10) 0.0313(8) 0.0158(6) -0.0031(6) 0.0029(6) -0.0165(7) Pt1 0.01219(3) 0.01103(3) 0.01292(3) 0.00069(2) 0.00408(2) 0.00011(2) P1 0.01333(18) 0.01357(19) 0.01638(19) -0.00031(15) 0.00462(15) 0.00101(15) P2 0.01361(18) 0.01325(18) 0.01411(18) 0.00228(15) 0.00385(14) -0.00023(15) C11 0.0151(7) 0.0201(8) 0.0151(7) 0.0004(6) 0.0039(6) -0.0031(6) C12 0.0196(8) 0.0225(9) 0.0200(8) 0.0003(7) 0.0070(6) -0.0026(7) C13 0.0229(9) 0.0307(11) 0.0259(9) -0.0058(8) 0.0120(7) -0.0031(8) C14 0.0248(10) 0.0464(13) 0.0188(9) -0.0066(8) 0.0107(7) -0.0120(9) C15 0.0311(11) 0.0416(13) 0.0181(9) 0.0081(8) 0.0069(8) -0.0061(9) C16 0.0260(9) 0.0266(10) 0.0196(8) 0.0047(7) 0.0065(7) -0.0016(8) C21 0.0158(7) 0.0134(7) 0.0169(7) 0.0017(6) 0.0039(6) 0.0006(6) C22 0.0167(8) 0.0217(9) 0.0197(8) 0.0044(7) 0.0034(6) -0.0027(6) C23 0.0188(8) 0.0258(10) 0.0264(9) 0.0025(7) 0.0042(7) -0.0070(7) C24 0.0220(9) 0.0234(9) 0.0237(9) -0.0020(7) -0.0012(7) -0.0041(7) C25 0.0274(9) 0.0234(9) 0.0180(8) 0.0022(7) -0.0003(7) -0.0020(7) C26 0.0218(8) 0.0202(8) 0.0168(8) 0.0039(6) 0.0036(6) -0.0028(7) C27 0.0164(7) 0.0134(7) 0.0212(8) 0.0043(6) 0.0048(6) 0.0001(6) C28 0.0188(8) 0.0134(7) 0.0194(8) 0.0005(6) 0.0050(6) 0.0026(6) C31 0.0207(8) 0.0169(8) 0.0215(8) 0.0006(6) 0.0098(7) 0.0033(6) C32 0.0180(8) 0.0459(13) 0.0204(9) -0.0008(8) 0.0048(7) 0.0045(8) C33 0.0279(10) 0.0567(16) 0.0185(9) -0.0020(9) 0.0063(8) 0.0094(10) C34 0.0325(11) 0.0355(12) 0.0266(10) 0.0019(9) 0.0169(9) 0.0082(9) C35 0.0298(11) 0.0477(15) 0.0374(12) -0.0077(11) 0.0208(10) -0.0096(10) C36 0.0267(10) 0.0383(12) 0.0318(11) -0.0109(9) 0.0148(8) -0.0122(9) C41 0.0142(7) 0.0228(9) 0.0229(9) 0.0035(7) 0.0030(6) 0.0007(6) C42 0.0199(9) 0.0294(11) 0.0437(13) -0.0023(9) -0.0002(9) 0.0066(8) C43 0.0218(10) 0.0406(14) 0.0544(15) 0.0100(12) -0.0060(10) 0.0090(9) C44 0.0220(10) 0.0486(15) 0.0401(13) 0.0107(11) -0.0098(9) -0.0059(10) C45 0.0265(10) 0.0434(13) 0.0271(10) 0.0002(9) -0.0047(8) -0.0097(9) C46 0.0197(8) 0.0291(10) 0.0205(8) 0.0015(7) 0.0022(7) -0.0025(7) N1 0.0145(7) 0.0383(10) 0.0213(8) 0.0076(7) 0.0005(6) -0.0036(7) C51 0.0165(10) 0.0478(16) 0.0248(11) 0.0065(10) 0.0039(8) -0.0063(10) C52 0.0268(13) 0.0471(16) 0.0222(12) 0.0033(11) 0.0059(10) -0.0055(12) C53 0.0277(13) 0.0403(16) 0.0474(17) -0.0009(12) 0.0133(12) -0.0095(11) C54 0.060(3) 0.040(2) 0.090(4) 0.014(3) 0.034(4) 0.0068(18) C55 0.0218(11) 0.0479(15) 0.0177(10) 0.0091(10) 0.0002(8) 0.0064(10) C56 0.048(2) 0.0439(19) 0.0321(18) 0.0108(14) 0.0095(16) 0.0093(19) C57 0.0198(10) 0.0554(17) 0.0193(10) 0.0130(11) 0.0001(8) -0.0023(11) C58 0.023(2) 0.051(2) 0.0199(15) 0.0081(15) 0.0024(15) -0.0058(19) C51' 0.0165(10) 0.0478(16) 0.0248(11) 0.0065(10) 0.0039(8) -0.0063(10) C52' 0.0268(13) 0.0471(16) 0.0222(12) 0.0033(11) 0.0059(10) -0.0055(12) C55' 0.0218(11) 0.0479(15) 0.0177(10) 0.0091(10) 0.0002(8) 0.0064(10) C53' 0.0277(13) 0.0403(16) 0.0474(17) -0.0009(12) 0.0133(12) -0.0095(11) C54' 0.060(3) 0.040(2) 0.090(4) 0.014(3) 0.034(4) 0.0068(18) C56' 0.048(2) 0.0439(19) 0.0321(18) 0.0108(14) 0.0095(16) 0.0093(19) C57' 0.0198(10) 0.0554(17) 0.0193(10) 0.0130(11) 0.0001(8) -0.0023(11) C58' 0.023(2) 0.051(2) 0.0199(15) 0.0081(15) 0.0024(15) -0.0058(19) C1S 0.034(2) 0.036(3) 0.046(3) -0.012(2) -0.005(2) -0.002(2) Cl1 0.0523(5) 0.0884(7) 0.0759(6) 0.0128(5) -0.0115(4) 0.0089(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C102 2.0124(18) . ? Mo1 C101 2.0194(18) . ? Mo1 C103 2.0200(19) . ? Mo1 C2 2.2111(17) . ? Mo1 B3 2.3172(19) . ? Mo1 B4 2.453(2) . ? Mo1 B5 2.4812(19) . ? Mo1 B7 2.4926(19) . ? Mo1 B6 2.6169(19) . ? Mo1 Pt1 2.7114(2) . ? C2 C3 1.506(2) . ? C2 B5 1.613(3) . ? C2 B4 1.628(3) . ? C2 B8 1.644(2) . ? B3 H3 1.11(2) . ? B3 B7 1.743(3) . ? B3 B9 1.766(3) . ? B3 B6 1.768(3) . ? B3 Pt1 2.3114(19) . ? B4 B10 1.825(3) . ? B4 B7 1.843(3) . ? B4 B8 1.845(3) . ? B5 B11 1.814(3) . ? B5 B8 1.834(3) . ? B5 B6 1.895(3) . ? B6 H6 1.13(2) . ? B6 B11 1.814(3) . ? B6 B9 1.817(3) . ? B6 Pt1 2.4063(19) . ? B7 B10 1.789(3) . ? B7 B9 1.834(3) . ? B8 B11 1.752(3) . ? B8 B10 1.775(3) . ? B9 B10 1.750(3) . ? B9 B11 1.752(3) . ? B10 B11 1.803(3) . ? C3 C8 1.401(3) . ? C3 C4 1.406(3) . ? C4 C5 1.395(3) . ? C5 C6 1.389(3) . ? C6 C7 1.383(3) . ? C7 C8 1.393(3) . ? C101 O101 1.147(2) . ? C102 O102 1.153(2) . ? C103 O103 1.165(2) . ? C103 Pt1 2.6201(18) . ? Pt1 P1 2.2344(4) . ? Pt1 P2 2.2753(4) . ? Pt1 H3 2.48(2) . ? Pt1 H6 2.50(2) . ? P1 C31 1.8233(18) . ? P1 C41 1.8283(19) . ? P1 C28 1.8486(18) . ? P2 C11 1.8198(17) . ? P2 C21 1.8313(18) . ? P2 C27 1.8424(18) . ? C11 C16 1.396(3) . ? C11 C12 1.403(3) . ? C12 C13 1.398(3) . ? C13 C14 1.394(3) . ? C14 C15 1.381(3) . ? C15 C16 1.397(3) . ? C21 C22 1.400(2) . ? C21 C26 1.404(2) . ? C22 C23 1.391(3) . ? C23 C24 1.395(3) . ? C24 C25 1.387(3) . ? C25 C26 1.398(3) . ? C27 C28 1.536(2) . ? C31 C32 1.391(3) . ? C31 C36 1.398(3) . ? C32 C33 1.402(3) . ? C33 C34 1.387(3) . ? C34 C35 1.374(3) . ? C35 C36 1.397(3) . ? C41 C42 1.398(3) . ? C41 C46 1.401(3) . ? C42 C43 1.405(3) . ? C43 C44 1.384(4) . ? C44 C45 1.386(4) . ? C45 C46 1.398(3) . ? N1 C53' 1.485(18) . ? N1 C51' 1.490(14) . ? N1 C55 1.508(3) . ? N1 C57 1.520(3) . ? N1 C51 1.525(3) . ? N1 C53 1.540(3) . ? N1 C57' 1.564(14) . ? N1 C55' 1.564(17) . ? C51 C52 1.521(3) . ? C53 C54 1.533(8) . ? C55 C56 1.506(5) . ? C57 C58 1.521(8) . ? C51' C52' 1.524(19) . ? C55' C56' 1.40(3) . ? C53' C54' 1.56(5) . ? C57' C58' 1.43(5) . ? C1S Cl1 1.582(5) . ? C1S Cl1 1.782(5) 3_757 ? Cl1 C1S 1.782(5) 3_757 ? 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 C102 Mo1 C101 86.79(7) . . ? C102 Mo1 C103 99.36(8) . . ? C101 Mo1 C103 79.32(7) . . ? C102 Mo1 C2 90.28(7) . . ? C101 Mo1 C2 90.29(7) . . ? C103 Mo1 C2 165.33(7) . . ? C102 Mo1 B3 132.64(7) . . ? C101 Mo1 B3 135.98(7) . . ? C103 Mo1 B3 75.92(7) . . ? C2 Mo1 B3 105.56(6) . . ? C102 Mo1 B4 129.54(7) . . ? C101 Mo1 B4 84.12(7) . . ? C103 Mo1 B4 127.12(7) . . ? C2 Mo1 B4 40.43(6) . . ? B3 Mo1 B4 82.63(7) . . ? C102 Mo1 B5 83.76(7) . . ? C101 Mo1 B5 128.72(7) . . ? C103 Mo1 B5 151.96(7) . . ? C2 Mo1 B5 39.70(6) . . ? B3 Mo1 B5 81.54(6) . . ? B4 Mo1 B5 64.84(6) . . ? C102 Mo1 B7 164.29(7) . . ? C101 Mo1 B7 104.76(7) . . ? C103 Mo1 B7 93.32(7) . . ? C2 Mo1 B7 79.22(6) . . ? B3 Mo1 B7 42.31(7) . . ? B4 Mo1 B7 43.74(6) . . ? B5 Mo1 B7 80.69(6) . . ? C102 Mo1 B6 102.49(6) . . ? C101 Mo1 B6 165.75(7) . . ? C103 Mo1 B6 109.30(7) . . ? C2 Mo1 B6 79.00(6) . . ? B3 Mo1 B6 41.44(6) . . ? B4 Mo1 B6 81.63(6) . . ? B5 Mo1 B6 43.54(6) . . ? B7 Mo1 B6 64.24(6) . . ? C102 Mo1 Pt1 80.75(5) . . ? C101 Mo1 Pt1 139.71(5) . . ? C103 Mo1 Pt1 65.36(5) . . ? C2 Mo1 Pt1 127.64(4) . . ? B3 Mo1 Pt1 54.04(5) . . ? B4 Mo1 Pt1 132.45(5) . . ? B5 Mo1 Pt1 87.95(5) . . ? B7 Mo1 Pt1 96.34(5) . . ? B6 Mo1 Pt1 53.66(4) . . ? C3 C2 B5 123.52(15) . . ? C3 C2 B4 124.53(15) . . ? B5 C2 B4 109.41(13) . . ? C3 C2 B8 114.75(14) . . ? B5 C2 B8 68.52(11) . . ? B4 C2 B8 68.66(12) . . ? C3 C2 Mo1 124.61(11) . . ? B5 C2 Mo1 79.21(10) . . ? B4 C2 Mo1 77.80(9) . . ? B8 C2 Mo1 120.64(11) . . ? H3 B3 B7 117.0(11) . . ? H3 B3 B9 118.8(11) . . ? B7 B3 B9 63.01(11) . . ? H3 B3 B6 137.0(11) . . ? B7 B3 B6 101.47(13) . . ? B9 B3 B6 61.90(11) . . ? H3 B3 Pt1 85.6(11) . . ? B7 B3 Pt1 145.93(12) . . ? B9 B3 Pt1 130.23(12) . . ? B6 B3 Pt1 70.88(9) . . ? H3 B3 Mo1 128.3(11) . . ? B7 B3 Mo1 74.23(9) . . ? B9 B3 Mo1 111.11(11) . . ? B6 B3 Mo1 78.40(9) . . ? Pt1 B3 Mo1 71.72(5) . . ? C2 B4 B10 107.61(13) . . ? C2 B4 B7 119.97(14) . . ? B10 B4 B7 58.39(10) . . ? C2 B4 B8 56.09(10) . . ? B10 B4 B8 57.85(10) . . ? B7 B4 B8 106.75(13) . . ? C2 B4 Mo1 61.77(9) . . ? B10 B4 Mo1 108.96(11) . . ? B7 B4 Mo1 69.28(9) . . ? B8 B4 Mo1 101.96(10) . . ? C2 B5 B11 107.91(13) . . ? C2 B5 B8 56.53(10) . . ? B11 B5 B8 57.41(10) . . ? C2 B5 B6 123.03(14) . . ? B11 B5 B6 58.50(10) . . ? B8 B5 B6 107.80(12) . . ? C2 B5 Mo1 61.09(8) . . ? B11 B5 Mo1 109.13(10) . . ? B8 B5 Mo1 101.26(10) . . ? B6 B5 Mo1 72.04(8) . . ? H6 B6 B3 130.5(11) . . ? H6 B6 B11 107.9(11) . . ? B3 B6 B11 110.42(13) . . ? H6 B6 B9 124.8(11) . . ? B3 B6 B9 59.00(11) . . ? B11 B6 B9 57.69(10) . . ? H6 B6 B5 108.6(11) . . ? B3 B6 B5 117.72(13) . . ? B11 B6 B5 58.50(10) . . ? B9 B6 B5 105.03(13) . . ? H6 B6 Pt1 81.5(11) . . ? B3 B6 Pt1 65.16(8) . . ? B11 B6 Pt1 168.93(12) . . ? B9 B6 Pt1 122.04(11) . . ? B5 B6 Pt1 113.55(10) . . ? H6 B6 Mo1 136.1(11) . . ? B3 B6 Mo1 60.16(8) . . ? B11 B6 Mo1 103.75(10) . . ? B9 B6 Mo1 97.76(10) . . ? B5 B6 Mo1 64.42(8) . . ? Pt1 B6 Mo1 65.18(5) . . ? B3 B7 B10 112.12(14) . . ? B3 B7 B9 59.09(11) . . ? B10 B7 B9 57.75(11) . . ? B3 B7 B4 122.94(14) . . ? B10 B7 B4 60.32(11) . . ? B9 B7 B4 107.66(13) . . ? B3 B7 Mo1 63.46(8) . . ? B10 B7 Mo1 108.59(11) . . ? B9 B7 Mo1 101.73(10) . . ? B4 B7 Mo1 66.98(8) . . ? C2 B8 B11 109.47(14) . . ? C2 B8 B10 109.24(14) . . ? B11 B8 B10 61.48(11) . . ? C2 B8 B5 54.95(10) . . ? B11 B8 B5 60.71(11) . . ? B10 B8 B5 103.87(13) . . ? C2 B8 B4 55.25(10) . . ? B11 B8 B4 104.41(13) . . ? B10 B8 B4 60.51(10) . . ? B5 B8 B4 91.95(12) . . ? B10 B9 B11 61.98(11) . . ? B10 B9 B3 112.93(14) . . ? B11 B9 B3 113.48(13) . . ? B10 B9 B6 107.31(13) . . ? B11 B9 B6 61.05(11) . . ? B3 B9 B6 59.11(10) . . ? B10 B9 B7 59.83(11) . . ? B11 B9 B7 104.39(13) . . ? B3 B9 B7 57.90(11) . . ? B6 B9 B7 96.24(12) . . ? B9 B10 B8 112.48(14) . . ? B9 B10 B7 62.41(11) . . ? B8 B10 B7 112.26(13) . . ? B9 B10 B11 59.05(11) . . ? B8 B10 B11 58.62(11) . . ? B7 B10 B11 104.15(13) . . ? B9 B10 B4 112.21(14) . . ? B8 B10 B4 61.64(11) . . ? B7 B10 B4 61.29(11) . . ? B11 B10 B4 103.18(13) . . ? B9 B11 B8 113.56(14) . . ? B9 B11 B10 58.97(11) . . ? B8 B11 B10 59.90(11) . . ? B9 B11 B5 111.45(13) . . ? B8 B11 B5 61.88(11) . . ? B10 B11 B5 103.58(13) . . ? B9 B11 B6 61.26(11) . . ? B8 B11 B6 115.36(13) . . ? B10 B11 B6 105.24(13) . . ? B5 B11 B6 63.00(11) . . ? C8 C3 C4 117.42(17) . . ? C8 C3 C2 121.41(16) . . ? C4 C3 C2 121.09(16) . . ? C5 C4 C3 120.6(2) . . ? C6 C5 C4 120.8(2) . . ? C7 C6 C5 119.39(19) . . ? C6 C7 C8 120.0(2) . . ? C7 C8 C3 121.67(19) . . ? O101 C101 Mo1 177.47(17) . . ? O102 C102 Mo1 176.09(17) . . ? O103 C103 Mo1 174.74(17) . . ? O103 C103 Pt1 114.67(14) . . ? Mo1 C103 Pt1 70.16(5) . . ? P1 Pt1 P2 85.341(17) . . ? P1 Pt1 B3 166.82(5) . . ? P2 Pt1 B3 103.39(5) . . ? P1 Pt1 B6 144.20(5) . . ? P2 Pt1 B6 103.28(5) . . ? B3 Pt1 B6 43.96(7) . . ? P1 Pt1 H3 149.2(5) . . ? P2 Pt1 H3 85.4(5) . . ? B3 Pt1 H3 26.3(5) . . ? B6 Pt1 H3 66.6(5) . . ? P1 Pt1 H6 124.9(5) . . ? P2 Pt1 H6 84.7(5) . . ? B3 Pt1 H6 66.5(5) . . ? B6 Pt1 H6 26.5(5) . . ? H3 Pt1 H6 83.3(7) . . ? P1 Pt1 C103 101.38(4) . . ? P2 Pt1 C103 132.16(4) . . ? B3 Pt1 C103 65.44(6) . . ? B6 Pt1 C103 98.06(6) . . ? H3 Pt1 C103 64.8(5) . . ? H6 Pt1 C103 124.5(5) . . ? P1 Pt1 Mo1 116.807(12) . . ? P2 Pt1 Mo1 157.612(12) . . ? B3 Pt1 Mo1 54.24(5) . . ? B6 Pt1 Mo1 61.16(5) . . ? H3 Pt1 Mo1 73.8(5) . . ? H6 Pt1 Mo1 84.8(5) . . ? C103 Pt1 Mo1 44.49(4) . . ? C31 P1 C41 105.30(9) . . ? C31 P1 C28 103.87(8) . . ? C41 P1 C28 101.54(8) . . ? C31 P1 Pt1 123.81(6) . . ? C41 P1 Pt1 111.81(6) . . ? C28 P1 Pt1 108.07(6) . . ? C11 P2 C21 104.21(8) . . ? C11 P2 C27 105.76(8) . . ? C21 P2 C27 102.63(8) . . ? C11 P2 Pt1 121.48(6) . . ? C21 P2 Pt1 113.23(6) . . ? C27 P2 Pt1 107.75(6) . . ? C16 C11 C12 119.47(17) . . ? C16 C11 P2 121.75(14) . . ? C12 C11 P2 118.78(13) . . ? C13 C12 C11 120.12(18) . . ? C14 C13 C12 119.75(19) . . ? C15 C14 C13 120.19(18) . . ? C14 C15 C16 120.5(2) . . ? C11 C16 C15 119.9(2) . . ? C22 C21 C26 118.94(16) . . ? C22 C21 P2 120.44(13) . . ? C26 C21 P2 120.57(13) . . ? C23 C22 C21 120.37(17) . . ? C22 C23 C24 120.28(18) . . ? C25 C24 C23 120.00(18) . . ? C24 C25 C26 119.99(18) . . ? C25 C26 C21 120.42(17) . . ? C28 C27 P2 106.93(11) . . ? C27 C28 P1 106.97(12) . . ? C32 C31 C36 118.63(17) . . ? C32 C31 P1 119.83(14) . . ? C36 C31 P1 121.54(15) . . ? C31 C32 C33 120.49(19) . . ? C34 C33 C32 120.1(2) . . ? C35 C34 C33 119.83(19) . . ? C34 C35 C36 120.5(2) . . ? C35 C36 C31 120.5(2) . . ? C42 C41 C46 119.10(18) . . ? C42 C41 P1 120.19(16) . . ? C46 C41 P1 120.48(14) . . ? C41 C42 C43 120.0(2) . . ? C44 C43 C42 120.4(2) . . ? C43 C44 C45 119.8(2) . . ? C44 C45 C46 120.5(2) . . ? C45 C46 C41 120.2(2) . . ? C53' N1 C51' 117.5(9) . . ? C53' N1 C55 175.9(7) . . ? C51' N1 C55 65.4(6) . . ? C53' N1 C57 66.5(7) . . ? C51' N1 C57 169.7(5) . . ? C55 N1 C57 111.18(18) . . ? C53' N1 C51 67.4(6) . . ? C51' N1 C51 83.1(5) . . ? C55 N1 C51 110.83(18) . . ? C57 N1 C51 107.09(17) . . ? C53' N1 C53 77.1(7) . . ? C51' N1 C53 62.8(6) . . ? C55 N1 C53 106.93(19) . . ? C57 N1 C53 110.8(2) . . ? C51 N1 C53 110.07(19) . . ? C53' N1 C57' 111.3(8) . . ? C51' N1 C57' 104.9(7) . . ? C55 N1 C57' 69.8(6) . . ? C57 N1 C57' 65.0(5) . . ? C51 N1 C57' 170.9(6) . . ? C53 N1 C57' 77.9(7) . . ? C53' N1 C55' 105.1(8) . . ? C51' N1 C55' 112.0(8) . . ? C55 N1 C55' 70.9(5) . . ? C57 N1 C55' 74.5(5) . . ? C51 N1 C55' 67.0(5) . . ? C53 N1 C55' 174.7(5) . . ? C57' N1 C55' 105.5(9) . . ? C52 C51 N1 114.7(2) . . ? C54 C53 N1 115.3(3) . . ? C56 C55 N1 115.1(2) . . ? N1 C57 C58 115.1(3) . . ? N1 C51' C52' 113.4(11) . . ? C56' C55' N1 122.0(15) . . ? N1 C53' C54' 109(2) . . ? C58' C57' N1 121.1(19) . . ? Cl1 C1S Cl1 120.4(3) . 3_757 ? C1S Cl1 C1S 59.6(3) . 3_757 ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.131 _refine_diff_density_min -1.922 _refine_diff_density_rms 0.115 #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 270995' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H38 B9 Mn Mo O6 P2 Pt, 1.125(C H2 Cl2)' _chemical_formula_sum 'C40.125 H40.25 B9 Cl2.25 Mn Mo O6 P2 Pt' _chemical_formula_weight 1203.44 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 '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' Pt Pt -1.7033 8.3905 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 56.424(3) _cell_length_b 11.4786(5) _cell_length_c 38.7221(17) _cell_angle_alpha 90.00 _cell_angle_beta 129.6520(10) _cell_angle_gamma 90.00 _cell_volume 19309.1(15) _cell_formula_units_Z 16 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9727 _cell_measurement_theta_min 2.2555 _cell_measurement_theta_max 27.803 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9396 _exptl_absorpt_coefficient_mu 3.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3743 _exptl_absorpt_correction_T_max 0.6247 _exptl_absorpt_process_details 'SADABS (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102923 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0687 _diffrn_reflns_limit_h_min -76 _diffrn_reflns_limit_h_max 72 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 29.35 _reflns_number_total 23919 _reflns_number_gt 17245 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2001)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2001)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2001)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+73.3249P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23919 _refine_ls_number_parameters 1232 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.088534(10) 0.18463(4) 0.449314(13) 0.01910(10) Uani 1 1 d . . . C2 C 0.09557(12) 0.3386(5) 0.48975(17) 0.0243(12) Uani 1 1 d . . . B3 B 0.03743(13) 0.1347(5) 0.40623(18) 0.0195(12) Uani 1 1 d . . . H3 H 0.0272(11) 0.089(5) 0.3756(17) 0.023 Uiso 1 1 d . . . B4 B 0.08031(14) 0.2461(6) 0.50208(19) 0.0245(13) Uani 1 1 d . . . H4 H 0.0954 0.2105 0.5371 0.029 Uiso 1 1 calc R . . B5 B 0.06990(14) 0.3831(6) 0.43906(19) 0.0227(13) Uani 1 1 d . . . H5 H 0.0764 0.4520 0.4260 0.027 Uiso 1 1 calc R . . B6 B 0.03976(14) 0.2822(5) 0.39888(19) 0.0226(13) Uani 1 1 d . . . H6 H 0.0253(12) 0.296(5) 0.3618(18) 0.027 Uiso 1 1 d . . . B7 B 0.04801(13) 0.1427(5) 0.46008(18) 0.0195(12) Uani 1 1 d . . . H7 H 0.0467(12) 0.069(5) 0.4816(17) 0.023 Uiso 1 1 d . . . B8 B 0.06618(14) 0.3949(6) 0.4833(2) 0.0259(14) Uani 1 1 d . . . H8 H 0.0687 0.4727 0.5029 0.031 Uiso 1 1 calc R . . B9 B 0.01732(13) 0.2344(5) 0.41462(19) 0.0225(13) Uani 1 1 d . . . H9 H -0.0081 0.2223 0.3941 0.027 Uiso 1 1 calc R . . B10 B 0.03995(14) 0.2847(5) 0.4702(2) 0.0218(12) Uani 1 1 d . . . H10 H 0.0291 0.2912 0.4863 0.026 Uiso 1 1 calc R . . B11 B 0.03240(15) 0.3773(6) 0.42660(19) 0.0247(13) Uani 1 1 d . . . H11 H 0.0157 0.4513 0.4094 0.030 Uiso 1 1 calc R . . C3 C 0.12649(12) 0.3964(5) 0.52350(17) 0.0244(12) Uani 1 1 d . . . C4 C 0.14322(13) 0.3825(5) 0.56976(18) 0.0321(13) Uani 1 1 d . . . H4P H 0.1354 0.3337 0.5802 0.039 Uiso 1 1 calc R . . C5 C 0.17128(14) 0.4398(6) 0.6006(2) 0.0383(15) Uani 1 1 d . . . H5P H 0.1823 0.4300 0.6318 0.046 Uiso 1 1 calc R . . C6 C 0.18311(13) 0.5100(5) 0.5863(2) 0.0375(15) Uani 1 1 d . . . H6P H 0.2022 0.5486 0.6074 0.045 Uiso 1 1 calc R . . C7 C 0.16709(13) 0.5244(5) 0.5406(2) 0.0334(13) Uani 1 1 d . . . H7P H 0.1751 0.5739 0.5305 0.040 Uiso 1 1 calc R . . C8 C 0.13958(13) 0.4669(5) 0.50992(19) 0.0265(12) Uani 1 1 d . . . H8P H 0.1292 0.4752 0.4788 0.032 Uiso 1 1 calc R . . C101 C 0.12798(12) 0.1320(5) 0.51069(18) 0.0274(12) Uani 1 1 d . . . O101 O 0.14923(9) 0.1053(4) 0.54547(13) 0.0405(11) Uani 1 1 d . . . C102 C 0.11465(14) 0.2577(5) 0.43542(19) 0.0320(13) Uani 1 1 d . . . O102 O 0.13034(10) 0.2948(4) 0.42894(15) 0.0440(11) Uani 1 1 d . . . C103 C 0.09587(12) 0.0431(5) 0.42404(16) 0.0239(12) Uani 1 1 d . . . O103 O 0.10483(9) -0.0223(3) 0.41243(12) 0.0281(9) Uani 1 1 d . . . Mn1 Mn 0.036089(18) 0.17731(7) 0.34911(2) 0.02339(18) Uani 1 1 d . . . C201 C 0.05482(14) 0.2723(6) 0.33553(18) 0.0319(14) Uani 1 1 d . . . O201 O 0.06633(11) 0.3358(4) 0.32771(15) 0.0503(13) Uani 1 1 d . . . C202 C -0.00088(13) 0.1847(5) 0.29466(18) 0.0283(12) Uani 1 1 d . . . O202 O -0.02472(9) 0.1886(4) 0.25913(12) 0.0366(10) Uani 1 1 d . . . C203 C 0.04385(12) 0.0513(5) 0.32925(17) 0.0246(12) Uani 1 1 d . . . O203 O 0.04763(9) -0.0255(4) 0.31433(13) 0.0341(10) Uani 1 1 d . . . Pt1 Pt 0.064589(4) -0.026338(18) 0.445601(6) 0.01748(5) Uani 1 1 d . . . P1 P 0.09660(3) -0.17886(12) 0.48397(4) 0.0186(3) Uani 1 1 d . . . P2 P 0.02668(3) -0.15557(12) 0.42455(4) 0.0195(3) Uani 1 1 d . . . C15 C 0.04499(12) -0.2842(5) 0.46074(18) 0.0261(12) Uani 1 1 d . . . H15A H 0.0514 -0.2677 0.4908 0.031 Uiso 1 1 calc R . . H15B H 0.0305 -0.3508 0.4475 0.031 Uiso 1 1 calc R . . C16 C 0.07294(11) -0.3120(5) 0.46434(17) 0.0242(12) Uani 1 1 d . . . H16A H 0.0663 -0.3358 0.4347 0.029 Uiso 1 1 calc R . . H16B H 0.0850 -0.3764 0.4858 0.029 Uiso 1 1 calc R . . C21 C 0.11494(11) -0.1747(5) 0.54357(16) 0.0221(11) Uani 1 1 d . . . C22 C 0.13189(13) -0.2706(5) 0.57014(18) 0.0291(13) Uani 1 1 d . . . H22A H 0.1343 -0.3357 0.5575 0.035 Uiso 1 1 calc R . . C23 C 0.14538(14) -0.2714(6) 0.61552(19) 0.0363(14) Uani 1 1 d . . . H23A H 0.1571 -0.3368 0.6337 0.044 Uiso 1 1 calc R . . C24 C 0.14172(13) -0.1783(6) 0.63382(18) 0.0367(15) Uani 1 1 d . . . H24A H 0.1508 -0.1793 0.6646 0.044 Uiso 1 1 calc R . . C25 C 0.12474(13) -0.0826(6) 0.60732(19) 0.0342(14) Uani 1 1 d . . . H25A H 0.1222 -0.0180 0.6201 0.041 Uiso 1 1 calc R . . C26 C 0.11129(12) -0.0803(5) 0.56209(17) 0.0272(12) Uani 1 1 d . . . H26A H 0.0997 -0.0145 0.5441 0.033 Uiso 1 1 calc R . . C31 C 0.12710(11) -0.2096(5) 0.48207(16) 0.0209(11) Uani 1 1 d . . . C32 C 0.12134(12) -0.2719(5) 0.44611(17) 0.0264(12) Uani 1 1 d . . . H32A H 0.1014 -0.3028 0.4232 0.032 Uiso 1 1 calc R . . C33 C 0.14493(13) -0.2881(6) 0.44424(19) 0.0337(14) Uani 1 1 d . . . H33A H 0.1412 -0.3312 0.4202 0.040 Uiso 1 1 calc R . . C34 C 0.17402(14) -0.2415(6) 0.4774(2) 0.0358(14) Uani 1 1 d . . . H34A H 0.1900 -0.2531 0.4759 0.043 Uiso 1 1 calc R . . C35 C 0.17966(13) -0.1789(6) 0.51220(19) 0.0340(14) Uani 1 1 d . . . H35A H 0.1995 -0.1467 0.5346 0.041 Uiso 1 1 calc R . . C36 C 0.15659(12) -0.1630(5) 0.51459(17) 0.0269(12) Uani 1 1 d . . . H36A H 0.1607 -0.1194 0.5388 0.032 Uiso 1 1 calc R . . C41 C 0.00644(12) -0.2151(5) 0.36866(17) 0.0268(12) Uani 1 1 d . . . C42 C -0.02097(13) -0.2768(6) 0.34741(19) 0.0338(14) Uani 1 1 d . . . H42A H -0.0297 -0.2847 0.3616 0.041 Uiso 1 1 calc R . . C43 C -0.03536(16) -0.3263(7) 0.3059(2) 0.053(2) Uani 1 1 d . . . H43A H -0.0542 -0.3668 0.2914 0.063 Uiso 1 1 calc R . . C44 C -0.02245(18) -0.3172(8) 0.2854(2) 0.066(2) Uani 1 1 d . . . H44A H -0.0325 -0.3517 0.2568 0.079 Uiso 1 1 calc R . . C45 C 0.00521(17) -0.2579(8) 0.3064(2) 0.061(2) Uani 1 1 d . . . H45A H 0.0144 -0.2529 0.2927 0.073 Uiso 1 1 calc R . . C46 C 0.01926(15) -0.2060(6) 0.3481(2) 0.0439(17) Uani 1 1 d . . . H46A H 0.0379 -0.1638 0.3624 0.053 Uiso 1 1 calc R . . C51 C -0.00298(11) -0.1051(5) 0.42627(16) 0.0210(11) Uani 1 1 d . . . C52 C -0.02464(12) -0.0255(5) 0.39390(19) 0.0295(13) Uani 1 1 d . . . H52A H -0.0247 -0.0040 0.3701 0.035 Uiso 1 1 calc R . . C53 C -0.04615(13) 0.0223(6) 0.3965(2) 0.0370(14) Uani 1 1 d . . . H53A H -0.0611 0.0759 0.3743 0.044 Uiso 1 1 calc R . . C54 C -0.04593(14) -0.0077(5) 0.4312(2) 0.0362(15) Uani 1 1 d . . . H54A H -0.0601 0.0274 0.4335 0.043 Uiso 1 1 calc R . . C55 C -0.02497(13) -0.0893(5) 0.46273(19) 0.0324(14) Uani 1 1 d . . . H55A H -0.0254 -0.1119 0.4860 0.039 Uiso 1 1 calc R . . C56 C -0.00339(13) -0.1381(5) 0.46059(18) 0.0281(12) Uani 1 1 d . . . H56A H 0.0110 -0.1936 0.4824 0.034 Uiso 1 1 calc R . . Mo2 Mo 0.179516(10) 0.04649(4) 0.845690(14) 0.01999(10) Uani 1 1 d . . . C12 C 0.20278(12) -0.1052(5) 0.84290(16) 0.0228(11) Uani 1 1 d . . . B103 B 0.13934(14) 0.0983(6) 0.77366(18) 0.0233(13) Uani 1 1 d . . . H103 H 0.1186(12) 0.145(5) 0.7660(17) 0.028 Uiso 1 1 d . . . B104 B 0.20350(15) -0.0084(5) 0.81282(19) 0.0236(13) Uani 1 1 d . . . H104 H 0.2266 0.0278 0.8271 0.028 Uiso 1 1 calc R . . B105 B 0.16788(14) -0.1520(6) 0.8149(2) 0.0240(13) Uani 1 1 d . . . H105 H 0.1635 -0.2247 0.8295 0.029 Uiso 1 1 calc R . . B106 B 0.13703(14) -0.0500(6) 0.7785(2) 0.0254(14) Uani 1 1 d . . . H106 H 0.1165(13) -0.066(5) 0.7741(18) 0.030 Uiso 1 1 d . . . B107 B 0.17075(15) 0.0961(6) 0.77330(19) 0.0270(14) Uani 1 1 d . . . H107 H 0.1780(12) 0.169(5) 0.7631(18) 0.032 Uiso 1 1 d . . . B108 B 0.18914(15) -0.1550(6) 0.7934(2) 0.0267(14) Uani 1 1 d . . . H108 H 0.2002 -0.2304 0.7902 0.032 Uiso 1 1 calc R . . B109 B 0.13758(15) 0.0048(6) 0.73478(19) 0.0262(14) Uani 1 1 d . . . H109 H 0.1187 0.0197 0.6980 0.031 Uiso 1 1 calc R . . B110 B 0.17332(15) -0.0421(6) 0.7537(2) 0.0274(14) Uani 1 1 d . . . H110 H 0.1777 -0.0440 0.7294 0.033 Uiso 1 1 calc R . . B111 B 0.14877(15) -0.1389(6) 0.7551(2) 0.0284(14) Uani 1 1 d . . . H111 H 0.1342 -0.2117 0.7313 0.034 Uiso 1 1 calc R . . C3A C 0.23074(13) -0.1643(5) 0.88445(18) 0.0264(12) Uani 1 1 d . . . C4A C 0.22865(13) -0.2250(5) 0.91395(18) 0.0276(12) Uani 1 1 d . . . H4Q H 0.2094 -0.2295 0.9075 0.033 Uiso 1 1 calc R . . C5A C 0.25418(14) -0.2785(5) 0.95234(19) 0.0335(14) Uani 1 1 d . . . H5Q H 0.2523 -0.3196 0.9717 0.040 Uiso 1 1 calc R . . C6A C 0.28278(15) -0.2716(5) 0.9624(2) 0.0392(15) Uani 1 1 d . . . H6Q H 0.3005 -0.3057 0.9891 0.047 Uiso 1 1 calc R . . C7A C 0.28499(14) -0.2146(6) 0.9331(2) 0.0396(15) Uani 1 1 d . . . H7Q H 0.3042 -0.2112 0.9394 0.048 Uiso 1 1 calc R . . C8A C 0.25917(13) -0.1621(5) 0.8943(2) 0.0348(14) Uani 1 1 d . . . H8Q H 0.2610 -0.1242 0.8743 0.042 Uiso 1 1 calc R . . C301 C 0.18046(13) -0.0241(5) 0.89505(18) 0.0299(13) Uani 1 1 d . . . O301 O 0.18080(10) -0.0601(4) 0.92298(13) 0.0392(10) Uani 1 1 d . . . C302 C 0.22436(13) 0.0998(5) 0.89273(17) 0.0242(12) Uani 1 1 d . . . O302 O 0.24936(9) 0.1296(4) 0.91770(12) 0.0325(9) Uani 1 1 d . . . C303 C 0.16938(12) 0.1882(5) 0.86634(16) 0.0242(12) Uani 1 1 d . . . O303 O 0.16615(9) 0.2521(3) 0.88680(12) 0.0283(9) Uani 1 1 d . . . Mn2 Mn 0.109598(18) 0.04507(8) 0.78999(3) 0.02633(19) Uani 1 1 d . . . C401 C 0.10873(13) -0.0534(5) 0.82541(19) 0.0300(13) Uani 1 1 d . . . O401 O 0.10796(10) -0.1178(4) 0.84751(15) 0.0432(11) Uani 1 1 d . . . C402 C 0.06860(14) 0.0315(6) 0.7436(2) 0.0348(14) Uani 1 1 d . . . O402 O 0.04320(10) 0.0213(5) 0.71434(15) 0.0516(13) Uani 1 1 d . . . C403 C 0.10221(12) 0.1677(6) 0.81182(18) 0.0300(13) Uani 1 1 d . . . O403 O 0.09626(10) 0.2405(4) 0.82537(15) 0.0440(11) Uani 1 1 d . . . Pt2 Pt 0.168112(4) 0.261704(18) 0.807789(6) 0.01890(6) Uani 1 1 d . . . P3 P 0.20063(3) 0.41053(12) 0.85168(4) 0.0200(3) Uani 1 1 d . . . P4 P 0.14293(3) 0.40217(13) 0.75333(4) 0.0216(3) Uani 1 1 d . . . C115 C 0.17046(12) 0.5211(5) 0.77094(17) 0.0259(12) Uani 1 1 d . . . H11B H 0.1862 0.4967 0.7686 0.031 Uiso 1 1 calc R . . H11C H 0.1597 0.5908 0.7520 0.031 Uiso 1 1 calc R . . C116 C 0.18530(12) 0.5469(5) 0.81990(17) 0.0261(12) Uani 1 1 d . . . H11D H 0.1698 0.5799 0.8215 0.031 Uiso 1 1 calc R . . H11E H 0.2021 0.6044 0.8327 0.031 Uiso 1 1 calc R . . C121 C 0.23686(11) 0.4002(5) 0.86156(16) 0.0233(12) Uani 1 1 d . . . C122 C 0.24303(12) 0.3071(5) 0.84560(17) 0.0283(12) Uani 1 1 d . . . H12A H 0.2295 0.2419 0.8323 0.034 Uiso 1 1 calc R . . C123 C 0.26924(14) 0.3101(6) 0.84928(19) 0.0353(14) Uani 1 1 d . . . H12B H 0.2736 0.2460 0.8386 0.042 Uiso 1 1 calc R . . C124 C 0.28871(13) 0.4029(6) 0.86782(19) 0.0372(15) Uani 1 1 d . . . H12C H 0.3063 0.4037 0.8696 0.045 Uiso 1 1 calc R . . C125 C 0.28291(13) 0.4965(6) 0.88414(19) 0.0359(15) Uani 1 1 d . . . H12D H 0.2966 0.5612 0.8973 0.043 Uiso 1 1 calc R . . C126 C 0.25684(12) 0.4953(5) 0.88114(18) 0.0296(13) Uani 1 1 d . . . H12E H 0.2528 0.5589 0.8924 0.035 Uiso 1 1 calc R . . C131 C 0.20991(11) 0.4445(5) 0.90495(16) 0.0224(11) Uani 1 1 d . . . C132 C 0.23621(12) 0.3989(5) 0.94505(17) 0.0259(12) Uani 1 1 d . . . H13A H 0.2500 0.3518 0.9450 0.031 Uiso 1 1 calc R . . C133 C 0.24218(14) 0.4229(5) 0.98537(18) 0.0329(14) Uani 1 1 d . . . H13B H 0.2600 0.3913 1.0126 0.039 Uiso 1 1 calc R . . C134 C 0.22243(15) 0.4917(5) 0.98601(19) 0.0336(14) Uani 1 1 d . . . H13C H 0.2270 0.5089 1.0137 0.040 Uiso 1 1 calc R . . C135 C 0.19592(14) 0.5359(5) 0.94616(19) 0.0329(13) Uani 1 1 d . . . H13D H 0.1822 0.5828 0.9465 0.039 Uiso 1 1 calc R . . C136 C 0.18956(13) 0.5113(5) 0.90588(18) 0.0290(13) Uani 1 1 d . . . H13E H 0.1712 0.5401 0.8786 0.035 Uiso 1 1 calc R . . C141 C 0.11374(12) 0.4768(5) 0.75198(17) 0.0256(12) Uani 1 1 d . . . C142 C 0.09455(14) 0.5606(6) 0.71848(19) 0.0374(15) Uani 1 1 d . . . H14A H 0.0955 0.5735 0.6952 0.045 Uiso 1 1 calc R . . C143 C 0.07442(16) 0.6237(7) 0.7197(2) 0.0512(19) Uani 1 1 d . . . H14B H 0.0612 0.6792 0.6969 0.061 Uiso 1 1 calc R . . C144 C 0.07337(16) 0.6066(7) 0.7541(2) 0.0499(19) Uani 1 1 d . . . H14C H 0.0597 0.6519 0.7551 0.060 Uiso 1 1 calc R . . C145 C 0.09187(14) 0.5252(6) 0.78693(19) 0.0371(15) Uani 1 1 d . . . H14D H 0.0908 0.5135 0.8102 0.045 Uiso 1 1 calc R . . C146 C 0.11223(12) 0.4598(5) 0.78601(17) 0.0284(13) Uani 1 1 d . . . H14E H 0.1251 0.4035 0.8087 0.034 Uiso 1 1 calc R . . C151 C 0.12385(12) 0.3732(5) 0.69484(16) 0.0261(12) Uani 1 1 d . . . C152 C 0.10109(14) 0.2889(6) 0.67335(18) 0.0341(14) Uani 1 1 d . . . H15C H 0.0974 0.2437 0.6901 0.041 Uiso 1 1 calc R . . C153 C 0.08354(15) 0.2694(6) 0.6276(2) 0.0443(17) Uani 1 1 d . . . H15D H 0.0683 0.2100 0.6132 0.053 Uiso 1 1 calc R . . C154 C 0.08863(16) 0.3388(6) 0.6031(2) 0.0447(17) Uani 1 1 d . . . H15E H 0.0767 0.3271 0.5718 0.054 Uiso 1 1 calc R . . C155 C 0.11107(15) 0.4243(7) 0.6246(2) 0.0430(16) Uani 1 1 d . . . H15F H 0.1145 0.4708 0.6078 0.052 Uiso 1 1 calc R . . C156 C 0.12861(14) 0.4427(6) 0.67028(19) 0.0339(14) Uani 1 1 d . . . H15G H 0.1438 0.5024 0.6847 0.041 Uiso 1 1 calc R . . Cl2S Cl 0.07077(17) -0.3032(9) 0.5849(3) 0.0718(19) Uani 0.535(7) 1 d PDU A 1 Cl1S Cl 0.02458(13) -0.4508(5) 0.52794(17) 0.091(2) Uani 0.535(7) 1 d PD . 1 C1S C 0.0425(4) -0.387(2) 0.5806(6) 0.074(6) Uani 0.535(7) 1 d PDU A 1 H1SA H 0.0519 -0.4464 0.6046 0.089 Uiso 0.535(7) 1 calc PR A 1 H1SB H 0.0282 -0.3379 0.5806 0.089 Uiso 0.535(7) 1 calc PR A 1 Cl2A Cl 0.03824(12) -0.4737(6) 0.5959(2) 0.086(2) Uani 0.465(7) 1 d PD A 2 Cl1A Cl 0.0723(3) -0.3079(13) 0.6025(6) 0.135(6) Uani 0.465(7) 1 d PDU A 2 C1SA C 0.0393(8) -0.385(3) 0.5596(7) 0.172(17) Uani 0.465(7) 1 d PDU A 2 H1SC H 0.0423 -0.4299 0.5408 0.207 Uiso 0.465(7) 1 calc PR A 2 H1SD H 0.0210 -0.3338 0.5404 0.207 Uiso 0.465(7) 1 calc PR A 2 Cl8S Cl 0.0565(2) -0.3842(10) 0.3358(3) 0.092(3) Uani 0.25 1 d PD B 2 Cl7S Cl 0.0016(3) -0.5229(11) 0.2697(4) 0.102(4) Uani 0.25 1 d PD . 2 C4S C 0.0261(7) -0.468(3) 0.3249(9) 0.110(17) Uani 0.25 1 d PD B 2 H4SA H 0.0348 -0.5341 0.3463 0.132 Uiso 0.25 1 calc PR B 2 H4SB H 0.0140 -0.4195 0.3297 0.132 Uiso 0.25 1 calc PR B 2 C3S C 0.2543(4) 0.127(2) 0.7296(7) 0.033(2) Uani 0.26 1 d PD C 1 H3SA H 0.2520 0.0416 0.7265 0.040 Uiso 0.26 1 calc PR C 1 H3SF H 0.2541 0.1528 0.7050 0.040 Uiso 0.26 1 calc PR C 1 Cl5S Cl 0.2915(3) 0.1432(15) 0.7751(4) 0.055(3) Uani 0.26 1 d PDU C 1 Cl6S Cl 0.2178(7) 0.174(3) 0.7108(11) 0.39(2) Uani 0.26 1 d PDU C 1 C3SA C 0.2564(4) 0.0644(16) 0.7346(6) 0.033(2) Uani 0.32 1 d PD D 2 H3SB H 0.2612 0.0006 0.7228 0.040 Uiso 0.32 1 calc PR D 2 H3SC H 0.2406 0.1158 0.7095 0.040 Uiso 0.32 1 calc PR D 2 Cl6A Cl 0.24369(16) 0.0093(6) 0.7620(3) 0.077(2) Uani 0.32 1 d PD D 2 Cl5A Cl 0.2868(5) 0.137(2) 0.7728(7) 0.162(9) Uani 0.32 1 d PDU D 2 C3SB C 0.1748(3) 0.2004(11) 0.6831(4) 0.033(2) Uani 0.42 1 d PD E 3 H3SD H 0.1765 0.1339 0.7008 0.040 Uiso 0.42 1 calc PR E 3 H3SE H 0.1540 0.2345 0.6667 0.040 Uiso 0.42 1 calc PR E 3 Cl5B Cl 0.20319(10) 0.3092(4) 0.72151(14) 0.0576(12) Uani 0.42 1 d PD E 3 Cl6B Cl 0.17783(13) 0.1517(4) 0.64697(16) 0.0598(12) Uani 0.42 1 d PD E 3 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 0.0211(2) 0.0191(3) 0.0196(2) -0.00220(17) 0.01411(18) -0.00279(18) C2 0.030(3) 0.022(3) 0.025(3) -0.002(2) 0.019(2) -0.001(2) B3 0.024(3) 0.014(3) 0.017(3) -0.001(2) 0.012(2) -0.002(2) B4 0.032(3) 0.023(4) 0.020(3) -0.004(2) 0.017(3) -0.005(3) B5 0.027(3) 0.018(3) 0.024(3) 0.002(2) 0.016(3) 0.000(2) B6 0.025(3) 0.016(3) 0.019(3) 0.001(2) 0.010(2) 0.000(2) B7 0.023(3) 0.017(3) 0.021(3) -0.002(2) 0.015(2) -0.001(2) B8 0.030(3) 0.025(4) 0.026(3) -0.005(3) 0.020(3) -0.003(3) B9 0.020(3) 0.021(4) 0.025(3) 0.005(2) 0.013(2) 0.002(2) B10 0.033(3) 0.014(3) 0.030(3) 0.000(2) 0.025(3) 0.003(2) B11 0.035(3) 0.016(3) 0.022(3) -0.001(2) 0.018(3) 0.002(3) C3 0.026(3) 0.019(3) 0.024(3) -0.006(2) 0.014(2) -0.003(2) C4 0.038(3) 0.030(4) 0.028(3) -0.004(2) 0.021(3) -0.002(3) C5 0.035(3) 0.040(4) 0.028(3) -0.004(3) 0.014(3) 0.003(3) C6 0.025(3) 0.027(4) 0.043(3) -0.013(3) 0.013(3) -0.003(3) C7 0.031(3) 0.027(4) 0.043(3) -0.003(3) 0.024(3) 0.000(3) C8 0.032(3) 0.017(3) 0.035(3) -0.004(2) 0.023(3) -0.001(2) C101 0.026(3) 0.024(3) 0.032(3) -0.008(2) 0.018(3) -0.006(2) O101 0.025(2) 0.043(3) 0.030(2) -0.0031(19) 0.0064(19) 0.0034(19) C102 0.036(3) 0.029(4) 0.032(3) -0.007(2) 0.022(3) -0.003(3) O102 0.052(3) 0.046(3) 0.056(3) -0.015(2) 0.044(2) -0.019(2) C103 0.023(3) 0.028(3) 0.021(2) 0.002(2) 0.015(2) 0.002(2) O103 0.034(2) 0.030(2) 0.0269(19) 0.0012(17) 0.0225(18) 0.0021(18) Mn1 0.0278(4) 0.0258(5) 0.0181(4) -0.0004(3) 0.0154(3) -0.0017(4) C201 0.041(3) 0.035(4) 0.026(3) -0.008(2) 0.025(3) -0.008(3) O201 0.071(3) 0.053(3) 0.043(3) -0.007(2) 0.044(3) -0.025(3) C202 0.037(3) 0.027(3) 0.030(3) -0.002(2) 0.026(3) 0.001(3) O202 0.033(2) 0.044(3) 0.0219(19) 0.0043(18) 0.0123(18) 0.007(2) C203 0.023(3) 0.033(4) 0.022(2) 0.000(2) 0.016(2) -0.004(2) O203 0.038(2) 0.036(3) 0.034(2) -0.0064(19) 0.0257(19) 0.0010(19) Pt1 0.01725(9) 0.01689(12) 0.01790(9) -0.00104(7) 0.01103(8) -0.00065(8) P1 0.0178(6) 0.0189(8) 0.0188(6) -0.0020(5) 0.0115(5) -0.0004(5) P2 0.0194(6) 0.0195(8) 0.0180(6) -0.0012(5) 0.0112(5) -0.0016(5) C15 0.029(3) 0.019(3) 0.028(3) 0.001(2) 0.017(2) -0.005(2) C16 0.022(3) 0.024(3) 0.025(3) -0.003(2) 0.014(2) -0.001(2) C21 0.020(2) 0.025(3) 0.020(2) -0.003(2) 0.013(2) -0.003(2) C22 0.034(3) 0.031(4) 0.026(3) 0.002(2) 0.021(2) 0.006(3) C23 0.038(3) 0.043(4) 0.027(3) 0.004(3) 0.020(3) 0.004(3) C24 0.037(3) 0.049(4) 0.023(3) 0.000(3) 0.019(3) -0.005(3) C25 0.033(3) 0.044(4) 0.029(3) -0.011(3) 0.021(3) -0.004(3) C26 0.024(3) 0.031(4) 0.027(3) 0.001(2) 0.017(2) 0.003(2) C31 0.022(3) 0.015(3) 0.023(2) 0.004(2) 0.013(2) 0.004(2) C32 0.026(3) 0.031(3) 0.023(3) 0.001(2) 0.016(2) 0.003(2) C33 0.041(3) 0.043(4) 0.029(3) 0.000(3) 0.027(3) 0.006(3) C34 0.037(3) 0.041(4) 0.042(3) 0.002(3) 0.031(3) 0.007(3) C35 0.023(3) 0.045(4) 0.033(3) -0.004(3) 0.017(3) -0.002(3) C36 0.026(3) 0.027(3) 0.026(3) -0.004(2) 0.016(2) 0.002(2) C41 0.025(3) 0.028(3) 0.025(3) -0.005(2) 0.015(2) -0.002(2) C42 0.031(3) 0.041(4) 0.030(3) -0.010(3) 0.019(3) -0.010(3) C43 0.044(4) 0.070(6) 0.044(4) -0.029(4) 0.028(3) -0.030(4) C44 0.065(5) 0.094(7) 0.036(4) -0.032(4) 0.031(4) -0.031(5) C45 0.056(5) 0.098(7) 0.040(4) -0.026(4) 0.036(4) -0.032(4) C46 0.046(4) 0.053(5) 0.034(3) -0.017(3) 0.027(3) -0.020(3) C51 0.019(2) 0.026(3) 0.023(2) -0.003(2) 0.015(2) -0.006(2) C52 0.025(3) 0.029(3) 0.036(3) 0.007(3) 0.020(3) 0.003(2) C53 0.028(3) 0.034(4) 0.048(4) 0.001(3) 0.023(3) -0.001(3) C54 0.032(3) 0.032(4) 0.058(4) -0.019(3) 0.035(3) -0.011(3) C55 0.038(3) 0.034(4) 0.037(3) -0.006(3) 0.030(3) -0.007(3) C56 0.030(3) 0.027(3) 0.029(3) -0.002(2) 0.019(2) -0.004(2) Mo2 0.0241(2) 0.0172(3) 0.0183(2) -0.00142(17) 0.01334(18) -0.00197(18) C12 0.027(3) 0.019(3) 0.024(2) 0.000(2) 0.017(2) 0.000(2) B103 0.025(3) 0.025(4) 0.014(2) 0.001(2) 0.010(2) 0.002(3) B104 0.032(3) 0.019(4) 0.020(3) -0.001(2) 0.017(3) 0.001(3) B105 0.026(3) 0.019(4) 0.026(3) -0.001(2) 0.016(3) -0.002(2) B106 0.025(3) 0.026(4) 0.024(3) -0.005(3) 0.015(3) -0.007(3) B107 0.034(3) 0.027(4) 0.019(3) -0.006(2) 0.016(3) -0.008(3) B108 0.037(4) 0.015(3) 0.032(3) -0.009(3) 0.023(3) -0.010(3) B109 0.032(3) 0.026(4) 0.016(3) -0.006(2) 0.014(3) -0.005(3) B110 0.038(4) 0.021(4) 0.026(3) -0.007(3) 0.021(3) -0.005(3) B111 0.034(3) 0.025(4) 0.025(3) -0.006(3) 0.018(3) -0.008(3) C3A 0.033(3) 0.017(3) 0.031(3) -0.005(2) 0.022(3) -0.005(2) C4A 0.036(3) 0.020(3) 0.028(3) -0.002(2) 0.021(3) 0.000(2) C5A 0.043(3) 0.024(3) 0.031(3) -0.003(2) 0.022(3) -0.001(3) C6A 0.041(4) 0.018(3) 0.033(3) -0.002(3) 0.012(3) 0.001(3) C7A 0.032(3) 0.032(4) 0.047(4) 0.000(3) 0.022(3) -0.002(3) C8A 0.035(3) 0.028(4) 0.042(3) 0.002(3) 0.025(3) -0.003(3) C301 0.035(3) 0.024(3) 0.030(3) -0.005(2) 0.020(3) -0.006(3) O301 0.049(3) 0.045(3) 0.030(2) 0.0084(19) 0.028(2) 0.001(2) C302 0.038(3) 0.016(3) 0.025(3) 0.001(2) 0.024(3) 0.000(2) O302 0.027(2) 0.035(3) 0.0221(19) -0.0028(17) 0.0091(17) -0.0035(18) C303 0.025(3) 0.025(3) 0.021(2) 0.006(2) 0.013(2) 0.000(2) O303 0.038(2) 0.027(2) 0.0275(19) -0.0044(16) 0.0246(18) -0.0034(17) Mn2 0.0247(4) 0.0288(5) 0.0245(4) -0.0011(3) 0.0153(4) -0.0040(4) C401 0.027(3) 0.028(4) 0.035(3) 0.003(3) 0.019(3) -0.001(2) O401 0.049(3) 0.042(3) 0.049(3) 0.007(2) 0.036(2) 0.002(2) C402 0.035(3) 0.036(4) 0.035(3) 0.000(3) 0.023(3) -0.010(3) O402 0.028(2) 0.068(4) 0.036(2) 0.004(2) 0.009(2) -0.013(2) C403 0.025(3) 0.033(4) 0.028(3) -0.003(3) 0.015(2) -0.005(3) O403 0.046(3) 0.048(3) 0.042(2) -0.009(2) 0.030(2) -0.003(2) Pt2 0.02016(10) 0.01747(12) 0.01657(9) -0.00207(7) 0.01057(8) -0.00173(8) P3 0.0193(6) 0.0178(8) 0.0178(6) -0.0021(5) 0.0095(5) -0.0010(5) P4 0.0207(6) 0.0234(8) 0.0165(6) -0.0013(5) 0.0099(5) -0.0008(6) C115 0.027(3) 0.017(3) 0.027(3) 0.002(2) 0.015(2) 0.000(2) C116 0.023(3) 0.020(3) 0.027(3) -0.001(2) 0.012(2) 0.000(2) C121 0.017(2) 0.028(3) 0.018(2) 0.001(2) 0.008(2) 0.000(2) C122 0.030(3) 0.029(4) 0.021(2) 0.006(2) 0.014(2) 0.003(2) C123 0.037(3) 0.040(4) 0.035(3) 0.006(3) 0.026(3) 0.008(3) C124 0.028(3) 0.055(5) 0.032(3) 0.008(3) 0.020(3) 0.005(3) C125 0.025(3) 0.043(4) 0.031(3) 0.002(3) 0.014(3) -0.004(3) C126 0.024(3) 0.029(4) 0.029(3) -0.001(2) 0.014(2) -0.002(2) C131 0.021(2) 0.021(3) 0.022(2) -0.006(2) 0.012(2) -0.005(2) C132 0.026(3) 0.023(3) 0.024(3) -0.003(2) 0.013(2) 0.000(2) C133 0.036(3) 0.034(4) 0.023(3) 0.000(2) 0.016(2) -0.003(3) C134 0.053(4) 0.025(4) 0.030(3) -0.005(2) 0.030(3) -0.007(3) C135 0.043(3) 0.027(4) 0.036(3) -0.005(3) 0.029(3) 0.000(3) C136 0.029(3) 0.024(3) 0.026(3) -0.003(2) 0.014(2) 0.000(2) C141 0.025(3) 0.025(3) 0.023(2) -0.001(2) 0.013(2) 0.002(2) C142 0.044(4) 0.042(4) 0.030(3) 0.008(3) 0.025(3) 0.011(3) C143 0.056(4) 0.056(5) 0.043(4) 0.019(3) 0.032(4) 0.030(4) C144 0.052(4) 0.058(5) 0.047(4) 0.010(3) 0.035(4) 0.023(4) C145 0.036(3) 0.045(4) 0.031(3) 0.000(3) 0.022(3) 0.012(3) C146 0.029(3) 0.027(3) 0.022(3) -0.001(2) 0.013(2) 0.003(2) C151 0.031(3) 0.025(3) 0.019(2) -0.002(2) 0.015(2) 0.001(2) C152 0.042(3) 0.034(4) 0.025(3) -0.004(2) 0.020(3) -0.009(3) C153 0.043(4) 0.049(5) 0.025(3) -0.011(3) 0.015(3) -0.014(3) C154 0.053(4) 0.053(5) 0.023(3) -0.006(3) 0.022(3) 0.003(4) C155 0.050(4) 0.056(5) 0.033(3) 0.005(3) 0.032(3) 0.007(4) C156 0.035(3) 0.040(4) 0.030(3) -0.005(3) 0.023(3) -0.004(3) Cl2S 0.052(3) 0.058(4) 0.101(4) 0.019(3) 0.047(3) 0.004(2) Cl1S 0.103(4) 0.096(4) 0.081(3) 0.009(3) 0.062(3) 0.037(3) C1S 0.051(10) 0.127(16) 0.077(13) -0.022(13) 0.056(11) -0.018(11) Cl2A 0.069(3) 0.105(5) 0.104(4) 0.024(3) 0.064(3) 0.016(3) Cl1A 0.147(8) 0.063(5) 0.252(16) 0.051(9) 0.154(11) 0.034(5) C1SA 0.12(2) 0.18(3) 0.07(2) -0.02(2) -0.003(18) -0.01(2) Cl8S 0.091(7) 0.097(8) 0.074(6) -0.011(6) 0.047(6) -0.016(6) Cl7S 0.091(7) 0.110(9) 0.082(7) -0.001(6) 0.044(7) -0.020(7) C4S 0.09(3) 0.06(3) 0.10(3) -0.06(2) 0.03(2) -0.06(2) C3S 0.040(6) 0.009(6) 0.053(6) -0.006(5) 0.031(5) -0.004(5) Cl5S 0.044(5) 0.081(9) 0.041(5) -0.021(5) 0.028(4) -0.027(5) Cl6S 0.77(6) 0.23(3) 0.56(5) 0.01(3) 0.60(5) 0.06(4) C3SA 0.040(6) 0.009(6) 0.053(6) -0.006(5) 0.031(5) -0.004(5) Cl6A 0.063(4) 0.069(5) 0.127(6) 0.019(4) 0.075(5) 0.011(3) Cl5A 0.168(18) 0.20(2) 0.126(14) 0.004(14) 0.097(14) 0.040(15) C3SB 0.040(6) 0.009(6) 0.053(6) -0.006(5) 0.031(5) -0.004(5) Cl5B 0.061(3) 0.063(3) 0.045(2) -0.004(2) 0.032(2) 0.000(2) Cl6B 0.100(4) 0.043(3) 0.070(3) -0.002(2) 0.070(3) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C102 2.044(6) . ? Mo1 C101 2.053(6) . ? Mo1 C103 2.070(6) . ? Mo1 C2 2.223(5) . ? Mo1 B3 2.300(6) . ? Mo1 B6 2.404(6) . ? Mo1 B5 2.433(6) . ? Mo1 B4 2.469(6) . ? Mo1 B7 2.617(6) . ? Mo1 Pt1 2.7318(5) . ? Mo1 Mn1 3.0275(9) . ? C2 C3 1.511(7) . ? C2 B5 1.607(8) . ? C2 B4 1.619(8) . ? C2 B8 1.643(8) . ? B3 H3 1.07(5) . ? B3 B6 1.735(9) . ? B3 B7 1.767(8) . ? B3 B9 1.781(9) . ? B3 Mn1 2.219(6) . ? B3 Pt1 2.260(6) . ? B4 B10 1.822(9) . ? B4 B8 1.829(9) . ? B4 B7 1.895(8) . ? B5 B6 1.810(9) . ? B5 B11 1.847(9) . ? B5 B8 1.858(8) . ? B6 H6 1.12(5) . ? B6 B11 1.757(9) . ? B6 B9 1.806(8) . ? B6 Mn1 2.167(6) . ? B7 H7 1.22(5) . ? B7 B10 1.801(8) . ? B7 B9 1.821(8) . ? B7 Pt1 2.371(6) . ? B8 B10 1.758(9) . ? B8 B11 1.776(8) . ? B9 B10 1.757(8) . ? B9 B11 1.768(9) . ? B10 B11 1.800(8) . ? C3 C4 1.402(7) . ? C3 C8 1.405(8) . ? C4 C5 1.397(8) . ? C5 C6 1.369(9) . ? C6 C7 1.389(8) . ? C7 C8 1.380(8) . ? C101 O101 1.133(6) . ? C102 O102 1.145(7) . ? C103 O103 1.145(6) . ? C103 Pt1 2.516(5) . ? Mn1 H6 1.69(5) . ? Mn1 H3 1.73(5) . ? Mn1 C202 1.786(6) . ? Mn1 C201 1.814(6) . ? Mn1 C203 1.817(6) . ? C201 O201 1.139(7) . ? C202 O202 1.159(6) . ? C203 O203 1.147(6) . ? Pt1 P1 2.2605(13) . ? Pt1 P2 2.2834(13) . ? Pt1 H7 2.44(5) . ? Pt1 H3 2.50(5) . ? P1 C31 1.804(5) . ? P1 C21 1.831(5) . ? P1 C16 1.844(6) . ? P2 C51 1.812(5) . ? P2 C41 1.816(5) . ? P2 C15 1.834(6) . ? C15 C16 1.526(7) . ? C21 C26 1.385(8) . ? C21 C22 1.389(8) . ? C22 C23 1.400(7) . ? C23 C24 1.368(9) . ? C24 C25 1.387(9) . ? C25 C26 1.396(7) . ? C31 C36 1.403(7) . ? C31 C32 1.407(7) . ? C32 C33 1.391(7) . ? C33 C34 1.392(9) . ? C34 C35 1.374(8) . ? C35 C36 1.375(7) . ? C41 C46 1.381(8) . ? C41 C42 1.395(8) . ? C42 C43 1.377(8) . ? C43 C44 1.382(10) . ? C44 C45 1.393(10) . ? C45 C46 1.398(9) . ? C51 C52 1.394(7) . ? C51 C56 1.396(7) . ? C52 C53 1.394(8) . ? C53 C54 1.377(9) . ? C54 C55 1.387(9) . ? C55 C56 1.390(8) . ? Mo2 C301 2.045(6) . ? Mo2 C303 2.049(6) . ? Mo2 C302 2.053(6) . ? Mo2 C12 2.224(5) . ? Mo2 B103 2.281(6) . ? Mo2 B106 2.405(6) . ? Mo2 B104 2.459(6) . ? Mo2 B105 2.459(7) . ? Mo2 B107 2.580(6) . ? Mo2 Pt2 2.7323(5) . ? Mo2 Mn2 3.0588(9) . ? C12 C3A 1.516(7) . ? C12 B105 1.618(8) . ? C12 B104 1.629(8) . ? C12 B108 1.646(8) . ? B103 H103 1.14(5) . ? B103 B106 1.726(9) . ? B103 B107 1.781(9) . ? B103 B109 1.799(8) . ? B103 Mn2 2.223(6) . ? B103 Pt2 2.272(6) . ? B104 B108 1.810(9) . ? B104 B110 1.820(8) . ? B104 B107 1.893(9) . ? B105 B106 1.805(9) . ? B105 B111 1.834(8) . ? B105 B108 1.845(9) . ? B106 H106 1.07(5) . ? B106 B111 1.753(9) . ? B106 B109 1.824(9) . ? B106 Mn2 2.159(7) . ? B107 H107 1.11(6) . ? B107 B110 1.803(9) . ? B107 B109 1.806(9) . ? B107 Pt2 2.382(7) . ? B108 B110 1.756(9) . ? B108 B111 1.764(9) . ? B109 B110 1.734(9) . ? B109 B111 1.761(10) . ? B110 B111 1.802(9) . ? C3A C8A 1.393(8) . ? C3A C4A 1.406(7) . ? C4A C5A 1.389(8) . ? C5A C6A 1.400(9) . ? C6A C7A 1.381(9) . ? C7A C8A 1.397(8) . ? C301 O301 1.146(6) . ? C302 O302 1.141(6) . ? C303 O303 1.176(6) . ? C303 Pt2 2.377(5) . ? Mn2 H106 1.57(6) . ? Mn2 H103 1.74(5) . ? Mn2 C401 1.802(6) . ? Mn2 C402 1.816(6) . ? Mn2 C403 1.822(6) . ? C401 O401 1.152(7) . ? C402 O402 1.131(7) . ? C403 O403 1.145(7) . ? Pt2 P3 2.2790(14) . ? Pt2 P4 2.2894(14) . ? Pt2 H107 2.38(5) . ? Pt2 H103 2.54(5) . ? P3 C131 1.817(5) . ? P3 C121 1.828(5) . ? P3 C116 1.832(6) . ? P4 C151 1.813(5) . ? P4 C141 1.827(6) . ? P4 C115 1.841(6) . ? C115 C116 1.535(7) . ? C121 C122 1.386(8) . ? C121 C126 1.395(8) . ? C122 C123 1.392(8) . ? C123 C124 1.361(9) . ? C124 C125 1.387(9) . ? C125 C126 1.400(8) . ? C131 C132 1.395(7) . ? C131 C136 1.400(8) . ? C132 C133 1.398(7) . ? C133 C134 1.379(8) . ? C134 C135 1.389(8) . ? C135 C136 1.388(8) . ? C141 C146 1.388(7) . ? C141 C142 1.410(8) . ? C142 C143 1.374(9) . ? C143 C144 1.384(9) . ? C144 C145 1.373(9) . ? C145 C146 1.391(8) . ? C151 C152 1.384(8) . ? C151 C156 1.393(8) . ? C152 C153 1.388(8) . ? C153 C154 1.402(9) . ? C154 C155 1.383(10) . ? C155 C156 1.385(8) . ? Cl2S C1S 1.778(14) . ? Cl1S C1S 1.754(13) . ? Cl1S Cl1S 2.448(12) 5_546 ? Cl2A C1SA 1.770(19) . ? Cl1A C1SA 1.747(18) . ? Cl8S C4S 1.768(18) . ? Cl7S Cl7S 1.42(2) 2 ? Cl7S C4S 1.761(18) . ? C3S Cl5S 1.679(16) . ? C3S Cl6S 1.772(19) . ? C3SA Cl5A 1.609(17) . ? C3SA Cl6A 1.732(15) . ? C3SB Cl6B 1.612(12) . ? C3SB Cl5B 1.816(11) . ? 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 C102 Mo1 C101 89.7(2) . . ? C102 Mo1 C103 78.6(2) . . ? C101 Mo1 C103 85.4(2) . . ? C102 Mo1 C2 91.4(2) . . ? C101 Mo1 C2 81.0(2) . . ? C103 Mo1 C2 163.2(2) . . ? C102 Mo1 B3 133.8(2) . . ? C101 Mo1 B3 134.2(2) . . ? C103 Mo1 B3 89.9(2) . . ? C2 Mo1 B3 106.7(2) . . ? C102 Mo1 B6 103.8(2) . . ? C101 Mo1 B6 155.6(2) . . ? C103 Mo1 B6 116.9(2) . . ? C2 Mo1 B6 78.4(2) . . ? B3 Mo1 B6 43.2(2) . . ? C102 Mo1 B5 83.2(2) . . ? C101 Mo1 B5 120.1(2) . . ? C103 Mo1 B5 148.6(2) . . ? C2 Mo1 B5 40.07(19) . . ? B3 Mo1 B5 84.5(2) . . ? B6 Mo1 B5 44.0(2) . . ? C102 Mo1 B4 130.4(2) . . ? C101 Mo1 B4 76.3(2) . . ? C103 Mo1 B4 144.6(2) . . ? C2 Mo1 B4 39.9(2) . . ? B3 Mo1 B4 82.0(2) . . ? B6 Mo1 B4 79.5(2) . . ? B5 Mo1 B4 65.0(2) . . ? C102 Mo1 B7 165.3(2) . . ? C101 Mo1 B7 100.0(2) . . ? C103 Mo1 B7 112.9(2) . . ? C2 Mo1 B7 79.36(19) . . ? B3 Mo1 B7 41.50(18) . . ? B6 Mo1 B7 63.4(2) . . ? B5 Mo1 B7 82.4(2) . . ? B4 Mo1 B7 43.63(19) . . ? C102 Mo1 Pt1 139.95(17) . . ? C101 Mo1 Pt1 86.23(16) . . ? C103 Mo1 Pt1 61.37(15) . . ? C2 Mo1 Pt1 127.00(14) . . ? B3 Mo1 Pt1 52.53(15) . . ? B6 Mo1 Pt1 95.66(15) . . ? B5 Mo1 Pt1 132.34(15) . . ? B4 Mo1 Pt1 87.07(15) . . ? B7 Mo1 Pt1 52.57(13) . . ? C102 Mo1 Mn1 87.32(16) . . ? C101 Mo1 Mn1 157.86(16) . . ? C103 Mo1 Mn1 72.48(14) . . ? C2 Mo1 Mn1 120.94(14) . . ? B3 Mo1 Mn1 46.81(14) . . ? B6 Mo1 Mn1 45.24(14) . . ? B5 Mo1 Mn1 81.35(14) . . ? B4 Mo1 Mn1 121.49(15) . . ? B7 Mo1 Mn1 87.72(12) . . ? Pt1 Mo1 Mn1 82.06(2) . . ? C3 C2 B5 124.1(5) . . ? C3 C2 B4 124.8(4) . . ? B5 C2 B4 109.5(4) . . ? C3 C2 B8 117.1(4) . . ? B5 C2 B8 69.7(4) . . ? B4 C2 B8 68.2(4) . . ? C3 C2 Mo1 123.2(4) . . ? B5 C2 Mo1 77.0(3) . . ? B4 C2 Mo1 78.3(3) . . ? B8 C2 Mo1 119.8(4) . . ? H3 B3 B6 110(3) . . ? H3 B3 B7 151(3) . . ? B6 B3 B7 98.0(4) . . ? H3 B3 B9 124(3) . . ? B6 B3 B9 61.8(4) . . ? B7 B3 B9 61.7(3) . . ? H3 B3 Mn1 49(3) . . ? B6 B3 Mn1 65.1(3) . . ? B7 B3 Mn1 159.3(4) . . ? B9 B3 Mn1 114.8(3) . . ? H3 B3 Pt1 90(3) . . ? B6 B3 Pt1 144.9(4) . . ? B7 B3 Pt1 70.9(3) . . ? B9 B3 Pt1 129.7(3) . . ? Mn1 B3 Pt1 115.5(3) . . ? H3 B3 Mo1 118(3) . . ? B6 B3 Mo1 71.6(3) . . ? B7 B3 Mo1 78.9(3) . . ? B9 B3 Mo1 110.9(3) . . ? Mn1 B3 Mo1 84.1(2) . . ? Pt1 B3 Mo1 73.61(17) . . ? C2 B4 B10 108.1(4) . . ? C2 B4 B8 56.5(3) . . ? B10 B4 B8 57.6(3) . . ? C2 B4 B7 124.0(4) . . ? B10 B4 B7 57.9(3) . . ? B8 B4 B7 107.9(4) . . ? C2 B4 Mo1 61.8(3) . . ? B10 B4 Mo1 108.8(3) . . ? B8 B4 Mo1 101.6(3) . . ? B7 B4 Mo1 72.3(2) . . ? C2 B5 B6 117.8(5) . . ? C2 B5 B11 107.3(4) . . ? B6 B5 B11 57.4(3) . . ? C2 B5 B8 56.0(3) . . ? B6 B5 B8 104.0(4) . . ? B11 B5 B8 57.3(3) . . ? C2 B5 Mo1 62.9(3) . . ? B6 B5 Mo1 67.2(3) . . ? B11 B5 Mo1 108.2(3) . . ? B8 B5 Mo1 102.1(3) . . ? H6 B6 B3 106(3) . . ? H6 B6 B11 115(3) . . ? B3 B6 B11 115.7(4) . . ? H6 B6 B9 112(3) . . ? B3 B6 B9 60.4(3) . . ? B11 B6 B9 59.5(4) . . ? H6 B6 B5 122(3) . . ? B3 B6 B5 127.7(4) . . ? B11 B6 B5 62.3(3) . . ? B9 B6 B5 112.4(4) . . ? H6 B6 Mn1 51(3) . . ? B3 B6 Mn1 68.3(3) . . ? B11 B6 Mn1 164.3(4) . . ? B9 B6 Mn1 116.2(4) . . ? B5 B6 Mn1 128.6(4) . . ? H6 B6 Mo1 129(3) . . ? B3 B6 Mo1 65.2(3) . . ? B11 B6 Mo1 112.8(3) . . ? B9 B6 Mo1 105.7(3) . . ? B5 B6 Mo1 68.9(3) . . ? Mn1 B6 Mo1 82.8(2) . . ? H7 B7 B3 130(3) . . ? H7 B7 B10 110(2) . . ? B3 B7 B10 111.2(4) . . ? H7 B7 B9 129(2) . . ? B3 B7 B9 59.5(3) . . ? B10 B7 B9 58.0(3) . . ? H7 B7 B4 107(2) . . ? B3 B7 B4 117.4(4) . . ? B10 B7 B4 59.0(3) . . ? B9 B7 B4 105.5(4) . . ? H7 B7 Pt1 79(2) . . ? B3 B7 Pt1 64.3(3) . . ? B10 B7 Pt1 169.8(4) . . ? B9 B7 Pt1 121.3(3) . . ? B4 B7 Pt1 114.0(3) . . ? H7 B7 Mo1 132(2) . . ? B3 B7 Mo1 59.6(2) . . ? B10 B7 Mo1 103.6(3) . . ? B9 B7 Mo1 97.4(3) . . ? B4 B7 Mo1 64.0(2) . . ? Pt1 B7 Mo1 66.19(14) . . ? C2 B8 B10 110.0(5) . . ? C2 B8 B11 109.1(4) . . ? B10 B8 B11 61.3(3) . . ? C2 B8 B4 55.3(3) . . ? B10 B8 B4 61.0(4) . . ? B11 B8 B4 103.7(4) . . ? C2 B8 B5 54.2(3) . . ? B10 B8 B5 104.5(4) . . ? B11 B8 B5 61.0(3) . . ? B4 B8 B5 91.2(4) . . ? B10 B9 B11 61.4(3) . . ? B10 B9 B3 112.6(4) . . ? B11 B9 B3 112.9(4) . . ? B10 B9 B6 101.3(4) . . ? B11 B9 B6 58.9(3) . . ? B3 B9 B6 57.9(3) . . ? B10 B9 B7 60.4(3) . . ? B11 B9 B7 106.3(4) . . ? B3 B9 B7 58.8(3) . . ? B6 B9 B7 93.6(4) . . ? B9 B10 B8 114.2(4) . . ? B9 B10 B11 59.6(3) . . ? B8 B10 B11 59.9(3) . . ? B9 B10 B7 61.5(3) . . ? B8 B10 B7 115.6(4) . . ? B11 B10 B7 105.8(4) . . ? B9 B10 B4 111.6(4) . . ? B8 B10 B4 61.4(4) . . ? B11 B10 B4 103.0(4) . . ? B7 B10 B4 63.1(3) . . ? B6 B11 B9 61.6(4) . . ? B6 B11 B8 109.9(4) . . ? B9 B11 B8 112.8(4) . . ? B6 B11 B10 101.5(4) . . ? B9 B11 B10 59.0(3) . . ? B8 B11 B10 58.9(3) . . ? B6 B11 B5 60.2(3) . . ? B9 B11 B5 112.4(4) . . ? B8 B11 B5 61.7(3) . . ? B10 B11 B5 103.3(4) . . ? C4 C3 C8 117.2(5) . . ? C4 C3 C2 121.3(5) . . ? C8 C3 C2 121.5(5) . . ? C5 C4 C3 120.7(6) . . ? C6 C5 C4 120.7(6) . . ? C5 C6 C7 119.8(6) . . ? C8 C7 C6 120.0(6) . . ? C7 C8 C3 121.6(5) . . ? O101 C101 Mo1 176.7(5) . . ? O102 C102 Mo1 176.7(6) . . ? O103 C103 Mo1 166.3(5) . . ? O103 C103 Pt1 120.1(4) . . ? Mo1 C103 Pt1 72.39(15) . . ? H6 Mn1 H3 90(3) . . ? H6 Mn1 C202 86.5(18) . . ? H3 Mn1 C202 99.5(17) . . ? H6 Mn1 C201 89.1(18) . . ? H3 Mn1 C201 165.4(17) . . ? C202 Mn1 C201 95.0(3) . . ? H6 Mn1 C203 173.8(19) . . ? H3 Mn1 C203 91.5(18) . . ? C202 Mn1 C203 87.3(2) . . ? C201 Mn1 C203 90.8(2) . . ? H6 Mn1 B6 30.7(18) . . ? H3 Mn1 B6 72.3(18) . . ? C202 Mn1 B6 113.6(2) . . ? C201 Mn1 B6 100.4(2) . . ? C203 Mn1 B6 154.9(2) . . ? H6 Mn1 B3 71.1(18) . . ? H3 Mn1 B3 28.0(18) . . ? C202 Mn1 B3 117.3(2) . . ? C201 Mn1 B3 140.0(2) . . ? C203 Mn1 B3 112.5(2) . . ? B6 Mn1 B3 46.6(2) . . ? H6 Mn1 Mo1 81.0(18) . . ? H3 Mn1 Mo1 70.9(17) . . ? C202 Mn1 Mo1 164.08(17) . . ? C201 Mn1 Mo1 94.65(18) . . ? C203 Mn1 Mo1 105.19(16) . . ? B6 Mn1 Mo1 51.99(16) . . ? B3 Mn1 Mo1 49.07(15) . . ? O201 C201 Mn1 177.1(6) . . ? O202 C202 Mn1 179.2(5) . . ? O203 C203 Mn1 176.1(5) . . ? B3 Pt1 P1 172.00(15) . . ? B3 Pt1 P2 102.30(15) . . ? P1 Pt1 P2 84.55(5) . . ? B3 Pt1 B7 44.8(2) . . ? P1 Pt1 B7 138.47(14) . . ? P2 Pt1 B7 101.25(15) . . ? B3 Pt1 H7 70.6(12) . . ? P1 Pt1 H7 114.9(12) . . ? P2 Pt1 H7 82.1(12) . . ? B7 Pt1 H7 29.3(12) . . ? B3 Pt1 H3 25.2(12) . . ? P1 Pt1 H3 153.0(12) . . ? P2 Pt1 H3 90.4(12) . . ? B7 Pt1 H3 68.6(12) . . ? H7 Pt1 H3 90.6(17) . . ? B3 Pt1 C103 80.46(19) . . ? P1 Pt1 C103 91.61(13) . . ? P2 Pt1 C103 141.54(13) . . ? B7 Pt1 C103 106.58(19) . . ? H7 Pt1 C103 132.8(13) . . ? H3 Pt1 C103 76.0(11) . . ? B3 Pt1 Mo1 53.86(15) . . ? P1 Pt1 Mo1 119.41(4) . . ? P2 Pt1 Mo1 156.04(4) . . ? B7 Pt1 Mo1 61.23(14) . . ? H7 Pt1 Mo1 86.7(13) . . ? H3 Pt1 Mo1 68.5(12) . . ? C103 Pt1 Mo1 46.24(13) . . ? C31 P1 C21 105.7(2) . . ? C31 P1 C16 106.2(2) . . ? C21 P1 C16 102.7(2) . . ? C31 P1 Pt1 120.52(17) . . ? C21 P1 Pt1 112.35(18) . . ? C16 P1 Pt1 107.83(17) . . ? C51 P2 C41 105.7(2) . . ? C51 P2 C15 108.2(2) . . ? C41 P2 C15 103.1(3) . . ? C51 P2 Pt1 117.12(18) . . ? C41 P2 Pt1 113.80(19) . . ? C15 P2 Pt1 107.93(18) . . ? C16 C15 P2 106.4(4) . . ? C15 C16 P1 107.4(4) . . ? C26 C21 C22 119.7(5) . . ? C26 C21 P1 121.5(4) . . ? C22 C21 P1 118.8(4) . . ? C21 C22 C23 120.0(5) . . ? C24 C23 C22 120.3(6) . . ? C23 C24 C25 119.8(5) . . ? C24 C25 C26 120.6(6) . . ? C21 C26 C25 119.6(5) . . ? C36 C31 C32 118.4(5) . . ? C36 C31 P1 120.3(4) . . ? C32 C31 P1 121.1(4) . . ? C33 C32 C31 119.7(5) . . ? C32 C33 C34 120.3(5) . . ? C35 C34 C33 120.3(5) . . ? C34 C35 C36 120.0(5) . . ? C35 C36 C31 121.4(5) . . ? C46 C41 C42 119.3(5) . . ? C46 C41 P2 119.8(4) . . ? C42 C41 P2 120.8(4) . . ? C43 C42 C41 120.2(6) . . ? C42 C43 C44 120.3(6) . . ? C43 C44 C45 120.4(6) . . ? C44 C45 C46 118.7(6) . . ? C41 C46 C45 120.9(6) . . ? C52 C51 C56 119.8(5) . . ? C52 C51 P2 118.5(4) . . ? C56 C51 P2 121.7(4) . . ? C53 C52 C51 119.8(5) . . ? C54 C53 C52 120.4(6) . . ? C53 C54 C55 120.0(5) . . ? C54 C55 C56 120.4(5) . . ? C55 C56 C51 119.6(5) . . ? C301 Mo2 C303 78.3(2) . . ? C301 Mo2 C302 90.4(2) . . ? C303 Mo2 C302 84.8(2) . . ? C301 Mo2 C12 94.1(2) . . ? C303 Mo2 C12 163.95(19) . . ? C302 Mo2 C12 81.1(2) . . ? C301 Mo2 B103 131.2(2) . . ? C303 Mo2 B103 87.9(2) . . ? C302 Mo2 B103 135.1(2) . . ? C12 Mo2 B103 107.6(2) . . ? C301 Mo2 B106 104.0(2) . . ? C303 Mo2 B106 117.0(2) . . ? C302 Mo2 B106 155.6(2) . . ? C12 Mo2 B106 78.4(2) . . ? B103 Mo2 B106 43.1(2) . . ? C301 Mo2 B104 133.4(2) . . ? C303 Mo2 B104 142.0(2) . . ? C302 Mo2 B104 76.2(2) . . ? C12 Mo2 B104 40.33(19) . . ? B103 Mo2 B104 83.1(2) . . ? B106 Mo2 B104 79.6(2) . . ? C301 Mo2 B105 85.8(2) . . ? C303 Mo2 B105 150.5(2) . . ? C302 Mo2 B105 120.2(2) . . ? C12 Mo2 B105 40.02(19) . . ? B103 Mo2 B105 84.2(2) . . ? B106 Mo2 B105 43.5(2) . . ? B104 Mo2 B105 64.9(2) . . ? C301 Mo2 B107 167.3(2) . . ? C303 Mo2 B107 109.9(2) . . ? C302 Mo2 B107 99.9(2) . . ? C12 Mo2 B107 80.2(2) . . ? B103 Mo2 B107 42.4(2) . . ? B106 Mo2 B107 63.8(2) . . ? B104 Mo2 B107 44.1(2) . . ? B105 Mo2 B107 82.6(2) . . ? C301 Mo2 Pt2 135.80(17) . . ? C303 Mo2 Pt2 57.51(14) . . ? C302 Mo2 Pt2 86.64(15) . . ? C12 Mo2 Pt2 128.74(13) . . ? B103 Mo2 Pt2 52.97(17) . . ? B106 Mo2 Pt2 96.01(16) . . ? B104 Mo2 Pt2 88.41(15) . . ? B105 Mo2 Pt2 132.75(14) . . ? B107 Mo2 Pt2 53.19(16) . . ? C301 Mo2 Mn2 84.81(16) . . ? C303 Mo2 Mn2 73.97(15) . . ? C302 Mo2 Mn2 158.78(15) . . ? C12 Mo2 Mn2 119.81(14) . . ? B103 Mo2 Mn2 46.44(16) . . ? B106 Mo2 Mn2 44.59(16) . . ? B104 Mo2 Mn2 121.45(14) . . ? B105 Mo2 Mn2 80.10(14) . . ? B107 Mo2 Mn2 88.18(15) . . ? Pt2 Mo2 Mn2 82.55(2) . . ? C3A C12 B105 124.1(5) . . ? C3A C12 B104 125.5(5) . . ? B105 C12 B104 108.8(4) . . ? C3A C12 B108 118.5(5) . . ? B105 C12 B108 68.8(4) . . ? B104 C12 B108 67.1(4) . . ? C3A C12 Mo2 123.1(3) . . ? B105 C12 Mo2 77.8(3) . . ? B104 C12 Mo2 77.6(3) . . ? B108 C12 Mo2 118.5(4) . . ? H103 B103 B106 111(3) . . ? H103 B103 B107 150(3) . . ? B106 B103 B107 97.5(4) . . ? H103 B103 B109 124(3) . . ? B106 B103 B109 62.3(4) . . ? B107 B103 B109 60.6(3) . . ? H103 B103 Mn2 51(3) . . ? B106 B103 Mn2 64.9(3) . . ? B107 B103 Mn2 159.0(4) . . ? B109 B103 Mn2 115.2(4) . . ? H103 B103 Pt2 90(3) . . ? B106 B103 Pt2 145.7(4) . . ? B107 B103 Pt2 70.8(3) . . ? B109 B103 Pt2 128.1(4) . . ? Mn2 B103 Pt2 116.8(3) . . ? H103 B103 Mo2 120(3) . . ? B106 B103 Mo2 72.3(3) . . ? B107 B103 Mo2 77.8(3) . . ? B109 B103 Mo2 110.4(4) . . ? Mn2 B103 Mo2 85.5(2) . . ? Pt2 B103 Mo2 73.76(17) . . ? C12 B104 B108 56.9(3) . . ? C12 B104 B110 108.9(5) . . ? B108 B104 B110 57.9(3) . . ? C12 B104 B107 123.6(5) . . ? B108 B104 B107 107.8(4) . . ? B110 B104 B107 58.1(3) . . ? C12 B104 Mo2 62.1(3) . . ? B108 B104 Mo2 101.8(3) . . ? B110 B104 Mo2 108.8(4) . . ? B107 B104 Mo2 71.4(3) . . ? C12 B105 B106 117.6(5) . . ? C12 B105 B111 107.6(4) . . ? B106 B105 B111 57.6(3) . . ? C12 B105 B108 56.3(3) . . ? B106 B105 B108 103.9(4) . . ? B111 B105 B108 57.3(3) . . ? C12 B105 Mo2 62.1(3) . . ? B106 B105 Mo2 66.6(3) . . ? B111 B105 Mo2 107.2(4) . . ? B108 B105 Mo2 100.7(3) . . ? H106 B106 B103 107(3) . . ? H106 B106 B111 123(3) . . ? B103 B106 B111 116.0(5) . . ? H106 B106 B105 115(3) . . ? B103 B106 B105 128.5(5) . . ? B111 B106 B105 62.1(4) . . ? H106 B106 B109 125(3) . . ? B103 B106 B109 60.8(3) . . ? B111 B106 B109 59.0(4) . . ? B105 B106 B109 111.7(4) . . ? H106 B106 Mn2 44(3) . . ? B103 B106 Mn2 68.8(3) . . ? B111 B106 Mn2 163.4(4) . . ? B105 B106 Mn2 128.9(4) . . ? B109 B106 Mn2 117.1(4) . . ? H106 B106 Mo2 119(3) . . ? B103 B106 Mo2 64.6(3) . . ? B111 B106 Mo2 112.5(4) . . ? B105 B106 Mo2 69.8(3) . . ? B109 B106 Mo2 104.5(3) . . ? Mn2 B106 Mo2 84.0(2) . . ? H107 B107 B103 126(3) . . ? H107 B107 B110 112(3) . . ? B103 B107 B110 111.3(5) . . ? H107 B107 B109 125(3) . . ? B103 B107 B109 60.2(3) . . ? B110 B107 B109 57.4(4) . . ? H107 B107 B104 112(3) . . ? B103 B107 B104 117.7(4) . . ? B110 B107 B104 58.9(3) . . ? B109 B107 B104 105.2(5) . . ? H107 B107 Pt2 77(3) . . ? B103 B107 Pt2 64.3(3) . . ? B110 B107 Pt2 171.2(4) . . ? B109 B107 Pt2 121.6(4) . . ? B104 B107 Pt2 115.5(3) . . ? H107 B107 Mo2 134(3) . . ? B103 B107 Mo2 59.8(2) . . ? B110 B107 Mo2 104.6(4) . . ? B109 B107 Mo2 98.5(3) . . ? B104 B107 Mo2 64.6(2) . . ? Pt2 B107 Mo2 66.68(15) . . ? C12 B108 B110 111.2(5) . . ? C12 B108 B111 109.7(5) . . ? B110 B108 B111 61.6(4) . . ? C12 B108 B104 56.0(3) . . ? B110 B108 B104 61.3(3) . . ? B111 B108 B104 104.3(5) . . ? C12 B108 B105 54.9(3) . . ? B110 B108 B105 105.5(5) . . ? B111 B108 B105 61.0(3) . . ? B104 B108 B105 92.5(4) . . ? B110 B109 B111 62.0(4) . . ? B110 B109 B103 113.7(4) . . ? B111 B109 B103 111.9(4) . . ? B110 B109 B107 61.2(4) . . ? B111 B109 B107 106.7(4) . . ? B103 B109 B107 59.2(3) . . ? B110 B109 B106 101.8(4) . . ? B111 B109 B106 58.5(4) . . ? B103 B109 B106 56.9(3) . . ? B107 B109 B106 93.2(4) . . ? B109 B110 B108 113.8(5) . . ? B109 B110 B111 59.7(4) . . ? B108 B110 B111 59.4(4) . . ? B109 B110 B107 61.4(4) . . ? B108 B110 B107 114.4(4) . . ? B111 B110 B107 105.1(4) . . ? B109 B110 B104 111.6(4) . . ? B108 B110 B104 60.8(3) . . ? B111 B110 B104 102.4(4) . . ? B107 B110 B104 63.0(3) . . ? B106 B111 B109 62.6(4) . . ? B106 B111 B108 109.7(4) . . ? B109 B111 B108 112.1(5) . . ? B106 B111 B110 102.0(5) . . ? B109 B111 B110 58.2(4) . . ? B108 B111 B110 59.0(4) . . ? B106 B111 B105 60.4(3) . . ? B109 B111 B105 113.2(4) . . ? B108 B111 B105 61.7(3) . . ? B110 B111 B105 104.1(4) . . ? C8A C3A C4A 117.8(5) . . ? C8A C3A C12 121.3(5) . . ? C4A C3A C12 120.9(5) . . ? C5A C4A C3A 121.4(6) . . ? C4A C5A C6A 119.8(6) . . ? C7A C6A C5A 119.4(6) . . ? C6A C7A C8A 120.6(6) . . ? C3A C8A C7A 121.0(6) . . ? O301 C301 Mo2 177.8(5) . . ? O302 C302 Mo2 177.6(4) . . ? O303 C303 Mo2 163.7(4) . . ? O303 C303 Pt2 119.9(4) . . ? Mo2 C303 Pt2 75.85(17) . . ? H106 Mn2 H103 95(3) . . ? H106 Mn2 C401 86(2) . . ? H103 Mn2 C401 167.7(18) . . ? H106 Mn2 C402 91(2) . . ? H103 Mn2 C402 98.7(17) . . ? C401 Mn2 C402 93.6(3) . . ? H106 Mn2 C403 176(2) . . ? H103 Mn2 C403 88.3(18) . . ? C401 Mn2 C403 90.4(3) . . ? C402 Mn2 C403 90.0(3) . . ? H106 Mn2 B106 28(2) . . ? H103 Mn2 B106 74.4(18) . . ? C401 Mn2 B106 102.2(3) . . ? C402 Mn2 B106 112.4(3) . . ? C403 Mn2 B106 153.2(2) . . ? H106 Mn2 B103 72(2) . . ? H103 Mn2 B103 30.4(18) . . ? C401 Mn2 B103 141.3(2) . . ? C402 Mn2 B103 117.3(2) . . ? C403 Mn2 B103 110.9(3) . . ? B106 Mn2 B103 46.4(2) . . ? H106 Mn2 Mo2 76(2) . . ? H103 Mn2 Mo2 71.8(18) . . ? C401 Mn2 Mo2 96.65(18) . . ? C402 Mn2 Mo2 162.5(2) . . ? C403 Mn2 Mo2 104.04(17) . . ? B106 Mn2 Mo2 51.43(16) . . ? B103 Mn2 Mo2 48.02(15) . . ? O401 C401 Mn2 178.9(5) . . ? O402 C402 Mn2 178.5(6) . . ? O403 C403 Mn2 175.7(5) . . ? B103 Pt2 P3 171.50(14) . . ? B103 Pt2 P4 104.63(15) . . ? P3 Pt2 P4 83.69(5) . . ? B103 Pt2 C303 80.6(2) . . ? P3 Pt2 C303 91.99(14) . . ? P4 Pt2 C303 138.74(14) . . ? B103 Pt2 B107 44.9(2) . . ? P3 Pt2 B107 135.05(16) . . ? P4 Pt2 B107 105.65(16) . . ? C303 Pt2 B107 106.1(2) . . ? B103 Pt2 H107 67.7(14) . . ? P3 Pt2 H107 115.2(14) . . ? P4 Pt2 H107 86.6(14) . . ? C303 Pt2 H107 131.0(15) . . ? B107 Pt2 H107 26.9(14) . . ? B103 Pt2 H103 26.7(13) . . ? P3 Pt2 H103 154.9(12) . . ? P4 Pt2 H103 90.1(12) . . ? C303 Pt2 H103 76.8(12) . . ? B107 Pt2 H103 70.0(13) . . ? H107 Pt2 H103 88.5(18) . . ? B103 Pt2 Mo2 53.27(14) . . ? P3 Pt2 Mo2 118.40(4) . . ? P4 Pt2 Mo2 157.90(4) . . ? C303 Pt2 Mo2 46.64(14) . . ? B107 Pt2 Mo2 60.13(15) . . ? H107 Pt2 Mo2 84.4(14) . . ? H103 Pt2 Mo2 69.6(12) . . ? C131 P3 C121 107.6(2) . . ? C131 P3 C116 104.5(3) . . ? C121 P3 C116 100.5(3) . . ? C131 P3 Pt2 121.25(18) . . ? C121 P3 Pt2 111.59(19) . . ? C116 P3 Pt2 109.23(18) . . ? C151 P4 C141 104.1(2) . . ? C151 P4 C115 106.7(3) . . ? C141 P4 C115 101.3(3) . . ? C151 P4 Pt2 123.1(2) . . ? C141 P4 Pt2 112.02(18) . . ? C115 P4 Pt2 107.45(17) . . ? C116 C115 P4 105.5(4) . . ? C115 C116 P3 108.4(4) . . ? C122 C121 C126 120.0(5) . . ? C122 C121 P3 121.5(4) . . ? C126 C121 P3 118.1(4) . . ? C121 C122 C123 119.2(6) . . ? C124 C123 C122 121.4(6) . . ? C123 C124 C125 120.1(6) . . ? C124 C125 C126 119.7(6) . . ? C121 C126 C125 119.7(6) . . ? C132 C131 C136 119.0(5) . . ? C132 C131 P3 120.9(4) . . ? C136 C131 P3 120.0(4) . . ? C131 C132 C133 119.8(5) . . ? C134 C133 C132 120.7(5) . . ? C133 C134 C135 119.9(5) . . ? C136 C135 C134 119.8(5) . . ? C135 C136 C131 120.8(5) . . ? C146 C141 C142 119.5(5) . . ? C146 C141 P4 120.5(4) . . ? C142 C141 P4 119.7(4) . . ? C143 C142 C141 119.6(6) . . ? C142 C143 C144 120.2(6) . . ? C145 C144 C143 120.8(6) . . ? C144 C145 C146 119.8(6) . . ? C141 C146 C145 120.0(5) . . ? C152 C151 C156 120.0(5) . . ? C152 C151 P4 117.6(4) . . ? C156 C151 P4 121.9(4) . . ? C151 C152 C153 120.9(6) . . ? C152 C153 C154 118.9(6) . . ? C155 C154 C153 120.0(5) . . ? C154 C155 C156 120.7(6) . . ? C155 C156 C151 119.5(6) . . ? C1S Cl1S Cl1S 135.0(6) . 5_546 ? Cl1S C1S Cl2S 98.8(8) . . ? Cl1A C1SA Cl2A 95.2(10) . . ? Cl7S Cl7S C4S 140.3(14) 2 . ? Cl7S C4S Cl8S 112.0(15) . . ? Cl5S C3S Cl6S 138(2) . . ? Cl5A C3SA Cl6A 104.1(13) . . ? Cl6B C3SB Cl5B 115.1(8) . . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.720 _refine_diff_density_min -1.586 _refine_diff_density_rms 0.163 #===END #============================================================================= #= #= NOTE THAT THIS IS A PRELIMINARY STRUCTURE DETERMINATION AND THAT #= THE DATA ARE VERY POOR DUE TO SEVERE CRYSTAL TWINNING #= data_3 _database_code_depnum_ccdc_archive 'CCDC 271639' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C8 H20 N), C13 H14 B9 Mn Mo O6 ' _chemical_formula_sum 'C29 H54 B9 Mn Mo N2 O6' _chemical_formula_weight 774.91 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' Mn Mn 0.3368 0.7283 '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 15.8482(7) _cell_length_b 24.0593(12) _cell_length_c 20.0462(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.259(2) _cell_angle_gamma 90.00 _cell_volume 7643.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4509 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 19.25 _exptl_crystal_description block _exptl_crystal_colour 'dark green-black' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3216 _exptl_absorpt_coefficient_mu 0.699 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.37 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'TWINABS (Bruker, 2003)' _exptl_special_details ; Crystals of compound 3 were badly twinned and although the unresolved data could be solved and partially refined in various cell settings and space groups, the refinement was not stable and anisotropic refinement could not be achieved. However, use of CELL_NOW (Bruker, 2003) resolved two main domains and allowed their separate integration and data reduction (Bruker, 2003). The resulting (somewhat approximate) intensity data were used in space group determination, structure solution and preliminary refinement. However, the poor quality of the data so obtained precluded an accurate determination. ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8 Apex CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40303 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.1120 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.05 _reflns_number_total 14329 _reflns_number_gt 7857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 (Bruker, 2003)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2003)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2003)' _computing_structure_solution 'Bruker SHELXTL (Bruker, 2000)' _computing_structure_refinement 'Bruker SHELXTL (Bruker, 2000)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 2000)' _computing_publication_material 'Bruker SHELXTL (Bruker, 2000)' _refine_special_details ; Two independents. Only the Mo and Mn atoms were allowed anisotropic refinement. All H atoms were set riding on their parent atoms, with U(iso) = 1.2 x U(eq) of the parent, or U(iso) = 1.5 x U(eq) of the parent for Me groups. The atoms H3, H6, H3a, B6a, H6a all had fixed coordinates after they were located or added. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14329 _refine_ls_number_parameters 402 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2872 _refine_ls_R_factor_gt 0.2150 _refine_ls_wR_factor_ref 0.5836 _refine_ls_wR_factor_gt 0.5617 _refine_ls_goodness_of_fit_ref 2.036 _refine_ls_restrained_S_all 2.036 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.18932(9) 0.38693(7) 0.46493(8) 0.0543(6) Uani 1 1 d . . . C2 C 0.1664(11) 0.2962(8) 0.4831(9) 0.054(4) Uiso 1 1 d . . . B3 B 0.2460(17) 0.3865(11) 0.3634(14) 0.076(7) Uiso 1 1 d . . . H3 H 0.2600 0.4278 0.3430 0.091 Uiso 1 1 d . . . B4 B 0.1175(14) 0.2997(9) 0.4150(11) 0.057(5) Uiso 1 1 d . . . H4 H 0.0475 0.2934 0.4170 0.069 Uiso 1 1 calc R . . B5 B 0.2646(13) 0.2972(9) 0.4706(11) 0.056(5) Uiso 1 1 d . . . H5 H 0.3073 0.2878 0.5138 0.068 Uiso 1 1 calc R . . B6 B 0.3094(15) 0.3466(11) 0.4042(13) 0.069(6) Uiso 1 1 d . . . H6 H 0.3735 0.3608 0.4127 0.083 Uiso 1 1 d . . . B7 B 0.1533(15) 0.3421(11) 0.3471(12) 0.070(6) Uiso 1 1 d . . . H7 H 0.1034 0.3578 0.3121 0.084 Uiso 1 1 calc R . . B8 B 0.1982(13) 0.2524(10) 0.4311(11) 0.060(6) Uiso 1 1 d . . . H8 H 0.1938 0.2068 0.4416 0.072 Uiso 1 1 calc R . . B9 B 0.2608(18) 0.3178(12) 0.3269(16) 0.090(8) Uiso 1 1 d . . . H9 H 0.2914 0.3115 0.2773 0.108 Uiso 1 1 calc R . . B10 B 0.1755(16) 0.2764(12) 0.3489(13) 0.076(7) Uiso 1 1 d . . . H10 H 0.1449 0.2497 0.3100 0.091 Uiso 1 1 calc R . . B11 B 0.2844(14) 0.2732(10) 0.3874(11) 0.058(6) Uiso 1 1 d . . . H11 H 0.3364 0.2430 0.3768 0.070 Uiso 1 1 calc R . . Mn1 Mn 0.34264(18) 0.43478(14) 0.40479(15) 0.0652(9) Uani 1 1 d . . . C11 C 0.0809(12) 0.3959(8) 0.5178(10) 0.059(5) Uiso 1 1 d . . . O11 O 0.0364(11) 0.4085(8) 0.5563(9) 0.101(5) Uiso 1 1 d . . . C12 C 0.2459(10) 0.4087(7) 0.5500(9) 0.050(4) Uiso 1 1 d . . . O12 O 0.2769(8) 0.4144(6) 0.6006(7) 0.064(3) Uiso 1 1 d . . . C13 C 0.1537(19) 0.4561(13) 0.4371(16) 0.118(9) Uiso 1 1 d . . . O13 O 0.1330(14) 0.5064(10) 0.4166(11) 0.136(7) Uiso 1 1 d . . . C14 C 0.4032(11) 0.4470(8) 0.4802(9) 0.055(5) Uiso 1 1 d . . . O14 O 0.4342(9) 0.4560(6) 0.5315(8) 0.080(4) Uiso 1 1 d . . . C15 C 0.3291(14) 0.5064(11) 0.3990(12) 0.086(7) Uiso 1 1 d . . . O15 O 0.3102(10) 0.5531(7) 0.3900(8) 0.088(5) Uiso 1 1 d . . . C16 C 0.4251(16) 0.4441(11) 0.3501(13) 0.092(7) Uiso 1 1 d . . . O16 O 0.4866(14) 0.4483(9) 0.3171(11) 0.134(7) Uiso 1 1 d . . . C21 C 0.1307(11) 0.2795(8) 0.5486(9) 0.055(5) Uiso 1 1 d . . . C22 C 0.0436(16) 0.2507(11) 0.5465(14) 0.096(8) Uiso 1 1 d . . . H22 H 0.0040 0.2509 0.5108 0.115 Uiso 1 1 calc R . . C23 C 0.0344(17) 0.2217(11) 0.6140(13) 0.103(8) Uiso 1 1 d . . . H23 H -0.0164 0.2016 0.6210 0.124 Uiso 1 1 calc R . . C24 C 0.0904(15) 0.2217(11) 0.6643(13) 0.090(7) Uiso 1 1 d . . . H24 H 0.0754 0.2005 0.7025 0.108 Uiso 1 1 calc R . . C25 C 0.1609(14) 0.2464(10) 0.6671(12) 0.083(7) Uiso 1 1 d . . . H25 H 0.1983 0.2468 0.7042 0.100 Uiso 1 1 calc R . . C26 C 0.1745(12) 0.2740(8) 0.6032(10) 0.063(5) Uiso 1 1 d . . . H26 H 0.2276 0.2921 0.6010 0.076 Uiso 1 1 calc R . . Mo1A Mo 0.31138(11) 0.61353(8) 0.96565(9) 0.0637(6) Uani 1 1 d . . . C2A C 0.3322(10) 0.7032(7) 0.9835(9) 0.051(4) Uiso 1 1 d . . . B3A B 0.2653(18) 0.6139(12) 0.8622(15) 0.081(8) Uiso 1 1 d . . . H3A H 0.2537 0.5729 0.8428 0.097 Uiso 1 1 d . . . B4A B 0.3867(19) 0.6977(12) 0.9189(14) 0.085(8) Uiso 1 1 d . . . H4A H 0.4569 0.7027 0.9225 0.102 Uiso 1 1 calc R . . B5A B 0.2313(14) 0.7011(10) 0.9700(12) 0.063(6) Uiso 1 1 d . . . H5A H 0.1859 0.7093 1.0115 0.075 Uiso 1 1 calc R . . B6A B 0.2072 0.6600 0.9065 0.175(19) Uiso 1 1 d . . . H6A H 0.1423 0.6441 0.9174 0.210 Uiso 1 1 d . . . B7A B 0.3515(19) 0.6506(13) 0.8454(15) 0.093(9) Uiso 1 1 d . . . H7A H 0.3996 0.6317 0.8115 0.111 Uiso 1 1 calc R . . B8A B 0.3020(14) 0.7505(11) 0.9327(12) 0.068(6) Uiso 1 1 d . . . H8A H 0.3067 0.7961 0.9433 0.081 Uiso 1 1 calc R . . B9A B 0.257(2) 0.6831(15) 0.822(2) 0.116(11) Uiso 1 1 d . . . H9A H 0.2369 0.6905 0.7688 0.139 Uiso 1 1 calc R . . B10A B 0.3228(16) 0.7229(12) 0.8518(14) 0.079(7) Uiso 1 1 d . . . H10A H 0.3517 0.7531 0.8160 0.095 Uiso 1 1 calc R . . B11A B 0.2120(16) 0.7227(11) 0.8835(13) 0.076(7) Uiso 1 1 d . . . H11A H 0.1544 0.7469 0.8691 0.091 Uiso 1 1 calc R . . Mn1A Mn 0.1589(2) 0.56465(14) 0.90454(16) 0.0704(10) Uani 1 1 d . . . C11A C 0.2609(11) 0.5902(8) 1.0517(10) 0.057(5) Uiso 1 1 d . . . O11A O 0.2224(9) 0.5801(6) 1.1004(8) 0.081(4) Uiso 1 1 d . . . C12A C 0.3510(16) 0.5389(12) 0.9354(13) 0.096(8) Uiso 1 1 d . . . O12A O 0.3733(14) 0.4976(10) 0.9179(11) 0.134(7) Uiso 1 1 d . . . C13A C 0.4072(16) 0.6077(10) 1.0202(13) 0.085(7) Uiso 1 1 d . . . O13A O 0.4767(15) 0.5960(10) 1.0521(12) 0.143(8) Uiso 1 1 d . . . C14A C 0.1740(15) 0.4937(11) 0.8976(12) 0.090(7) Uiso 1 1 d . . . O14A O 0.1834(12) 0.4468(9) 0.8902(10) 0.115(6) Uiso 1 1 d . . . C15A C 0.0766(18) 0.5626(12) 0.8473(14) 0.103(8) Uiso 1 1 d . . . O15A O 0.0110(16) 0.5485(10) 0.8164(13) 0.156(9) Uiso 1 1 d . . . C16A C 0.0976(14) 0.5551(10) 0.9820(12) 0.080(6) Uiso 1 1 d . . . O16A O 0.0624(10) 0.5462(7) 1.0316(8) 0.090(5) Uiso 1 1 d . . . C21A C 0.3624(12) 0.7281(8) 1.0488(10) 0.065(5) Uiso 1 1 d . . . C22A C 0.3214(12) 0.7259(8) 1.1066(9) 0.059(5) Uiso 1 1 d . . . H22A H 0.2706 0.7049 1.1075 0.071 Uiso 1 1 calc R . . C23A C 0.3457(12) 0.7513(9) 1.1655(10) 0.069(5) Uiso 1 1 d . . . H23A H 0.3116 0.7495 1.2043 0.083 Uiso 1 1 calc R . . C24A C 0.4214(15) 0.7792(11) 1.1655(13) 0.091(7) Uiso 1 1 d . . . H24A H 0.4380 0.7990 1.2045 0.109 Uiso 1 1 calc R . . C25A C 0.4722(15) 0.7796(10) 1.1128(12) 0.086(7) Uiso 1 1 d . . . H25A H 0.5238 0.7995 1.1156 0.103 Uiso 1 1 calc R . . C26A C 0.4520(16) 0.7508(11) 1.0517(14) 0.097(8) Uiso 1 1 d . . . H26A H 0.4911 0.7464 1.0164 0.117 Uiso 1 1 calc R . . N1 N 0.0332(11) 0.6346(8) 0.2336(9) 0.072(5) Uiso 1 1 d . . . C31 C 0.1101(19) 0.6111(12) 0.2578(16) 0.111(9) Uiso 1 1 d . . . H31A H 0.1054 0.5701 0.2559 0.133 Uiso 1 1 calc R . . H31B H 0.1563 0.6222 0.2276 0.133 Uiso 1 1 calc R . . C32 C 0.132(3) 0.6267(18) 0.324(2) 0.193(18) Uiso 1 1 d . . . H32A H 0.1845 0.6076 0.3374 0.289 Uiso 1 1 calc R . . H32B H 0.0869 0.6163 0.3547 0.289 Uiso 1 1 calc R . . H32C H 0.1413 0.6670 0.3262 0.289 Uiso 1 1 calc R . . C33 C -0.0430(15) 0.6362(11) 0.2641(13) 0.090(7) Uiso 1 1 d . . . H33A H -0.0836 0.6543 0.2333 0.108 Uiso 1 1 calc R . . H33B H -0.0378 0.6604 0.3038 0.108 Uiso 1 1 calc R . . C34 C -0.079(3) 0.5834(17) 0.285(2) 0.177(16) Uiso 1 1 d . . . H34A H -0.1300 0.5904 0.3118 0.266 Uiso 1 1 calc R . . H34B H -0.0379 0.5631 0.3125 0.266 Uiso 1 1 calc R . . H34C H -0.0941 0.5612 0.2460 0.266 Uiso 1 1 calc R . . C35 C 0.0601(19) 0.7012(14) 0.2312(16) 0.127(10) Uiso 1 1 d . . . H35A H 0.0111 0.7234 0.2159 0.152 Uiso 1 1 calc R . . H35B H 0.0753 0.7138 0.2767 0.152 Uiso 1 1 calc R . . C36 C 0.128(3) 0.7105(18) 0.189(2) 0.191(17) Uiso 1 1 d . . . H36A H 0.1440 0.7498 0.1902 0.287 Uiso 1 1 calc R . . H36B H 0.1117 0.7006 0.1428 0.287 Uiso 1 1 calc R . . H36C H 0.1760 0.6875 0.2026 0.287 Uiso 1 1 calc R . . C37 C 0.021(2) 0.6100(12) 0.1659(15) 0.117(10) Uiso 1 1 d . . . H37A H -0.0052 0.5727 0.1689 0.140 Uiso 1 1 calc R . . H37B H 0.0756 0.6067 0.1424 0.140 Uiso 1 1 calc R . . C38 C -0.0361(19) 0.6500(13) 0.1310(15) 0.128(10) Uiso 1 1 d . . . H38A H -0.0503 0.6356 0.0866 0.191 Uiso 1 1 calc R . . H38B H -0.0076 0.6860 0.1264 0.191 Uiso 1 1 calc R . . H38C H -0.0879 0.6548 0.1569 0.191 Uiso 1 1 calc R . . N2 N 0.4650(11) 0.3647(8) 0.7309(9) 0.077(5) Uiso 1 1 d . . . C41 C 0.440(2) 0.3023(16) 0.7300(19) 0.157(14) Uiso 1 1 d . . . H41A H 0.4861 0.2810 0.7087 0.188 Uiso 1 1 calc R . . H41B H 0.4356 0.2892 0.7767 0.188 Uiso 1 1 calc R . . C42 C 0.359(3) 0.2891(18) 0.694(2) 0.187(17) Uiso 1 1 d . . . H42A H 0.3481 0.2490 0.6968 0.281 Uiso 1 1 calc R . . H42B H 0.3631 0.3004 0.6476 0.281 Uiso 1 1 calc R . . H42C H 0.3124 0.3092 0.7157 0.281 Uiso 1 1 calc R . . C43 C 0.393(2) 0.3960(15) 0.7557(18) 0.138(12) Uiso 1 1 d . . . H43A H 0.3475 0.3894 0.7227 0.166 Uiso 1 1 calc R . . H43B H 0.4092 0.4355 0.7507 0.166 Uiso 1 1 calc R . . C44 C 0.348(3) 0.392(2) 0.827(3) 0.22(2) Uiso 1 1 d . . . H44A H 0.3016 0.4193 0.8290 0.335 Uiso 1 1 calc R . . H44B H 0.3890 0.4006 0.8625 0.335 Uiso 1 1 calc R . . H44C H 0.3253 0.3548 0.8337 0.335 Uiso 1 1 calc R . . C45 C 0.5368(15) 0.3568(11) 0.7713(12) 0.088(7) Uiso 1 1 d . . . H45A H 0.5507 0.3167 0.7691 0.106 Uiso 1 1 calc R . . H45B H 0.5191 0.3644 0.8177 0.106 Uiso 1 1 calc R . . C46 C 0.619(3) 0.3881(17) 0.761(2) 0.176(17) Uiso 1 1 d . . . H46A H 0.6597 0.3771 0.7952 0.263 Uiso 1 1 calc R . . H46B H 0.6083 0.4281 0.7638 0.263 Uiso 1 1 calc R . . H46C H 0.6413 0.3792 0.7166 0.263 Uiso 1 1 calc R . . C47 C 0.4816(18) 0.3950(11) 0.6653(14) 0.106(9) Uiso 1 1 d . . . H47A H 0.5119 0.4305 0.6725 0.127 Uiso 1 1 calc R . . H47B H 0.4289 0.4019 0.6400 0.127 Uiso 1 1 calc R . . C48 C 0.539(2) 0.3499(16) 0.630(2) 0.179(16) Uiso 1 1 d . . . H48A H 0.5548 0.3630 0.5857 0.269 Uiso 1 1 calc R . . H48B H 0.5081 0.3149 0.6265 0.269 Uiso 1 1 calc R . . H48C H 0.5903 0.3440 0.6571 0.269 Uiso 1 1 calc R . . N3 N 0.2834(13) 0.4088(9) 0.1070(10) 0.090(6) Uiso 1 1 d . . . C51 C 0.358(2) 0.4544(15) 0.1024(18) 0.139(12) Uiso 1 1 d . . . H51A H 0.3926 0.4528 0.0616 0.166 Uiso 1 1 calc R . . H51B H 0.3414 0.4928 0.1144 0.166 Uiso 1 1 calc R . . C52 C 0.385(5) 0.421(3) 0.155(4) 0.37(5) Uiso 1 1 d . . . H52A H 0.4389 0.4351 0.1716 0.561 Uiso 1 1 calc R . . H52B H 0.3912 0.3830 0.1393 0.561 Uiso 1 1 calc R . . H52C H 0.3429 0.4225 0.1907 0.561 Uiso 1 1 calc R . . C53 C 0.303(4) 0.366(3) 0.075(3) 0.27(3) Uiso 1 1 d . . . H53A H 0.2483 0.3470 0.0710 0.325 Uiso 1 1 calc R . . H53B H 0.3352 0.3449 0.1087 0.325 Uiso 1 1 calc R . . C54 C 0.342(2) 0.3512(14) 0.0173(17) 0.137(11) Uiso 1 1 d . . . H54A H 0.3429 0.3105 0.0140 0.205 Uiso 1 1 calc R . . H54B H 0.4000 0.3653 0.0174 0.205 Uiso 1 1 calc R . . H54C H 0.3112 0.3667 -0.0209 0.205 Uiso 1 1 calc R . . C55 C 0.216(2) 0.4309(16) 0.0524(19) 0.154(13) Uiso 1 1 d . . . H55A H 0.2148 0.4719 0.0570 0.184 Uiso 1 1 calc R . . H55B H 0.2408 0.4231 0.0082 0.184 Uiso 1 1 calc R . . C56 C 0.120(2) 0.4114(16) 0.048(2) 0.162(14) Uiso 1 1 d . . . H56A H 0.0893 0.4346 0.0155 0.243 Uiso 1 1 calc R . . H56B H 0.0931 0.4153 0.0918 0.243 Uiso 1 1 calc R . . H56C H 0.1171 0.3725 0.0338 0.243 Uiso 1 1 calc R . . C57 C 0.215(2) 0.4114(16) 0.1796(19) 0.153(13) Uiso 1 1 d . . . H57A H 0.1588 0.3959 0.1679 0.184 Uiso 1 1 calc R . . H57B H 0.2391 0.3883 0.2158 0.184 Uiso 1 1 calc R . . C58 C 0.2043(17) 0.4725(11) 0.2049(14) 0.103(8) Uiso 1 1 d . . . H58A H 0.1695 0.4728 0.2452 0.155 Uiso 1 1 calc R . . H58B H 0.1769 0.4949 0.1701 0.155 Uiso 1 1 calc R . . H58C H 0.2599 0.4882 0.2152 0.155 Uiso 1 1 calc R . . N4 N 0.2158(12) 0.5843(9) 0.6052(10) 0.087(5) Uiso 1 1 d . . . C61 C 0.272(2) 0.5870(16) 0.6730(19) 0.158(14) Uiso 1 1 d . . . H61A H 0.3232 0.6088 0.6637 0.190 Uiso 1 1 calc R . . H61B H 0.2390 0.6076 0.7069 0.190 Uiso 1 1 calc R . . C62 C 0.2973(16) 0.5342(11) 0.7020(13) 0.095(7) Uiso 1 1 d . . . H62A H 0.3295 0.5410 0.7431 0.142 Uiso 1 1 calc R . . H62B H 0.3326 0.5140 0.6702 0.142 Uiso 1 1 calc R . . H62C H 0.2471 0.5120 0.7123 0.142 Uiso 1 1 calc R . . C63 C 0.1491(19) 0.5484(13) 0.6005(16) 0.117(10) Uiso 1 1 d . . . H63A H 0.1302 0.5446 0.5536 0.140 Uiso 1 1 calc R . . H63B H 0.1648 0.5112 0.6176 0.140 Uiso 1 1 calc R . . C64 C 0.095(4) 0.568(3) 0.634(3) 0.30(3) Uiso 1 1 d . . . H64A H 0.0447 0.5449 0.6320 0.453 Uiso 1 1 calc R . . H64B H 0.0812 0.6055 0.6166 0.453 Uiso 1 1 calc R . . H64C H 0.1148 0.5715 0.6800 0.453 Uiso 1 1 calc R . . C65 C 0.188(2) 0.6480(16) 0.5745(19) 0.159(14) Uiso 1 1 d . . . H65A H 0.1524 0.6658 0.6087 0.191 Uiso 1 1 calc R . . H65B H 0.2408 0.6701 0.5721 0.191 Uiso 1 1 calc R . . C66 C 0.1462(19) 0.6551(13) 0.5127(15) 0.122(10) Uiso 1 1 d . . . H66A H 0.1313 0.6943 0.5069 0.182 Uiso 1 1 calc R . . H66B H 0.0948 0.6324 0.5120 0.182 Uiso 1 1 calc R . . H66C H 0.1834 0.6434 0.4764 0.182 Uiso 1 1 calc R . . C67 C 0.2835(14) 0.5640(10) 0.5537(12) 0.084(6) Uiso 1 1 d . . . H67A H 0.3029 0.5264 0.5669 0.100 Uiso 1 1 calc R . . H67B H 0.2563 0.5607 0.5093 0.100 Uiso 1 1 calc R . . C68 C 0.3615(17) 0.6023(11) 0.5474(15) 0.105(9) Uiso 1 1 d . . . H68A H 0.4010 0.5863 0.5153 0.158 Uiso 1 1 calc R . . H68B H 0.3893 0.6057 0.5910 0.158 Uiso 1 1 calc R . . H68C H 0.3435 0.6391 0.5321 0.158 Uiso 1 1 calc R . . 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 0.0440(9) 0.0691(12) 0.0498(11) -0.0033(8) -0.0106(6) -0.0004(8) Mn1 0.0603(18) 0.075(2) 0.061(2) -0.0022(16) 0.0071(14) -0.0179(15) Mo1A 0.0648(12) 0.0674(12) 0.0591(12) 0.0042(9) 0.0128(8) 0.0030(9) Mn1A 0.092(2) 0.061(2) 0.058(2) -0.0029(16) -0.0059(16) -0.0158(17) _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 C13 1.84(3) . ? Mo1 C12 1.993(18) . ? Mo1 C11 2.04(2) . ? Mo1 B3 2.23(3) . ? Mo1 C2 2.243(18) . ? Mo1 B5 2.47(2) . ? Mo1 B6 2.46(2) . ? Mo1 B4 2.59(2) . ? Mo1 B7 2.66(2) . ? Mo1 Mn1 2.951(3) . ? C2 C21 1.49(2) . ? C2 B8 1.57(3) . ? C2 B4 1.57(3) . ? C2 B5 1.58(3) . ? B3 B6 1.61(4) . ? B3 B9 1.82(4) . ? B3 B7 1.84(4) . ? B3 Mn1 2.09(3) . ? B4 B10 1.71(3) . ? B4 B8 1.74(3) . ? B4 B7 1.80(3) . ? B5 B8 1.70(3) . ? B5 B11 1.79(3) . ? B5 B6 1.92(3) . ? B6 B11 1.84(3) . ? B6 B9 1.86(4) . ? B6 Mn1 2.19(3) . ? B7 B10 1.62(4) . ? B7 B9 1.85(4) . ? B8 B11 1.70(3) . ? B8 B10 1.78(3) . ? B9 B11 1.66(4) . ? B9 B10 1.74(4) . ? B10 B11 1.89(3) . ? Mn1 C16 1.72(3) . ? Mn1 C15 1.74(3) . ? Mn1 H3 1.806(3) . ? Mn1 C14 1.810(19) . ? Mn1 H6 1.854(3) . ? C11 O11 1.09(2) . ? C12 O12 1.133(19) . ? C13 O13 1.32(3) . ? C14 O14 1.16(2) . ? C15 O15 1.18(3) . ? C16 O16 1.18(3) . ? C21 C26 1.30(2) . ? C21 C22 1.55(3) . ? C22 C23 1.53(4) . ? C23 C24 1.34(3) . ? C24 C25 1.27(3) . ? C25 C26 1.46(3) . ? Mo1A C13A 1.87(3) . ? Mo1A C11A 1.985(19) . ? Mo1A C12A 2.00(3) . ? Mo1A B3A 2.20(3) . ? Mo1A C2A 2.212(18) . ? Mo1A B6A 2.3153(19) . ? Mo1A B5A 2.46(2) . ? Mo1A B4A 2.53(3) . ? Mo1A B7A 2.65(3) . ? Mo1A Mn1A 2.949(4) . ? C2A C21A 1.51(3) . ? C2A B4A 1.57(3) . ? C2A B8A 1.60(3) . ? C2A B5A 1.62(3) . ? B3A B7A 1.66(4) . ? B3A B6A 1.69(3) . ? B3A B9A 1.86(5) . ? B3A Mn1A 2.23(3) . ? B4A B10A 1.79(4) . ? B4A B8A 1.87(4) . ? B4A B7A 1.94(4) . ? B5A B6A 1.66(2) . ? B5A B8A 1.80(3) . ? B5A B11A 1.84(3) . ? B6A B11A 1.58(3) . ? B6A B9A 1.96(4) . ? B6A Mn1A 2.418(3) . ? B7A B9A 1.76(5) . ? B7A B10A 1.80(4) . ? B8A B10A 1.79(4) . ? B8A B11A 1.86(4) . ? B9A B10A 1.54(4) . ? B9A B11A 1.72(4) . ? B10A B11A 1.87(4) . ? Mn1A C15A 1.73(3) . ? Mn1A C14A 1.73(3) . ? Mn1A C16A 1.85(2) . ? Mn1A H6A 1.948(3) . ? Mn1A H3A 1.960(3) . ? C11A O11A 1.18(2) . ? C12A O12A 1.11(3) . ? C13A O13A 1.30(3) . ? C14A O14A 1.15(3) . ? C15A O15A 1.25(3) . ? C16A O16A 1.16(2) . ? C21A C22A 1.33(3) . ? C21A C26A 1.52(3) . ? C22A C23A 1.38(3) . ? C23A C24A 1.38(3) . ? C24A C25A 1.33(3) . ? C25A C26A 1.44(3) . ? N1 C33 1.36(3) . ? N1 C31 1.43(3) . ? N1 C37 1.49(3) . ? N1 C35 1.66(4) . ? C31 C32 1.43(5) . ? C33 C34 1.46(4) . ? C35 C36 1.40(4) . ? C37 C38 1.50(4) . ? N2 C45 1.41(3) . ? N2 C43 1.46(4) . ? N2 C47 1.53(3) . ? N2 C41 1.55(4) . ? C41 C42 1.50(4) . ? C43 C44 1.61(5) . ? C45 C46 1.52(4) . ? C47 C48 1.58(4) . ? N3 C53 1.25(6) . ? N3 C55 1.62(4) . ? N3 C51 1.61(4) . ? N3 C57 1.82(4) . ? N3 C52 1.89(8) . ? C51 C52 1.38(8) . ? C53 C54 1.36(6) . ? C55 C56 1.60(5) . ? C57 C58 1.57(4) . ? N4 C63 1.37(3) . ? N4 C67 1.57(3) . ? N4 C61 1.62(4) . ? N4 C65 1.71(4) . ? C61 C62 1.45(4) . ? C63 C64 1.19(6) . ? C65 C66 1.41(4) . ? C67 C68 1.55(3) . ? 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 C13 Mo1 C12 99.1(11) . . ? C13 Mo1 C11 78.7(11) . . ? C12 Mo1 C11 84.5(7) . . ? C13 Mo1 B3 81.5(12) . . ? C12 Mo1 B3 126.9(8) . . ? C11 Mo1 B3 145.2(9) . . ? C13 Mo1 C2 151.4(10) . . ? C12 Mo1 C2 100.9(7) . . ? C11 Mo1 C2 83.2(7) . . ? B3 Mo1 C2 102.1(8) . . ? C13 Mo1 B5 161.9(11) . . ? C12 Mo1 B5 88.6(7) . . ? C11 Mo1 B5 118.6(7) . . ? B3 Mo1 B5 80.9(9) . . ? C2 Mo1 B5 38.7(7) . . ? C13 Mo1 B6 116.2(11) . . ? C12 Mo1 B6 100.5(8) . . ? C11 Mo1 B6 162.9(8) . . ? B3 Mo1 B6 39.7(9) . . ? C2 Mo1 B6 79.8(7) . . ? B5 Mo1 B6 45.9(8) . . ? C13 Mo1 B4 118.8(11) . . ? C12 Mo1 B4 137.7(7) . . ? C11 Mo1 B4 85.2(7) . . ? B3 Mo1 B4 79.7(8) . . ? C2 Mo1 B4 37.1(7) . . ? B5 Mo1 B4 61.3(7) . . ? B6 Mo1 B4 80.2(8) . . ? C13 Mo1 B7 91.8(11) . . ? C12 Mo1 B7 164.1(7) . . ? C11 Mo1 B7 109.1(8) . . ? B3 Mo1 B7 43.3(9) . . ? C2 Mo1 B7 73.4(7) . . ? B5 Mo1 B7 77.8(8) . . ? B6 Mo1 B7 64.1(8) . . ? B4 Mo1 B7 40.0(7) . . ? C13 Mo1 Mn1 77.0(10) . . ? C12 Mo1 Mn1 83.1(5) . . ? C11 Mo1 Mn1 150.5(5) . . ? B3 Mo1 Mn1 45.0(7) . . ? C2 Mo1 Mn1 125.5(5) . . ? B5 Mo1 Mn1 87.8(5) . . ? B6 Mo1 Mn1 46.5(6) . . ? B4 Mo1 Mn1 121.3(5) . . ? B7 Mo1 Mn1 88.2(5) . . ? C21 C2 B8 122.0(17) . . ? C21 C2 B4 126.4(16) . . ? B8 C2 B4 67.5(13) . . ? C21 C2 B5 121.6(15) . . ? B8 C2 B5 65.5(13) . . ? B4 C2 B5 110.2(16) . . ? C21 C2 Mo1 118.0(12) . . ? B8 C2 Mo1 119.6(13) . . ? B4 C2 Mo1 83.5(11) . . ? B5 C2 Mo1 78.4(11) . . ? B6 B3 B9 65.3(16) . . ? B6 B3 B7 103.9(19) . . ? B9 B3 B7 60.5(15) . . ? B6 B3 Mn1 71.1(14) . . ? B9 B3 Mn1 124.6(17) . . ? B7 B3 Mn1 166.8(18) . . ? B6 B3 Mo1 78.0(14) . . ? B9 B3 Mo1 115.1(17) . . ? B7 B3 Mo1 80.8(13) . . ? Mn1 B3 Mo1 86.1(10) . . ? C2 B4 B10 113.0(17) . . ? C2 B4 B8 56.2(12) . . ? B10 B4 B8 62.1(14) . . ? C2 B4 B7 122.2(17) . . ? B10 B4 B7 55.0(14) . . ? B8 B4 B7 106.1(16) . . ? C2 B4 Mo1 59.5(10) . . ? B10 B4 Mo1 109.2(14) . . ? B8 B4 Mo1 97.9(12) . . ? B7 B4 Mo1 72.1(11) . . ? C2 B5 B8 57.0(12) . . ? C2 B5 B11 108.6(15) . . ? B8 B5 B11 58.2(13) . . ? C2 B5 B6 119.1(16) . . ? B8 B5 B6 107.4(16) . . ? B11 B5 B6 59.3(12) . . ? C2 B5 Mo1 62.9(10) . . ? B8 B5 Mo1 103.6(13) . . ? B11 B5 Mo1 109.0(13) . . ? B6 B5 Mo1 66.9(10) . . ? B3 B6 B11 110.3(18) . . ? B3 B6 B9 62.9(16) . . ? B11 B6 B9 53.3(13) . . ? B3 B6 B5 119.3(18) . . ? B11 B6 B5 56.9(12) . . ? B9 B6 B5 101.2(17) . . ? B3 B6 Mn1 64.8(13) . . ? B11 B6 Mn1 169.7(16) . . ? B9 B6 Mn1 117.7(15) . . ? B5 B6 Mn1 133.3(15) . . ? B3 B6 Mo1 62.3(13) . . ? B11 B6 Mo1 107.6(13) . . ? B9 B6 Mo1 103.9(14) . . ? B5 B6 Mo1 67.2(10) . . ? Mn1 B6 Mo1 78.6(8) . . ? B10 B7 B4 59.8(14) . . ? B10 B7 B3 112.8(19) . . ? B4 B7 B3 116.7(18) . . ? B10 B7 B9 59.7(15) . . ? B4 B7 B9 106.3(18) . . ? B3 B7 B9 59.1(14) . . ? B10 B7 Mo1 109.3(16) . . ? B4 B7 Mo1 67.9(11) . . ? B3 B7 Mo1 55.9(11) . . ? B9 B7 Mo1 97.4(14) . . ? C2 B8 B5 57.6(12) . . ? C2 B8 B11 114.0(17) . . ? B5 B8 B11 63.7(13) . . ? C2 B8 B4 56.3(12) . . ? B5 B8 B4 97.1(16) . . ? B11 B8 B4 107.6(17) . . ? C2 B8 B10 109.4(17) . . ? B5 B8 B10 110.3(18) . . ? B11 B8 B10 65.6(14) . . ? B4 B8 B10 58.1(13) . . ? B11 B9 B10 67.5(16) . . ? B11 B9 B3 109(2) . . ? B10 B9 B3 108(2) . . ? B11 B9 B7 104(2) . . ? B10 B9 B7 53.6(14) . . ? B3 B9 B7 60.4(15) . . ? B11 B9 B6 62.8(15) . . ? B10 B9 B6 109(2) . . ? B3 B9 B6 51.8(14) . . ? B7 B9 B6 94.5(18) . . ? B7 B10 B4 65.2(15) . . ? B7 B10 B9 66.7(17) . . ? B4 B10 B9 115(2) . . ? B7 B10 B8 112(2) . . ? B4 B10 B8 59.8(13) . . ? B9 B10 B8 105.5(19) . . ? B7 B10 B11 104.3(19) . . ? B4 B10 B11 101.0(17) . . ? B9 B10 B11 54.3(14) . . ? B8 B10 B11 55.1(12) . . ? B9 B11 B8 112.8(18) . . ? B9 B11 B5 115.4(19) . . ? B8 B11 B5 58.1(13) . . ? B9 B11 B6 63.9(15) . . ? B8 B11 B6 111.1(16) . . ? B5 B11 B6 63.8(13) . . ? B9 B11 B10 58.2(15) . . ? B8 B11 B10 59.2(13) . . ? B5 B11 B10 101.7(15) . . ? B6 B11 B10 103.3(16) . . ? C16 Mn1 C15 85.5(11) . . ? C16 Mn1 H3 97.1(9) . . ? C15 Mn1 H3 87.5(8) . . ? C16 Mn1 C14 96.3(10) . . ? C15 Mn1 C14 87.7(10) . . ? H3 Mn1 C14 165.3(6) . . ? C16 Mn1 H6 88.8(9) . . ? C15 Mn1 H6 171.7(8) . . ? H3 Mn1 H6 99.21(15) . . ? C14 Mn1 H6 86.9(6) . . ? C16 Mn1 B3 112.0(11) . . ? C15 Mn1 B3 115.7(11) . . ? H3 Mn1 B3 31.7(8) . . ? C14 Mn1 B3 143.7(10) . . ? H6 Mn1 B3 72.1(8) . . ? C16 Mn1 B6 107.8(11) . . ? C15 Mn1 B6 158.5(10) . . ? H3 Mn1 B6 74.5(7) . . ? C14 Mn1 B6 106.8(9) . . ? H6 Mn1 B6 29.7(6) . . ? B3 Mn1 B6 44.1(10) . . ? C16 Mn1 Mo1 159.8(9) . . ? C15 Mn1 Mo1 108.2(8) . . ? H3 Mn1 Mo1 69.43(9) . . ? C14 Mn1 Mo1 99.0(6) . . ? H6 Mn1 Mo1 78.92(10) . . ? B3 Mn1 Mo1 48.9(8) . . ? B6 Mn1 Mo1 54.9(6) . . ? O11 C11 Mo1 161.5(19) . . ? O12 C12 Mo1 171.6(16) . . ? O13 C13 Mo1 177(3) . . ? O14 C14 Mn1 173.0(16) . . ? O15 C15 Mn1 171(2) . . ? O16 C16 Mn1 174(2) . . ? C26 C21 C2 124.6(17) . . ? C26 C21 C22 116.7(18) . . ? C2 C21 C22 116.2(17) . . ? C23 C22 C21 106(2) . . ? C24 C23 C22 127(3) . . ? C25 C24 C23 128(3) . . ? C24 C25 C26 108(2) . . ? C21 C26 C25 135(2) . . ? C13A Mo1A C11A 78.5(9) . . ? C13A Mo1A C12A 81.6(11) . . ? C11A Mo1A C12A 97.9(9) . . ? C13A Mo1A B3A 144.8(11) . . ? C11A Mo1A B3A 133.5(9) . . ? C12A Mo1A B3A 79.7(11) . . ? C13A Mo1A C2A 81.9(9) . . ? C11A Mo1A C2A 101.3(7) . . ? C12A Mo1A C2A 151.6(9) . . ? B3A Mo1A C2A 101.4(9) . . ? C13A Mo1A B6A 155.5(7) . . ? C11A Mo1A B6A 107.0(5) . . ? C12A Mo1A B6A 120.2(8) . . ? B3A Mo1A B6A 44.0(7) . . ? C2A Mo1A B6A 73.6(5) . . ? C13A Mo1A B5A 117.4(9) . . ? C11A Mo1A B5A 90.1(8) . . ? C12A Mo1A B5A 160.6(9) . . ? B3A Mo1A B5A 82.0(9) . . ? C2A Mo1A B5A 40.2(7) . . ? B6A Mo1A B5A 40.4(5) . . ? C13A Mo1A B4A 83.9(10) . . ? C11A Mo1A B4A 137.7(9) . . ? C12A Mo1A B4A 117.2(10) . . ? B3A Mo1A B4A 78.6(10) . . ? C2A Mo1A B4A 37.8(8) . . ? B6A Mo1A B4A 76.2(7) . . ? B5A Mo1A B4A 64.7(9) . . ? C13A Mo1A B7A 111.1(10) . . ? C11A Mo1A B7A 169.9(9) . . ? C12A Mo1A B7A 87.1(10) . . ? B3A Mo1A B7A 38.7(10) . . ? C2A Mo1A B7A 77.4(8) . . ? B6A Mo1A B7A 62.9(7) . . ? B5A Mo1A B7A 82.5(9) . . ? B4A Mo1A B7A 43.9(9) . . ? C13A Mo1A Mn1A 150.8(7) . . ? C11A Mo1A Mn1A 85.1(5) . . ? C12A Mo1A Mn1A 76.9(8) . . ? B3A Mo1A Mn1A 48.8(7) . . ? C2A Mo1A Mn1A 125.3(5) . . ? B6A Mo1A Mn1A 53.05(8) . . ? B5A Mo1A Mn1A 86.2(5) . . ? B4A Mo1A Mn1A 123.5(7) . . ? B7A Mo1A Mn1A 87.5(6) . . ? C21A C2A B4A 125.1(17) . . ? C21A C2A B8A 111.2(16) . . ? B4A C2A B8A 72.5(16) . . ? C21A C2A B5A 117.6(16) . . ? B4A C2A B5A 114.0(18) . . ? B8A C2A B5A 67.9(14) . . ? C21A C2A Mo1A 124.9(13) . . ? B4A C2A Mo1A 82.3(13) . . ? B8A C2A Mo1A 123.1(14) . . ? B5A C2A Mo1A 78.2(11) . . ? B7A B3A B6A 102.0(19) . . ? B7A B3A B9A 59.6(18) . . ? B6A B3A B9A 66.7(15) . . ? B7A B3A Mo1A 85.6(16) . . ? B6A B3A Mo1A 71.7(11) . . ? B9A B3A Mo1A 116.1(18) . . ? B7A B3A Mn1A 169(2) . . ? B6A B3A Mn1A 74.6(11) . . ? B9A B3A Mn1A 126.1(19) . . ? Mo1A B3A Mn1A 83.5(10) . . ? C2A B4A B10A 106(2) . . ? C2A B4A B8A 54.6(14) . . ? B10A B4A B8A 58.4(14) . . ? C2A B4A B7A 121(2) . . ? B10A B4A B7A 57.7(15) . . ? B8A B4A B7A 107.7(19) . . ? C2A B4A Mo1A 60.0(12) . . ? B10A B4A Mo1A 106.4(16) . . ? B8A B4A Mo1A 98.5(14) . . ? B7A B4A Mo1A 71.3(13) . . ? C2A B5A B6A 111.8(15) . . ? C2A B5A B8A 55.4(12) . . ? B6A B5A B8A 102.5(15) . . ? C2A B5A B11A 108.0(16) . . ? B6A B5A B11A 53.5(11) . . ? B8A B5A B11A 61.4(14) . . ? C2A B5A Mo1A 61.6(10) . . ? B6A B5A Mo1A 65.1(8) . . ? B8A B5A Mo1A 103.2(13) . . ? B11A B5A Mo1A 107.0(13) . . ? B11A B6A B5A 69.1(12) . . ? B11A B6A B3A 116.4(14) . . ? B5A B6A B3A 132.1(13) . . ? B11A B6A B9A 56.9(14) . . ? B5A B6A B9A 114.0(14) . . ? B3A B6A B9A 60.6(14) . . ? B11A B6A Mo1A 125.2(10) . . ? B5A B6A Mo1A 74.5(8) . . ? B3A B6A Mo1A 64.3(10) . . ? B9A B6A Mo1A 107.1(11) . . ? B11A B6A Mn1A 156.4(10) . . ? B5A B6A Mn1A 130.6(8) . . ? B3A B6A Mn1A 62.9(10) . . ? B9A B6A Mn1A 112.6(11) . . ? Mo1A B6A Mn1A 77.02(9) . . ? B3A B7A B9A 65.7(19) . . ? B3A B7A B10A 107(2) . . ? B9A B7A B10A 51.3(17) . . ? B3A B7A B4A 113(2) . . ? B9A B7A B4A 101(2) . . ? B10A B7A B4A 56.9(15) . . ? B3A B7A Mo1A 55.7(14) . . ? B9A B7A Mo1A 100.8(18) . . ? B10A B7A Mo1A 101.4(16) . . ? B4A B7A Mo1A 64.8(12) . . ? C2A B8A B10A 104.9(18) . . ? C2A B8A B5A 56.7(13) . . ? B10A B8A B5A 104.4(18) . . ? C2A B8A B11A 108.0(18) . . ? B10A B8A B11A 61.8(14) . . ? B5A B8A B11A 60.3(13) . . ? C2A B8A B4A 52.9(13) . . ? B10A B8A B4A 58.5(14) . . ? B5A B8A B4A 93.5(17) . . ? B11A B8A B4A 103.1(17) . . ? B10A B9A B11A 70(2) . . ? B10A B9A B7A 66(2) . . ? B11A B9A B7A 114(3) . . ? B10A B9A B3A 110(3) . . ? B11A B9A B3A 102(2) . . ? B7A B9A B3A 54.7(17) . . ? B10A B9A B6A 96(2) . . ? B11A B9A B6A 50.4(14) . . ? B7A B9A B6A 89(2) . . ? B3A B9A B6A 52.7(14) . . ? B9A B10A B8A 117(2) . . ? B9A B10A B4A 118(3) . . ? B8A B10A B4A 63.2(15) . . ? B9A B10A B7A 63(2) . . ? B8A B10A B7A 118(2) . . ? B4A B10A B7A 65.4(16) . . ? B9A B10A B11A 59.6(18) . . ? B8A B10A B11A 61.0(14) . . ? B4A B10A B11A 105.9(19) . . ? B7A B10A B11A 105.0(19) . . ? B6A B11A B9A 72.6(17) . . ? B6A B11A B5A 57.4(12) . . ? B9A B11A B5A 117(2) . . ? B6A B11A B8A 103.1(17) . . ? B9A B11A B8A 105(2) . . ? B5A B11A B8A 58.3(13) . . ? B6A B11A B10A 98.5(17) . . ? B9A B11A B10A 50.6(16) . . ? B5A B11A B10A 99.7(17) . . ? B8A B11A B10A 57.3(13) . . ? C15A Mn1A C14A 91.3(12) . . ? C15A Mn1A C16A 98.9(12) . . ? C14A Mn1A C16A 91.0(11) . . ? C15A Mn1A H6A 90.8(9) . . ? C14A Mn1A H6A 177.0(8) . . ? C16A Mn1A H6A 86.5(7) . . ? C15A Mn1A H3A 99.3(9) . . ? C14A Mn1A H3A 86.7(8) . . ? C16A Mn1A H3A 161.7(7) . . ? H6A Mn1A H3A 95.07(14) . . ? C15A Mn1A B3A 109.3(12) . . ? C14A Mn1A B3A 112.9(11) . . ? C16A Mn1A B3A 141.8(11) . . ? H6A Mn1A B3A 68.4(7) . . ? H3A Mn1A B3A 28.8(7) . . ? C15A Mn1A B6A 105.9(9) . . ? C14A Mn1A B6A 153.4(8) . . ? C16A Mn1A B6A 105.7(7) . . ? H6A Mn1A B6A 27.08(4) . . ? H3A Mn1A B6A 70.77(10) . . ? B3A Mn1A B6A 42.5(7) . . ? C15A Mn1A Mo1A 154.0(9) . . ? C14A Mn1A Mo1A 108.3(8) . . ? C16A Mn1A Mo1A 97.7(7) . . ? H6A Mn1A Mo1A 70.40(10) . . ? H3A Mn1A Mo1A 65.98(9) . . ? B3A Mn1A Mo1A 47.7(8) . . ? B6A Mn1A Mo1A 49.92(7) . . ? O11A C11A Mo1A 171.8(17) . . ? O12A C12A Mo1A 179(3) . . ? O13A C13A Mo1A 170(2) . . ? O14A C14A Mn1A 177(2) . . ? O15A C15A Mn1A 162(3) . . ? O16A C16A Mn1A 176(2) . . ? C22A C21A C2A 125.7(18) . . ? C22A C21A C26A 116.0(19) . . ? C2A C21A C26A 117.8(18) . . ? C21A C22A C23A 126.2(19) . . ? C24A C23A C22A 117(2) . . ? C25A C24A C23A 122(2) . . ? C24A C25A C26A 123(2) . . ? C25A C26A C21A 114(2) . . ? C33 N1 C31 128(2) . . ? C33 N1 C37 108(2) . . ? C31 N1 C37 105(2) . . ? C33 N1 C35 102.4(19) . . ? C31 N1 C35 100(2) . . ? C37 N1 C35 113(2) . . ? C32 C31 N1 115(3) . . ? N1 C33 C34 117(3) . . ? C36 C35 N1 112(3) . . ? N1 C37 C38 104(2) . . ? C45 N2 C43 120(2) . . ? C45 N2 C47 115(2) . . ? C43 N2 C47 101(2) . . ? C45 N2 C41 95(2) . . ? C43 N2 C41 108(2) . . ? C47 N2 C41 120(2) . . ? C42 C41 N2 115(3) . . ? N2 C43 C44 129(3) . . ? N2 C45 C46 123(2) . . ? N2 C47 C48 99(2) . . ? C53 N3 C55 95(3) . . ? C53 N3 C51 110(4) . . ? C55 N3 C51 103(2) . . ? C53 N3 C57 126(4) . . ? C55 N3 C57 98(2) . . ? C51 N3 C57 117(2) . . ? C53 N3 C52 100(4) . . ? C55 N3 C52 148(3) . . ? C51 N3 C52 46(2) . . ? C57 N3 C52 96(3) . . ? C52 C51 N3 78(4) . . ? C51 C52 N3 56(4) . . ? N3 C53 C54 141(6) . . ? C56 C55 N3 125(3) . . ? C58 C57 N3 111(3) . . ? C63 N4 C67 107(2) . . ? C63 N4 C61 120(2) . . ? C67 N4 C61 101(2) . . ? C63 N4 C65 110(2) . . ? C67 N4 C65 102.5(19) . . ? C61 N4 C65 114(2) . . ? C62 C61 N4 117(3) . . ? C64 C63 N4 105(4) . . ? C66 C65 N4 123(3) . . ? C68 C67 N4 115(2) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 4.596 _refine_diff_density_min -2.440 _refine_diff_density_rms 0.220