Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Incarvito, Christopher' 'Liable-Sands, L. M.' 'Rheingold, Arnold' 'Trofimenko, S.' _publ_contact_author_name 'Prof S Trofimenko' _publ_contact_author_address ; Department of Chemistry & Biochemistry University of Delaware Newark Delaware 19716-2522 USA ; _publ_contact_author_email 'TROFIMEN@UDEL.EDU' _publ_section_title ; Novel and unique scorpionate ligands: BpBr3 and TpBr3 ; data_1 _database_code_CSD 172549 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H9 B Br6 Mo N4 O2' _chemical_formula_weight 827.44 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' '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5258(2) _cell_length_b 10.3977(2) _cell_length_c 13.2707(3) _cell_angle_alpha 87.2664(11) _cell_angle_beta 86.3381(8) _cell_angle_gamma 69.5095(7) _cell_volume 1099.35(6) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 28.0 _exptl_crystal_description 'orange-red' _exptl_crystal_colour block _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 11.515 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.356 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Siemens P4_CCD' _diffrn_measurement_method 'omega/phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6844 _diffrn_reflns_av_R_equivalents 0.0900 _diffrn_reflns_av_sigmaI/netI 0.0868 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4119 _reflns_number_gt 3257 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SAINT' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1000P)^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 4119 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1677 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _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 Mo Mo 0.77154(8) 0.65915(7) 0.26852(5) 0.0268(2) Uani 1 1 d . . . Br11 Br 0.48658(13) 1.23744(9) 0.35438(9) 0.0463(3) Uani 1 1 d . . . Br12 Br 0.13194(12) 1.12262(11) 0.44010(8) 0.0469(3) Uani 1 1 d . . . Br13 Br 0.29743(13) 0.74980(11) 0.39773(8) 0.0462(3) Uani 1 1 d . . . Br21 Br 0.81561(12) 1.16981(10) 0.09416(8) 0.0464(3) Uani 1 1 d . . . Br22 Br 0.71463(13) 1.02686(14) -0.13353(7) 0.0585(4) Uani 1 1 d . . . Br23 Br 0.64517(13) 0.71297(12) -0.04001(8) 0.0541(3) Uani 1 1 d . . . O6 O 0.5614(10) 0.4825(8) 0.2131(8) 0.066(2) Uani 1 1 d . . . O5 O 0.7547(12) 0.5034(9) 0.4766(6) 0.068(2) Uani 1 1 d . . . N11 N 0.5660(8) 0.8360(7) 0.3331(5) 0.0282(15) Uani 1 1 d . . . N12 N 0.6121(8) 0.9506(6) 0.3274(5) 0.0264(14) Uani 1 1 d . . . N21 N 0.7403(9) 0.8103(7) 0.1327(5) 0.0296(15) Uani 1 1 d . . . N22 N 0.7772(8) 0.9187(7) 0.1626(5) 0.0259(14) Uani 1 1 d . . . C1 C 0.9306(12) 0.4927(9) 0.1506(8) 0.041(2) Uani 1 1 d . . . H1A H 0.9423 0.3970 0.1670 0.050 Uiso 1 1 calc R . . H1B H 0.9151 0.5181 0.0789 0.050 Uiso 1 1 calc R . . C2 C 1.0348(11) 0.5479(9) 0.2018(8) 0.041(2) Uani 1 1 d . . . C3 C 1.0393(12) 0.5150(10) 0.3096(9) 0.049(3) Uani 1 1 d . . . H3A H 1.1035 0.5548 0.3491 0.059 Uiso 1 1 calc R . . H3B H 1.0521 0.4202 0.3300 0.059 Uiso 1 1 calc R . . C4 C 1.1246(12) 0.6351(10) 0.1510(8) 0.045(2) Uani 1 1 d . . . H4A H 1.1874 0.6606 0.2000 0.068 Uiso 1 1 calc R . . H4B H 1.0438 0.7173 0.1222 0.068 Uiso 1 1 calc R . . H4C H 1.2010 0.5840 0.0977 0.068 Uiso 1 1 calc R . . C5 C 0.7612(13) 0.5634(10) 0.3990(8) 0.045(2) Uani 1 1 d . . . C6 C 0.6416(12) 0.5465(9) 0.2313(8) 0.039(2) Uani 1 1 d . . . C11 C 0.4788(11) 1.0604(8) 0.3585(6) 0.0294(18) Uani 1 1 d . . . C12 C 0.3458(10) 1.0164(9) 0.3894(6) 0.0300(18) Uani 1 1 d . . . C13 C 0.4064(11) 0.8757(9) 0.3726(6) 0.0313(19) Uani 1 1 d . . . C21 C 0.7754(10) 1.0056(9) 0.0812(6) 0.0298(18) Uani 1 1 d . . . C22 C 0.7321(11) 0.9531(9) -0.0016(7) 0.034(2) Uani 1 1 d . . . C23 C 0.7104(10) 0.8314(9) 0.0331(6) 0.0290(17) Uani 1 1 d . . . B B 0.7911(11) 0.9270(10) 0.2786(7) 0.0276(19) Uani 1 1 d . . . H10A H 0.8280 1.0032 0.2931 0.033 Uiso 1 1 calc R . . H10B H 0.8718 0.8414 0.3050 0.033 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 Mo 0.0253(4) 0.0187(4) 0.0345(4) 0.0058(3) 0.0013(3) -0.0066(3) Br11 0.0497(6) 0.0255(5) 0.0627(7) -0.0042(4) 0.0064(5) -0.0129(4) Br12 0.0318(5) 0.0491(6) 0.0500(6) -0.0022(5) 0.0127(4) -0.0042(4) Br13 0.0422(5) 0.0476(6) 0.0570(6) 0.0015(5) 0.0115(4) -0.0285(5) Br21 0.0394(5) 0.0399(6) 0.0622(7) 0.0227(5) -0.0022(4) -0.0199(4) Br22 0.0404(6) 0.0886(9) 0.0293(5) 0.0214(5) -0.0006(4) -0.0041(6) Br23 0.0424(6) 0.0562(7) 0.0550(7) -0.0238(5) -0.0121(5) -0.0017(5) O6 0.054(5) 0.037(4) 0.114(7) -0.007(4) 0.001(5) -0.026(4) O5 0.085(6) 0.054(5) 0.063(5) 0.035(4) 0.004(4) -0.028(5) N11 0.027(3) 0.026(4) 0.027(4) 0.005(3) 0.004(3) -0.005(3) N12 0.028(4) 0.017(3) 0.032(4) 0.005(3) 0.003(3) -0.006(3) N21 0.025(3) 0.025(4) 0.032(4) 0.007(3) 0.003(3) -0.003(3) N22 0.022(3) 0.029(4) 0.023(3) 0.011(3) -0.001(3) -0.006(3) C1 0.034(5) 0.027(5) 0.057(6) -0.007(4) 0.005(4) -0.004(4) C2 0.030(5) 0.026(5) 0.061(6) 0.002(4) -0.004(4) -0.003(4) C3 0.030(5) 0.034(5) 0.072(7) 0.013(5) -0.005(5) 0.001(4) C4 0.031(5) 0.040(6) 0.058(6) 0.002(5) 0.007(4) -0.007(4) C5 0.044(6) 0.036(5) 0.050(6) 0.011(5) 0.000(4) -0.010(5) C6 0.039(5) 0.023(4) 0.058(6) -0.005(4) 0.011(4) -0.015(4) C11 0.033(4) 0.025(4) 0.030(4) 0.008(3) -0.002(3) -0.011(4) C12 0.029(4) 0.031(5) 0.024(4) 0.004(3) 0.001(3) -0.004(4) C13 0.036(5) 0.040(5) 0.023(4) 0.009(4) 0.003(3) -0.021(4) C21 0.020(4) 0.037(5) 0.025(4) 0.013(4) 0.001(3) -0.003(3) C22 0.026(4) 0.034(5) 0.034(5) 0.011(4) 0.000(3) 0.000(4) C23 0.019(4) 0.034(5) 0.028(4) -0.006(3) -0.003(3) -0.001(3) B 0.024(4) 0.029(5) 0.029(5) 0.004(4) -0.003(4) -0.009(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 Mo C5 1.969(10) . ? Mo C6 1.969(9) . ? Mo N11 2.211(7) . ? Mo C2 2.277(9) . ? Mo N21 2.300(7) . ? Mo C3 2.333(9) . ? Mo C1 2.372(9) . ? Br11 C11 1.863(8) . ? Br12 C12 1.871(8) . ? Br13 C13 1.859(8) . ? Br21 C21 1.872(9) . ? Br22 C22 1.871(9) . ? Br23 C23 1.852(8) . ? O6 C6 1.150(12) . ? O5 C5 1.186(12) . ? N11 C13 1.354(10) . ? N11 N12 1.377(10) . ? N12 C11 1.357(11) . ? N12 B 1.561(11) . ? N21 C23 1.356(11) . ? N21 N22 1.354(10) . ? N22 C21 1.372(10) . ? N22 B 1.561(11) . ? C1 C2 1.432(14) . ? C2 C3 1.455(15) . ? C2 C4 1.491(13) . ? C11 C12 1.396(11) . ? C12 C13 1.395(12) . ? C21 C22 1.375(13) . ? C22 C23 1.394(13) . ? 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 C5 Mo C6 80.6(4) . . ? C5 Mo N11 86.4(3) . . ? C6 Mo N11 99.6(3) . . ? C5 Mo C2 104.6(4) . . ? C6 Mo C2 104.2(4) . . ? N11 Mo C2 155.1(3) . . ? C5 Mo N21 167.6(3) . . ? C6 Mo N21 102.2(4) . . ? N11 Mo N21 81.3(2) . . ? C2 Mo N21 86.6(3) . . ? C5 Mo C3 69.8(4) . . ? C6 Mo C3 109.1(4) . . ? N11 Mo C3 138.3(4) . . ? C2 Mo C3 36.8(4) . . ? N21 Mo C3 119.6(3) . . ? C5 Mo C1 107.9(4) . . ? C6 Mo C1 69.8(4) . . ? N11 Mo C1 159.8(3) . . ? C2 Mo C1 35.8(3) . . ? N21 Mo C1 84.2(3) . . ? C3 Mo C1 61.6(4) . . ? C13 N11 N12 107.0(6) . . ? C13 N11 Mo 143.1(6) . . ? N12 N11 Mo 109.8(5) . . ? C11 N12 N11 108.8(6) . . ? C11 N12 B 136.1(7) . . ? N11 N12 B 114.7(6) . . ? C23 N21 N22 106.9(6) . . ? C23 N21 Mo 145.5(6) . . ? N22 N21 Mo 107.4(5) . . ? N21 N22 C21 109.4(7) . . ? N21 N22 B 115.8(6) . . ? C21 N22 B 134.4(8) . . ? C2 C1 Mo 68.5(5) . . ? C1 C2 C3 113.2(9) . . ? C1 C2 C4 123.7(9) . . ? C3 C2 C4 123.0(9) . . ? C1 C2 Mo 75.7(5) . . ? C3 C2 Mo 73.7(5) . . ? C4 C2 Mo 116.7(6) . . ? C2 C3 Mo 69.5(5) . . ? O5 C5 Mo 178.5(10) . . ? O6 C6 Mo 177.1(9) . . ? N12 C11 C12 109.0(7) . . ? N12 C11 Br11 121.9(6) . . ? C12 C11 Br11 129.0(7) . . ? C11 C12 C13 104.8(7) . . ? C11 C12 Br12 127.8(7) . . ? C13 C12 Br12 127.4(6) . . ? N11 C13 C12 110.3(7) . . ? N11 C13 Br13 121.2(7) . . ? C12 C13 Br13 128.5(6) . . ? N22 C21 C22 108.3(8) . . ? N22 C21 Br21 121.6(7) . . ? C22 C21 Br21 130.0(6) . . ? C21 C22 C23 105.4(7) . . ? C21 C22 Br22 126.9(7) . . ? C23 C22 Br22 127.6(7) . . ? N21 C23 C22 110.0(8) . . ? N21 C23 Br23 122.6(6) . . ? C22 C23 Br23 127.4(7) . . ? N22 B N12 106.1(6) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.415 _refine_diff_density_min -1.766 _refine_diff_density_rms 0.321 #===END data_2 _database_code_CSD 172550 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H23 B Mo N4 O2' _chemical_formula_weight 410.13 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 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 9.9584(5) _cell_length_b 14.4109(8) _cell_length_c 12.9238(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.5410(10) _cell_angle_gamma 90.00 _cell_volume 1803.13(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.8079 _exptl_absorpt_correction_T_max 0.8657 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 8822 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 28.37 _reflns_number_total 4084 _reflns_number_gt 3554 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0387P)^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 4084 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0866 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.368 _refine_ls_restrained_S_all 1.368 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.003 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 0.311804(17) 0.159190(14) 0.693442(16) 0.01965(8) Uani 1 1 d . . . O1 O 0.5042(2) 0.00837(15) 0.64110(18) 0.0471(6) Uani 1 1 d . . . O2 O 0.53083(19) 0.12983(17) 0.90558(17) 0.0437(5) Uani 1 1 d . . . N1 N 0.17998(17) 0.07776(15) 0.77204(16) 0.0218(4) Uani 1 1 d . . . N2 N 0.06099(18) 0.12526(14) 0.77265(16) 0.0215(4) Uani 1 1 d . . . N3 N 0.12957(19) 0.14612(14) 0.55879(17) 0.0223(4) Uani 1 1 d . . . N4 N 0.01615(18) 0.18297(14) 0.58712(16) 0.0215(4) Uani 1 1 d . . . B1 B 0.0435(3) 0.2137(2) 0.7039(2) 0.0237(6) Uani 1 1 d . . . H1 H 0.148(2) 0.2457(19) 0.721(2) 0.026(7) Uiso 1 1 d . . . H2 H -0.033(3) 0.2604(19) 0.721(2) 0.032(7) Uiso 1 1 d . . . C1 C -0.0142(2) 0.07642(18) 0.82792(19) 0.0253(5) Uani 1 1 d . . . C2 C 0.0575(2) -0.00300(18) 0.8639(2) 0.0275(5) Uani 1 1 d . . . H2A H 0.0299 -0.0507 0.9053 0.033 Uiso 1 1 calc R . . C3 C 0.1786(2) -0.00006(18) 0.82799(19) 0.0236(5) Uani 1 1 d . . . C4 C -0.1516(3) 0.1106(2) 0.8399(2) 0.0372(7) Uani 1 1 d . . . H4A H -0.1718 0.1707 0.8040 0.056 Uiso 1 1 calc R . . H4B H -0.1497 0.1178 0.9156 0.056 Uiso 1 1 calc R . . H4C H -0.2233 0.0658 0.8078 0.056 Uiso 1 1 calc R . . C5 C 0.2951(2) -0.0674(2) 0.8452(2) 0.0334(6) Uani 1 1 d . . . H5A H 0.3654 -0.0451 0.8092 0.050 Uiso 1 1 calc R . . H5B H 0.2608 -0.1280 0.8160 0.050 Uiso 1 1 calc R . . H5C H 0.3360 -0.0734 0.9216 0.050 Uiso 1 1 calc R . . C6 C -0.0972(2) 0.16535(17) 0.5102(2) 0.0265(5) Uani 1 1 d . . . C7 C -0.0569(2) 0.1188(2) 0.4302(2) 0.0305(6) Uani 1 1 d . . . H7A H -0.1148 0.0981 0.3650 0.037 Uiso 1 1 calc R . . C8 C 0.0859(2) 0.10785(18) 0.4633(2) 0.0251(5) Uani 1 1 d . . . C9 C -0.2391(2) 0.1930(2) 0.5203(2) 0.0380(7) Uani 1 1 d . . . H9A H -0.2322 0.2259 0.5877 0.057 Uiso 1 1 calc R . . H9B H -0.2962 0.1374 0.5187 0.057 Uiso 1 1 calc R . . H9C H -0.2815 0.2339 0.4609 0.057 Uiso 1 1 calc R . . C10 C 0.1797(3) 0.0611(2) 0.4057(2) 0.0341(6) Uani 1 1 d . . . H10A H 0.2747 0.0637 0.4489 0.051 Uiso 1 1 calc R . . H10B H 0.1748 0.0927 0.3377 0.051 Uiso 1 1 calc R . . H10C H 0.1517 -0.0038 0.3924 0.051 Uiso 1 1 calc R . . C11 C 0.4300(2) 0.0647(2) 0.6591(2) 0.0290(6) Uani 1 1 d . . . C12 C 0.4480(2) 0.14428(19) 0.8296(2) 0.0287(6) Uani 1 1 d . . . C13 C 0.4124(3) 0.2192(2) 0.5603(2) 0.0367(7) Uani 1 1 d . . . H13A H 0.5119 0.2065 0.5677 0.044 Uiso 1 1 calc R . . H13B H 0.3567 0.2153 0.4861 0.044 Uiso 1 1 calc R . . C14 C 0.3788(2) 0.28960(19) 0.6231(2) 0.0312(6) Uani 1 1 d . . . C15 C 0.4516(3) 0.2880(2) 0.7316(3) 0.0390(7) Uani 1 1 d . . . H15A H 0.4248 0.3351 0.7788 0.047 Uiso 1 1 calc R . . H15B H 0.5524 0.2771 0.7460 0.047 Uiso 1 1 calc R . . C16 C 0.2691(3) 0.3600(2) 0.5813(3) 0.0459(8) Uani 1 1 d . . . H16A H 0.3102 0.4134 0.5533 0.069 Uiso 1 1 calc R . . H16B H 0.2272 0.3804 0.6389 0.069 Uiso 1 1 calc R . . H16C H 0.1980 0.3322 0.5242 0.069 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 0.01526(11) 0.02190(13) 0.02188(14) 0.00130(8) 0.00453(8) 0.00045(7) O1 0.0435(11) 0.0447(14) 0.0587(15) 0.0066(11) 0.0231(10) 0.0232(10) O2 0.0331(10) 0.0579(14) 0.0326(12) 0.0024(10) -0.0073(8) 0.0004(9) N1 0.0197(8) 0.0248(11) 0.0207(11) -0.0002(9) 0.0044(7) 0.0016(8) N2 0.0195(8) 0.0246(11) 0.0215(11) -0.0029(9) 0.0071(7) -0.0009(8) N3 0.0175(9) 0.0273(12) 0.0227(11) 0.0015(9) 0.0056(8) 0.0047(8) N4 0.0188(8) 0.0225(11) 0.0240(11) 0.0023(8) 0.0066(7) 0.0055(8) B1 0.0208(11) 0.0241(15) 0.0267(15) -0.0021(12) 0.0067(10) 0.0012(10) C1 0.0254(11) 0.0315(15) 0.0203(13) -0.0042(11) 0.0077(9) -0.0072(10) C2 0.0308(11) 0.0302(15) 0.0223(13) 0.0001(11) 0.0075(9) -0.0094(10) C3 0.0270(11) 0.0249(14) 0.0168(12) -0.0016(10) 0.0006(9) -0.0037(9) C4 0.0303(12) 0.0464(19) 0.0404(18) 0.0010(14) 0.0193(12) -0.0005(12) C5 0.0349(13) 0.0288(15) 0.0334(16) 0.0078(12) 0.0019(11) 0.0033(11) C6 0.0213(11) 0.0300(15) 0.0265(14) 0.0055(11) 0.0020(9) 0.0021(9) C7 0.0269(11) 0.0383(16) 0.0225(14) -0.0032(12) -0.0018(9) -0.0001(11) C8 0.0280(11) 0.0265(14) 0.0203(13) 0.0001(10) 0.0047(9) 0.0007(10) C9 0.0206(11) 0.0502(18) 0.0411(17) 0.0035(14) 0.0027(10) 0.0069(12) C10 0.0372(13) 0.0384(17) 0.0283(15) -0.0043(12) 0.0106(11) 0.0055(12) C11 0.0243(11) 0.0359(16) 0.0268(14) 0.0071(12) 0.0060(9) 0.0042(10) C12 0.0238(11) 0.0317(15) 0.0301(15) -0.0008(11) 0.0055(10) -0.0018(10) C13 0.0289(12) 0.0429(18) 0.0432(18) 0.0108(14) 0.0186(11) -0.0025(12) C14 0.0253(11) 0.0283(15) 0.0425(17) 0.0063(12) 0.0128(11) -0.0029(10) C15 0.0338(13) 0.0308(16) 0.0507(19) 0.0005(14) 0.0067(12) -0.0129(12) C16 0.0459(16) 0.0337(17) 0.060(2) 0.0196(15) 0.0166(15) 0.0040(13) _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 C11 1.918(3) . ? Mo1 C12 1.966(3) . ? Mo1 N1 2.1810(19) . ? Mo1 N3 2.209(2) . ? Mo1 C14 2.255(3) . ? Mo1 C15 2.303(3) . ? Mo1 C13 2.349(3) . ? O1 C11 1.158(3) . ? O2 C12 1.144(3) . ? N1 C3 1.336(3) . ? N1 N2 1.370(2) . ? N2 C1 1.348(3) . ? N2 B1 1.540(4) . ? N3 C8 1.329(3) . ? N3 N4 1.373(2) . ? N4 C6 1.342(3) . ? N4 B1 1.535(4) . ? C1 C2 1.371(4) . ? C1 C4 1.496(3) . ? C2 C3 1.390(3) . ? C3 C5 1.489(3) . ? C6 C7 1.369(4) . ? C6 C9 1.504(3) . ? C7 C8 1.395(3) . ? C8 C10 1.486(3) . ? C13 C14 1.389(4) . ? C14 C15 1.420(4) . ? C14 C16 1.496(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Mo1 C12 78.32(11) . . ? C11 Mo1 N1 101.22(9) . . ? C12 Mo1 N1 83.59(9) . . ? C11 Mo1 N3 101.12(9) . . ? C12 Mo1 N3 164.43(9) . . ? N1 Mo1 N3 81.26(7) . . ? C11 Mo1 C14 104.05(10) . . ? C12 Mo1 C14 104.16(10) . . ? N1 Mo1 C14 154.57(8) . . ? N3 Mo1 C14 91.12(8) . . ? C11 Mo1 C15 104.40(11) . . ? C12 Mo1 C15 68.94(11) . . ? N1 Mo1 C15 137.16(10) . . ? N3 Mo1 C15 125.55(9) . . ? C14 Mo1 C15 36.28(10) . . ? C11 Mo1 C13 72.65(11) . . ? C12 Mo1 C13 111.90(10) . . ? N1 Mo1 C13 160.99(9) . . ? N3 Mo1 C13 82.34(9) . . ? C14 Mo1 C13 35.04(10) . . ? C15 Mo1 C13 61.36(11) . . ? C3 N1 N2 107.33(18) . . ? C3 N1 Mo1 141.92(15) . . ? N2 N1 Mo1 110.46(15) . . ? C1 N2 N1 109.3(2) . . ? C1 N2 B1 137.43(19) . . ? N1 N2 B1 113.02(17) . . ? C8 N3 N4 107.29(19) . . ? C8 N3 Mo1 142.87(16) . . ? N4 N3 Mo1 109.41(15) . . ? C6 N4 N3 109.3(2) . . ? C6 N4 B1 135.09(19) . . ? N3 N4 B1 113.94(18) . . ? N4 B1 N2 107.4(2) . . ? N2 C1 C2 107.8(2) . . ? N2 C1 C4 121.2(2) . . ? C2 C1 C4 131.0(2) . . ? C1 C2 C3 106.5(2) . . ? N1 C3 C2 109.0(2) . . ? N1 C3 C5 121.4(2) . . ? C2 C3 C5 129.6(2) . . ? N4 C6 C7 108.0(2) . . ? N4 C6 C9 122.0(2) . . ? C7 C6 C9 130.0(2) . . ? C6 C7 C8 106.3(2) . . ? N3 C8 C7 109.1(2) . . ? N3 C8 C10 123.1(2) . . ? C7 C8 C10 127.8(2) . . ? O1 C11 Mo1 178.0(2) . . ? O2 C12 Mo1 174.8(2) . . ? C14 C13 Mo1 68.79(15) . . ? C13 C14 C15 115.4(2) . . ? C13 C14 C16 122.6(3) . . ? C15 C14 C16 121.9(3) . . ? C13 C14 Mo1 76.17(16) . . ? C15 C14 Mo1 73.69(15) . . ? C16 C14 Mo1 116.78(17) . . ? C14 C15 Mo1 70.03(15) . . ? _diffrn_measured_fraction_theta_max 0.905 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.905 _refine_diff_density_max 0.496 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.073 #===END data_3 _database_code_CSD 172551 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H10 B Br9 Cl2 Mo N6 O2' _chemical_formula_weight 1215.14 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 19.3440(11) _cell_length_b 20.8714(12) _cell_length_c 16.7739(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6772.2(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 11.191 _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.1342 _exptl_absorpt_correction_T_max 0.2131 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25325 _diffrn_reflns_av_R_equivalents 0.0822 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5682 _reflns_number_gt 4096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.1000P)^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 5682 _refine_ls_number_parameters 310 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1320 _refine_ls_goodness_of_fit_ref 0.907 _refine_ls_restrained_S_all 0.907 _refine_ls_shift/su_max 0.000 _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 0.16862(3) 0.18318(4) 0.10686(4) 0.02324(19) Uani 1 1 d . . . B1 B 0.2492(5) 0.3237(5) 0.1146(5) 0.026(2) Uani 1 1 d D . . H1 H 0.273(4) 0.3714(18) 0.118(4) 0.033 Uiso 1 1 d D . . Br1 Br 0.42098(5) 0.34484(6) 0.13457(7) 0.0518(3) Uani 1 1 d . . . Br2 Br 0.48836(4) 0.18272(6) 0.13177(6) 0.0496(3) Uani 1 1 d . . . Br3 Br 0.33929(4) 0.08065(5) 0.11174(5) 0.0307(2) Uani 1 1 d . . . Br4 Br 0.23059(5) 0.44804(5) -0.01132(5) 0.0413(3) Uani 1 1 d . . . Br5 Br 0.16455(5) 0.37109(5) -0.18794(5) 0.0424(3) Uani 1 1 d . . . Br6 Br 0.14896(4) 0.20472(5) -0.13810(5) 0.0369(3) Uani 1 1 d . . . Br7 Br 0.22566(5) 0.44156(5) 0.24955(6) 0.0432(3) Uani 1 1 d . . . Br8 Br 0.15624(5) 0.35392(6) 0.41818(5) 0.0468(3) Uani 1 1 d . . . Br9 Br 0.14074(5) 0.19126(5) 0.35272(5) 0.0380(3) Uani 1 1 d . . . O1 O 0.1875(3) 0.0703(3) -0.0119(4) 0.0448(17) Uani 1 1 d . . . O2 O 0.1809(3) 0.0626(3) 0.2131(4) 0.0442(17) Uani 1 1 d . . . N1 N 0.3016(3) 0.2685(3) 0.1160(4) 0.0260(16) Uani 1 1 d . . . N2 N 0.2818(3) 0.2045(3) 0.1117(3) 0.0224(15) Uani 1 1 d . . . N3 N 0.2080(3) 0.3201(3) 0.0380(4) 0.0244(15) Uani 1 1 d . . . N4 N 0.1852(3) 0.2612(3) 0.0098(4) 0.0253(15) Uani 1 1 d . . . N5 N 0.2026(3) 0.3162(3) 0.1895(4) 0.0237(15) Uani 1 1 d . . . N6 N 0.1801(3) 0.2571(3) 0.2104(4) 0.0250(15) Uani 1 1 d . . . C1 C 0.3719(4) 0.2703(4) 0.1248(4) 0.028(2) Uani 1 1 d . . . C2 C 0.3979(4) 0.2092(5) 0.1224(4) 0.029(2) Uani 1 1 d . . . C3 C 0.3392(4) 0.1687(5) 0.1146(5) 0.029(2) Uani 1 1 d . . . C4 C 0.2032(4) 0.3631(4) -0.0212(5) 0.0260(19) Uani 1 1 d . . . C5 C 0.1783(4) 0.3340(4) -0.0895(5) 0.0242(18) Uani 1 1 d . . . C6 C 0.1714(4) 0.2706(4) -0.0664(5) 0.0269(19) Uani 1 1 d . . . C7 C 0.1966(4) 0.3562(4) 0.2527(5) 0.0290(19) Uani 1 1 d . . . C8 C 0.1718(4) 0.3235(5) 0.3168(5) 0.031(2) Uani 1 1 d . . . C9 C 0.1634(4) 0.2611(4) 0.2878(5) 0.028(2) Uani 1 1 d . . . C10 C 0.0634(4) 0.1636(5) 0.1735(6) 0.042(2) Uani 1 1 d . . . H10A H 0.0449 0.1205 0.1702 0.050 Uiso 1 1 calc R . . H10B H 0.0574 0.1836 0.2252 0.050 Uiso 1 1 calc R . . C11 C 0.0547(4) 0.2036(5) 0.1051(6) 0.038(2) Uani 1 1 d . . . C12 C 0.0659(4) 0.1710(5) 0.0326(6) 0.040(2) Uani 1 1 d . . . H12A H 0.0620 0.1960 -0.0159 0.047 Uiso 1 1 calc R . . H12B H 0.0472 0.1280 0.0284 0.047 Uiso 1 1 calc R . . C13 C 0.0358(5) 0.2734(5) 0.1093(7) 0.056(3) Uani 1 1 d . . . H13A H -0.0136 0.2778 0.1073 0.083 Uiso 1 1 calc R . . H13B H 0.0561 0.2957 0.0650 0.083 Uiso 1 1 calc R . . H13C H 0.0528 0.2913 0.1582 0.083 Uiso 1 1 calc R . . C14 C 0.1805(4) 0.1151(5) 0.0295(6) 0.036(2) Uani 1 1 d . . . C15 C 0.1776(4) 0.1094(5) 0.1768(6) 0.034(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0131(3) 0.0239(5) 0.0327(4) -0.0001(3) 0.0011(3) -0.0012(3) B1 0.024(5) 0.034(7) 0.019(4) -0.004(4) -0.003(3) 0.000(4) Br1 0.0284(5) 0.0473(7) 0.0797(8) 0.0051(6) -0.0043(5) -0.0160(5) Br2 0.0161(4) 0.0642(8) 0.0684(7) 0.0070(5) -0.0014(4) 0.0035(4) Br3 0.0249(4) 0.0339(6) 0.0334(5) -0.0014(4) -0.0002(3) 0.0067(4) Br4 0.0520(6) 0.0328(6) 0.0391(5) 0.0050(4) -0.0038(4) -0.0101(5) Br5 0.0410(5) 0.0590(7) 0.0271(5) 0.0092(4) -0.0041(4) -0.0055(5) Br6 0.0294(5) 0.0432(7) 0.0382(5) -0.0141(4) -0.0078(4) 0.0048(4) Br7 0.0570(6) 0.0326(6) 0.0400(5) -0.0079(4) 0.0008(4) -0.0090(5) Br8 0.0442(6) 0.0694(8) 0.0268(5) -0.0115(5) 0.0046(4) -0.0089(5) Br9 0.0306(5) 0.0429(7) 0.0404(5) 0.0139(4) 0.0090(4) 0.0044(4) O1 0.049(4) 0.027(4) 0.058(4) -0.014(3) -0.006(3) 0.005(3) O2 0.041(4) 0.035(5) 0.057(4) 0.018(3) 0.012(3) 0.002(3) N1 0.016(3) 0.026(5) 0.036(4) -0.005(3) 0.003(3) -0.008(3) N2 0.010(3) 0.035(5) 0.023(3) -0.001(3) 0.001(2) -0.002(3) N3 0.024(3) 0.026(4) 0.023(3) 0.003(3) 0.003(3) -0.004(3) N4 0.016(3) 0.022(4) 0.037(4) 0.005(3) 0.005(3) 0.006(3) N5 0.023(3) 0.025(4) 0.023(3) -0.005(3) 0.000(3) -0.001(3) N6 0.016(3) 0.028(5) 0.031(4) -0.001(3) 0.001(3) -0.002(3) C1 0.017(4) 0.034(6) 0.034(5) 0.004(4) 0.004(3) -0.011(4) C2 0.022(4) 0.040(6) 0.026(4) 0.009(4) 0.005(3) 0.002(4) C3 0.014(4) 0.041(6) 0.031(4) -0.001(4) 0.000(3) -0.003(4) C4 0.015(4) 0.035(6) 0.028(4) 0.001(4) -0.002(3) 0.010(3) C5 0.021(4) 0.021(5) 0.031(4) 0.002(3) 0.003(3) 0.003(3) C6 0.021(4) 0.025(6) 0.035(5) -0.015(4) -0.008(3) 0.001(3) C7 0.030(4) 0.031(6) 0.026(4) -0.002(4) -0.005(3) 0.001(4) C8 0.021(4) 0.041(6) 0.029(4) 0.000(4) 0.000(3) 0.002(4) C9 0.010(3) 0.038(6) 0.036(4) 0.015(4) 0.002(3) -0.003(4) C10 0.021(4) 0.049(7) 0.055(6) 0.013(5) 0.011(4) -0.007(4) C11 0.009(4) 0.046(7) 0.059(6) -0.002(5) -0.001(4) 0.002(4) C12 0.014(4) 0.044(7) 0.060(6) 0.009(5) -0.005(4) -0.013(4) C13 0.014(4) 0.054(8) 0.099(9) -0.004(6) 0.006(5) 0.016(5) C14 0.015(4) 0.031(6) 0.063(6) 0.001(5) 0.000(4) -0.003(4) C15 0.022(4) 0.025(6) 0.054(6) -0.001(4) 0.005(4) 0.001(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 C14 1.939(10) . ? Mo1 C15 1.944(10) . ? Mo1 N2 2.236(6) . ? Mo1 C11 2.244(8) . ? Mo1 N4 2.325(7) . ? Mo1 N6 2.334(7) . ? Mo1 C10 2.358(8) . ? Mo1 C12 2.358(8) . ? B1 N3 1.515(10) . ? B1 N1 1.534(12) . ? B1 N5 1.555(10) . ? Br1 C1 1.830(8) . ? Br2 C2 1.843(8) . ? Br3 C3 1.838(10) . ? Br4 C4 1.858(9) . ? Br5 C5 1.843(8) . ? Br6 C6 1.877(8) . ? Br7 C7 1.869(9) . ? Br8 C8 1.840(8) . ? Br9 C9 1.872(8) . ? O1 C14 1.171(10) . ? O2 C15 1.153(10) . ? N1 C1 1.368(10) . ? N1 N2 1.392(10) . ? N2 C3 1.339(10) . ? N3 C4 1.341(10) . ? N3 N4 1.391(9) . ? N4 C6 1.320(10) . ? N5 C7 1.354(10) . ? N5 N6 1.354(9) . ? N6 C9 1.339(10) . ? C1 C2 1.372(12) . ? C2 C3 1.421(12) . ? C4 C5 1.383(11) . ? C5 C6 1.384(12) . ? C7 C8 1.361(11) . ? C8 C9 1.401(12) . ? C10 C11 1.429(13) . ? C11 C12 1.409(13) . ? C11 C13 1.504(14) . ? 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 C14 Mo1 C15 79.2(4) . . ? C14 Mo1 N2 93.1(3) . . ? C15 Mo1 N2 92.8(3) . . ? C14 Mo1 C11 104.3(3) . . ? C15 Mo1 C11 104.2(3) . . ? N2 Mo1 C11 157.5(3) . . ? C14 Mo1 N4 91.6(3) . . ? C15 Mo1 N4 164.9(3) . . ? N2 Mo1 N4 75.6(2) . . ? C11 Mo1 N4 89.6(3) . . ? C14 Mo1 N6 166.3(3) . . ? C15 Mo1 N6 93.8(3) . . ? N2 Mo1 N6 75.4(2) . . ? C11 Mo1 N6 88.7(3) . . ? N4 Mo1 N6 92.6(2) . . ? C14 Mo1 C10 107.0(4) . . ? C15 Mo1 C10 69.7(3) . . ? N2 Mo1 C10 149.6(3) . . ? C11 Mo1 C10 36.1(3) . . ? N4 Mo1 C10 124.9(3) . . ? N6 Mo1 C10 81.0(3) . . ? C14 Mo1 C12 70.6(3) . . ? C15 Mo1 C12 108.0(3) . . ? N2 Mo1 C12 149.9(3) . . ? C11 Mo1 C12 35.6(3) . . ? N4 Mo1 C12 79.7(3) . . ? N6 Mo1 C12 123.0(3) . . ? C10 Mo1 C12 60.3(3) . . ? N3 B1 N1 108.9(7) . . ? N3 B1 N5 112.0(7) . . ? N1 B1 N5 107.2(7) . . ? C1 N1 N2 107.7(7) . . ? C1 N1 B1 129.6(7) . . ? N2 N1 B1 122.6(6) . . ? C3 N2 N1 107.9(6) . . ? C3 N2 Mo1 134.5(6) . . ? N1 N2 Mo1 117.5(5) . . ? C4 N3 N4 108.5(6) . . ? C4 N3 B1 129.2(7) . . ? N4 N3 B1 120.0(7) . . ? C6 N4 N3 105.2(6) . . ? C6 N4 Mo1 139.0(6) . . ? N3 N4 Mo1 115.1(5) . . ? C7 N5 N6 109.4(6) . . ? C7 N5 B1 128.3(7) . . ? N6 N5 B1 119.2(6) . . ? C9 N6 N5 105.7(7) . . ? C9 N6 Mo1 137.7(6) . . ? N5 N6 Mo1 116.1(4) . . ? N1 C1 C2 109.6(7) . . ? N1 C1 Br1 123.2(7) . . ? C2 C1 Br1 127.1(6) . . ? C1 C2 C3 105.3(7) . . ? C1 C2 Br2 128.6(7) . . ? C3 C2 Br2 126.0(7) . . ? N2 C3 C2 109.4(8) . . ? N2 C3 Br3 124.0(6) . . ? C2 C3 Br3 126.6(7) . . ? N3 C4 C5 110.1(8) . . ? N3 C4 Br4 123.5(6) . . ? C5 C4 Br4 126.3(6) . . ? C4 C5 C6 102.8(7) . . ? C4 C5 Br5 127.4(7) . . ? C6 C5 Br5 129.6(6) . . ? N4 C6 C5 113.2(7) . . ? N4 C6 Br6 123.9(7) . . ? C5 C6 Br6 122.9(6) . . ? N5 C7 C8 109.8(8) . . ? N5 C7 Br7 122.7(6) . . ? C8 C7 Br7 127.3(7) . . ? C7 C8 C9 103.4(7) . . ? C7 C8 Br8 128.0(7) . . ? C9 C8 Br8 128.6(6) . . ? N6 C9 C8 111.5(7) . . ? N6 C9 Br9 124.9(7) . . ? C8 C9 Br9 123.3(6) . . ? C11 C10 Mo1 67.6(4) . . ? C12 C11 C10 113.1(9) . . ? C12 C11 C13 123.0(9) . . ? C10 C11 C13 123.8(9) . . ? C12 C11 Mo1 76.6(5) . . ? C10 C11 Mo1 76.3(5) . . ? C13 C11 Mo1 115.0(6) . . ? C11 C12 Mo1 67.8(5) . . ? O1 C14 Mo1 174.2(8) . . ? O2 C15 Mo1 174.3(8) . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.602 _refine_diff_density_min -1.171 _refine_diff_density_rms 0.196 #===END data_4 _database_code_CSD 172552 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H29 B Mo N6 O2' _chemical_formula_weight 504.25 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 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 10.2604(6) _cell_length_b 27.6907(16) _cell_length_c 8.7327(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.8130(10) _cell_angle_gamma 90.00 _cell_volume 2252.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.613 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.8873 _exptl_absorpt_correction_T_max 0.8873 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 7977 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 24.00 _reflns_number_total 3224 _reflns_number_gt 2730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0646P)^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 SHELXL _refine_ls_extinction_coef 0.0004(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3224 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.708 _refine_ls_restrained_S_all 1.708 _refine_ls_shift/su_max 0.000 _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 0.81270(4) 0.105149(13) 0.14617(6) 0.0230(2) Uani 1 1 d . . . B1 B 0.5086(7) 0.13701(19) -0.1711(8) 0.0226(13) Uani 1 1 d . . . H1 H 0.405(6) 0.1448(18) -0.278(7) 0.027(13) Uiso 1 1 d . . . O1 O 1.0051(5) 0.15492(16) 0.4842(6) 0.0478(11) Uani 1 1 d . . . O2 O 0.8636(5) 0.03019(14) 0.4293(5) 0.0433(10) Uani 1 1 d . . . N1 N 0.4947(4) 0.13945(13) 0.0005(5) 0.0239(10) Uani 1 1 d . . . N2 N 0.6069(4) 0.12828(13) 0.1493(5) 0.0224(10) Uani 1 1 d . . . N3 N 0.6266(5) 0.17285(14) -0.1605(6) 0.0263(10) Uani 1 1 d . . . N4 N 0.7523(5) 0.17411(13) -0.0174(6) 0.0256(10) Uani 1 1 d . . . N5 N 0.5436(4) 0.08447(14) -0.1979(5) 0.0233(9) Uani 1 1 d . . . N6 N 0.6440(4) 0.05985(13) -0.0652(6) 0.0243(10) Uani 1 1 d . . . C1 C 0.3787(5) 0.15259(17) 0.0255(7) 0.0290(12) Uani 1 1 d . . . C2 C 0.4180(5) 0.14971(18) 0.1970(7) 0.0288(13) Uani 1 1 d . . . H2A H 0.3589 0.1567 0.2538 0.035 Uiso 1 1 calc R . . C3 C 0.5605(5) 0.13461(16) 0.2711(7) 0.0245(12) Uani 1 1 d . . . C4 C 0.2399(6) 0.1674(2) -0.1135(7) 0.0344(13) Uani 1 1 d . . . H4A H 0.2477 0.1655 -0.2214 0.052 Uiso 1 1 calc R . . H4B H 0.2171 0.2006 -0.0944 0.052 Uiso 1 1 calc R . . H4C H 0.1634 0.1457 -0.1162 0.052 Uiso 1 1 calc R . . C5 C 0.6524(6) 0.1273(2) 0.4513(7) 0.0350(13) Uani 1 1 d . . . H5A H 0.7479 0.1167 0.4653 0.052 Uiso 1 1 calc R . . H5B H 0.6097 0.1027 0.4966 0.052 Uiso 1 1 calc R . . H5C H 0.6610 0.1577 0.5121 0.052 Uiso 1 1 calc R . . C6 C 0.6081(6) 0.21562(17) -0.2463(7) 0.0289(13) Uani 1 1 d . . . C7 C 0.7243(6) 0.24403(18) -0.1562(7) 0.0332(13) Uani 1 1 d . . . H7A H 0.7419 0.2757 -0.1851 0.040 Uiso 1 1 calc R . . C8 C 0.8118(6) 0.21784(18) -0.0145(7) 0.0299(13) Uani 1 1 d . . . C9 C 0.4808(7) 0.22614(19) -0.4069(7) 0.0391(14) Uani 1 1 d . . . H9A H 0.4157 0.1983 -0.4380 0.059 Uiso 1 1 calc R . . H9B H 0.5123 0.2324 -0.4965 0.059 Uiso 1 1 calc R . . H9C H 0.4305 0.2546 -0.3918 0.059 Uiso 1 1 calc R . . C10 C 0.9443(6) 0.23648(19) 0.1245(7) 0.0377(14) Uani 1 1 d . . . H10A H 0.9858 0.2114 0.2104 0.056 Uiso 1 1 calc R . . H10B H 0.9209 0.2649 0.1751 0.056 Uiso 1 1 calc R . . H10C H 1.0139 0.2455 0.0796 0.056 Uiso 1 1 calc R . . C11 C 0.4578(6) 0.05339(18) -0.3180(7) 0.0279(12) Uani 1 1 d . . . C12 C 0.5054(6) 0.00778(17) -0.2624(7) 0.0313(13) Uani 1 1 d . . . H12A H 0.4681 -0.0215 -0.3212 0.038 Uiso 1 1 calc R . . C13 C 0.6185(6) 0.01224(16) -0.1037(7) 0.0268(12) Uani 1 1 d . . . C14 C 0.3341(6) 0.0688(2) -0.4740(8) 0.0400(15) Uani 1 1 d . . . H14A H 0.3281 0.1041 -0.4773 0.060 Uiso 1 1 calc R . . H14B H 0.2454 0.0553 -0.4752 0.060 Uiso 1 1 calc R . . H14C H 0.3471 0.0571 -0.5727 0.060 Uiso 1 1 calc R . . C15 C 0.6937(6) -0.02886(17) 0.0123(8) 0.0344(13) Uani 1 1 d . . . H15A H 0.7695 -0.0161 0.1161 0.052 Uiso 1 1 calc R . . H15B H 0.7362 -0.0503 -0.0435 0.052 Uiso 1 1 calc R . . H15C H 0.6243 -0.0470 0.0400 0.052 Uiso 1 1 calc R . . C16 C 1.0332(6) 0.12414(19) 0.1434(7) 0.0305(13) Uani 1 1 d . . . H16A H 1.0381 0.1547 0.0870 0.037 Uiso 1 1 calc R . . H16B H 1.1200 0.1175 0.2481 0.037 Uiso 1 1 calc R . . C17 C 0.9701(6) 0.08480(18) 0.0394(7) 0.0305(13) Uani 1 1 d . . . C18 C 0.9624(6) 0.04343(18) 0.1286(8) 0.0335(13) Uani 1 1 d . . . H18A H 1.0484 0.0357 0.2331 0.040 Uiso 1 1 calc R . . H18B H 0.9147 0.0147 0.0607 0.040 Uiso 1 1 calc R . . C19 C 0.9099(6) 0.0873(2) -0.1505(7) 0.0393(14) Uani 1 1 d . . . H19A H 0.9844 0.0781 -0.1875 0.059 Uiso 1 1 calc R . . H19B H 0.8778 0.1203 -0.1878 0.059 Uiso 1 1 calc R . . H19C H 0.8283 0.0651 -0.1997 0.059 Uiso 1 1 calc R . . C20 C 0.9310(6) 0.13905(18) 0.3524(8) 0.0320(13) Uani 1 1 d . . . C21 C 0.8402(5) 0.05572(18) 0.3193(7) 0.0279(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0179(3) 0.0250(3) 0.0236(4) 0.00060(17) 0.0062(3) 0.00121(16) B1 0.019(3) 0.026(3) 0.018(3) 0.001(2) 0.003(3) 0.001(2) O1 0.036(2) 0.055(3) 0.033(3) -0.015(2) -0.005(2) 0.002(2) O2 0.047(3) 0.044(2) 0.036(3) 0.017(2) 0.015(2) 0.014(2) N1 0.018(2) 0.025(2) 0.024(3) 0.0022(19) 0.004(2) 0.0041(17) N2 0.020(2) 0.024(2) 0.019(3) 0.0023(18) 0.004(2) 0.0023(17) N3 0.023(2) 0.032(2) 0.025(3) 0.0077(19) 0.011(2) 0.0046(19) N4 0.022(2) 0.026(2) 0.025(3) 0.0032(19) 0.006(2) 0.0000(18) N5 0.019(2) 0.026(2) 0.021(3) 0.001(2) 0.004(2) 0.0030(18) N6 0.019(2) 0.024(2) 0.031(3) -0.0048(19) 0.011(2) -0.0021(18) C1 0.020(3) 0.028(2) 0.036(4) 0.000(2) 0.009(3) -0.002(2) C2 0.027(3) 0.033(3) 0.031(4) -0.002(2) 0.016(3) -0.002(2) C3 0.025(3) 0.024(2) 0.024(3) -0.003(2) 0.010(3) -0.002(2) C4 0.023(3) 0.045(3) 0.031(4) 0.006(3) 0.008(3) 0.007(3) C5 0.034(3) 0.041(3) 0.029(4) 0.001(3) 0.012(3) 0.005(3) C6 0.038(3) 0.024(2) 0.030(3) 0.005(2) 0.019(3) 0.005(2) C7 0.039(3) 0.025(3) 0.035(4) 0.001(2) 0.015(3) -0.005(2) C8 0.025(3) 0.033(3) 0.031(3) 0.000(3) 0.011(3) 0.000(2) C9 0.048(4) 0.031(3) 0.032(4) 0.014(3) 0.010(3) 0.006(3) C10 0.034(3) 0.034(3) 0.039(4) 0.000(3) 0.010(3) -0.009(2) C11 0.024(3) 0.036(3) 0.026(3) -0.007(3) 0.012(3) -0.005(2) C12 0.031(3) 0.023(3) 0.036(4) -0.011(2) 0.011(3) -0.009(2) C13 0.025(3) 0.027(2) 0.031(4) -0.003(2) 0.014(3) -0.004(2) C14 0.031(3) 0.044(3) 0.038(4) 0.000(3) 0.007(3) -0.003(3) C15 0.031(3) 0.026(2) 0.048(4) -0.002(3) 0.018(3) -0.002(2) C16 0.018(3) 0.039(3) 0.034(4) 0.003(3) 0.010(3) -0.001(2) C17 0.022(3) 0.035(3) 0.037(4) 0.002(3) 0.016(3) 0.004(2) C18 0.020(3) 0.037(3) 0.039(4) -0.003(3) 0.008(3) 0.008(2) C19 0.034(3) 0.060(4) 0.029(4) 0.001(3) 0.018(3) 0.000(3) C20 0.025(3) 0.032(3) 0.039(4) 0.004(3) 0.014(3) 0.007(2) C21 0.020(3) 0.031(3) 0.028(3) -0.003(3) 0.006(3) 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 C20 1.940(6) . ? Mo1 C21 1.970(6) . ? Mo1 N2 2.218(4) . ? Mo1 C17 2.249(5) . ? Mo1 N6 2.301(4) . ? Mo1 N4 2.308(4) . ? Mo1 C16 2.332(5) . ? Mo1 C18 2.346(5) . ? B1 N3 1.538(7) . ? B1 N5 1.540(7) . ? B1 N1 1.566(7) . ? O1 C20 1.167(7) . ? O2 C21 1.134(6) . ? N1 C1 1.347(6) . ? N1 N2 1.361(6) . ? N2 C3 1.346(6) . ? N3 N4 1.369(6) . ? N3 C6 1.371(6) . ? N4 C8 1.352(6) . ? N5 C11 1.357(7) . ? N5 N6 1.366(6) . ? N6 C13 1.358(6) . ? C1 C2 1.381(8) . ? C1 C4 1.489(8) . ? C2 C3 1.392(7) . ? C3 C5 1.470(8) . ? C6 C7 1.368(8) . ? C6 C9 1.491(8) . ? C7 C8 1.390(8) . ? C8 C10 1.484(8) . ? C11 C12 1.368(7) . ? C11 C14 1.482(8) . ? C12 C13 1.390(8) . ? C13 C15 1.504(7) . ? C16 C17 1.392(8) . ? C17 C18 1.406(7) . ? C17 C19 1.509(8) . ? 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 C20 Mo1 C21 78.0(2) . . ? C20 Mo1 N2 94.40(18) . . ? C21 Mo1 N2 91.26(17) . . ? C20 Mo1 C17 103.2(2) . . ? C21 Mo1 C17 104.33(19) . . ? N2 Mo1 C17 158.50(19) . . ? C20 Mo1 N6 167.27(18) . . ? C21 Mo1 N6 93.11(18) . . ? N2 Mo1 N6 76.57(14) . . ? C17 Mo1 N6 87.71(17) . . ? C20 Mo1 N4 94.30(18) . . ? C21 Mo1 N4 164.69(17) . . ? N2 Mo1 N4 76.04(14) . . ? C17 Mo1 N4 90.22(17) . . ? N6 Mo1 N4 92.20(15) . . ? C20 Mo1 C16 70.7(2) . . ? C21 Mo1 C16 109.7(2) . . ? N2 Mo1 C16 150.18(17) . . ? C17 Mo1 C16 35.32(19) . . ? N6 Mo1 C16 121.40(17) . . ? N4 Mo1 C16 79.45(17) . . ? C20 Mo1 C18 104.0(2) . . ? C21 Mo1 C18 69.94(19) . . ? N2 Mo1 C18 149.81(16) . . ? C17 Mo1 C18 35.56(19) . . ? N6 Mo1 C18 80.98(17) . . ? N4 Mo1 C18 125.14(17) . . ? C16 Mo1 C18 59.93(18) . . ? N3 B1 N5 113.0(4) . . ? N3 B1 N1 107.5(4) . . ? N5 B1 N1 107.9(4) . . ? C1 N1 N2 111.0(4) . . ? C1 N1 B1 127.5(4) . . ? N2 N1 B1 121.6(4) . . ? C3 N2 N1 106.7(4) . . ? C3 N2 Mo1 134.5(4) . . ? N1 N2 Mo1 118.8(3) . . ? N4 N3 C6 109.8(4) . . ? N4 N3 B1 119.2(4) . . ? C6 N3 B1 126.9(5) . . ? C8 N4 N3 106.6(4) . . ? C8 N4 Mo1 136.7(4) . . ? N3 N4 Mo1 116.7(3) . . ? C11 N5 N6 110.6(4) . . ? C11 N5 B1 126.9(4) . . ? N6 N5 B1 118.9(4) . . ? C13 N6 N5 106.0(4) . . ? C13 N6 Mo1 136.8(4) . . ? N5 N6 Mo1 117.0(3) . . ? N1 C1 C2 106.5(5) . . ? N1 C1 C4 123.4(5) . . ? C2 C1 C4 130.1(5) . . ? C1 C2 C3 107.0(4) . . ? N2 C3 C2 108.8(5) . . ? N2 C3 C5 123.2(5) . . ? C2 C3 C5 128.0(5) . . ? C7 C6 N3 107.2(5) . . ? C7 C6 C9 129.6(5) . . ? N3 C6 C9 123.3(5) . . ? C6 C7 C8 107.0(4) . . ? N4 C8 C7 109.5(5) . . ? N4 C8 C10 125.4(5) . . ? C7 C8 C10 125.0(5) . . ? N5 C11 C12 107.0(5) . . ? N5 C11 C14 123.7(5) . . ? C12 C11 C14 129.2(5) . . ? C11 C12 C13 107.2(5) . . ? N6 C13 C12 109.1(5) . . ? N6 C13 C15 125.2(5) . . ? C12 C13 C15 125.6(4) . . ? C17 C16 Mo1 69.1(3) . . ? C16 C17 C18 113.2(5) . . ? C16 C17 C19 123.0(5) . . ? C18 C17 C19 123.7(5) . . ? C16 C17 Mo1 75.6(3) . . ? C18 C17 Mo1 76.0(3) . . ? C19 C17 Mo1 114.2(4) . . ? C17 C18 Mo1 68.5(3) . . ? O1 C20 Mo1 173.2(5) . . ? O2 C21 Mo1 173.8(5) . . ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.295 _refine_diff_density_min -0.761 _refine_diff_density_rms 0.101 #===END data_5 _database_code_CSD 172553 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H8 B Br9 N6 Pd' _chemical_formula_weight 1084.65 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1589(3) _cell_length_b 10.4504(3) _cell_length_c 12.6714(3) _cell_angle_alpha 101.967(2) _cell_angle_beta 92.483(2) _cell_angle_gamma 104.979(2) _cell_volume 1264.60(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 14.967 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.1176 _exptl_absorpt_correction_T_max 0.3160 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 12592 _diffrn_reflns_av_R_equivalents 0.0485 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.37 _reflns_number_total 5946 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0437P)^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 5946 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0950 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.006 _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 Pd1 Pd 0.27715(4) 0.71994(4) 0.33932(3) 0.02062(10) Uani 1 1 d . . . B1 B 0.1901(6) 0.9219(6) 0.1997(4) 0.0182(12) Uani 1 1 d . . . H1 H 0.156(5) 0.995(5) 0.160(4) 0.009(12) Uiso 1 1 d . . . Br1 Br -0.05087(6) 0.80133(6) -0.01711(5) 0.02777(14) Uani 1 1 d . . . Br2 Br -0.22589(6) 0.46248(6) 0.01885(5) 0.03085(14) Uani 1 1 d . . . Br3 Br -0.05884(6) 0.43995(6) 0.27151(5) 0.03198(15) Uani 1 1 d . . . Br4 Br 0.05970(7) 1.17648(7) 0.31833(6) 0.03959(17) Uani 1 1 d . . . Br5 Br 0.14078(8) 1.20765(7) 0.60608(5) 0.04043(17) Uani 1 1 d . . . Br6 Br 0.31813(8) 0.94708(7) 0.61696(5) 0.04348(18) Uani 1 1 d . . . Br7 Br 0.42754(7) 1.20406(6) 0.18570(6) 0.03930(17) Uani 1 1 d . . . Br8 Br 0.72089(6) 1.07685(7) 0.10509(5) 0.03449(16) Uani 1 1 d . . . Br9 Br 0.59923(7) 0.70828(7) 0.09929(6) 0.03635(16) Uani 1 1 d . . . N1 N 0.0940(4) 0.7767(4) 0.1699(3) 0.0164(9) Uani 1 1 d . . . N2 N 0.0949(4) 0.6875(4) 0.2364(3) 0.0178(9) Uani 1 1 d . . . N3 N 0.1961(4) 0.9753(4) 0.3250(3) 0.0178(9) Uani 1 1 d . . . N4 N 0.2569(5) 0.9194(4) 0.3951(4) 0.0202(9) Uani 1 1 d . . . N5 N 0.3352(5) 0.9212(4) 0.1711(3) 0.0183(9) Uani 1 1 d . . . N6 N 0.3752(5) 0.8039(5) 0.1507(4) 0.0220(10) Uani 1 1 d . . . C1 C -0.0119(5) 0.7179(5) 0.0922(4) 0.0201(11) Uani 1 1 d . . . C2 C -0.0813(5) 0.5924(5) 0.1070(4) 0.0218(11) Uani 1 1 d . . . C3 C -0.0111(6) 0.5802(5) 0.1989(4) 0.0213(11) Uani 1 1 d . . . C4 C 0.1511(5) 1.0764(5) 0.3819(4) 0.0208(11) Uani 1 1 d . . . C5 C 0.1822(6) 1.0871(6) 0.4909(5) 0.0242(12) Uani 1 1 d . . . C6 C 0.2465(6) 0.9869(5) 0.4938(4) 0.0239(12) Uani 1 1 d . . . C7 C 0.4395(6) 1.0265(6) 0.1608(4) 0.0222(11) Uani 1 1 d . . . C8 C 0.5505(6) 0.9781(6) 0.1318(4) 0.0238(12) Uani 1 1 d . . . C9 C 0.5039(6) 0.8406(6) 0.1283(4) 0.0242(12) Uani 1 1 d . . . C10 C 0.4622(6) 0.7200(7) 0.4205(6) 0.0360(15) Uani 1 1 d . . . H10A H 0.5426 0.7297 0.3784 0.043 Uiso 1 1 calc R . . H10B H 0.4838 0.7733 0.4964 0.043 Uiso 1 1 calc R . . C11 C 0.3724(6) 0.5884(6) 0.4039(5) 0.0314(14) Uani 1 1 d . . . C12 C 0.3200(7) 0.5303(6) 0.2952(6) 0.0341(15) Uani 1 1 d . . . H12A H 0.2404 0.4488 0.2820 0.041 Uiso 1 1 calc R . . H12B H 0.3882 0.5235 0.2423 0.041 Uiso 1 1 calc R . . C13 C 0.3130(8) 0.5295(8) 0.4950(7) 0.050(2) Uani 1 1 d . . . H13A H 0.3672 0.4718 0.5156 0.075 Uiso 1 1 calc R . . H13B H 0.2182 0.4749 0.4717 0.075 Uiso 1 1 calc R . . H13C H 0.3144 0.6033 0.5575 0.075 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 Pd1 0.0213(2) 0.0180(2) 0.0243(2) 0.00880(16) -0.00023(16) 0.00561(17) B1 0.028(3) 0.017(3) 0.011(3) 0.006(2) -0.001(2) 0.006(2) Br1 0.0261(3) 0.0337(3) 0.0245(3) 0.0125(2) -0.0015(2) 0.0058(2) Br2 0.0237(3) 0.0228(3) 0.0385(3) 0.0002(2) -0.0059(2) 0.0001(2) Br3 0.0347(3) 0.0206(3) 0.0438(4) 0.0158(3) 0.0081(3) 0.0056(3) Br4 0.0480(4) 0.0315(3) 0.0466(4) 0.0089(3) 0.0016(3) 0.0242(3) Br5 0.0503(4) 0.0295(3) 0.0339(4) -0.0058(3) 0.0186(3) 0.0056(3) Br6 0.0644(5) 0.0448(4) 0.0201(3) 0.0106(3) -0.0053(3) 0.0119(4) Br7 0.0445(4) 0.0190(3) 0.0522(4) 0.0123(3) 0.0057(3) 0.0013(3) Br8 0.0237(3) 0.0453(4) 0.0274(3) 0.0150(3) 0.0025(2) -0.0081(3) Br9 0.0289(3) 0.0404(4) 0.0462(4) 0.0137(3) 0.0130(3) 0.0160(3) N1 0.014(2) 0.018(2) 0.016(2) 0.0049(17) 0.0021(17) 0.0024(18) N2 0.021(2) 0.019(2) 0.017(2) 0.0062(17) 0.0027(17) 0.0085(19) N3 0.020(2) 0.016(2) 0.016(2) 0.0060(17) -0.0006(17) 0.0022(18) N4 0.025(2) 0.018(2) 0.018(2) 0.0075(18) 0.0021(18) 0.0040(19) N5 0.025(2) 0.014(2) 0.015(2) 0.0042(17) -0.0003(18) 0.0021(18) N6 0.020(2) 0.024(2) 0.024(2) 0.0081(19) 0.0078(19) 0.0068(19) C1 0.018(3) 0.025(3) 0.019(3) 0.004(2) 0.003(2) 0.008(2) C2 0.017(3) 0.020(3) 0.024(3) -0.002(2) 0.000(2) 0.003(2) C3 0.020(3) 0.018(3) 0.027(3) 0.002(2) 0.006(2) 0.008(2) C4 0.018(3) 0.016(3) 0.027(3) 0.001(2) 0.006(2) 0.003(2) C5 0.021(3) 0.021(3) 0.025(3) 0.000(2) 0.006(2) -0.001(2) C6 0.028(3) 0.022(3) 0.017(3) 0.005(2) 0.000(2) -0.002(2) C7 0.023(3) 0.026(3) 0.017(3) 0.011(2) 0.001(2) 0.000(2) C8 0.019(3) 0.031(3) 0.017(3) 0.008(2) 0.002(2) -0.002(2) C9 0.023(3) 0.033(3) 0.019(3) 0.012(2) 0.003(2) 0.007(2) C10 0.020(3) 0.043(4) 0.048(4) 0.022(3) -0.004(3) 0.005(3) C11 0.022(3) 0.034(3) 0.047(4) 0.022(3) -0.001(3) 0.014(3) C12 0.029(3) 0.027(3) 0.054(4) 0.018(3) 0.008(3) 0.015(3) C13 0.043(4) 0.049(4) 0.070(5) 0.038(4) 0.001(4) 0.015(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 Pd1 C10 2.103(6) . ? Pd1 C12 2.107(6) . ? Pd1 N4 2.124(4) . ? Pd1 N2 2.127(4) . ? Pd1 C11 2.141(5) . ? B1 N5 1.535(8) . ? B1 N1 1.537(7) . ? B1 N3 1.563(7) . ? Br1 C1 1.862(5) . ? Br2 C2 1.857(5) . ? Br3 C3 1.860(5) . ? Br4 C4 1.841(5) . ? Br5 C5 1.859(6) . ? Br6 C6 1.861(5) . ? Br7 C7 1.853(6) . ? Br8 C8 1.857(5) . ? Br9 C9 1.871(6) . ? N1 C1 1.348(7) . ? N1 N2 1.382(5) . ? N2 C3 1.324(7) . ? N3 C4 1.345(7) . ? N3 N4 1.365(5) . ? N4 C6 1.326(7) . ? N5 C7 1.349(7) . ? N5 N6 1.367(6) . ? N6 C9 1.324(7) . ? C1 C2 1.374(7) . ? C2 C3 1.384(8) . ? C4 C5 1.379(8) . ? C5 C6 1.376(8) . ? C7 C8 1.384(8) . ? C8 C9 1.382(7) . ? C10 C11 1.408(9) . ? C11 C12 1.404(10) . ? C11 C13 1.497(9) . ? 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 C10 Pd1 C12 68.1(3) . . ? C10 Pd1 N4 105.1(2) . . ? C12 Pd1 N4 173.2(2) . . ? C10 Pd1 N2 169.2(2) . . ? C12 Pd1 N2 101.7(2) . . ? N4 Pd1 N2 85.04(17) . . ? C10 Pd1 C11 38.7(2) . . ? C12 Pd1 C11 38.6(3) . . ? N4 Pd1 C11 135.7(2) . . ? N2 Pd1 C11 133.9(2) . . ? N5 B1 N1 110.4(4) . . ? N5 B1 N3 108.4(4) . . ? N1 B1 N3 107.7(4) . . ? C1 N1 N2 107.7(4) . . ? C1 N1 B1 131.0(4) . . ? N2 N1 B1 120.7(4) . . ? C3 N2 N1 106.5(4) . . ? C3 N2 Pd1 133.2(3) . . ? N1 N2 Pd1 117.8(3) . . ? C4 N3 N4 109.3(4) . . ? C4 N3 B1 130.1(4) . . ? N4 N3 B1 120.6(4) . . ? C6 N4 N3 106.0(4) . . ? C6 N4 Pd1 130.8(3) . . ? N3 N4 Pd1 118.6(3) . . ? C7 N5 N6 109.8(4) . . ? C7 N5 B1 128.6(4) . . ? N6 N5 B1 121.6(4) . . ? C9 N6 N5 105.2(4) . . ? N1 C1 C2 110.1(4) . . ? N1 C1 Br1 122.6(4) . . ? C2 C1 Br1 127.3(4) . . ? C1 C2 C3 103.8(5) . . ? C1 C2 Br2 128.5(4) . . ? C3 C2 Br2 127.5(4) . . ? N2 C3 C2 111.8(5) . . ? N2 C3 Br3 121.3(4) . . ? C2 C3 Br3 126.8(4) . . ? N3 C4 C5 108.7(5) . . ? N3 C4 Br4 123.3(4) . . ? C5 C4 Br4 128.0(4) . . ? C6 C5 C4 104.2(5) . . ? C6 C5 Br5 128.7(4) . . ? C4 C5 Br5 127.0(4) . . ? N4 C6 C5 111.8(5) . . ? N4 C6 Br6 121.4(4) . . ? C5 C6 Br6 126.7(4) . . ? N5 C7 C8 108.6(5) . . ? N5 C7 Br7 123.0(4) . . ? C8 C7 Br7 128.3(4) . . ? C9 C8 C7 103.5(5) . . ? C9 C8 Br8 128.9(4) . . ? C7 C8 Br8 127.6(4) . . ? N6 C9 C8 112.8(5) . . ? N6 C9 Br9 118.7(4) . . ? C8 C9 Br9 128.4(4) . . ? C11 C10 Pd1 72.1(3) . . ? C12 C11 C10 113.8(5) . . ? C12 C11 C13 122.0(6) . . ? C10 C11 C13 122.7(7) . . ? C12 C11 Pd1 69.4(3) . . ? C10 C11 Pd1 69.2(3) . . ? C13 C11 Pd1 119.0(4) . . ? C11 C12 Pd1 72.0(4) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.873 _refine_diff_density_min -1.059 _refine_diff_density_rms 0.184 #===END data_6 _database_code_CSD 172554 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H29 B N6 Pd' _chemical_formula_weight 458.69 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' 'Pd' 'Pd' -0.9988 1.0072 '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 16.0102(8) _cell_length_b 8.4061(4) _cell_length_c 17.2544(9) _cell_angle_alpha 90.00 _cell_angle_beta 114.7850(10) _cell_angle_gamma 90.00 _cell_volume 2108.25(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7513 _cell_measurement_theta_min 2.6005 _cell_measurement_theta_max 28.387 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.7158 _exptl_absorpt_correction_T_max 0.7749 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 10295 _diffrn_reflns_av_R_equivalents 0.0280 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 28.39 _reflns_number_total 4410 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0195P)^2^+1.8627P] 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 4410 _refine_ls_number_parameters 272 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.135 _refine_ls_restrained_S_all 1.135 _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 Pd1 Pd 0.254598(15) 0.10714(2) 0.407168(11) 0.02026(7) Uani 1 1 d . . . N1 N 0.14314(16) 0.2351(2) 0.31937(13) 0.0205(5) Uani 1 1 d . . . N2 N 0.13718(15) 0.2444(2) 0.23752(13) 0.0198(5) Uani 1 1 d . . . N3 N 0.22200(16) -0.0687(2) 0.31371(13) 0.0213(5) Uani 1 1 d . . . N4 N 0.20565(16) -0.0214(2) 0.23270(13) 0.0202(5) Uani 1 1 d . . . N5 N 0.30547(16) 0.2248(2) 0.26923(13) 0.0213(5) Uani 1 1 d . . . N6 N 0.31418(17) 0.3786(2) 0.29852(14) 0.0254(5) Uani 1 1 d . . . B1 B 0.2080(2) 0.1577(3) 0.21362(18) 0.0212(6) Uani 1 1 d . . . H1 H 0.1866(19) 0.176(3) 0.1467(17) 0.021(7) Uiso 1 1 d . . . C1 C 0.07391(19) 0.3184(3) 0.32210(17) 0.0251(6) Uani 1 1 d . . . C2 C 0.0216(2) 0.3825(3) 0.24156(18) 0.0289(6) Uani 1 1 d . . . H2 H -0.0318 0.4469 0.2256 0.035 Uiso 1 1 calc R . . C3 C 0.0629(2) 0.3341(3) 0.18992(17) 0.0250(6) Uani 1 1 d . . . C4 C 0.0589(2) 0.3293(4) 0.40142(19) 0.0360(7) Uani 1 1 d . . . H4A H 0.0061 0.2634 0.3955 0.054 Uiso 1 1 calc R . . H4B H 0.0469 0.4402 0.4110 0.054 Uiso 1 1 calc R . . H4C H 0.1140 0.2916 0.4500 0.054 Uiso 1 1 calc R . . C5 C 0.0350(2) 0.3680(3) 0.09726(18) 0.0349(7) Uani 1 1 d . . . H5A H 0.0839 0.4279 0.0903 0.052 Uiso 1 1 calc R . . H5B H -0.0218 0.4307 0.0750 0.052 Uiso 1 1 calc R . . H5C H 0.0247 0.2675 0.0658 0.052 Uiso 1 1 calc R . . C6 C 0.2135(2) -0.2264(3) 0.31240(17) 0.0260(6) Uani 1 1 d . . . C7 C 0.1934(2) -0.2832(3) 0.23047(18) 0.0287(6) Uani 1 1 d . . . H7 H 0.1848 -0.3909 0.2121 0.034 Uiso 1 1 calc R . . C8 C 0.1885(2) -0.1508(3) 0.18175(17) 0.0239(6) Uani 1 1 d . . . C9 C 0.2199(2) -0.3185(3) 0.3887(2) 0.0384(7) Uani 1 1 d . . . H9A H 0.2649 -0.2680 0.4406 0.058 Uiso 1 1 calc R . . H9B H 0.2394 -0.4277 0.3849 0.058 Uiso 1 1 calc R . . H9C H 0.1596 -0.3203 0.3906 0.058 Uiso 1 1 calc R . . C10 C 0.1698(2) -0.1410(3) 0.08960(17) 0.0329(7) Uani 1 1 d . . . H10A H 0.1169 -0.0712 0.0599 0.049 Uiso 1 1 calc R . . H10B H 0.1562 -0.2475 0.0643 0.049 Uiso 1 1 calc R . . H10C H 0.2239 -0.0980 0.0841 0.049 Uiso 1 1 calc R . . C11 C 0.3892(2) 0.1613(3) 0.28687(18) 0.0277(6) Uani 1 1 d . . . C12 C 0.4540(2) 0.2755(3) 0.32950(19) 0.0312(7) Uani 1 1 d . . . H12 H 0.5189 0.2662 0.3508 0.037 Uiso 1 1 calc R . . C13 C 0.4038(2) 0.4075(3) 0.33470(18) 0.0292(7) Uani 1 1 d . . . C14 C 0.4046(2) -0.0034(4) 0.2624(2) 0.0451(9) Uani 1 1 d . . . H14A H 0.3812 -0.0812 0.2908 0.068 Uiso 1 1 calc R . . H14B H 0.4706 -0.0208 0.2801 0.068 Uiso 1 1 calc R . . H14C H 0.3721 -0.0161 0.2004 0.068 Uiso 1 1 calc R . . C15 C 0.4398(3) 0.5681(4) 0.3729(2) 0.0454(9) Uani 1 1 d . . . H15A H 0.3894 0.6454 0.3529 0.068 Uiso 1 1 calc R . . H15B H 0.4878 0.6023 0.3554 0.068 Uiso 1 1 calc R . . H15C H 0.4656 0.5608 0.4353 0.068 Uiso 1 1 calc R . . C16 C 0.3427(2) 0.1151(3) 0.54095(17) 0.0304(7) Uani 1 1 d . . . C17 C 0.3140(2) 0.2697(3) 0.50918(19) 0.0337(7) Uani 1 1 d D . . H17A H 0.348(2) 0.331(4) 0.4872(19) 0.038(9) Uiso 1 1 d D . . H17B H 0.277(2) 0.333(4) 0.529(2) 0.050(10) Uiso 1 1 d D . . C18 C 0.3840(2) 0.0279(4) 0.49749(18) 0.0321(7) Uani 1 1 d D . . H18A H 0.4165(19) 0.087(3) 0.4727(18) 0.026(8) Uiso 1 1 d D . . H18B H 0.394(2) -0.078(3) 0.509(2) 0.037(9) Uiso 1 1 d D . . C19 C 0.3129(3) 0.0394(4) 0.60355(19) 0.0405(8) Uani 1 1 d . . . H19A H 0.3093 -0.0762 0.5952 0.061 Uiso 1 1 calc R . . H19B H 0.2523 0.0805 0.5948 0.061 Uiso 1 1 calc R . . H19C H 0.3576 0.0641 0.6617 0.061 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 Pd1 0.01947(14) 0.02192(9) 0.01865(10) 0.00039(7) 0.00727(9) 0.00177(7) N1 0.0190(14) 0.0222(10) 0.0205(10) 0.0004(8) 0.0085(10) 0.0012(8) N2 0.0190(14) 0.0200(9) 0.0196(10) 0.0006(7) 0.0072(10) 0.0008(8) N3 0.0242(14) 0.0178(9) 0.0248(10) 0.0009(8) 0.0130(10) 0.0014(8) N4 0.0241(14) 0.0178(9) 0.0210(10) 0.0008(7) 0.0116(10) 0.0012(8) N5 0.0207(14) 0.0201(9) 0.0244(10) 0.0026(8) 0.0107(10) 0.0003(8) N6 0.0268(16) 0.0208(10) 0.0269(11) 0.0016(8) 0.0095(11) -0.0008(9) B1 0.0238(19) 0.0186(12) 0.0216(13) 0.0012(10) 0.0097(13) 0.0011(10) C1 0.0180(17) 0.0265(12) 0.0308(13) -0.0049(10) 0.0102(12) -0.0013(10) C2 0.0203(18) 0.0278(12) 0.0362(15) 0.0001(11) 0.0095(13) 0.0057(10) C3 0.0210(17) 0.0208(11) 0.0282(13) 0.0011(10) 0.0054(12) 0.0006(10) C4 0.029(2) 0.0473(16) 0.0375(16) -0.0068(13) 0.0191(15) 0.0031(13) C5 0.033(2) 0.0357(15) 0.0288(14) 0.0058(11) 0.0054(14) 0.0072(12) C6 0.0285(18) 0.0197(11) 0.0305(13) 0.0021(10) 0.0129(13) 0.0007(10) C7 0.0323(19) 0.0184(11) 0.0349(14) -0.0030(10) 0.0136(14) -0.0002(10) C8 0.0222(17) 0.0235(12) 0.0261(12) -0.0032(9) 0.0104(12) -0.0003(10) C9 0.044(2) 0.0310(14) 0.0418(16) 0.0080(13) 0.0200(16) 0.0030(13) C10 0.046(2) 0.0283(13) 0.0274(13) -0.0054(10) 0.0179(14) -0.0014(12) C11 0.0219(18) 0.0294(13) 0.0366(15) 0.0081(11) 0.0168(13) 0.0040(11) C12 0.0175(18) 0.0356(14) 0.0387(15) 0.0108(12) 0.0101(14) 0.0012(11) C13 0.0256(19) 0.0279(13) 0.0301(14) 0.0053(11) 0.0076(13) -0.0043(11) C14 0.031(2) 0.0341(15) 0.076(3) -0.0023(15) 0.0283(19) 0.0072(13) C15 0.036(2) 0.0363(16) 0.053(2) -0.0065(14) 0.0074(17) -0.0110(14) C16 0.0192(18) 0.0417(15) 0.0212(12) -0.0038(11) -0.0005(12) -0.0002(12) C17 0.031(2) 0.0319(14) 0.0295(14) -0.0085(11) 0.0037(14) -0.0057(12) C18 0.0236(19) 0.0429(17) 0.0276(14) 0.0070(12) 0.0088(13) 0.0075(12) C19 0.041(2) 0.0545(19) 0.0259(14) -0.0003(13) 0.0136(15) 0.0050(15) _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 Pd1 N3 2.086(2) . ? Pd1 N1 2.090(2) . ? Pd1 C16 2.143(3) . ? N1 C1 1.328(3) . ? N1 N2 1.377(3) . ? N2 C3 1.356(3) . ? N2 B1 1.542(4) . ? N3 C6 1.332(3) . ? N3 N4 1.369(3) . ? N4 C8 1.353(3) . ? N4 B1 1.545(3) . ? N5 C11 1.354(4) . ? N5 N6 1.373(3) . ? N5 B1 1.556(4) . ? N6 C13 1.326(4) . ? C1 C2 1.395(4) . ? C1 C4 1.488(4) . ? C2 C3 1.374(4) . ? C3 C5 1.496(4) . ? C6 C7 1.396(4) . ? C6 C9 1.493(4) . ? C7 C8 1.377(4) . ? C8 C10 1.492(4) . ? C11 C12 1.377(4) . ? C11 C14 1.498(4) . ? C12 C13 1.395(4) . ? C13 C15 1.506(4) . ? C16 C18 1.397(4) . ? C16 C17 1.411(4) . ? C16 C19 1.494(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Pd1 N1 86.76(8) . . ? N3 Pd1 C16 133.89(10) . . ? N1 Pd1 C16 137.81(10) . . ? C1 N1 N2 107.8(2) . . ? C1 N1 Pd1 135.80(18) . . ? N2 N1 Pd1 116.32(16) . . ? C3 N2 N1 108.6(2) . . ? C3 N2 B1 131.1(2) . . ? N1 N2 B1 120.3(2) . . ? C6 N3 N4 107.3(2) . . ? C6 N3 Pd1 135.15(18) . . ? N4 N3 Pd1 117.56(14) . . ? C8 N4 N3 109.27(19) . . ? C8 N4 B1 131.4(2) . . ? N3 N4 B1 119.28(19) . . ? C11 N5 N6 110.5(2) . . ? C11 N5 B1 129.7(2) . . ? N6 N5 B1 119.3(2) . . ? C13 N6 N5 105.6(2) . . ? N2 B1 N4 108.5(2) . . ? N2 B1 N5 108.9(2) . . ? N4 B1 N5 109.2(2) . . ? N1 C1 C2 109.2(2) . . ? N1 C1 C4 121.6(2) . . ? C2 C1 C4 129.2(3) . . ? C3 C2 C1 106.3(2) . . ? N2 C3 C2 108.1(2) . . ? N2 C3 C5 123.1(3) . . ? C2 C3 C5 128.9(3) . . ? N3 C6 C7 109.6(2) . . ? N3 C6 C9 122.2(2) . . ? C7 C6 C9 128.1(2) . . ? C8 C7 C6 105.8(2) . . ? N4 C8 C7 108.0(2) . . ? N4 C8 C10 122.9(2) . . ? C7 C8 C10 129.1(2) . . ? N5 C11 C12 107.3(2) . . ? N5 C11 C14 124.4(3) . . ? C12 C11 C14 128.2(3) . . ? C11 C12 C13 105.3(3) . . ? N6 C13 C12 111.2(2) . . ? N6 C13 C15 120.7(3) . . ? C12 C13 C15 128.1(3) . . ? C18 C16 C17 115.1(3) . . ? C18 C16 C19 122.1(3) . . ? C17 C16 C19 121.6(3) . . ? C18 C16 Pd1 69.59(16) . . ? C17 C16 Pd1 69.53(16) . . ? C19 C16 Pd1 120.0(2) . . ? _diffrn_measured_fraction_theta_max 0.832 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.832 _refine_diff_density_max 0.974 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.069 #===END data_7 _database_code_CSD 172555 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H B Br9 N6 O2 Rh' _chemical_formula_weight 1082.09 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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 16.7656(16) _cell_length_b 14.2673(13) _cell_length_c 20.937(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.287(2) _cell_angle_gamma 90.00 _cell_volume 4634.0(8) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.102 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 16.281 _exptl_absorpt_correction_type 'Empirical from SADABS' _exptl_absorpt_correction_T_min 0.0845 _exptl_absorpt_correction_T_max 0.1392 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 11366 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.33 _reflns_number_total 5111 _reflns_number_gt 3995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0349P)^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 5111 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0709 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.014 _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 Rh1 Rh 1.01602(3) 0.13984(3) 0.333230(18) 0.02531(10) Uani 1 1 d . . . B1 B 0.8393(4) 0.0114(4) 0.2800(3) 0.0231(12) Uani 1 1 d . . . H1 H 0.788(3) -0.048(3) 0.2676(19) 0.007(10) Uiso 1 1 d . . . Br1 Br 0.81921(4) -0.19133(4) 0.35243(3) 0.03535(14) Uani 1 1 d . . . Br2 Br 1.02917(4) -0.22118(4) 0.49199(3) 0.04044(16) Uani 1 1 d . . . Br3 Br 1.14324(4) -0.00995(4) 0.49443(3) 0.03754(14) Uani 1 1 d . . . Br4 Br 0.66932(4) 0.03072(4) 0.32687(3) 0.03361(13) Uani 1 1 d . . . Br5 Br 0.69187(5) 0.26819(4) 0.39262(3) 0.04486(17) Uani 1 1 d . . . Br6 Br 0.87674(4) 0.36373(3) 0.35968(3) 0.03646(15) Uani 1 1 d . . . Br7 Br 0.75472(4) -0.08812(4) 0.12160(2) 0.03383(14) Uani 1 1 d . . . Br8 Br 0.90332(5) -0.01561(4) 0.04293(3) 0.04789(18) Uani 1 1 d . . . Br9 Br 1.06579(4) 0.11903(4) 0.17294(3) 0.03776(15) Uani 1 1 d . . . O1 O 1.1500(3) 0.2217(3) 0.4578(2) 0.0582(13) Uani 1 1 d . . . O2 O 1.0448(3) 0.3127(3) 0.2655(2) 0.0561(13) Uani 1 1 d . . . N1 N 0.9127(3) -0.0303(3) 0.34426(18) 0.0220(9) Uani 1 1 d . . . N2 N 0.9895(3) 0.0156(3) 0.37733(18) 0.0236(9) Uani 1 1 d . . . N3 N 0.8106(3) 0.1034(2) 0.30052(18) 0.0204(8) Uani 1 1 d . . . N4 N 0.8610(3) 0.1820(3) 0.30879(18) 0.0230(9) Uani 1 1 d . . . N5 N 0.8762(3) 0.0247(2) 0.22328(18) 0.0205(8) Uani 1 1 d . . . N6 N 0.9519(3) 0.0718(2) 0.23703(18) 0.0207(8) Uani 1 1 d . . . C1 C 0.9142(4) -0.1119(3) 0.3768(2) 0.0252(11) Uani 1 1 d . . . C2 C 0.9918(4) -0.1215(3) 0.4311(2) 0.0277(11) Uani 1 1 d . . . C3 C 1.0366(3) -0.0410(4) 0.4304(2) 0.0274(11) Uani 1 1 d . . . C4 C 0.7495(3) 0.1199(3) 0.3261(2) 0.0219(10) Uani 1 1 d . . . C5 C 0.7573(3) 0.2102(3) 0.3504(2) 0.0247(11) Uani 1 1 d . . . C6 C 0.8270(3) 0.2445(3) 0.3380(2) 0.0248(11) Uani 1 1 d . . . C7 C 0.8509(3) -0.0121(3) 0.1600(2) 0.0234(11) Uani 1 1 d . . . C8 C 0.9084(4) 0.0117(3) 0.1309(2) 0.0251(11) Uani 1 1 d . . . C9 C 0.9698(3) 0.0636(3) 0.1808(2) 0.0240(11) Uani 1 1 d . . . C10 C 1.0986(4) 0.1879(4) 0.4128(3) 0.0355(13) Uani 1 1 d . . . C11 C 1.0371(4) 0.2460(4) 0.2914(3) 0.0374(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0213(2) 0.0303(2) 0.02353(18) -0.00326(14) 0.00764(16) -0.00591(17) B1 0.020(3) 0.026(3) 0.023(3) 0.0045(19) 0.007(2) 0.005(2) Br1 0.0340(3) 0.0283(3) 0.0449(3) 0.0061(2) 0.0162(3) -0.0004(2) Br2 0.0453(4) 0.0439(3) 0.0298(3) 0.0155(2) 0.0116(3) 0.0143(3) Br3 0.0224(3) 0.0597(3) 0.0250(2) -0.0021(2) 0.0027(2) 0.0038(3) Br4 0.0287(3) 0.0411(3) 0.0365(3) 0.0001(2) 0.0185(2) -0.0052(2) Br5 0.0532(5) 0.0438(3) 0.0486(3) 0.0012(2) 0.0318(3) 0.0169(3) Br6 0.0483(4) 0.0229(2) 0.0345(3) 0.00029(19) 0.0117(3) -0.0006(2) Br7 0.0303(3) 0.0360(3) 0.0289(3) -0.0045(2) 0.0042(2) -0.0060(2) Br8 0.0615(5) 0.0624(4) 0.0236(3) -0.0065(2) 0.0205(3) -0.0065(3) Br9 0.0359(4) 0.0478(3) 0.0366(3) 0.0041(2) 0.0217(3) -0.0077(3) O1 0.049(3) 0.067(3) 0.043(2) -0.011(2) 0.000(2) -0.025(3) O2 0.071(4) 0.039(2) 0.056(3) -0.0010(19) 0.022(3) -0.023(2) N1 0.019(2) 0.0253(19) 0.0205(18) 0.0031(14) 0.0062(17) 0.0008(17) N2 0.020(2) 0.029(2) 0.0221(19) 0.0009(15) 0.0084(18) 0.0015(18) N3 0.017(2) 0.0212(18) 0.0206(18) 0.0008(14) 0.0045(17) 0.0006(17) N4 0.018(2) 0.025(2) 0.0236(19) 0.0015(15) 0.0057(17) -0.0001(17) N5 0.017(2) 0.0235(18) 0.0205(18) 0.0007(14) 0.0061(17) -0.0035(17) N6 0.016(2) 0.0229(18) 0.0235(19) 0.0027(14) 0.0087(17) -0.0023(17) C1 0.030(3) 0.023(2) 0.028(2) 0.0015(18) 0.016(2) 0.004(2) C2 0.029(3) 0.034(3) 0.023(2) 0.0050(18) 0.013(2) 0.010(2) C3 0.022(3) 0.040(3) 0.017(2) -0.0004(19) 0.005(2) 0.008(2) C4 0.016(3) 0.034(2) 0.019(2) 0.0044(17) 0.010(2) 0.002(2) C5 0.022(3) 0.031(2) 0.023(2) 0.0061(18) 0.010(2) 0.008(2) C6 0.026(3) 0.022(2) 0.019(2) 0.0030(16) 0.000(2) 0.001(2) C7 0.023(3) 0.023(2) 0.020(2) 0.0044(16) 0.003(2) 0.004(2) C8 0.029(3) 0.027(2) 0.018(2) -0.0010(17) 0.007(2) 0.004(2) C9 0.025(3) 0.025(2) 0.026(2) 0.0078(18) 0.014(2) 0.005(2) C10 0.026(3) 0.049(3) 0.032(3) -0.009(2) 0.012(3) -0.010(3) C11 0.038(4) 0.035(3) 0.037(3) -0.011(2) 0.013(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C10 1.847(5) . ? Rh1 C11 1.849(6) . ? Rh1 N6 2.124(4) . ? Rh1 N2 2.122(4) . ? Rh1 N4 2.523(4) . ? B1 N3 1.515(6) . ? B1 N5 1.544(7) . ? B1 N1 1.557(6) . ? Br1 C1 1.862(5) . ? Br2 C2 1.853(5) . ? Br3 C3 1.837(5) . ? Br4 C4 1.855(5) . ? Br5 C5 1.845(5) . ? Br6 C6 1.873(5) . ? Br7 C7 1.854(5) . ? Br8 C8 1.853(4) . ? Br9 C9 1.854(5) . ? O1 C10 1.117(6) . ? O2 C11 1.126(6) . ? N1 C1 1.344(5) . ? N1 N2 1.376(6) . ? N2 C3 1.358(6) . ? N3 C4 1.346(6) . ? N3 N4 1.375(5) . ? N4 C6 1.326(6) . ? N5 C7 1.337(5) . ? N5 N6 1.368(5) . ? N6 C9 1.327(6) . ? C1 C2 1.371(7) . ? C2 C3 1.375(7) . ? C4 C5 1.373(6) . ? C5 C6 1.380(7) . ? C7 C8 1.364(7) . ? C8 C9 1.372(7) . ? 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 C10 Rh1 C11 84.9(2) . . ? C10 Rh1 N6 164.0(2) . . ? C11 Rh1 N6 92.50(18) . . ? C10 Rh1 N2 97.3(2) . . ? C11 Rh1 N2 177.75(19) . . ? N6 Rh1 N2 85.24(14) . . ? C10 Rh1 N4 117.1(2) . . ? C11 Rh1 N4 94.3(2) . . ? N6 Rh1 N4 78.75(14) . . ? N2 Rh1 N4 85.30(14) . . ? N3 B1 N5 112.0(4) . . ? N3 B1 N1 108.5(4) . . ? N5 B1 N1 107.2(4) . . ? C1 N1 N2 108.8(4) . . ? C1 N1 B1 128.8(4) . . ? N2 N1 B1 122.3(4) . . ? C3 N2 N1 105.7(4) . . ? C3 N2 Rh1 134.5(4) . . ? N1 N2 Rh1 119.3(3) . . ? C4 N3 N4 109.4(4) . . ? C4 N3 B1 129.5(4) . . ? N4 N3 B1 119.7(4) . . ? C6 N4 N3 104.8(4) . . ? C6 N4 Rh1 131.0(3) . . ? N3 N4 Rh1 111.6(3) . . ? C7 N5 N6 108.8(4) . . ? C7 N5 B1 130.2(4) . . ? N6 N5 B1 120.6(4) . . ? C9 N6 N5 105.9(4) . . ? C9 N6 Rh1 132.8(3) . . ? N5 N6 Rh1 121.3(3) . . ? N1 C1 C2 109.7(5) . . ? N1 C1 Br1 122.5(4) . . ? C2 C1 Br1 127.6(4) . . ? C3 C2 C1 104.9(4) . . ? C3 C2 Br2 127.2(4) . . ? C1 C2 Br2 127.9(4) . . ? N2 C3 C2 110.8(5) . . ? N2 C3 Br3 123.8(4) . . ? C2 C3 Br3 125.4(4) . . ? N3 C4 C5 109.4(4) . . ? N3 C4 Br4 123.2(3) . . ? C5 C4 Br4 127.5(4) . . ? C4 C5 C6 103.4(4) . . ? C4 C5 Br5 127.4(4) . . ? C6 C5 Br5 129.2(4) . . ? N4 C6 C5 113.1(4) . . ? N4 C6 Br6 119.5(4) . . ? C5 C6 Br6 127.4(4) . . ? N5 C7 C8 109.4(4) . . ? N5 C7 Br7 123.8(4) . . ? C8 C7 Br7 126.8(3) . . ? C7 C8 C9 104.5(4) . . ? C7 C8 Br8 128.1(4) . . ? C9 C8 Br8 127.4(4) . . ? N6 C9 C8 111.4(4) . . ? N6 C9 Br9 122.4(4) . . ? C8 C9 Br9 126.1(4) . . ? O1 C10 Rh1 174.7(5) . . ? O2 C11 Rh1 175.5(6) . . ? _diffrn_measured_fraction_theta_max 0.885 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.885 _refine_diff_density_max 0.729 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.138 #===END