Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Mike Ward' _publ_contact_author_address ; Department of Chemistry University of Sheffield Dainton Building Sheffield S3 7HF UK ; _publ_contact_author_email M.D.WARD@SHEFFIELD.AC.UK _publ_contact_author_fax '0114 2229346' _publ_section_title ; New third-generation bis-, tris- and tetrakis(pyrazolyl)borate ligands with 3-pyridyl and 4-pyridyl substituents: synthesis and coordination chemistry ; loop_ _publ_author_name 'Mike Ward' 'Harry Adams' 'S. Batten' 'Simon Coles' 'Graham M. Davies' 'Martin B. Duriska' ; M.Hursthouse ; 'J. Jeffery' 'Paul Jensen' 'Jinzhen Lu.' 'Graham R. Motson' data_4pypz _database_code_depnum_ccdc_archive 'CCDC 264755' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H7 N3' _chemical_formula_sum 'C8 H7 N3' _chemical_formula_weight 145.17 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' 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 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 6.9317(6) _cell_length_b 9.0964(8) _cell_length_c 11.0059(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.2630(10) _cell_angle_gamma 90.00 _cell_volume 693.42(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5322 _cell_measurement_theta_min 4.478 _cell_measurement_theta_max 55.092 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.55 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9474 _exptl_absorpt_correction_T_max 0.9814 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7586 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.55 _reflns_number_total 1590 _reflns_number_gt 1458 _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^)+(0.0639P)^2^+0.1638P] 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 1590 _refine_ls_number_parameters 104 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1061 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _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 N1 N 0.17631(13) 0.24244(10) 0.74777(8) 0.0255(2) Uani 1 1 d . . . N2 N 0.05128(13) 0.17976(11) 0.82332(9) 0.0272(2) Uani 1 1 d . . . H2 H -0.037(2) 0.2355(18) 0.8615(15) 0.044(4) Uiso 1 1 d . . . C3 C 0.08244(16) 0.03512(13) 0.83818(10) 0.0281(3) Uani 1 1 d . . . H3 H 0.0109 -0.0298 0.8868 0.034 Uiso 1 1 calc R . . C4 C 0.23682(16) -0.00141(12) 0.77007(9) 0.0256(3) Uani 1 1 d . . . H4 H 0.2949 -0.0953 0.7619 0.031 Uiso 1 1 calc R . . C5 C 0.28991(14) 0.13140(11) 0.71494(9) 0.0215(2) Uani 1 1 d . . . C6 C 0.44903(14) 0.15825(11) 0.63363(9) 0.0214(2) Uani 1 1 d . . . C7 C 0.61685(15) 0.07307(12) 0.64144(9) 0.0245(2) Uani 1 1 d . . . H7 H 0.6286 -0.0055 0.6981 0.029 Uiso 1 1 calc R . . C8 C 0.76571(16) 0.10484(13) 0.56536(10) 0.0292(3) Uani 1 1 d . . . H8 H 0.8796 0.0469 0.5726 0.035 Uiso 1 1 calc R . . N9 N 0.75885(14) 0.21244(12) 0.48208(9) 0.0309(3) Uani 1 1 d . . . C10 C 0.59613(17) 0.29209(13) 0.47425(10) 0.0297(3) Uani 1 1 d . . . H10 H 0.5873 0.3683 0.4152 0.036 Uiso 1 1 calc R . . C11 C 0.44044(16) 0.27007(12) 0.54682(10) 0.0262(3) Uani 1 1 d . . . H11 H 0.3289 0.3304 0.5377 0.031 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 N1 0.0210(4) 0.0281(5) 0.0277(5) -0.0013(3) 0.0054(4) 0.0004(3) N2 0.0211(4) 0.0344(5) 0.0266(5) -0.0039(4) 0.0065(4) -0.0005(4) C3 0.0276(5) 0.0335(6) 0.0235(5) -0.0009(4) 0.0049(4) -0.0070(4) C4 0.0286(5) 0.0250(5) 0.0235(5) -0.0008(4) 0.0043(4) -0.0021(4) C5 0.0201(5) 0.0241(5) 0.0204(5) -0.0015(4) 0.0017(4) -0.0003(4) C6 0.0208(5) 0.0236(5) 0.0199(5) -0.0030(4) 0.0023(4) -0.0017(4) C7 0.0246(5) 0.0272(5) 0.0221(5) -0.0010(4) 0.0041(4) 0.0026(4) C8 0.0237(5) 0.0371(6) 0.0274(6) -0.0050(4) 0.0061(4) 0.0025(4) N9 0.0285(5) 0.0408(6) 0.0239(5) -0.0041(4) 0.0080(4) -0.0067(4) C10 0.0322(6) 0.0347(6) 0.0225(5) 0.0032(4) 0.0030(4) -0.0071(5) C11 0.0243(5) 0.0289(5) 0.0253(5) 0.0021(4) 0.0005(4) 0.0000(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 N1 C5 1.3392(14) . ? N1 N2 1.3507(13) . ? N2 C3 1.3423(16) . ? N2 H2 0.909(17) . ? C3 C4 1.3714(15) . ? C3 H3 0.9500 . ? C4 C5 1.4074(14) . ? C4 H4 0.9500 . ? C5 C6 1.4680(14) . ? C6 C11 1.3952(15) . ? C6 C7 1.3975(14) . ? C7 C8 1.3848(15) . ? C7 H7 0.9500 . ? C8 N9 1.3404(16) . ? C8 H8 0.9500 . ? N9 C10 1.3405(16) . ? C10 C11 1.3823(15) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? 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 N1 N2 104.25(9) . . ? C3 N2 N1 112.63(9) . . ? C3 N2 H2 126.8(10) . . ? N1 N2 H2 120.5(10) . . ? N2 C3 C4 107.23(9) . . ? N2 C3 H3 126.4 . . ? C4 C3 H3 126.4 . . ? C3 C4 C5 104.51(10) . . ? C3 C4 H4 127.7 . . ? C5 C4 H4 127.7 . . ? N1 C5 C4 111.38(9) . . ? N1 C5 C6 120.20(10) . . ? C4 C5 C6 128.40(10) . . ? C11 C6 C7 117.34(10) . . ? C11 C6 C5 121.73(9) . . ? C7 C6 C5 120.92(9) . . ? C8 C7 C6 119.04(10) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? N9 C8 C7 123.96(10) . . ? N9 C8 H8 118.0 . . ? C7 C8 H8 118.0 . . ? C8 N9 C10 116.47(10) . . ? N9 C10 C11 123.96(10) . . ? N9 C10 H10 118.0 . . ? C11 C10 H10 118.0 . . ? C10 C11 C6 119.22(10) . . ? C10 C11 H11 120.4 . . ? C6 C11 H11 120.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.187 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.093 #=END data_3pypz(polymorphI) _database_code_depnum_ccdc_archive 'CCDC 264756' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3pypz _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H7 N3' _chemical_formula_weight 145.17 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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 21.853(4) _cell_length_b 8.4566(17) _cell_length_c 3.8270(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 707.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4602 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 28.08 _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector CCD _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4596 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 3 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 28.08 _reflns_number_total 934 _reflns_number_gt 601 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0635P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(10) _refine_ls_number_reflns 934 _refine_ls_number_parameters 104 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1035 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.035 _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 C6 C 0.63287(12) 0.0157(3) 0.9768(9) 0.0188(7) Uani 1 1 d . . . N8 N 0.63104(10) 0.3010(3) 0.9878(7) 0.0239(7) Uani 1 1 d . . . C7 C 0.60652(12) 0.1598(3) 1.0617(8) 0.0208(8) Uani 1 1 d . . . H7 H 0.5684 0.1582 1.1806 0.025 Uiso 1 1 calc R . . C9 C 0.68575(13) 0.3011(4) 0.8273(9) 0.0254(8) Uani 1 1 d . . . H9 H 0.7039 0.3998 0.7706 0.030 Uiso 1 1 calc R . . C11 C 0.68988(12) 0.0203(3) 0.8116(9) 0.0229(8) Uani 1 1 d . . . H11 H 0.7100 -0.0751 0.7483 0.027 Uiso 1 1 calc R . . C5 C 0.60203(12) -0.1339(3) 1.0582(8) 0.0188(7) Uani 1 1 d . . . C10 C 0.71676(13) 0.1645(3) 0.7411(9) 0.0245(8) Uani 1 1 d . . . H10 H 0.7560 0.1695 0.6349 0.029 Uiso 1 1 calc R . . N1 N 0.63065(10) -0.2718(3) 1.0017(7) 0.0226(7) Uani 1 1 d . . . C4 C 0.54270(12) -0.1588(3) 1.1936(9) 0.0225(8) Uani 1 1 d . . . H4 H 0.5133 -0.0809 1.2560 0.027 Uiso 1 1 calc R . . N2 N 0.58955(10) -0.3838(3) 1.0996(9) 0.0264(7) Uani 1 1 d . . . C3 C 0.53671(13) -0.3197(4) 1.2155(9) 0.0263(8) Uani 1 1 d . . . H3 H 0.5019 -0.3759 1.2970 0.032 Uiso 1 1 calc R . . H2 H 0.6011(12) -0.503(3) 1.075(10) 0.039(9) Uiso 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 C6 0.0155(14) 0.0209(17) 0.0200(19) -0.0019(15) -0.0034(13) 0.0017(12) N8 0.0190(12) 0.0207(15) 0.0321(19) 0.0007(15) -0.0027(12) -0.0009(11) C7 0.0155(13) 0.0224(19) 0.0246(19) -0.0021(15) -0.0010(14) -0.0017(12) C9 0.0218(15) 0.025(2) 0.0289(19) 0.0022(17) -0.0042(15) -0.0064(14) C11 0.0207(15) 0.0194(19) 0.029(2) 0.0003(16) -0.0008(14) 0.0020(13) C5 0.0185(14) 0.0176(17) 0.0205(18) 0.0008(15) -0.0039(14) 0.0025(12) C10 0.0187(14) 0.0266(19) 0.028(2) 0.0030(16) 0.0007(14) -0.0008(13) N1 0.0184(12) 0.0158(15) 0.0336(19) 0.0025(15) -0.0004(12) -0.0019(10) C4 0.0190(14) 0.020(2) 0.029(2) -0.0016(15) 0.0024(13) 0.0022(12) N2 0.0260(14) 0.0156(14) 0.0375(17) 0.0007(13) -0.0020(14) -0.0021(11) C3 0.0212(15) 0.028(2) 0.030(2) -0.0052(18) 0.0034(14) 0.0000(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 C6 C7 1.386(4) . ? C6 C11 1.398(4) . ? C6 C5 1.467(4) . ? N8 C7 1.339(3) . ? N8 C9 1.344(4) . ? C9 C10 1.379(4) . ? C11 C10 1.380(4) . ? C5 N1 1.341(3) . ? C5 C4 1.412(4) . ? N1 N2 1.358(3) . ? C4 C3 1.370(4) . ? N2 C3 1.351(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 C7 C6 C11 116.9(2) . . ? C7 C6 C5 121.2(3) . . ? C11 C6 C5 122.0(2) . . ? C7 N8 C9 116.9(2) . . ? N8 C7 C6 124.6(3) . . ? N8 C9 C10 123.1(3) . . ? C10 C11 C6 119.5(3) . . ? N1 C5 C4 110.9(3) . . ? N1 C5 C6 120.1(2) . . ? C4 C5 C6 128.9(2) . . ? C9 C10 C11 118.9(3) . . ? C5 N1 N2 104.7(2) . . ? C3 C4 C5 105.0(2) . . ? C3 N2 N1 112.1(2) . . ? N2 C3 C4 107.3(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N8 1.05(3) 1.81(3) 2.847(4) 171(3) 1_545 _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.248 _refine_diff_density_min -0.359 _refine_diff_density_rms 0.079 #=END data_3pypzpolymorphII _database_code_depnum_ccdc_archive 'CCDC 264757' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '3pypz polymorph II' _chemical_melting_point ? _chemical_formula_moiety 'C8 H7 N3' _chemical_formula_sum 'C8 H7 N3' _chemical_formula_weight 145.17 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' 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 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 15.009(2) _cell_length_b 5.8998(9) _cell_length_c 16.526(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.308(3) _cell_angle_gamma 90.00 _cell_volume 1463.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2333 _cell_measurement_theta_min 7.253 _cell_measurement_theta_max 50.549 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.085 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.9668 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16023 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.0848 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.53 _reflns_number_total 3347 _reflns_number_gt 1775 _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^)+(0.0529P)^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 3347 _refine_ls_number_parameters 207 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1200 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _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 N1 N 0.70900(11) 0.0176(3) 0.61580(10) 0.0330(4) Uani 1 1 d . . . N2 N 0.77591(12) 0.1527(3) 0.64295(10) 0.0345(4) Uani 1 1 d . . . H2 H 0.8361(16) 0.120(4) 0.6335(14) 0.063(8) Uiso 1 1 d . . . C3 C 0.74673(15) 0.3311(4) 0.68506(13) 0.0402(6) Uani 1 1 d . . . H3 H 0.7824 0.4466 0.7094 0.048 Uiso 1 1 calc R . . C4 C 0.65613(14) 0.3154(3) 0.68640(13) 0.0374(5) Uani 1 1 d . . . H4 H 0.6159 0.4160 0.7117 0.045 Uiso 1 1 calc R . . C5 C 0.63521(13) 0.1184(3) 0.64237(11) 0.0296(5) Uani 1 1 d . . . C6 C 0.54674(13) 0.0231(3) 0.62193(11) 0.0274(5) Uani 1 1 d . . . C7 C 0.47029(13) 0.1484(3) 0.63554(11) 0.0313(5) Uani 1 1 d . . . H7 H 0.4768 0.2899 0.6625 0.038 Uiso 1 1 calc R . . N8 N 0.38792(11) 0.0829(3) 0.61316(10) 0.0341(4) Uani 1 1 d . . . C9 C 0.37952(14) -0.1178(3) 0.57603(12) 0.0338(5) Uani 1 1 d . . . H9 H 0.3219 -0.1656 0.5583 0.041 Uiso 1 1 calc R . . C10 C 0.45148(13) -0.2586(3) 0.56241(12) 0.0324(5) Uani 1 1 d . . . H10 H 0.4428 -0.4025 0.5377 0.039 Uiso 1 1 calc R . . C11 C 0.53580(14) -0.1875(3) 0.58513(11) 0.0310(5) Uani 1 1 d . . . H11 H 0.5860 -0.2813 0.5758 0.037 Uiso 1 1 calc R . . N101 N 0.21391(11) 0.5544(3) 0.63935(10) 0.0334(4) Uani 1 1 d . . . N102 N 0.24300(12) 0.3902(3) 0.58955(11) 0.0371(5) Uani 1 1 d . . . H102 H 0.2930(15) 0.284(4) 0.6044(12) 0.054(7) Uiso 1 1 d . . . C103 C 0.19592(15) 0.3819(4) 0.51898(14) 0.0421(6) Uani 1 1 d . . . H103 H 0.2054 0.2810 0.4752 0.051 Uiso 1 1 calc R . . C104 C 0.13230(14) 0.5462(3) 0.52258(13) 0.0379(5) Uani 1 1 d . . . H104 H 0.0883 0.5827 0.4824 0.045 Uiso 1 1 calc R . . C105 C 0.14563(12) 0.6504(3) 0.59864(12) 0.0284(5) Uani 1 1 d . . . C106 C 0.09823(12) 0.8427(3) 0.63315(11) 0.0264(5) Uani 1 1 d . . . C107 C 0.01212(13) 0.8973(3) 0.60716(12) 0.0320(5) Uani 1 1 d . . . H107 H -0.0156 0.8030 0.5674 0.038 Uiso 1 1 calc R . . N108 N -0.03432(11) 1.0747(3) 0.63461(10) 0.0355(4) Uani 1 1 d . . . C109 C 0.00636(14) 1.2073(4) 0.68986(12) 0.0372(5) Uani 1 1 d . . . H109 H -0.0246 1.3364 0.7089 0.045 Uiso 1 1 calc R . . C110 C 0.09104(14) 1.1656(4) 0.72043(12) 0.0356(5) Uani 1 1 d . . . H110 H 0.1170 1.2624 0.7604 0.043 Uiso 1 1 calc R . . C111 C 0.13744(14) 0.9820(3) 0.69229(12) 0.0330(5) Uani 1 1 d . . . H111 H 0.1957 0.9501 0.7129 0.040 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 N1 0.0287(10) 0.0371(10) 0.0331(10) -0.0034(8) -0.0031(8) 0.0053(8) N2 0.0272(10) 0.0396(11) 0.0364(11) -0.0041(9) -0.0026(8) 0.0033(9) C3 0.0402(14) 0.0371(12) 0.0429(14) -0.0083(11) -0.0046(11) 0.0020(10) C4 0.0356(13) 0.0365(12) 0.0401(13) -0.0099(10) -0.0011(10) 0.0091(10) C5 0.0318(12) 0.0325(11) 0.0244(11) 0.0013(9) -0.0001(9) 0.0070(9) C6 0.0294(11) 0.0291(11) 0.0236(10) 0.0046(9) 0.0011(9) 0.0060(9) C7 0.0328(12) 0.0326(11) 0.0285(11) 0.0036(9) 0.0007(9) 0.0057(9) N8 0.0298(10) 0.0386(10) 0.0340(10) 0.0050(8) 0.0019(8) 0.0054(8) C9 0.0316(12) 0.0385(12) 0.0313(12) 0.0085(10) 0.0005(9) 0.0010(10) C10 0.0352(12) 0.0315(11) 0.0305(11) 0.0037(9) -0.0011(9) -0.0005(10) C11 0.0346(12) 0.0313(11) 0.0272(11) 0.0024(9) 0.0013(9) 0.0075(10) N101 0.0247(9) 0.0335(10) 0.0418(11) 0.0035(8) -0.0015(8) 0.0018(8) N102 0.0274(10) 0.0331(10) 0.0507(12) 0.0050(9) 0.0026(9) 0.0066(8) C103 0.0400(14) 0.0426(13) 0.0440(14) -0.0058(11) 0.0029(11) 0.0053(11) C104 0.0370(13) 0.0414(13) 0.0351(12) -0.0052(10) -0.0036(10) 0.0086(10) C105 0.0220(10) 0.0297(11) 0.0335(11) 0.0015(9) -0.0004(9) -0.0015(9) C106 0.0250(11) 0.0273(10) 0.0268(11) 0.0028(8) 0.0006(9) -0.0018(8) C107 0.0318(12) 0.0320(11) 0.0319(11) -0.0060(9) -0.0031(9) 0.0012(9) N108 0.0314(10) 0.0356(10) 0.0393(11) -0.0061(8) -0.0008(8) 0.0053(8) C109 0.0419(13) 0.0349(12) 0.0351(12) -0.0053(10) 0.0084(10) 0.0010(10) C110 0.0375(13) 0.0421(13) 0.0273(11) -0.0066(10) 0.0030(10) -0.0093(10) C111 0.0298(12) 0.0412(12) 0.0280(11) 0.0008(10) -0.0028(9) -0.0057(10) _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 N1 C5 1.340(2) . ? N1 N2 1.351(2) . ? N2 C3 1.341(3) . ? N2 H2 0.94(2) . ? C3 C4 1.364(3) . ? C3 H3 0.9500 . ? C4 C5 1.403(3) . ? C4 H4 0.9500 . ? C5 C6 1.474(3) . ? C6 C7 1.388(3) . ? C6 C11 1.391(3) . ? C7 N8 1.339(2) . ? C7 H7 0.9500 . ? N8 C9 1.338(2) . ? C9 C10 1.385(3) . ? C9 H9 0.9500 . ? C10 C11 1.377(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? N101 C105 1.339(2) . ? N101 N102 1.350(2) . ? N102 C103 1.351(3) . ? N102 H102 1.00(2) . ? C103 C104 1.363(3) . ? C103 H103 0.9500 . ? C104 C105 1.409(3) . ? C104 H104 0.9500 . ? C105 C106 1.462(3) . ? C106 C107 1.390(3) . ? C106 C111 1.397(3) . ? C107 N108 1.342(2) . ? C107 H107 0.9500 . ? N108 C109 1.339(3) . ? C109 C110 1.379(3) . ? C109 H109 0.9500 . ? C110 C111 1.374(3) . ? C110 H110 0.9500 . ? C111 H111 0.9500 . ? 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 N1 N2 104.08(16) . . ? C3 N2 N1 112.73(18) . . ? C3 N2 H2 125.0(14) . . ? N1 N2 H2 122.3(14) . . ? N2 C3 C4 107.01(19) . . ? N2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C3 C4 C5 105.04(19) . . ? C3 C4 H4 127.5 . . ? C5 C4 H4 127.5 . . ? N1 C5 C4 111.14(18) . . ? N1 C5 C6 120.17(17) . . ? C4 C5 C6 128.66(18) . . ? C7 C6 C11 117.19(18) . . ? C7 C6 C5 120.21(18) . . ? C11 C6 C5 122.52(18) . . ? N8 C7 C6 124.26(19) . . ? N8 C7 H7 117.9 . . ? C6 C7 H7 117.9 . . ? C9 N8 C7 117.29(18) . . ? N8 C9 C10 122.7(2) . . ? N8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C11 C10 C9 119.2(2) . . ? C11 C10 H10 120.4 . . ? C9 C10 H10 120.4 . . ? C10 C11 C6 119.32(19) . . ? C10 C11 H11 120.3 . . ? C6 C11 H11 120.3 . . ? C105 N101 N102 104.57(16) . . ? N101 N102 C103 112.46(18) . . ? N101 N102 H102 123.3(12) . . ? C103 N102 H102 124.2(12) . . ? N102 C103 C104 106.9(2) . . ? N102 C103 H103 126.6 . . ? C104 C103 H103 126.6 . . ? C103 C104 C105 105.29(19) . . ? C103 C104 H104 127.4 . . ? C105 C104 H104 127.4 . . ? N101 C105 C104 110.82(17) . . ? N101 C105 C106 120.39(17) . . ? C104 C105 C106 128.74(18) . . ? C107 C106 C111 116.97(18) . . ? C107 C106 C105 121.11(17) . . ? C111 C106 C105 121.91(17) . . ? N108 C107 C106 124.23(18) . . ? N108 C107 H107 117.9 . . ? C106 C107 H107 117.9 . . ? C109 N108 C107 116.99(17) . . ? N108 C109 C110 123.21(19) . . ? N108 C109 H109 118.4 . . ? C110 C109 H109 118.4 . . ? C111 C110 C109 119.11(19) . . ? C111 C110 H110 120.4 . . ? C109 C110 H110 120.4 . . ? C110 C111 C106 119.45(19) . . ? C110 C111 H111 120.3 . . ? C106 C111 H111 120.3 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.161 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.049 #=END data_TlBp3py _database_code_depnum_ccdc_archive 'CCDC 264758' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H30 B2 Cl2 N12 Tl2' _chemical_formula_sum 'C33 H30 B2 Cl2 N12 Tl2' _chemical_formula_weight 1095.95 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' Tl Tl -2.8358 9.6688 '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)/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 8.1673(13) _cell_length_b 16.983(3) _cell_length_c 27.131(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.016(3) _cell_angle_gamma 90.00 _cell_volume 3760.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5556 _cell_measurement_theta_min 4.797 _cell_measurement_theta_max 45.673 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 8.743 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.1076 _exptl_absorpt_correction_T_max 0.5414 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41391 _diffrn_reflns_av_R_equivalents 0.1369 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.54 _reflns_number_total 8548 _reflns_number_gt 4928 _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^)+(0.0527P)^2^+7.8946P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8548 _refine_ls_number_parameters 426 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1205 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.021 _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 C133 C -0.1042(14) 0.8161(6) 0.3177(4) 0.038(3) Uani 1 1 d . . . C132 C -0.0318(15) 0.7748(6) 0.3562(4) 0.044(3) Uani 1 1 d . . . C134 C -0.1648(18) 0.8903(8) 0.3281(6) 0.063(4) Uani 1 1 d . . . C135 C -0.1562(18) 0.9178(8) 0.3754(6) 0.065(4) Uani 1 1 d . . . C136 C -0.0776(18) 0.8720(8) 0.4117(5) 0.061(4) Uani 1 1 d . . . N131 N -0.0156(12) 0.8009(5) 0.4020(3) 0.046(2) Uani 1 1 d . . . Tl1 Tl 0.71414(5) 0.61443(3) 0.334430(15) 0.03906(14) Uani 1 1 d . . . Tl2 Tl 0.20348(5) 0.70692(3) 0.450735(16) 0.03891(14) Uani 1 1 d . . . B1 B 0.7925(19) 0.5985(9) 0.1988(6) 0.055(4) Uani 1 1 d . . . H1B H 0.8593 0.5591 0.2175 0.066 Uiso 1 1 calc R . . H1A H 0.8139 0.5923 0.1633 0.066 Uiso 1 1 calc R . . N101 N 0.6072(12) 0.5845(5) 0.2077(3) 0.042(2) Uani 1 1 d . . . N102 N 0.5577(11) 0.5621(5) 0.2538(3) 0.036(2) Uani 1 1 d . . . C103 C 0.3947(14) 0.5640(6) 0.2516(4) 0.039(3) Uani 1 1 d . . . C104 C 0.3348(14) 0.5873(6) 0.2045(4) 0.041(3) Uani 1 1 d . . . H104 H 0.2237 0.5935 0.1936 0.049 Uiso 1 1 calc R . . C105 C 0.4744(15) 0.5993(6) 0.1773(4) 0.043(3) Uani 1 1 d . . . H105 H 0.4765 0.6150 0.1437 0.052 Uiso 1 1 calc R . . N111 N 0.2779(14) 0.4812(7) 0.3749(5) 0.071(3) Uani 1 1 d . . . C112 C 0.3632(14) 0.4944(7) 0.3323(4) 0.043(3) Uani 1 1 d . . . H112 H 0.4646 0.4682 0.3282 0.051 Uiso 1 1 calc R . . C113 C 0.3036(13) 0.5450(6) 0.2955(4) 0.039(3) Uani 1 1 d . . . C114 C 0.1552(16) 0.5802(7) 0.3044(5) 0.054(3) Uani 1 1 d . . . H114 H 0.1119 0.6158 0.2802 0.065 Uiso 1 1 calc R . . C115 C 0.0684(12) 0.5679(6) 0.3443(4) 0.037(3) Uani 1 1 d . . . H115 H -0.0336 0.5935 0.3483 0.044 Uiso 1 1 calc R . . C116 C 0.1274(15) 0.5201(7) 0.3770(4) 0.047(3) Uani 1 1 d . . . H116 H 0.0635 0.5105 0.4050 0.057 Uiso 1 1 calc R . . N121 N 0.8400(12) 0.6825(5) 0.2160(3) 0.043(2) Uani 1 1 d . . . N122 N 0.8485(10) 0.7009(5) 0.2652(3) 0.032(2) Uani 1 1 d . . . C123 C 0.8801(14) 0.7774(7) 0.2681(4) 0.042(3) Uani 1 1 d . . . C124 C 0.8902(14) 0.8104(7) 0.2210(5) 0.051(3) Uani 1 1 d . . . H124 H 0.9093 0.8639 0.2128 0.061 Uiso 1 1 calc R . . C125 C 0.8657(15) 0.7470(8) 0.1889(5) 0.057(3) Uani 1 1 d . . . H125 H 0.8670 0.7492 0.1539 0.068 Uiso 1 1 calc R . . H132 H 0.0100 0.7240 0.3494 0.068 Uiso 1 1 d R . . H134 H -0.2128 0.9217 0.3025 0.068 Uiso 1 1 d R . . H135 H -0.2020 0.9673 0.3834 0.068 Uiso 1 1 d R . . H136 H -0.0676 0.8919 0.4444 0.068 Uiso 1 1 d R . . B2 B 0.2808(17) 0.8680(8) 0.5452(5) 0.041(3) Uani 1 1 d . . . H2A H 0.2939 0.9124 0.5687 0.049 Uiso 1 1 calc R . . H2B H 0.3590 0.8261 0.5554 0.049 Uiso 1 1 calc R . . N1 N 0.3170(11) 0.8966(5) 0.4919(3) 0.038(2) Uani 1 1 d . . . N2 N 0.3445(10) 0.8441(5) 0.4542(3) 0.0297(19) Uani 1 1 d . . . C3 C 0.3629(13) 0.8874(6) 0.4137(4) 0.037(3) Uani 1 1 d . . . C4 C 0.3452(14) 0.9672(6) 0.4248(4) 0.042(3) Uani 1 1 d . . . H4 H 0.3507 1.0106 0.4028 0.051 Uiso 1 1 calc R . . C5 C 0.3176(14) 0.9693(7) 0.4750(4) 0.042(3) Uani 1 1 d . . . H5 H 0.3017 1.0155 0.4940 0.050 Uiso 1 1 calc R . . N11 N 0.5041(11) 0.7407(6) 0.3226(3) 0.043(2) Uani 1 1 d . . . C12 C 0.4749(13) 0.7795(6) 0.3637(4) 0.038(3) Uani 1 1 d . . . H12 H 0.5121 0.7561 0.3939 0.045 Uiso 1 1 calc R . . C13 C 0.3945(12) 0.8514(6) 0.3666(4) 0.034(2) Uani 1 1 d . . . C14 C 0.3434(15) 0.8851(7) 0.3223(4) 0.046(3) Uani 1 1 d . . . H14 H 0.2872 0.9341 0.3220 0.056 Uiso 1 1 calc R . . C15 C 0.3745(16) 0.8473(8) 0.2789(5) 0.057(3) Uani 1 1 d . . . H15 H 0.3411 0.8702 0.2482 0.069 Uiso 1 1 calc R . . C16 C 0.4546(17) 0.7758(8) 0.2802(5) 0.058(4) Uani 1 1 d . . . H16 H 0.4757 0.7503 0.2500 0.069 Uiso 1 1 calc R . . N21 N 0.1006(11) 0.8356(5) 0.5459(3) 0.035(2) Uani 1 1 d . A . N22 N 0.0554(11) 0.7646(5) 0.5271(3) 0.038(2) Uani 1 1 d . A . C23 C -0.1030(13) 0.7582(5) 0.5308(4) 0.045(3) Uiso 1 1 d D . . C24 C -0.1659(16) 0.8260(9) 0.5515(5) 0.060(4) Uani 1 1 d . A . H24 H -0.2775 0.8371 0.5574 0.072 Uiso 1 1 calc R . . C25 C -0.0311(16) 0.8744(8) 0.5618(4) 0.054(4) Uani 1 1 d . . . H25 H -0.0321 0.9248 0.5771 0.065 Uiso 1 1 calc R A . C1S C 0.2717(17) 0.7996(8) 0.1333(7) 0.082(5) Uani 1 1 d . . . H2S H 0.2400 0.7717 0.1024 0.099 Uiso 1 1 calc R . . H1S H 0.2240 0.7705 0.1610 0.099 Uiso 1 1 calc R . . C36A C -0.4045(15) 0.5759(7) 0.4718(5) 0.027(5) Uiso 0.51(2) 1 d PG A 1 H36A H -0.4703 0.5347 0.4581 0.033 Uiso 0.51(2) 1 calc PR A 1 N31A N -0.4687(12) 0.6513(8) 0.4759(5) 0.054(6) Uiso 0.51(2) 1 d PG A 1 C32A C -0.3724(17) 0.7116(6) 0.4960(6) 0.051(7) Uiso 0.51(2) 1 d PG A 1 H32A H -0.4163 0.7632 0.4988 0.061 Uiso 0.51(2) 1 calc PR A 1 C33A C -0.2120(16) 0.6965(7) 0.5119(6) 0.033(6) Uiso 0.51(2) 1 d PGD A 1 C34A C -0.1477(12) 0.6210(8) 0.5079(5) 0.029(5) Uiso 0.51(2) 1 d PG A 1 H34A H -0.0381 0.6107 0.5188 0.035 Uiso 0.51(2) 1 calc PR A 1 C35A C -0.2440(15) 0.5608(6) 0.4878(6) 0.050(7) Uiso 0.51(2) 1 d PG A 1 H35A H -0.2001 0.5092 0.4850 0.060 Uiso 0.51(2) 1 calc PR A 1 C35B C -0.130(2) 0.5435(7) 0.4945(7) 0.048(7) Uiso 0.49(2) 1 d PG A 2 H35B H -0.0616 0.4982 0.4949 0.058 Uiso 0.49(2) 1 calc PR A 2 C36B C -0.290(2) 0.5387(7) 0.4754(8) 0.089(11) Uiso 0.49(2) 1 d PG A 2 H36B H -0.3307 0.4901 0.4628 0.107 Uiso 0.49(2) 1 calc PR A 2 N31B N -0.3895(18) 0.6050(10) 0.4748(7) 0.075(9) Uiso 0.49(2) 1 d PG A 2 C32B C -0.329(2) 0.6761(8) 0.4933(7) 0.059(8) Uiso 0.49(2) 1 d PG A 2 H32B H -0.3976 0.7215 0.4929 0.071 Uiso 0.49(2) 1 calc PR A 2 C33B C -0.169(2) 0.6809(7) 0.5124(7) 0.043(7) Uiso 0.49(2) 1 d PGD A 2 C34B C -0.0697(18) 0.6146(10) 0.5130(7) 0.067(9) Uiso 0.49(2) 1 d PG A 2 H34B H 0.0396 0.6179 0.5260 0.081 Uiso 0.49(2) 1 calc PR A 2 Cl1S Cl 0.4881(5) 0.7993(2) 0.14095(16) 0.0764(11) Uani 1 1 d . . . Cl2S Cl 0.1917(6) 0.8943(3) 0.13127(19) 0.0973(15) 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 C133 0.052(7) 0.020(5) 0.042(7) -0.008(5) -0.002(6) -0.001(5) C132 0.057(8) 0.033(7) 0.040(7) -0.002(5) -0.005(6) 0.001(5) C134 0.072(10) 0.044(8) 0.072(10) -0.002(7) -0.010(8) 0.014(7) C135 0.086(11) 0.043(8) 0.065(10) -0.026(7) -0.017(8) 0.014(7) C136 0.076(10) 0.062(9) 0.045(8) -0.023(7) 0.000(7) -0.007(7) N131 0.070(7) 0.036(6) 0.031(5) -0.009(4) -0.006(5) 0.001(5) Tl1 0.0487(3) 0.0405(3) 0.0281(2) 0.00005(19) 0.00349(19) 0.0022(2) Tl2 0.0412(3) 0.0331(2) 0.0423(3) -0.0022(2) -0.00084(19) 0.00397(19) B1 0.063(10) 0.054(10) 0.049(9) -0.016(7) 0.025(8) -0.012(7) N101 0.054(6) 0.042(6) 0.029(5) -0.017(4) 0.006(5) -0.011(5) N102 0.054(6) 0.029(5) 0.026(5) -0.003(4) 0.007(4) -0.005(4) C103 0.045(7) 0.032(6) 0.039(7) -0.010(5) 0.003(5) 0.004(5) C104 0.046(7) 0.036(7) 0.041(7) -0.010(5) -0.003(6) 0.002(5) C105 0.061(8) 0.037(7) 0.032(6) -0.015(5) -0.006(6) -0.007(6) N111 0.061(7) 0.064(8) 0.089(9) -0.017(7) 0.017(7) 0.009(6) C112 0.045(7) 0.042(7) 0.042(7) 0.000(6) 0.006(6) 0.007(5) C113 0.032(6) 0.035(7) 0.050(7) -0.010(5) 0.004(5) -0.003(5) C114 0.067(9) 0.043(8) 0.052(8) -0.005(6) -0.010(7) 0.005(7) C115 0.027(6) 0.034(6) 0.050(7) 0.012(6) 0.016(5) 0.012(5) C116 0.059(8) 0.037(7) 0.048(8) -0.008(6) 0.034(6) -0.009(6) N121 0.061(6) 0.041(6) 0.028(5) -0.005(4) 0.002(5) -0.003(5) N122 0.042(5) 0.033(5) 0.022(5) -0.001(4) -0.001(4) 0.001(4) C123 0.049(7) 0.039(7) 0.037(7) 0.002(5) -0.003(5) 0.001(5) C124 0.049(7) 0.050(8) 0.054(8) 0.020(6) -0.004(6) -0.014(6) C125 0.060(8) 0.056(9) 0.054(8) 0.009(7) -0.015(7) -0.018(7) B2 0.058(9) 0.031(7) 0.035(8) -0.002(6) 0.009(6) 0.004(6) N1 0.042(5) 0.034(5) 0.040(6) -0.009(4) 0.005(4) 0.001(4) N2 0.038(5) 0.024(4) 0.027(5) -0.003(4) -0.002(4) 0.006(4) C3 0.032(6) 0.037(6) 0.041(7) 0.005(5) -0.004(5) 0.001(5) C4 0.057(7) 0.025(6) 0.046(7) 0.004(5) 0.011(6) -0.006(5) C5 0.058(7) 0.030(6) 0.038(7) 0.001(5) 0.001(6) -0.005(5) N11 0.042(6) 0.053(6) 0.035(6) -0.005(5) 0.003(4) 0.007(5) C12 0.036(6) 0.049(7) 0.029(6) -0.001(5) 0.009(5) 0.013(5) C13 0.033(6) 0.034(6) 0.036(6) 0.005(5) 0.006(5) 0.004(5) C14 0.058(8) 0.046(7) 0.036(7) 0.011(6) -0.004(6) 0.005(6) C15 0.077(9) 0.051(8) 0.044(8) 0.018(7) 0.004(7) 0.005(7) C16 0.090(10) 0.056(9) 0.028(7) -0.003(6) 0.003(7) 0.004(7) N21 0.053(6) 0.034(5) 0.020(5) 0.004(4) 0.008(4) 0.012(4) N22 0.048(6) 0.032(5) 0.034(5) -0.007(4) 0.001(4) 0.005(4) C24 0.044(8) 0.077(10) 0.059(9) 0.014(7) 0.023(7) 0.018(7) C25 0.058(8) 0.065(9) 0.041(8) 0.008(6) 0.022(6) 0.010(7) C1S 0.056(9) 0.063(10) 0.126(15) -0.036(10) -0.006(9) -0.006(8) Cl1S 0.072(2) 0.059(2) 0.098(3) -0.016(2) -0.005(2) -0.0058(19) Cl2S 0.100(3) 0.078(3) 0.113(4) 0.004(3) -0.004(3) 0.031(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 C133 C132 1.373(15) . ? C133 C134 1.387(16) . ? C133 C123 1.501(15) 1_455 ? C132 N131 1.324(14) . ? C132 H132 0.9482 . ? C134 C135 1.364(19) . ? C134 H134 0.9507 . ? C135 C136 1.394(19) . ? C135 H135 0.9487 . ? C136 N131 1.338(16) . ? C136 H136 0.9508 . ? N131 Tl2 2.708(10) . ? Tl1 N102 2.648(9) . ? Tl1 N122 2.653(8) . ? Tl1 N11 2.758(9) . ? Tl2 N2 2.599(8) . ? Tl2 N22 2.624(8) . ? B1 N121 1.546(16) . ? B1 N101 1.559(16) . ? B1 H1B 0.9900 . ? B1 H1A 0.9900 . ? N101 C105 1.363(14) . ? N101 N102 1.382(11) . ? N102 C103 1.331(13) . ? C103 C104 1.410(15) . ? C103 C113 1.462(15) . ? C104 C105 1.395(15) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? N111 C112 1.389(15) . ? N111 C116 1.399(15) . ? C112 C113 1.393(15) . ? C112 H112 0.9500 . ? C113 C114 1.380(16) . ? C114 C115 1.331(16) . ? C114 H114 0.9500 . ? C115 C116 1.285(15) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.342(15) . ? N121 N122 1.369(11) . ? N122 C123 1.325(13) . ? C123 C124 1.400(16) . ? C123 C133 1.501(15) 1_655 ? C124 C125 1.395(17) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? B2 N1 1.564(15) . ? B2 N21 1.571(16) . ? B2 H2A 0.9900 . ? B2 H2B 0.9900 . ? N1 C5 1.317(13) . ? N1 N2 1.381(11) . ? N2 C3 1.334(13) . ? C3 C4 1.398(14) . ? C3 C13 1.448(15) . ? C4 C5 1.389(15) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? N11 C12 1.322(13) . ? N11 C16 1.345(15) . ? C12 C13 1.391(14) . ? C12 H12 0.9500 . ? C13 C14 1.381(15) . ? C14 C15 1.375(17) . ? C14 H14 0.9500 . ? C15 C16 1.378(17) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? N21 C25 1.346(14) . ? N21 N22 1.356(12) . ? N22 C23 1.306(13) . ? C23 C24 1.388(16) . ? C23 C33A 1.456(5) . ? C23 C33B 1.500(5) . ? C24 C25 1.395(18) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C1S Cl2S 1.736(14) . ? C1S Cl1S 1.772(14) . ? C1S H2S 0.9900 . ? C1S H1S 0.9900 . ? C36A N31A 1.3900 . ? C36A C35A 1.3900 . ? C36A H36A 0.9500 . ? N31A C32A 1.3900 . ? C32A C33A 1.3900 . ? C32A H32A 0.9500 . ? C33A C34A 1.3900 . ? C34A C35A 1.3900 . ? C34A H34A 0.9500 . ? C35A H35A 0.9500 . ? C35B C36B 1.3900 . ? C35B C34B 1.3900 . ? C35B H35B 0.9500 . ? C36B N31B 1.3900 . ? C36B H36B 0.9500 . ? N31B C32B 1.3900 . ? C32B C33B 1.3900 . ? C32B H32B 0.9500 . ? C33B C34B 1.3900 . ? C34B H34B 0.9500 . ? 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 C132 C133 C134 117.3(11) . . ? C132 C133 C123 118.5(9) . 1_455 ? C134 C133 C123 124.2(11) . 1_455 ? N131 C132 C133 124.6(10) . . ? N131 C132 H132 117.6 . . ? C133 C132 H132 117.8 . . ? C135 C134 C133 119.7(13) . . ? C135 C134 H134 120.2 . . ? C133 C134 H134 120.1 . . ? C134 C135 C136 118.7(12) . . ? C134 C135 H135 120.7 . . ? C136 C135 H135 120.6 . . ? N131 C136 C135 122.2(12) . . ? N131 C136 H136 118.9 . . ? C135 C136 H136 118.9 . . ? C132 N131 C136 117.5(11) . . ? C132 N131 Tl2 107.6(7) . . ? C136 N131 Tl2 133.1(8) . . ? N102 Tl1 N122 78.5(3) . . ? N102 Tl1 N11 83.4(3) . . ? N122 Tl1 N11 76.0(3) . . ? N2 Tl2 N22 81.5(3) . . ? N2 Tl2 N131 76.9(3) . . ? N22 Tl2 N131 81.4(3) . . ? N121 B1 N101 109.1(10) . . ? N121 B1 H1B 109.9 . . ? N101 B1 H1B 109.9 . . ? N121 B1 H1A 109.9 . . ? N101 B1 H1A 109.9 . . ? H1B B1 H1A 108.3 . . ? C105 N101 N102 110.3(9) . . ? C105 N101 B1 129.5(11) . . ? N102 N101 B1 119.9(10) . . ? C103 N102 N101 106.1(9) . . ? C103 N102 Tl1 118.7(7) . . ? N101 N102 Tl1 120.5(6) . . ? N102 C103 C104 111.2(10) . . ? N102 C103 C113 119.7(10) . . ? C104 C103 C113 129.1(11) . . ? C105 C104 C103 104.9(10) . . ? C105 C104 H104 127.6 . . ? C103 C104 H104 127.6 . . ? N101 C105 C104 107.5(10) . . ? N101 C105 H105 126.2 . . ? C104 C105 H105 126.2 . . ? C112 N111 C116 115.2(11) . . ? N111 C112 C113 121.5(11) . . ? N111 C112 H112 119.2 . . ? C113 C112 H112 119.2 . . ? C114 C113 C112 115.4(11) . . ? C114 C113 C103 121.4(11) . . ? C112 C113 C103 123.0(10) . . ? C115 C114 C113 124.7(12) . . ? C115 C114 H114 117.6 . . ? C113 C114 H114 117.6 . . ? C116 C115 C114 117.7(10) . . ? C116 C115 H115 121.2 . . ? C114 C115 H115 121.2 . . ? C115 C116 N111 125.3(11) . . ? C115 C116 H116 117.3 . . ? N111 C116 H116 117.3 . . ? C125 N121 N122 110.1(9) . . ? C125 N121 B1 129.1(11) . . ? N122 N121 B1 120.6(9) . . ? C123 N122 N121 106.6(9) . . ? C123 N122 Tl1 125.8(7) . . ? N121 N122 Tl1 123.7(6) . . ? N122 C123 C124 110.8(11) . . ? N122 C123 C133 119.6(10) . 1_655 ? C124 C123 C133 129.6(11) . 1_655 ? C125 C124 C123 104.4(11) . . ? C125 C124 H124 127.8 . . ? C123 C124 H124 127.8 . . ? N121 C125 C124 108.0(11) . . ? N121 C125 H125 126.0 . . ? C124 C125 H125 126.0 . . ? N1 B2 N21 109.1(10) . . ? N1 B2 H2A 109.9 . . ? N21 B2 H2A 109.9 . . ? N1 B2 H2B 109.9 . . ? N21 B2 H2B 109.9 . . ? H2A B2 H2B 108.3 . . ? C5 N1 N2 110.2(9) . . ? C5 N1 B2 128.0(9) . . ? N2 N1 B2 121.7(9) . . ? C3 N2 N1 106.3(8) . . ? C3 N2 Tl2 121.7(7) . . ? N1 N2 Tl2 121.5(6) . . ? N2 C3 C4 110.0(10) . . ? N2 C3 C13 121.6(10) . . ? C4 C3 C13 128.4(10) . . ? C5 C4 C3 104.9(10) . . ? C5 C4 H4 127.6 . . ? C3 C4 H4 127.6 . . ? N1 C5 C4 108.7(10) . . ? N1 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? C12 N11 C16 116.2(10) . . ? C12 N11 Tl1 114.8(7) . . ? C16 N11 Tl1 127.7(8) . . ? N11 C12 C13 125.8(11) . . ? N11 C12 H12 117.1 . . ? C13 C12 H12 117.1 . . ? C14 C13 C12 116.3(10) . . ? C14 C13 C3 122.4(10) . . ? C12 C13 C3 121.3(10) . . ? C15 C14 C13 119.6(11) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C16 119.3(12) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? N11 C16 C15 122.8(12) . . ? N11 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? C25 N21 N22 110.3(10) . . ? C25 N21 B2 126.2(10) . . ? N22 N21 B2 123.4(8) . . ? C23 N22 N21 107.6(8) . . ? C23 N22 Tl2 121.1(7) . . ? N21 N22 Tl2 120.2(6) . . ? N22 C23 C24 110.1(9) . . ? N22 C23 C33A 128.8(11) . . ? C24 C23 C33A 120.6(12) . . ? N22 C23 C33B 113.3(12) . . ? C24 C23 C33B 136.6(13) . . ? C33A C23 C33B 16.9(9) . . ? C23 C24 C25 105.7(10) . . ? C23 C24 H24 127.2 . . ? C25 C24 H24 127.2 . . ? N21 C25 C24 106.3(12) . . ? N21 C25 H25 126.8 . . ? C24 C25 H25 126.8 . . ? Cl2S C1S Cl1S 112.3(8) . . ? Cl2S C1S H2S 109.1 . . ? Cl1S C1S H2S 109.1 . . ? Cl2S C1S H1S 109.1 . . ? Cl1S C1S H1S 109.1 . . ? H2S C1S H1S 107.9 . . ? N31A C36A C35A 120.0 . . ? N31A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C36A N31A C32A 120.0 . . ? C33A C32A N31A 120.0 . . ? C33A C32A H32A 120.0 . . ? N31A C32A H32A 120.0 . . ? C34A C33A C32A 120.0 . . ? C34A C33A C23 117.6(11) . . ? C32A C33A C23 122.3(11) . . ? C33A C34A C35A 120.0 . . ? C33A C34A H34A 120.0 . . ? C35A C34A H34A 120.0 . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C36B C35B C34B 120.0 . . ? C36B C35B H35B 120.0 . . ? C34B C35B H35B 120.0 . . ? N31B C36B C35B 120.0 . . ? N31B C36B H36B 120.0 . . ? C35B C36B H36B 120.0 . . ? C36B N31B C32B 120.0 . . ? C33B C32B N31B 120.0 . . ? C33B C32B H32B 120.0 . . ? N31B C32B H32B 120.0 . . ? C32B C33B C34B 120.0 . . ? C32B C33B C23 120.0(13) . . ? C34B C33B C23 120.0(13) . . ? C33B C34B C35B 120.0 . . ? C33B C34B H34B 120.0 . . ? C35B C34B H34B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 2.839 _refine_diff_density_min -1.575 _refine_diff_density_rms 0.212 #=END data_TlTp3py _database_code_depnum_ccdc_archive 'CCDC 264759' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H19 B N9 Tl' _chemical_formula_sum 'C24 H19 B N9 Tl' _chemical_formula_weight 648.66 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' Tl Tl -2.8358 9.6688 '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 9.2506(13) _cell_length_b 12.3819(17) _cell_length_c 19.887(3) _cell_angle_alpha 90.00 _cell_angle_beta 94.968(2) _cell_angle_gamma 90.00 _cell_volume 2269.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6652 _cell_measurement_theta_min 5.034 _cell_measurement_theta_max 55.041 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1248 _exptl_absorpt_coefficient_mu 7.151 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.1306 _exptl_absorpt_correction_T_max 0.4566 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23976 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 27.55 _reflns_number_total 5118 _reflns_number_gt 4484 _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^)+(0.0367P)^2^+0.5710P] 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 5118 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0631 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _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 Tl1 Tl 0.892350(13) 0.814886(10) 0.054150(6) 0.02402(6) Uani 1 1 d . . . B1 B 0.7795(4) 0.7191(3) 0.22085(19) 0.0231(7) Uani 1 1 d . . . H1 H 0.732(4) 0.687(3) 0.2666(19) 0.025(10) Uiso 1 1 d . . . N101 N 0.8768(3) 0.8162(2) 0.24124(14) 0.0203(6) Uani 1 1 d . . . N102 N 0.9393(3) 0.8818(2) 0.19631(13) 0.0228(6) Uani 1 1 d . . . C103 C 1.0201(3) 0.9518(3) 0.23442(16) 0.0223(6) Uani 1 1 d . . . C104 C 1.0105(4) 0.9327(3) 0.30341(16) 0.0257(7) Uani 1 1 d . . . H104 H 1.0577 0.9709 0.3405 0.031 Uiso 1 1 calc R . . C105 C 0.9179(4) 0.8469(3) 0.30535(16) 0.0245(7) Uani 1 1 d . . . H105 H 0.8875 0.8144 0.3450 0.029 Uiso 1 1 calc R . . C115 C 1.2885(4) 1.1755(3) 0.21857(19) 0.0287(8) Uani 1 1 d . . . H115 H 1.3663 1.2100 0.2445 0.034 Uiso 1 1 calc R . . C114 C 1.2189(4) 1.0870(3) 0.24379(17) 0.0271(7) Uani 1 1 d . . . H114 H 1.2494 1.0594 0.2873 0.033 Uiso 1 1 calc R . . C113 C 1.1043(3) 1.0387(3) 0.20497(16) 0.0224(7) Uani 1 1 d . . . C112 C 1.0672(4) 1.0806(3) 0.14124(17) 0.0281(7) Uani 1 1 d . . . H112 H 0.9903 1.0470 0.1141 0.034 Uiso 1 1 calc R . . N111 N 1.1334(4) 1.1656(3) 0.11539(16) 0.0333(7) Uani 1 1 d . . . C116 C 1.2415(4) 1.2123(3) 0.15460(19) 0.0300(8) Uani 1 1 d . . . H116 H 1.2881 1.2736 0.1376 0.036 Uiso 1 1 calc R . . N121 N 0.8634(3) 0.6274(2) 0.18886(13) 0.0228(6) Uani 1 1 d . . . N122 N 0.9565(3) 0.6407(2) 0.14000(13) 0.0227(6) Uani 1 1 d . . . C123 C 1.0045(3) 0.5414(3) 0.12714(16) 0.0229(7) Uani 1 1 d . . . C124 C 0.9442(4) 0.4647(3) 0.16790(18) 0.0310(8) Uani 1 1 d . . . H124 H 0.9604 0.3890 0.1687 0.037 Uiso 1 1 calc R . . C125 C 0.8563(4) 0.5232(3) 0.20663(18) 0.0287(8) Uani 1 1 d . . . H125 H 0.8000 0.4947 0.2402 0.034 Uiso 1 1 calc R . . N131 N 1.2198(3) 0.3876(2) 0.00894(15) 0.0301(7) Uani 1 1 d . . . C132 C 1.1278(4) 0.4165(3) 0.05318(17) 0.0251(7) Uani 1 1 d . . . H132 H 1.0689 0.3615 0.0699 0.030 Uiso 1 1 calc R . . C133 C 1.1102(4) 0.5207(3) 0.07712(16) 0.0233(7) Uani 1 1 d . . . C134 C 1.1976(4) 0.6006(3) 0.05120(18) 0.0290(8) Uani 1 1 d . . . H134 H 1.1918 0.6734 0.0659 0.035 Uiso 1 1 calc R . . C135 C 1.2917(4) 0.5724(3) 0.00433(19) 0.0335(8) Uani 1 1 d . . . H135 H 1.3506 0.6258 -0.0141 0.040 Uiso 1 1 calc R . . C136 C 1.3001(4) 0.4662(3) -0.01585(19) 0.0332(8) Uani 1 1 d . . . H136 H 1.3652 0.4479 -0.0485 0.040 Uiso 1 1 calc R . . N141 N 0.6412(3) 0.7545(2) 0.17648(13) 0.0224(6) Uani 1 1 d . . . N142 N 0.6330(3) 0.7863(2) 0.11065(13) 0.0229(6) Uani 1 1 d . . . C143 C 0.4946(4) 0.8173(3) 0.09567(18) 0.0241(7) Uani 1 1 d . . . C144 C 0.4137(4) 0.8046(3) 0.15164(18) 0.0290(8) Uani 1 1 d . . . H144 H 0.3139 0.8202 0.1545 0.035 Uiso 1 1 calc R . . C145 C 0.5111(4) 0.7647(3) 0.20109(17) 0.0275(7) Uani 1 1 d . . . H145 H 0.4902 0.7471 0.2457 0.033 Uiso 1 1 calc R . . N151 N 0.2529(3) 0.9591(3) -0.03700(16) 0.0351(7) Uani 1 1 d . . . C152 C 0.3120(4) 0.9182(3) 0.02128(19) 0.0316(8) Uani 1 1 d . . . H152 H 0.2632 0.9306 0.0606 0.038 Uiso 1 1 calc R . . C153 C 0.4402(4) 0.8585(3) 0.02836(17) 0.0234(7) Uani 1 1 d . . . C154 C 0.5105(4) 0.8419(3) -0.02993(18) 0.0281(7) Uani 1 1 d . . . H154 H 0.5977 0.8011 -0.0281 0.034 Uiso 1 1 calc R . . C155 C 0.4523(4) 0.8854(3) -0.09065(17) 0.0297(8) Uani 1 1 d . . . H155 H 0.4997 0.8761 -0.1307 0.036 Uiso 1 1 calc R . . C156 C 0.3234(4) 0.9425(3) -0.09153(17) 0.0318(8) Uani 1 1 d . . . H156 H 0.2833 0.9714 -0.1333 0.038 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 Tl1 0.02244(8) 0.02029(9) 0.02938(8) -0.00021(5) 0.00253(5) 0.00053(5) B1 0.0225(19) 0.0193(19) 0.0276(18) 0.0031(15) 0.0020(15) -0.0014(15) N101 0.0204(14) 0.0167(14) 0.0237(13) 0.0022(10) 0.0010(11) 0.0015(10) N102 0.0222(14) 0.0195(15) 0.0265(13) 0.0010(11) 0.0005(11) -0.0002(11) C103 0.0171(15) 0.0199(16) 0.0295(15) -0.0004(14) -0.0003(12) 0.0046(13) C104 0.0259(17) 0.0262(19) 0.0244(15) -0.0017(14) -0.0017(13) 0.0030(14) C105 0.0256(17) 0.0235(17) 0.0241(15) 0.0013(14) 0.0008(13) 0.0057(14) C115 0.0175(17) 0.033(2) 0.0354(19) -0.0031(15) 0.0006(14) -0.0048(14) C114 0.0213(16) 0.0296(19) 0.0296(16) 0.0012(14) -0.0028(13) 0.0017(14) C113 0.0184(15) 0.0210(17) 0.0278(15) -0.0014(13) 0.0023(12) 0.0023(12) C112 0.0262(18) 0.0265(19) 0.0306(17) 0.0001(15) -0.0039(14) -0.0031(14) N111 0.0361(18) 0.0306(18) 0.0319(16) 0.0060(13) -0.0045(14) -0.0071(14) C116 0.0244(18) 0.0288(19) 0.0364(19) 0.0038(16) 0.0003(15) -0.0049(15) N121 0.0218(14) 0.0183(14) 0.0278(14) 0.0014(11) -0.0003(11) -0.0027(11) N122 0.0227(14) 0.0169(14) 0.0282(14) 0.0026(12) 0.0001(11) -0.0009(11) C123 0.0206(16) 0.0171(17) 0.0301(16) -0.0018(13) -0.0037(13) 0.0012(12) C124 0.038(2) 0.0160(18) 0.0392(19) 0.0010(15) 0.0041(16) 0.0000(14) C125 0.0332(19) 0.0179(18) 0.0357(18) 0.0025(14) 0.0060(15) -0.0021(14) N131 0.0284(16) 0.0265(17) 0.0349(15) -0.0022(13) 0.0000(12) 0.0039(13) C132 0.0264(17) 0.0182(17) 0.0299(16) 0.0003(13) -0.0017(13) 0.0010(13) C133 0.0224(16) 0.0188(17) 0.0273(15) 0.0007(13) -0.0058(13) 0.0013(13) C134 0.0258(18) 0.0205(18) 0.0402(19) -0.0035(15) -0.0007(15) -0.0033(14) C135 0.0311(19) 0.027(2) 0.043(2) 0.0040(16) 0.0031(15) -0.0061(15) C136 0.0281(19) 0.035(2) 0.0375(19) -0.0017(16) 0.0073(15) 0.0035(16) N141 0.0209(14) 0.0211(15) 0.0252(13) 0.0005(11) 0.0028(10) -0.0018(11) N142 0.0210(14) 0.0211(14) 0.0266(14) 0.0007(11) 0.0026(11) 0.0014(11) C143 0.0208(17) 0.0208(18) 0.0304(17) -0.0058(13) 0.0002(14) -0.0009(13) C144 0.0194(17) 0.035(2) 0.0336(18) -0.0026(15) 0.0055(14) -0.0005(14) C145 0.0227(17) 0.030(2) 0.0297(17) -0.0006(15) 0.0046(13) -0.0032(14) N151 0.0317(17) 0.0338(19) 0.0379(16) -0.0073(14) -0.0075(13) 0.0122(14) C152 0.0259(18) 0.032(2) 0.0364(18) -0.0077(16) -0.0009(14) 0.0053(15) C153 0.0222(16) 0.0174(17) 0.0294(16) -0.0035(14) -0.0042(13) -0.0001(13) C154 0.0269(18) 0.0237(18) 0.0331(18) -0.0019(15) -0.0010(14) 0.0046(14) C155 0.0292(19) 0.029(2) 0.0303(17) -0.0053(15) 0.0013(14) 0.0030(15) C156 0.036(2) 0.0263(19) 0.0310(17) -0.0040(16) -0.0102(15) 0.0031(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tl1 N142 2.759(3) . ? Tl1 N122 2.783(3) . ? B1 N101 1.535(5) . ? B1 N121 1.543(5) . ? B1 N141 1.553(5) . ? B1 H1 1.12(4) . ? N101 C105 1.353(4) . ? N101 N102 1.372(4) . ? N102 C103 1.337(4) . ? C103 C104 1.403(4) . ? C103 C113 1.479(5) . ? C104 C105 1.368(5) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? C115 C116 1.385(5) . ? C115 C114 1.387(5) . ? C115 H115 0.9500 . ? C114 C113 1.391(4) . ? C114 H114 0.9500 . ? C113 C112 1.385(5) . ? C112 N111 1.342(5) . ? C112 H112 0.9500 . ? N111 C116 1.345(5) . ? C116 H116 0.9500 . ? N121 C125 1.341(4) . ? N121 N122 1.363(4) . ? N122 C123 1.339(4) . ? C123 C124 1.396(5) . ? C123 C133 1.476(5) . ? C124 C125 1.374(5) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? N131 C132 1.326(4) . ? N131 C136 1.344(5) . ? C132 C133 1.389(5) . ? C132 H132 0.9500 . ? C133 C134 1.404(5) . ? C134 C135 1.374(5) . ? C134 H134 0.9500 . ? C135 C136 1.379(5) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.344(4) . ? N141 N142 1.363(4) . ? N142 C143 1.345(4) . ? C143 C144 1.403(5) . ? C143 C153 1.479(5) . ? C144 C145 1.367(5) . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? N151 C156 1.329(5) . ? N151 C152 1.338(5) . ? C152 C153 1.394(5) . ? C152 H152 0.9500 . ? C153 C154 1.392(5) . ? C154 C155 1.387(5) . ? C154 H154 0.9500 . ? C155 C156 1.385(5) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? 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 N142 Tl1 N122 78.31(8) . . ? N101 B1 N121 112.3(3) . . ? N101 B1 N141 111.4(3) . . ? N121 B1 N141 113.1(3) . . ? N101 B1 H1 109.1(18) . . ? N121 B1 H1 108.6(17) . . ? N141 B1 H1 102(2) . . ? C105 N101 N102 110.3(3) . . ? C105 N101 B1 125.4(3) . . ? N102 N101 B1 124.2(3) . . ? C103 N102 N101 105.1(3) . . ? N102 C103 C104 111.5(3) . . ? N102 C103 C113 122.4(3) . . ? C104 C103 C113 126.2(3) . . ? C105 C104 C103 104.6(3) . . ? C105 C104 H104 127.7 . . ? C103 C104 H104 127.7 . . ? N101 C105 C104 108.5(3) . . ? N101 C105 H105 125.8 . . ? C104 C105 H105 125.8 . . ? C116 C115 C114 118.3(3) . . ? C116 C115 H115 120.9 . . ? C114 C115 H115 120.9 . . ? C115 C114 C113 119.6(3) . . ? C115 C114 H114 120.2 . . ? C113 C114 H114 120.2 . . ? C112 C113 C114 117.6(3) . . ? C112 C113 C103 122.5(3) . . ? C114 C113 C103 119.7(3) . . ? N111 C112 C113 124.0(3) . . ? N111 C112 H112 118.0 . . ? C113 C112 H112 118.0 . . ? C112 N111 C116 117.1(3) . . ? N111 C116 C115 123.3(3) . . ? N111 C116 H116 118.3 . . ? C115 C116 H116 118.3 . . ? C125 N121 N122 110.6(3) . . ? C125 N121 B1 124.1(3) . . ? N122 N121 B1 125.2(3) . . ? C123 N122 N121 105.5(3) . . ? C123 N122 Tl1 130.6(2) . . ? N121 N122 Tl1 114.60(19) . . ? N122 C123 C124 111.0(3) . . ? N122 C123 C133 122.6(3) . . ? C124 C123 C133 126.4(3) . . ? C125 C124 C123 104.6(3) . . ? C125 C124 H124 127.7 . . ? C123 C124 H124 127.7 . . ? N121 C125 C124 108.3(3) . . ? N121 C125 H125 125.8 . . ? C124 C125 H125 125.8 . . ? C132 N131 C136 117.0(3) . . ? N131 C132 C133 125.4(3) . . ? N131 C132 H132 117.3 . . ? C133 C132 H132 117.3 . . ? C132 C133 C134 116.1(3) . . ? C132 C133 C123 119.8(3) . . ? C134 C133 C123 124.1(3) . . ? C135 C134 C133 119.2(3) . . ? C135 C134 H134 120.4 . . ? C133 C134 H134 120.4 . . ? C134 C135 C136 119.7(3) . . ? C134 C135 H135 120.2 . . ? C136 C135 H135 120.2 . . ? N131 C136 C135 122.5(3) . . ? N131 C136 H136 118.8 . . ? C135 C136 H136 118.8 . . ? C145 N141 N142 110.2(3) . . ? C145 N141 B1 122.6(3) . . ? N142 N141 B1 127.0(3) . . ? C143 N142 N141 105.6(3) . . ? C143 N142 Tl1 135.9(2) . . ? N141 N142 Tl1 116.75(18) . . ? N142 C143 C144 110.8(3) . . ? N142 C143 C153 122.8(3) . . ? C144 C143 C153 126.4(3) . . ? C145 C144 C143 104.3(3) . . ? C145 C144 H144 127.8 . . ? C143 C144 H144 127.8 . . ? N141 C145 C144 109.1(3) . . ? N141 C145 H145 125.4 . . ? C144 C145 H145 125.4 . . ? C156 N151 C152 117.1(3) . . ? N151 C152 C153 124.7(3) . . ? N151 C152 H152 117.7 . . ? C153 C152 H152 117.7 . . ? C154 C153 C152 116.6(3) . . ? C154 C153 C143 123.8(3) . . ? C152 C153 C143 119.6(3) . . ? C155 C154 C153 119.6(3) . . ? C155 C154 H154 120.2 . . ? C153 C154 H154 120.2 . . ? C156 C155 C154 118.5(3) . . ? C156 C155 H155 120.7 . . ? C154 C155 H155 120.7 . . ? N151 C156 C155 123.5(3) . . ? N151 C156 H156 118.3 . . ? C155 C156 H156 118.3 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.891 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.121 #=END data_TlTkp4py _database_code_depnum_ccdc_archive 'CCDC 264760' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TlTkp4py _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H32 B N12 O2 Tl' _chemical_formula_weight 855.90 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' Tl Tl -2.8358 9.6688 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.1323(3) _cell_length_b 11.8362(3) _cell_length_c 35.6666(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3433.11(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11168 _cell_measurement_theta_min 3.49 _cell_measurement_theta_max 28.14 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.656 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 4.756 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0254 _exptl_absorpt_correction_T_max 0.0503 _exptl_absorpt_process_details 'XPREP (Siemens, 1994)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector CCD _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11168 _diffrn_reflns_av_R_equivalents 0.0423 _diffrn_reflns_av_sigmaI/netI 0.0784 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.49 _diffrn_reflns_theta_max 28.14 _reflns_number_total 7573 _reflns_number_gt 5499 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0450P)^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 constr _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 0.005(10) _refine_ls_number_reflns 7573 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1069 _refine_ls_wR_factor_gt 0.0960 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.017 _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 Tl1 Tl 0.74827(5) 0.987743(17) 0.061987(8) 0.03189(8) Uani 1 1 d . . . N142 N 0.7026(7) 0.9621(5) 0.14101(18) 0.0298(15) Uani 1 1 d . . . N102 N 0.4210(7) 0.9951(5) 0.07915(18) 0.0254(13) Uani 1 1 d . . . N111 N 0.3096(8) 0.7384(6) -0.0327(2) 0.045(2) Uani 1 1 d . . . C105 C 0.2429(13) 1.1355(5) 0.0892(2) 0.0351(16) Uani 1 1 d . . . H105 H 0.1898 1.1986 0.1004 0.042 Uiso 1 1 calc R . . C103 C 0.3086(10) 0.9931(6) 0.0521(2) 0.0312(17) Uani 1 1 d . . . N141 N 0.5528(7) 0.9988(5) 0.15334(18) 0.0275(14) Uani 1 1 d . . . N101 N 0.3824(7) 1.0832(5) 0.10204(19) 0.0284(14) Uani 1 1 d . . . C104 C 0.1939(8) 1.0799(6) 0.0574(3) 0.0355(19) Uani 1 1 d . . . H104 H 0.1015 1.0968 0.0421 0.043 Uiso 1 1 calc R . . C153 C 1.0128(10) 0.8429(7) 0.1313(2) 0.0353(19) Uani 1 1 d . . . H153 H 1.0141 0.9216 0.1261 0.042 Uiso 1 1 calc R . . C154 C 0.8701(10) 0.7922(7) 0.1464(2) 0.0316(18) Uani 1 1 d . . . C145 C 0.4776(10) 0.9170(6) 0.1729(2) 0.0335(18) Uani 1 1 d . . . H145 H 0.3721 0.9227 0.1842 0.040 Uiso 1 1 calc R . . C155 C 0.8787(11) 0.6760(7) 0.1532(3) 0.038(2) Uani 1 1 d . . . H155 H 0.7866 0.6363 0.1630 0.046 Uiso 1 1 calc R . . C114 C 0.3113(9) 0.9065(6) 0.0225(3) 0.0347(19) Uani 1 1 d . . . B1 B 0.4842(11) 1.1104(7) 0.1366(3) 0.031(2) Uani 1 1 d . . . C144 C 0.5775(9) 0.8234(7) 0.1740(3) 0.038(2) Uani 1 1 d . . . H144 H 0.5561 0.7529 0.1858 0.045 Uiso 1 1 calc R . . N162 N 0.2418(10) 1.1150(4) 0.18122(15) 0.0285(12) Uani 1 1 d . . . C115 C 0.2481(14) 0.9261(5) -0.0128(2) 0.0388(16) Uani 1 1 d . . . H115 H 0.2014 0.9974 -0.0187 0.047 Uiso 1 1 calc R . . C125 C 0.7359(11) 1.2332(5) 0.1545(2) 0.0315(16) Uani 1 1 d . . . H125 H 0.7268 1.2261 0.1809 0.038 Uiso 1 1 calc R . . C164 C 0.2390(12) 1.2984(6) 0.1989(2) 0.0380(17) Uani 1 1 d . . . H164 H 0.2068 1.3669 0.2106 0.046 Uiso 1 1 calc R . . N161 N 0.3709(8) 1.1707(5) 0.1653(2) 0.0314(15) Uani 1 1 d . . . C163 C 0.1619(10) 1.1920(6) 0.2019(2) 0.0325(18) Uani 1 1 d . . . N122 N 0.6821(8) 1.2138(6) 0.09341(19) 0.0320(15) Uani 1 1 d . . . C165 C 0.3708(10) 1.2819(6) 0.1753(2) 0.0354(19) Uani 1 1 d . . . H165 H 0.4476 1.3376 0.1675 0.042 Uiso 1 1 calc R . . C123 C 0.8213(9) 1.2757(7) 0.0978(2) 0.0283(17) Uani 1 1 d . . . N151 N 1.1573(9) 0.6683(6) 0.1305(2) 0.048(2) Uani 1 1 d . . . C124 C 0.8548(9) 1.2899(7) 0.1356(3) 0.035(2) Uani 1 1 d . . . H124 H 0.9435 1.3312 0.1462 0.043 Uiso 1 1 calc R . . N121 N 0.6320(8) 1.1883(5) 0.12856(19) 0.0273(14) Uani 1 1 d . . . C113 C 0.3732(10) 0.7993(7) 0.0303(3) 0.039(2) Uani 1 1 d . . . H113 H 0.4167 0.7813 0.0543 0.046 Uiso 1 1 calc R . . C152 C 1.1489(10) 0.7787(7) 0.1242(3) 0.041(2) Uani 1 1 d . . . H152 H 1.2431 0.8153 0.1142 0.050 Uiso 1 1 calc R . . C156 C 1.0243(12) 0.6200(7) 0.1454(3) 0.050(3) Uani 1 1 d . . . H156 H 1.0297 0.5416 0.1510 0.060 Uiso 1 1 calc R . . C134 C 0.9124(8) 1.3196(5) 0.0654(2) 0.0278(16) Uani 1 1 d . . . C173 C -0.0692(9) 1.0584(6) 0.2159(2) 0.0301(18) Uani 1 1 d . . . H173 H -0.0286 1.0069 0.1977 0.036 Uiso 1 1 calc R . . C174 C 0.0129(9) 1.1592(6) 0.2229(3) 0.0341(18) Uani 1 1 d . . . C135 C 1.0335(10) 1.4019(6) 0.0705(2) 0.035(2) Uani 1 1 d . . . H135 H 1.0562 1.4312 0.0947 0.042 Uiso 1 1 calc R . . C175 C -0.0493(10) 1.2320(7) 0.2503(2) 0.039(2) Uani 1 1 d . . . H175 H 0.0029 1.3017 0.2560 0.046 Uiso 1 1 calc R . . C133 C 0.8877(9) 1.2796(6) 0.0293(2) 0.0318(18) Uani 1 1 d . . . H133 H 0.8063 1.2239 0.0244 0.038 Uiso 1 1 calc R . . C143 C 0.7196(8) 0.8558(6) 0.1537(2) 0.0267(18) Uani 1 1 d . . . N171 N -0.2748(9) 1.1003(6) 0.26182(19) 0.0419(18) Uani 1 1 d . . . C172 C -0.2105(9) 1.0343(7) 0.2357(2) 0.039(2) Uani 1 1 d . . . H172 H -0.2656 0.9655 0.2302 0.047 Uiso 1 1 calc R . . N131 N 1.1008(8) 1.4020(6) 0.0052(2) 0.0387(17) Uani 1 1 d . . . C136 C 1.1192(11) 1.4398(7) 0.0397(3) 0.042(2) Uani 1 1 d . . . H136 H 1.1980 1.4979 0.0436 0.051 Uiso 1 1 calc R . . C132 C 0.9847(10) 1.3225(6) 0.0001(2) 0.0330(19) Uani 1 1 d . . . H132 H 0.9676 1.2941 -0.0245 0.040 Uiso 1 1 calc R . . C176 C -0.1920(10) 1.1973(7) 0.2690(3) 0.047(2) Uani 1 1 d . . . H176 H -0.2339 1.2452 0.2881 0.056 Uiso 1 1 calc R . . C116 C 0.2530(14) 0.8411(6) -0.0398(2) 0.0439(18) Uani 1 1 d . . . H116 H 0.2140 0.8575 -0.0643 0.053 Uiso 1 1 calc R . . C112 C 0.3688(12) 0.7184(8) 0.0013(3) 0.050(3) Uani 1 1 d . . . H112 H 0.4110 0.6452 0.0064 0.060 Uiso 1 1 calc R . . O1 O -0.5580(7) 1.0319(6) 0.30183(19) 0.0514(17) Uani 1 1 d . . . C1 C -0.6618(11) 0.9748(9) 0.2750(3) 0.058(3) Uani 1 1 d . . . H1A H -0.7720 0.9651 0.2856 0.087 Uiso 1 1 calc R . . H1B H -0.6149 0.9006 0.2692 0.087 Uiso 1 1 calc R . . H1C H -0.6689 1.0199 0.2520 0.087 Uiso 1 1 calc R . . O2 O 1.4195(8) 0.5811(5) 0.0873(2) 0.0579(19) Uani 1 1 d . . . C2 C 1.4909(13) 0.4813(9) 0.0992(4) 0.069(3) Uani 1 1 d . . . H2A H 1.4090 0.4205 0.0984 0.103 Uiso 1 1 calc R . . H2B H 1.5311 0.4903 0.1249 0.103 Uiso 1 1 calc R . . H2C H 1.5830 0.4622 0.0827 0.103 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 Tl1 0.03206(13) 0.03074(12) 0.03287(13) -0.00217(11) 0.0017(2) 0.0036(2) N142 0.032(4) 0.029(3) 0.028(3) -0.002(3) 0.004(3) 0.000(2) N102 0.019(3) 0.026(3) 0.032(3) 0.000(3) 0.001(2) 0.003(2) N111 0.040(4) 0.037(4) 0.058(5) -0.011(4) -0.014(4) -0.001(3) C105 0.028(4) 0.027(3) 0.050(4) 0.006(3) 0.006(6) 0.012(5) C103 0.029(3) 0.026(4) 0.038(4) 0.003(3) -0.001(3) -0.002(3) N141 0.029(3) 0.027(3) 0.027(3) 0.000(3) -0.001(3) 0.002(3) N101 0.020(3) 0.031(3) 0.034(4) -0.001(3) -0.003(3) -0.001(3) C104 0.018(3) 0.036(4) 0.052(6) 0.011(4) -0.008(4) 0.000(3) C153 0.030(4) 0.038(4) 0.038(5) 0.006(4) 0.001(4) 0.002(4) C154 0.032(4) 0.030(4) 0.033(5) -0.001(3) -0.003(4) 0.001(3) C145 0.035(4) 0.031(4) 0.035(5) -0.007(4) 0.005(4) 0.000(3) C155 0.037(5) 0.031(4) 0.047(6) -0.002(4) 0.002(4) 0.005(4) C114 0.028(4) 0.028(4) 0.049(5) 0.004(4) 0.002(4) -0.001(3) B1 0.033(5) 0.028(4) 0.031(5) 0.001(4) 0.011(4) 0.008(4) C144 0.034(4) 0.029(4) 0.050(6) 0.002(4) 0.007(4) 0.001(3) N162 0.027(3) 0.029(2) 0.029(3) 0.002(2) 0.006(4) 0.004(4) C115 0.045(4) 0.031(3) 0.041(4) 0.002(3) -0.009(7) -0.007(6) C125 0.034(4) 0.036(3) 0.024(3) 0.002(3) 0.002(5) 0.009(5) C164 0.046(5) 0.030(3) 0.038(4) -0.007(3) 0.003(6) 0.005(6) N161 0.030(3) 0.023(3) 0.041(4) -0.001(3) 0.006(3) 0.003(3) C163 0.036(4) 0.027(4) 0.035(5) -0.001(3) -0.004(4) -0.002(3) N122 0.036(3) 0.027(3) 0.033(4) -0.005(3) 0.000(3) 0.005(3) C165 0.041(5) 0.030(4) 0.035(5) 0.003(4) 0.006(4) 0.000(4) C123 0.020(3) 0.026(4) 0.039(5) 0.001(4) -0.002(3) -0.002(3) N151 0.039(4) 0.036(4) 0.068(6) -0.004(4) 0.003(4) 0.006(3) C124 0.027(4) 0.036(4) 0.043(5) -0.008(4) -0.006(4) -0.004(3) N121 0.027(3) 0.025(3) 0.030(4) 0.003(3) 0.002(3) 0.002(3) C113 0.031(4) 0.032(4) 0.053(6) -0.001(4) -0.005(4) -0.001(4) C152 0.033(5) 0.044(5) 0.048(6) 0.001(4) 0.001(4) 0.002(4) C156 0.062(6) 0.026(4) 0.061(7) -0.006(4) 0.011(5) 0.003(4) C134 0.031(4) 0.021(3) 0.031(4) 0.007(3) -0.002(4) 0.007(3) C173 0.028(4) 0.031(4) 0.031(5) 0.003(3) 0.003(3) 0.004(3) C174 0.029(4) 0.034(4) 0.039(5) 0.004(4) 0.001(4) 0.009(3) C135 0.042(5) 0.029(4) 0.035(5) -0.005(3) 0.005(4) -0.007(3) C175 0.043(5) 0.041(5) 0.032(5) -0.004(4) 0.003(4) 0.004(4) C133 0.022(4) 0.028(4) 0.045(5) 0.001(4) -0.005(4) 0.008(3) C143 0.019(5) 0.027(3) 0.033(4) 0.000(3) -0.001(3) 0.001(3) N171 0.029(4) 0.049(4) 0.047(4) -0.001(3) 0.009(4) 0.004(3) C172 0.042(6) 0.039(4) 0.036(5) 0.005(3) 0.000(4) -0.006(4) N131 0.032(4) 0.033(4) 0.052(5) 0.009(3) 0.003(4) 0.002(3) C136 0.042(5) 0.036(4) 0.049(6) 0.007(4) -0.007(5) -0.007(4) C132 0.038(5) 0.035(4) 0.026(4) 0.001(3) 0.001(4) 0.009(4) C176 0.047(5) 0.047(5) 0.045(6) -0.004(4) 0.012(4) 0.008(4) C116 0.038(4) 0.051(4) 0.042(5) -0.002(3) -0.002(7) -0.017(7) C112 0.049(6) 0.034(5) 0.068(7) -0.015(5) -0.001(5) 0.008(4) O1 0.050(4) 0.051(4) 0.052(4) -0.008(3) 0.016(3) -0.003(3) C1 0.050(6) 0.066(6) 0.058(7) 0.008(6) 0.010(5) -0.001(5) O2 0.058(4) 0.040(3) 0.075(5) 0.011(3) 0.018(4) 0.013(3) C2 0.059(7) 0.062(6) 0.085(9) 0.023(6) 0.014(6) 0.008(6) _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 Tl1 N102 2.732(6) . ? Tl1 N142 2.859(6) . ? Tl1 N122 2.950(7) . ? Tl1 N111 2.916(7) 3_565 ? Tl1 N131 2.980(7) 3_475 ? N142 C143 1.344(9) . ? N142 N141 1.366(8) . ? N102 C103 1.330(10) . ? N102 N101 1.361(8) . ? N111 C112 1.325(12) . ? N111 C116 1.325(10) . ? C105 N101 1.370(10) . ? C105 C104 1.373(11) . ? C103 C104 1.400(10) . ? C103 C114 1.470(11) . ? N141 C145 1.341(10) . ? N141 B1 1.553(10) . ? N101 B1 1.519(11) . ? C153 C152 1.366(11) . ? C153 C154 1.412(11) . ? C154 C155 1.398(11) . ? C154 C143 1.461(10) . ? C145 C144 1.374(10) . ? C155 C156 1.386(11) . ? C114 C115 1.381(11) . ? C114 C113 1.393(11) . ? B1 N121 1.541(11) . ? B1 N161 1.551(10) . ? C144 C143 1.418(10) . ? N162 C163 1.340(9) . ? N162 N161 1.364(9) . ? C115 C116 1.392(10) . ? C125 C124 1.356(11) . ? C125 N121 1.361(10) . ? C164 C165 1.375(11) . ? C164 C163 1.411(10) . ? N161 C165 1.364(10) . ? C163 C174 1.478(11) . ? N122 N121 1.353(9) . ? N122 C123 1.358(9) . ? C123 C124 1.387(11) . ? C123 C134 1.467(11) . ? N151 C152 1.328(11) . ? N151 C156 1.333(11) . ? C113 C112 1.412(12) . ? C134 C133 1.388(11) . ? C134 C135 1.397(10) . ? C173 C172 1.378(10) . ? C173 C174 1.390(11) . ? C174 C175 1.398(11) . ? C135 C136 1.375(12) . ? C175 C176 1.400(11) . ? C133 C132 1.400(11) . ? N171 C172 1.323(10) . ? N171 C176 1.355(11) . ? N131 C136 1.318(11) . ? N131 C132 1.345(10) . ? O1 C1 1.444(12) . ? O2 C2 1.383(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 C143 N142 N141 106.4(6) . . ? C103 N102 N101 106.9(6) . . ? C103 N102 Tl1 120.4(5) . . ? N101 N102 Tl1 112.6(4) . . ? C112 N111 C116 117.7(8) . . ? N101 C105 C104 107.4(6) . . ? N102 C103 C104 110.3(7) . . ? N102 C103 C114 121.5(7) . . ? C104 C103 C114 128.2(7) . . ? C145 N141 N142 110.1(6) . . ? C145 N141 B1 130.6(6) . . ? N142 N141 B1 117.8(6) . . ? N102 N101 C105 109.7(6) . . ? N102 N101 B1 121.5(6) . . ? C105 N101 B1 128.8(6) . . ? C105 C104 C103 105.7(7) . . ? C152 C153 C154 120.0(8) . . ? C155 C154 C153 116.3(7) . . ? C155 C154 C143 121.2(7) . . ? C153 C154 C143 122.5(7) . . ? N141 C145 C144 109.2(7) . . ? C156 C155 C154 118.6(8) . . ? C115 C114 C113 118.0(8) . . ? C115 C114 C103 122.1(7) . . ? C113 C114 C103 119.8(8) . . ? N101 B1 N121 113.7(7) . . ? N101 B1 N161 108.0(7) . . ? N121 B1 N161 108.0(6) . . ? N101 B1 N141 109.2(6) . . ? N121 B1 N141 107.5(6) . . ? N161 B1 N141 110.5(7) . . ? C145 C144 C143 104.4(7) . . ? C163 N162 N161 105.9(5) . . ? C114 C115 C116 119.9(8) . . ? C124 C125 N121 107.4(7) . . ? C165 C164 C163 105.4(7) . . ? C165 N161 N162 110.9(6) . . ? C165 N161 B1 128.2(7) . . ? N162 N161 B1 120.6(6) . . ? N162 C163 C164 110.5(7) . . ? N162 C163 C174 119.9(7) . . ? C164 C163 C174 129.6(7) . . ? N121 N122 C123 105.4(6) . . ? N161 C165 C164 107.4(7) . . ? N122 C123 C124 109.9(7) . . ? N122 C123 C134 121.5(7) . . ? C124 C123 C134 128.6(7) . . ? C152 N151 C156 116.6(8) . . ? C125 C124 C123 106.4(7) . . ? N122 N121 C125 110.8(6) . . ? N122 N121 B1 122.7(7) . . ? C125 N121 B1 126.3(7) . . ? C114 C113 C112 117.5(9) . . ? N151 C152 C153 123.9(8) . . ? N151 C156 C155 124.6(8) . . ? C133 C134 C135 117.4(8) . . ? C133 C134 C123 122.5(7) . . ? C135 C134 C123 120.1(8) . . ? C172 C173 C174 119.1(8) . . ? C173 C174 C175 118.8(7) . . ? C173 C174 C163 121.9(7) . . ? C175 C174 C163 119.4(7) . . ? C136 C135 C134 118.8(8) . . ? C174 C175 C176 116.9(8) . . ? C134 C133 C132 118.9(7) . . ? N142 C143 C144 110.0(6) . . ? N142 C143 C154 120.6(6) . . ? C144 C143 C154 129.4(7) . . ? C172 N171 C176 115.9(7) . . ? N171 C172 C173 124.6(8) . . ? C136 N131 C132 116.3(8) . . ? N131 C136 C135 125.2(8) . . ? N131 C132 C133 123.4(8) . . ? N171 C176 C175 124.7(8) . . ? N111 C116 C115 122.7(8) . . ? N111 C112 C113 124.1(9) . . ? N102 Tl1 N122 73.0(2) . . ? N102 Tl1 N142 69.9(2) . . ? N122 Tl1 N142 72.4(2) . . ? N131 Tl1 N102 77.0(2) 3_475 . ? N131 Tl1 N122 80.5(2) 3_475 . ? N131 Tl1 N142 141.9(2) 3_475 . ? N111 Tl1 N102 106.0(2) 3_565 . ? N111 Tl1 N122 178.5(2) 3_565 . ? N111 Tl1 N142 106.1(2) 3_565 . ? N111 Tl1 N131 100.5(2) 3_565 3_475 ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.820 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.128 #=END data_TlTkp3py _database_code_depnum_ccdc_archive 'CCDC 264761' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TlTkp3py _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 B N12 O Tl' _chemical_formula_weight 809.83 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' Tl Tl -2.8358 9.6688 '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 11.0693(1) _cell_length_b 11.6639(2) _cell_length_c 13.9684(2) _cell_angle_alpha 84.381(1) _cell_angle_beta 72.825(1) _cell_angle_gamma 70.132(1) _cell_volume 1620.49(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 42072 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 28.21 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.04 _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.660 _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 5.030 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2581 _exptl_absorpt_correction_T_max 0.8099 _exptl_absorpt_process_details 'XPREP (Siemens, 1994)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector CCD _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42072 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0233 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 28.21 _reflns_number_total 7910 _reflns_number_gt 7381 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0346P)^2^+3.7648P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7910 _refine_ls_number_parameters 423 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Tl1 Tl 0.272787(11) 0.390670(11) 0.275359(10) 0.02701(5) Uani 1 1 d . . . N101 N 0.6170(2) 0.2135(2) 0.23848(19) 0.0201(5) Uani 1 1 d . . . N142 N 0.4129(3) 0.1114(2) 0.2225(2) 0.0220(5) Uani 1 1 d . . . N122 N 0.3969(3) 0.3183(2) 0.4417(2) 0.0239(5) Uani 1 1 d . . . N161 N 0.6542(3) 0.0164(2) 0.3313(2) 0.0236(5) Uani 1 1 d . . . N121 N 0.5079(3) 0.2167(2) 0.4251(2) 0.0225(5) Uani 1 1 d . . . N102 N 0.5528(3) 0.3321(2) 0.2197(2) 0.0229(5) Uani 1 1 d . . . N141 N 0.4267(3) 0.1267(2) 0.3142(2) 0.0219(5) Uani 1 1 d . . . N171 N 1.1732(3) -0.3544(3) 0.3278(3) 0.0378(7) Uani 1 1 d . . . C105 C 0.7387(3) 0.1734(3) 0.1712(2) 0.0253(6) Uani 1 1 d . . . H105 H 0.8022 0.0941 0.1694 0.030 Uiso 1 1 calc R . . C123 C 0.3859(3) 0.3643(3) 0.5291(2) 0.0242(6) Uani 1 1 d . . . C173 C 0.9717(3) -0.1805(3) 0.3520(2) 0.0243(6) Uani 1 1 d . . . C125 C 0.5648(3) 0.2009(3) 0.5016(3) 0.0290(7) Uani 1 1 d . . . H125 H 0.6427 0.1366 0.5072 0.035 Uiso 1 1 calc R . . C143 C 0.3006(3) 0.0822(3) 0.2423(3) 0.0249(6) Uani 1 1 d . . . C103 C 0.6366(3) 0.3641(3) 0.1390(2) 0.0243(6) Uani 1 1 d . . . C134 C 0.2854(4) 0.5580(4) 0.6281(3) 0.0339(8) Uani 1 1 d . . . H134 H 0.3705 0.5512 0.6349 0.041 Uiso 1 1 calc R . . C113 C 0.5972(3) 0.4860(3) 0.0954(3) 0.0270(7) Uani 1 1 d . . . C104 C 0.7554(3) 0.2660(3) 0.1061(3) 0.0297(7) Uani 1 1 d . . . H104 H 0.8306 0.2643 0.0509 0.036 Uiso 1 1 calc R . . C153 C 0.2494(3) 0.0638(3) 0.1614(3) 0.0292(7) Uani 1 1 d . . . C144 C 0.2432(3) 0.0778(4) 0.3463(3) 0.0324(7) Uani 1 1 d . . . H144 H 0.1641 0.0590 0.3798 0.039 Uiso 1 1 calc R . . C133 C 0.2714(3) 0.4707(3) 0.5741(2) 0.0259(6) Uani 1 1 d . . . C132 C 0.1434(3) 0.4856(3) 0.5671(3) 0.0288(7) Uani 1 1 d . . . H132 H 0.1338 0.4267 0.5301 0.035 Uiso 1 1 calc R . . N151 N 0.0734(4) 0.0300(4) 0.1116(3) 0.0524(10) Uani 1 1 d . . . C114 C 0.4928(4) 0.5840(3) 0.1478(3) 0.0358(8) Uani 1 1 d . . . H114 H 0.4482 0.5757 0.2163 0.043 Uiso 1 1 calc R . . C176 C 1.2107(4) -0.3039(3) 0.3903(3) 0.0363(8) Uani 1 1 d . . . H176 H 1.2930 -0.3468 0.4050 0.044 Uiso 1 1 calc R . . C174 C 1.0152(4) -0.1289(3) 0.4149(3) 0.0309(7) Uani 1 1 d . . . H174 H 0.9628 -0.0510 0.4440 0.037 Uiso 1 1 calc R . . C172 C 1.0561(4) -0.2935(3) 0.3098(3) 0.0336(8) Uani 1 1 d . . . H172 H 1.0284 -0.3294 0.2655 0.040 Uiso 1 1 calc R . . B1 B 0.5531(3) 0.1444(3) 0.3273(3) 0.0208(6) Uani 1 1 d . . . C145 C 0.3255(3) 0.1062(3) 0.3888(3) 0.0288(7) Uani 1 1 d . . . H145 H 0.3140 0.1109 0.4586 0.035 Uiso 1 1 calc R . . C165 C 0.6516(3) -0.0869(3) 0.2970(3) 0.0329(8) Uani 1 1 d . . . H165 H 0.5804 -0.0948 0.2762 0.040 Uiso 1 1 calc R . . C124 C 0.4904(3) 0.2939(4) 0.5689(3) 0.0305(7) Uani 1 1 d . . . H124 H 0.5061 0.3076 0.6294 0.037 Uiso 1 1 calc R . . C115 C 0.4547(5) 0.6944(4) 0.0983(4) 0.0449(10) Uani 1 1 d . . . H115 H 0.3831 0.7620 0.1323 0.054 Uiso 1 1 calc R . . C175 C 1.1356(4) -0.1920(4) 0.4350(3) 0.0372(8) Uani 1 1 d . . . H175 H 1.1662 -0.1586 0.4789 0.045 Uiso 1 1 calc R . . C152 C 0.1279(4) 0.0438(5) 0.1813(3) 0.0449(10) Uani 1 1 d . . . H152 H 0.0799 0.0396 0.2495 0.054 Uiso 1 1 calc R . . C154 C 0.3216(5) 0.0608(6) 0.0633(4) 0.0621(16) Uani 1 1 d . . . H154 H 0.4080 0.0690 0.0459 0.075 Uiso 1 1 calc R . . C156 C 0.1402(5) 0.0360(6) 0.0176(4) 0.0579(14) Uani 1 1 d . . . H156 H 0.0999 0.0336 -0.0332 0.070 Uiso 1 1 calc R . . C155 C 0.2680(6) 0.0458(8) -0.0106(4) 0.081(2) Uani 1 1 d . . . H155 H 0.3174 0.0422 -0.0792 0.098 Uiso 1 1 calc R . . N162 N 0.7724(3) -0.0041(3) 0.3535(2) 0.0241(5) Uani 1 1 d . . . N131 N 0.0340(3) 0.5777(3) 0.6091(3) 0.0361(7) Uani 1 1 d . . . C163 C 0.8408(3) -0.1226(3) 0.3328(2) 0.0245(6) Uani 1 1 d . . . N111 N 0.6268(4) 0.6132(3) -0.0517(3) 0.0398(8) Uani 1 1 d . . . C112 C 0.6615(4) 0.5074(4) -0.0036(3) 0.0331(7) Uani 1 1 d . . . H112 H 0.7349 0.4422 -0.0393 0.040 Uiso 1 1 calc R . . C164 C 0.7688(4) -0.1785(3) 0.2971(3) 0.0358(8) Uani 1 1 d . . . H164 H 0.7950 -0.2611 0.2775 0.043 Uiso 1 1 calc R . . C116 C 0.5226(5) 0.7041(4) -0.0011(3) 0.0418(9) Uani 1 1 d . . . H116 H 0.4938 0.7787 -0.0349 0.050 Uiso 1 1 calc R . . C136 C 0.0507(4) 0.6596(4) 0.6608(3) 0.0414(9) Uani 1 1 d . . . H136 H -0.0261 0.7251 0.6921 0.050 Uiso 1 1 calc R . . C135 C 0.1734(4) 0.6545(4) 0.6714(3) 0.0429(10) Uani 1 1 d . . . H135 H 0.1801 0.7159 0.7075 0.051 Uiso 1 1 calc R . . O1 O 0.9411(9) -0.3896(9) 0.0674(7) 0.076(2) Uiso 0.50 1 d P . . O2 O 0.9596(9) -0.4563(9) 0.1116(7) 0.070(2) Uiso 0.50 1 d P . . 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 Tl1 0.02089(7) 0.02044(7) 0.03639(8) 0.00070(5) -0.01068(5) -0.00054(5) N101 0.0160(11) 0.0189(12) 0.0239(12) -0.0003(10) -0.0067(9) -0.0028(9) N142 0.0183(12) 0.0184(12) 0.0270(13) -0.0012(10) -0.0049(10) -0.0038(10) N122 0.0198(12) 0.0221(13) 0.0246(13) -0.0007(10) -0.0082(10) 0.0016(10) N161 0.0163(12) 0.0201(13) 0.0306(14) 0.0042(11) -0.0071(10) -0.0019(10) N121 0.0175(12) 0.0219(13) 0.0238(13) 0.0024(10) -0.0077(10) 0.0001(10) N102 0.0193(12) 0.0197(12) 0.0269(13) 0.0014(10) -0.0062(10) -0.0035(10) N141 0.0169(11) 0.0200(12) 0.0251(13) 0.0027(10) -0.0050(10) -0.0030(10) N171 0.0236(14) 0.0252(15) 0.058(2) -0.0061(14) -0.0119(14) 0.0021(12) C105 0.0184(14) 0.0276(16) 0.0261(15) -0.0008(13) -0.0053(12) -0.0035(12) C123 0.0198(14) 0.0268(16) 0.0238(14) 0.0007(12) -0.0057(11) -0.0054(12) C173 0.0195(14) 0.0204(15) 0.0278(15) 0.0040(12) -0.0048(12) -0.0025(11) C125 0.0216(15) 0.0345(18) 0.0272(16) 0.0045(14) -0.0120(12) -0.0014(13) C143 0.0171(13) 0.0187(14) 0.0355(17) -0.0027(12) -0.0045(12) -0.0036(11) C103 0.0232(15) 0.0278(16) 0.0241(15) 0.0026(12) -0.0080(12) -0.0104(13) C134 0.0290(17) 0.039(2) 0.0347(18) -0.0078(15) -0.0123(14) -0.0077(15) C113 0.0284(16) 0.0291(17) 0.0289(16) 0.0063(13) -0.0127(13) -0.0140(13) C104 0.0224(15) 0.0368(19) 0.0259(16) 0.0041(14) -0.0048(12) -0.0073(14) C153 0.0216(15) 0.0246(16) 0.0397(19) -0.0095(14) -0.0052(13) -0.0056(12) C144 0.0219(15) 0.0360(19) 0.0370(19) 0.0039(15) -0.0034(13) -0.0118(14) C133 0.0220(15) 0.0283(17) 0.0238(15) -0.0020(13) -0.0053(12) -0.0042(13) C132 0.0241(15) 0.0296(17) 0.0308(17) -0.0067(14) -0.0056(13) -0.0063(13) N151 0.0271(17) 0.075(3) 0.057(2) -0.025(2) -0.0056(16) -0.0185(18) C114 0.046(2) 0.0274(18) 0.0333(18) 0.0033(14) -0.0105(16) -0.0123(16) C176 0.0239(16) 0.0279(18) 0.055(2) 0.0057(16) -0.0172(16) -0.0023(14) C174 0.0281(17) 0.0239(16) 0.0347(18) -0.0015(14) -0.0097(14) 0.0002(13) C172 0.0238(16) 0.0239(17) 0.049(2) -0.0074(15) -0.0116(15) 0.0013(13) B1 0.0159(14) 0.0179(15) 0.0251(16) 0.0033(12) -0.0074(12) -0.0006(12) C145 0.0234(15) 0.0285(17) 0.0304(17) 0.0075(13) -0.0042(13) -0.0082(13) C165 0.0211(15) 0.0207(16) 0.058(2) 0.0016(15) -0.0149(15) -0.0050(13) C124 0.0242(16) 0.040(2) 0.0254(16) 0.0001(14) -0.0106(13) -0.0045(14) C115 0.058(3) 0.0252(19) 0.051(2) 0.0021(17) -0.019(2) -0.0107(18) C175 0.0357(19) 0.0310(19) 0.048(2) 0.0014(16) -0.0218(17) -0.0057(15) C152 0.0306(19) 0.062(3) 0.047(2) -0.008(2) -0.0079(17) -0.0222(19) C154 0.046(3) 0.112(5) 0.045(2) -0.024(3) 0.001(2) -0.052(3) C156 0.042(2) 0.090(4) 0.051(3) -0.036(3) -0.008(2) -0.028(3) C155 0.068(4) 0.156(7) 0.043(3) -0.031(3) 0.001(2) -0.071(4) N162 0.0184(12) 0.0222(13) 0.0271(13) 0.0019(10) -0.0078(10) 0.0001(10) N131 0.0232(14) 0.0370(17) 0.0433(18) -0.0109(14) -0.0069(13) -0.0027(13) C163 0.0179(14) 0.0204(15) 0.0284(15) 0.0030(12) -0.0038(12) -0.0010(11) N111 0.0448(19) 0.0436(19) 0.0382(17) 0.0158(15) -0.0168(15) -0.0233(16) C112 0.0313(18) 0.037(2) 0.0331(18) 0.0090(15) -0.0110(14) -0.0148(15) C164 0.0238(16) 0.0193(16) 0.063(3) -0.0021(16) -0.0150(16) -0.0020(13) C116 0.058(3) 0.0296(19) 0.047(2) 0.0126(17) -0.026(2) -0.0200(19) C136 0.0269(18) 0.039(2) 0.050(2) -0.0198(18) -0.0054(16) -0.0004(15) C135 0.038(2) 0.042(2) 0.049(2) -0.0211(19) -0.0129(18) -0.0075(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 Tl1 N102 2.815(3) . ? Tl1 N122 2.951(3) . ? Tl1 N141 3.055(3) . ? Tl1 N142 3.150(3) . ? Tl1 N131 3.209(3) 2_566 ? Tl1 N111 2.990(4) 2_665 ? Tl1 N171 2.884(3) 1_465 ? N101 C105 1.352(4) . ? N101 N102 1.363(4) . ? N101 B1 1.538(4) . ? N142 C143 1.343(4) . ? N142 N141 1.369(4) . ? N122 C123 1.338(4) . ? N122 N121 1.366(4) . ? N161 C165 1.352(5) . ? N161 N162 1.370(4) . ? N161 B1 1.539(4) . ? N121 C125 1.361(4) . ? N121 B1 1.537(4) . ? N102 C103 1.343(4) . ? N141 C145 1.357(4) . ? N141 B1 1.545(4) . ? N171 C176 1.328(5) . ? N171 C172 1.335(5) . ? C105 C104 1.368(5) . ? C123 C124 1.403(4) . ? C123 C133 1.468(4) . ? C173 C174 1.384(5) . ? C173 C172 1.396(5) . ? C173 C163 1.469(4) . ? C125 C124 1.369(5) . ? C143 C144 1.407(5) . ? C143 C153 1.467(5) . ? C103 C104 1.404(5) . ? C103 C113 1.466(5) . ? C134 C135 1.382(5) . ? C134 C133 1.399(5) . ? C113 C114 1.394(5) . ? C113 C112 1.398(5) . ? C153 C154 1.364(6) . ? C153 C152 1.386(5) . ? C144 C145 1.362(5) . ? C133 C132 1.399(5) . ? C132 N131 1.336(5) . ? N151 C156 1.311(7) . ? N151 C152 1.335(6) . ? C114 C115 1.393(6) . ? C176 C175 1.378(6) . ? C174 C175 1.382(5) . ? C165 C164 1.372(5) . ? C115 C116 1.385(6) . ? C154 C155 1.384(7) . ? C156 C155 1.393(7) . ? N162 C163 1.343(4) . ? N131 C136 1.342(5) . ? C163 C164 1.400(5) . ? N111 C116 1.337(6) . ? N111 C112 1.338(5) . ? C136 C135 1.390(6) . ? O1 O2 0.950(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 C105 N101 N102 110.1(3) . . ? C105 N101 B1 128.4(3) . . ? N102 N101 B1 121.4(2) . . ? C143 N142 N141 105.3(3) . . ? C123 N122 N121 105.8(3) . . ? C165 N161 N162 110.4(3) . . ? C165 N161 B1 125.3(3) . . ? N162 N161 B1 123.4(3) . . ? C125 N121 N122 110.1(3) . . ? C125 N121 B1 130.6(3) . . ? N122 N121 B1 119.3(2) . . ? C103 N102 N101 105.9(3) . . ? C103 N102 Tl1 130.9(2) . . ? N101 N102 Tl1 112.79(18) . . ? C145 N141 N142 110.5(3) . . ? C145 N141 B1 125.9(3) . . ? N142 N141 B1 122.9(2) . . ? C176 N171 C172 117.5(3) . . ? N101 C105 C104 108.7(3) . . ? N122 C123 C124 111.0(3) . . ? N122 C123 C133 120.8(3) . . ? C124 C123 C133 128.1(3) . . ? C174 C173 C172 117.0(3) . . ? C174 C173 C163 122.3(3) . . ? C172 C173 C163 120.7(3) . . ? N121 C125 C124 108.2(3) . . ? N142 C143 C144 110.7(3) . . ? N142 C143 C153 121.2(3) . . ? C144 C143 C153 128.0(3) . . ? N102 C103 C104 110.5(3) . . ? N102 C103 C113 120.7(3) . . ? C104 C103 C113 128.8(3) . . ? C135 C134 C133 118.9(3) . . ? C114 C113 C112 116.9(3) . . ? C114 C113 C103 122.7(3) . . ? C112 C113 C103 120.4(3) . . ? C105 C104 C103 104.8(3) . . ? C154 C153 C152 116.8(4) . . ? C154 C153 C143 121.5(3) . . ? C152 C153 C143 121.6(3) . . ? C145 C144 C143 105.2(3) . . ? C132 C133 C134 117.9(3) . . ? C132 C133 C123 120.8(3) . . ? C134 C133 C123 121.3(3) . . ? N131 C132 C133 124.0(3) . . ? C156 N151 C152 117.3(4) . . ? C115 C114 C113 119.1(4) . . ? N171 C176 C175 123.0(3) . . ? C175 C174 C173 119.3(3) . . ? N171 C172 C173 124.1(4) . . ? N121 B1 N101 110.5(3) . . ? N121 B1 N161 112.9(3) . . ? N101 B1 N161 108.3(2) . . ? N121 B1 N141 106.4(2) . . ? N101 B1 N141 111.6(2) . . ? N161 B1 N141 107.0(3) . . ? N141 C145 C144 108.2(3) . . ? N161 C165 C164 108.7(3) . . ? C125 C124 C123 104.9(3) . . ? C116 C115 C114 119.1(4) . . ? C176 C175 C174 119.1(4) . . ? N151 C152 C153 124.8(4) . . ? C153 C154 C155 119.5(4) . . ? N151 C156 C155 122.5(4) . . ? C154 C155 C156 118.7(5) . . ? C163 N162 N161 105.0(3) . . ? C132 N131 C136 116.7(3) . . ? N162 C163 C164 111.6(3) . . ? N162 C163 C173 121.0(3) . . ? C164 C163 C173 127.4(3) . . ? C116 N111 C112 117.2(3) . . ? N111 C112 C113 124.6(4) . . ? C165 C164 C163 104.3(3) . . ? N111 C116 C115 123.0(4) . . ? N131 C136 C135 124.1(4) . . ? C134 C135 C136 118.5(4) . . ? N102 Tl1 N122 64.77(8) . . ? N102 Tl1 N142 69.68(7) . . ? N122 Tl1 N142 82.07(7) . . ? N131 Tl1 N102 165.25(9) 2_566 . ? N131 Tl1 N122 100.99(8) 2_566 . ? N131 Tl1 N142 105.88(8) 2_566 . ? N111 Tl1 N102 71.32(9) 2_665 . ? N111 Tl1 N122 135.47(9) 2_665 . ? N111 Tl1 N142 76.17(9) 2_665 . ? N111 Tl1 N131 122.08(9) 2_665 2_566 ? N171 Tl1 N131 79.49(9) 1_465 2_566 ? N171 Tl1 N111 104.55(10) 1_465 2_665 ? N171 Tl1 N102 104.12(9) 1_465 . ? N171 Tl1 N122 93.09(9) 1_465 . ? N171 Tl1 N142 173.32(8) 1_465 . ? N141 Tl1 N102 65.05(7) . . ? N141 Tl1 N122 56.95(7) . . ? N141 Tl1 N142 25.44(7) . . ? N141 Tl1 N111 98.21(9) . 2_665 ? N141 Tl1 N131 104.64(8) . 2_566 ? N141 Tl1 N171 150.03(9) . 1_465 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.365 _refine_diff_density_min -1.420 _refine_diff_density_rms 0.190 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 0.00 1.00 0.0050 0.00 0.00 -1.00 0.0360 -3.00 9.00 -1.00 0.1910 3.00 -9.00 1.00 0.1890 -3.00 -2.00 -1.00 0.1270 3.00 2.00 1.00 0.1500 #=END data_CuTp4py _database_code_depnum_ccdc_archive 'CCDC 264762' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H19 B Cu N9' _chemical_formula_sum 'C24 H19 B Cu N9' _chemical_formula_weight 507.83 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' Cu Cu 0.3201 1.2651 '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 14.470(3) _cell_length_b 9.7387(17) _cell_length_c 17.593(3) _cell_angle_alpha 90.00 _cell_angle_beta 112.583(3) _cell_angle_gamma 90.00 _cell_volume 2289.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2743 _cell_measurement_theta_min 4.632 _cell_measurement_theta_max 48.113 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 0.987 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.6380 _exptl_absorpt_correction_T_max 0.9616 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 smart 1000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15501 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 27.52 _reflns_number_total 5172 _reflns_number_gt 3242 _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^)+(0.0313P)^2^+0.1740P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5172 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1220 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Cu1 Cu 0.52426(3) 0.90563(4) 0.81193(2) 0.02407(14) Uani 1 1 d . . . B1 B 0.3885(3) 0.9712(4) 0.6350(2) 0.0243(8) Uani 1 1 d . . . H1 H 0.3458 0.9848 0.5756 0.014(7) Uiso 1 1 d R . . N101 N 0.40544(19) 0.8148(3) 0.64701(15) 0.0222(6) Uani 1 1 d . . . N102 N 0.46740(19) 0.7602(3) 0.72056(15) 0.0215(6) Uani 1 1 d . . . C103 C 0.4645(2) 0.6234(3) 0.70908(19) 0.0231(7) Uani 1 1 d . . . C104 C 0.4008(2) 0.5902(3) 0.6291(2) 0.0277(8) Uani 1 1 d . . . H104 H 0.3853 0.5014 0.6053 0.033 Uiso 1 1 calc R . . C105 C 0.3653(2) 0.7136(3) 0.59222(19) 0.0275(8) Uani 1 1 d . . . H105 H 0.3198 0.7258 0.5369 0.033 Uiso 1 1 calc R . . N111 N 0.6298(2) 0.3461(3) 0.90220(18) 0.0371(8) Uani 1 1 d . . . C112 C 0.5419(3) 0.3141(4) 0.8435(2) 0.0382(9) Uani 1 1 d . . . H112 H 0.5155 0.2254 0.8455 0.046 Uiso 1 1 calc R . . C113 C 0.4861(3) 0.3995(3) 0.7800(2) 0.0338(8) Uani 1 1 d . . . H113 H 0.4235 0.3700 0.7406 0.041 Uiso 1 1 calc R . . C114 C 0.5229(2) 0.5291(3) 0.7746(2) 0.0239(7) Uani 1 1 d . . . C115 C 0.6166(3) 0.5629(3) 0.8332(2) 0.0282(8) Uani 1 1 d . . . H115 H 0.6460 0.6492 0.8309 0.034 Uiso 1 1 calc R . . C116 C 0.6668(3) 0.4702(4) 0.8949(2) 0.0363(9) Uani 1 1 d . . . H116 H 0.7308 0.4953 0.9341 0.044 Uiso 1 1 calc R . . N121 N 0.4892(2) 1.0449(3) 0.65664(16) 0.0231(6) Uani 1 1 d . . . N122 N 0.5651(2) 1.0312(2) 0.73217(15) 0.0211(6) Uani 1 1 d . . . C123 C 0.6389(2) 1.1146(3) 0.73147(19) 0.0216(7) Uani 1 1 d . . . C124 C 0.6100(3) 1.1822(3) 0.6554(2) 0.0335(9) Uani 1 1 d . . . H124 H 0.6477 1.2465 0.6386 0.040 Uiso 1 1 calc R . . C125 C 0.5157(3) 1.1351(3) 0.6110(2) 0.0323(9) Uani 1 1 d . . . H125 H 0.4753 1.1620 0.5563 0.039 Uiso 1 1 calc R . . N131 N 0.9155(2) 1.1621(3) 0.94013(17) 0.0344(7) Uani 1 1 d . . . C132 C 0.8771(3) 1.2606(4) 0.8839(2) 0.0359(9) Uani 1 1 d . . . H132 H 0.9127 1.3449 0.8918 0.043 Uiso 1 1 calc R . . C133 C 0.7896(3) 1.2487(3) 0.8152(2) 0.0316(8) Uani 1 1 d . . . H133 H 0.7678 1.3217 0.7766 0.038 Uiso 1 1 calc R . . C134 C 0.7334(2) 1.1287(3) 0.8030(2) 0.0231(7) Uani 1 1 d . . . C135 C 0.7725(2) 1.0256(3) 0.86086(18) 0.0236(7) Uani 1 1 d . . . H135 H 0.7374 0.9414 0.8554 0.028 Uiso 1 1 calc R . . C136 C 0.8626(3) 1.0454(4) 0.9267(2) 0.0310(8) Uani 1 1 d . . . H136 H 0.8884 0.9719 0.9644 0.037 Uiso 1 1 calc R . . N141 N 0.3367(2) 1.0281(3) 0.69059(15) 0.0234(6) Uani 1 1 d . . . N142 N 0.37892(19) 1.0080(3) 0.77348(15) 0.0230(6) Uani 1 1 d . . . C143 C 0.3288(2) 1.0922(3) 0.80515(19) 0.0227(7) Uani 1 1 d . . . C144 C 0.2554(3) 1.1657(3) 0.74303(19) 0.0303(8) Uani 1 1 d . . . H144 H 0.2100 1.2314 0.7488 0.036 Uiso 1 1 calc R . . C145 C 0.2634(2) 1.1221(3) 0.67190(19) 0.0269(8) Uani 1 1 d . . . H145 H 0.2236 1.1532 0.6180 0.032 Uiso 1 1 calc R . . N151 N 0.41242(19) 1.1018(2) 1.06737(16) 0.0222(6) Uani 1 1 d . . . C152 C 0.4119(2) 1.2168(3) 1.02387(19) 0.0256(8) Uani 1 1 d . . . H152 H 0.4324 1.3007 1.0530 0.031 Uiso 1 1 calc R . . C153 C 0.3832(2) 1.2185(3) 0.93916(19) 0.0257(8) Uani 1 1 d . . . H153 H 0.3817 1.3025 0.9113 0.031 Uiso 1 1 calc R . . C154 C 0.3565(2) 1.0964(3) 0.89512(19) 0.0209(7) Uani 1 1 d . . . C155 C 0.3568(2) 0.9784(3) 0.93942(19) 0.0238(7) Uani 1 1 d . . . H155 H 0.3395 0.8925 0.9119 0.029 Uiso 1 1 calc R . . C156 C 0.3818(2) 0.9854(3) 1.02267(19) 0.0237(7) Uani 1 1 d . . . H156 H 0.3775 0.9038 1.0507 0.028 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 Cu1 0.0234(3) 0.0252(2) 0.0191(2) 0.00162(17) 0.00312(17) 0.00141(17) B1 0.023(2) 0.030(2) 0.0180(19) 0.0004(16) 0.0056(17) 0.0039(16) N101 0.0165(15) 0.0263(14) 0.0196(14) -0.0035(12) 0.0021(12) 0.0005(11) N102 0.0170(15) 0.0233(14) 0.0206(14) -0.0004(11) 0.0033(12) 0.0001(11) C103 0.0195(19) 0.0228(17) 0.0283(18) -0.0012(13) 0.0108(15) -0.0022(13) C104 0.0225(19) 0.0269(18) 0.0304(19) -0.0099(15) 0.0063(16) -0.0061(14) C105 0.019(2) 0.036(2) 0.0220(18) -0.0045(15) 0.0011(15) -0.0028(15) N111 0.045(2) 0.0271(16) 0.0374(18) 0.0055(14) 0.0144(16) 0.0064(14) C112 0.038(3) 0.0220(18) 0.057(2) 0.0100(18) 0.021(2) 0.0006(16) C113 0.027(2) 0.0261(18) 0.046(2) -0.0031(17) 0.0109(18) -0.0025(15) C114 0.023(2) 0.0216(16) 0.0281(18) -0.0010(14) 0.0111(16) 0.0013(14) C115 0.032(2) 0.0226(17) 0.0256(19) -0.0041(14) 0.0057(17) -0.0023(14) C116 0.033(2) 0.031(2) 0.034(2) -0.0037(17) 0.0019(18) 0.0017(16) N121 0.0246(17) 0.0232(14) 0.0191(14) 0.0026(11) 0.0056(13) 0.0033(12) N122 0.0196(16) 0.0201(13) 0.0196(14) 0.0018(11) 0.0030(12) 0.0014(11) C123 0.0241(19) 0.0170(15) 0.0236(17) 0.0004(13) 0.0091(15) -0.0004(13) C124 0.037(2) 0.0293(19) 0.034(2) 0.0097(16) 0.0134(18) -0.0043(16) C125 0.041(2) 0.0327(19) 0.0218(18) 0.0088(15) 0.0106(17) 0.0079(16) N131 0.0304(19) 0.0435(19) 0.0282(16) -0.0050(14) 0.0102(14) -0.0100(14) C132 0.040(2) 0.038(2) 0.034(2) -0.0101(17) 0.0177(19) -0.0202(17) C133 0.040(2) 0.0276(18) 0.0281(19) 0.0012(15) 0.0147(18) -0.0059(16) C134 0.023(2) 0.0237(16) 0.0252(18) -0.0034(14) 0.0124(15) -0.0007(14) C135 0.022(2) 0.0216(17) 0.0242(18) -0.0014(14) 0.0062(15) -0.0023(14) C136 0.031(2) 0.038(2) 0.0237(18) 0.0016(15) 0.0100(17) 0.0002(16) N141 0.0191(16) 0.0272(14) 0.0186(14) 0.0016(12) 0.0013(12) 0.0061(11) N142 0.0214(16) 0.0271(15) 0.0170(14) -0.0002(11) 0.0034(12) 0.0050(12) C143 0.0157(18) 0.0252(16) 0.0235(17) 0.0018(14) 0.0034(14) 0.0017(13) C144 0.027(2) 0.0329(19) 0.0280(19) 0.0042(16) 0.0070(16) 0.0143(15) C145 0.023(2) 0.0331(19) 0.0183(17) 0.0056(14) 0.0009(15) 0.0106(14) N151 0.0177(15) 0.0201(13) 0.0272(15) 0.0033(12) 0.0067(12) 0.0044(11) C152 0.029(2) 0.0198(16) 0.0267(18) -0.0005(14) 0.0088(16) 0.0010(14) C153 0.029(2) 0.0213(17) 0.0259(18) 0.0092(14) 0.0093(16) 0.0078(14) C154 0.0131(17) 0.0271(17) 0.0217(16) 0.0016(14) 0.0059(13) 0.0036(13) C155 0.024(2) 0.0217(16) 0.0252(18) 0.0002(14) 0.0084(15) 0.0005(14) C156 0.0229(19) 0.0181(16) 0.0253(18) 0.0027(13) 0.0041(15) 0.0007(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 Cu1 N151 1.965(3) 3_677 ? Cu1 N102 2.062(2) . ? Cu1 N122 2.110(3) . ? Cu1 N142 2.187(3) . ? B1 N121 1.536(5) . ? B1 N101 1.545(4) . ? B1 N141 1.545(4) . ? B1 H1 0.9982 . ? N101 C105 1.344(4) . ? N101 N102 1.367(3) . ? N102 C103 1.346(4) . ? C103 C104 1.392(4) . ? C103 C114 1.463(4) . ? C104 C105 1.368(4) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? N111 C112 1.332(5) . ? N111 C116 1.348(4) . ? C112 C113 1.377(5) . ? C112 H112 0.9500 . ? C113 C114 1.387(4) . ? C113 H113 0.9500 . ? C114 C115 1.392(5) . ? C115 C116 1.383(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.342(4) . ? N121 N122 1.367(3) . ? N122 C123 1.346(4) . ? C123 C124 1.403(4) . ? C123 C134 1.466(4) . ? C124 C125 1.365(5) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? N131 C132 1.337(4) . ? N131 C136 1.339(4) . ? C132 C133 1.380(5) . ? C132 H132 0.9500 . ? C133 C134 1.392(4) . ? C133 H133 0.9500 . ? C134 C135 1.387(4) . ? C135 C136 1.385(4) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.343(4) . ? N141 N142 1.361(3) . ? N142 C143 1.349(4) . ? C143 C144 1.394(4) . ? C143 C154 1.477(4) . ? C144 C145 1.368(4) . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? N151 C156 1.354(4) . ? N151 C152 1.354(4) . ? N151 Cu1 1.965(3) 3_677 ? C152 C153 1.385(4) . ? C152 H152 0.9500 . ? C153 C154 1.390(4) . ? C153 H153 0.9500 . ? C154 C155 1.388(4) . ? C155 C156 1.369(4) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? 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 N151 Cu1 N102 134.27(10) 3_677 . ? N151 Cu1 N122 127.36(11) 3_677 . ? N102 Cu1 N122 90.54(10) . . ? N151 Cu1 N142 110.20(10) 3_677 . ? N102 Cu1 N142 91.36(10) . . ? N122 Cu1 N142 90.68(10) . . ? N121 B1 N101 110.0(3) . . ? N121 B1 N141 108.7(3) . . ? N101 B1 N141 110.9(3) . . ? N121 B1 H1 110.2 . . ? N101 B1 H1 106.0 . . ? N141 B1 H1 111.1 . . ? C105 N101 N102 109.8(3) . . ? C105 N101 B1 128.5(3) . . ? N102 N101 B1 121.7(2) . . ? C103 N102 N101 105.7(2) . . ? C103 N102 Cu1 141.0(2) . . ? N101 N102 Cu1 113.03(18) . . ? N102 C103 C104 110.6(3) . . ? N102 C103 C114 121.9(3) . . ? C104 C103 C114 127.5(3) . . ? C105 C104 C103 104.9(3) . . ? C105 C104 H104 127.5 . . ? C103 C104 H104 127.5 . . ? N101 C105 C104 108.9(3) . . ? N101 C105 H105 125.6 . . ? C104 C105 H105 125.6 . . ? C112 N111 C116 115.6(3) . . ? N111 C112 C113 125.1(3) . . ? N111 C112 H112 117.4 . . ? C113 C112 H112 117.4 . . ? C112 C113 C114 119.0(3) . . ? C112 C113 H113 120.5 . . ? C114 C113 H113 120.5 . . ? C113 C114 C115 117.0(3) . . ? C113 C114 C103 120.3(3) . . ? C115 C114 C103 122.6(3) . . ? C116 C115 C114 119.7(3) . . ? C116 C115 H115 120.1 . . ? C114 C115 H115 120.1 . . ? N111 C116 C115 123.5(3) . . ? N111 C116 H116 118.3 . . ? C115 C116 H116 118.3 . . ? C125 N121 N122 109.8(3) . . ? C125 N121 B1 128.3(3) . . ? N122 N121 B1 121.8(3) . . ? C123 N122 N121 106.0(2) . . ? C123 N122 Cu1 141.5(2) . . ? N121 N122 Cu1 112.17(19) . . ? N122 C123 C124 110.2(3) . . ? N122 C123 C134 122.1(3) . . ? C124 C123 C134 127.8(3) . . ? C125 C124 C123 104.8(3) . . ? C125 C124 H124 127.6 . . ? C123 C124 H124 127.6 . . ? N121 C125 C124 109.2(3) . . ? N121 C125 H125 125.4 . . ? C124 C125 H125 125.4 . . ? C132 N131 C136 115.6(3) . . ? N131 C132 C133 124.6(3) . . ? N131 C132 H132 117.7 . . ? C133 C132 H132 117.7 . . ? C132 C133 C134 119.5(3) . . ? C132 C133 H133 120.3 . . ? C134 C133 H133 120.3 . . ? C135 C134 C133 116.4(3) . . ? C135 C134 C123 123.0(3) . . ? C133 C134 C123 120.6(3) . . ? C136 C135 C134 120.1(3) . . ? C136 C135 H135 120.0 . . ? C134 C135 H135 120.0 . . ? N131 C136 C135 123.8(3) . . ? N131 C136 H136 118.1 . . ? C135 C136 H136 118.1 . . ? C145 N141 N142 110.3(2) . . ? C145 N141 B1 128.2(3) . . ? N142 N141 B1 120.0(3) . . ? C143 N142 N141 105.3(2) . . ? C143 N142 Cu1 139.1(2) . . ? N141 N142 Cu1 112.28(18) . . ? N142 C143 C144 110.9(3) . . ? N142 C143 C154 119.5(3) . . ? C144 C143 C154 129.6(3) . . ? C145 C144 C143 104.6(3) . . ? C145 C144 H144 127.7 . . ? C143 C144 H144 127.7 . . ? N141 C145 C144 108.9(3) . . ? N141 C145 H145 125.5 . . ? C144 C145 H145 125.5 . . ? C156 N151 C152 115.7(3) . . ? C156 N151 Cu1 120.6(2) . 3_677 ? C152 N151 Cu1 122.7(2) . 3_677 ? N151 C152 C153 123.5(3) . . ? N151 C152 H152 118.2 . . ? C153 C152 H152 118.2 . . ? C152 C153 C154 119.6(3) . . ? C152 C153 H153 120.2 . . ? C154 C153 H153 120.2 . . ? C155 C154 C153 117.1(3) . . ? C155 C154 C143 121.3(3) . . ? C153 C154 C143 121.6(3) . . ? C156 C155 C154 120.1(3) . . ? C156 C155 H155 119.9 . . ? C154 C155 H155 119.9 . . ? N151 C156 C155 123.8(3) . . ? N151 C156 H156 118.1 . . ? C155 C156 H156 118.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N121 B1 N101 C105 -124.4(3) . . . . ? N141 B1 N101 C105 115.4(3) . . . . ? N121 B1 N101 N102 56.0(4) . . . . ? N141 B1 N101 N102 -64.2(4) . . . . ? C105 N101 N102 C103 0.3(3) . . . . ? B1 N101 N102 C103 -180.0(3) . . . . ? C105 N101 N102 Cu1 -175.4(2) . . . . ? B1 N101 N102 Cu1 4.3(3) . . . . ? N151 Cu1 N102 C103 -11.0(4) 3_677 . . . ? N122 Cu1 N102 C103 137.9(4) . . . . ? N142 Cu1 N102 C103 -131.4(3) . . . . ? N151 Cu1 N102 N101 162.47(18) 3_677 . . . ? N122 Cu1 N102 N101 -48.6(2) . . . . ? N142 Cu1 N102 N101 42.1(2) . . . . ? N101 N102 C103 C104 -0.4(4) . . . . ? Cu1 N102 C103 C104 173.4(3) . . . . ? N101 N102 C103 C114 179.3(3) . . . . ? Cu1 N102 C103 C114 -6.9(5) . . . . ? N102 C103 C104 C105 0.3(4) . . . . ? C114 C103 C104 C105 -179.4(3) . . . . ? N102 N101 C105 C104 -0.2(4) . . . . ? B1 N101 C105 C104 -179.8(3) . . . . ? C103 C104 C105 N101 -0.1(4) . . . . ? C116 N111 C112 C113 -3.1(6) . . . . ? N111 C112 C113 C114 0.8(6) . . . . ? C112 C113 C114 C115 2.0(5) . . . . ? C112 C113 C114 C103 -178.6(3) . . . . ? N102 C103 C114 C113 147.0(3) . . . . ? C104 C103 C114 C113 -33.4(5) . . . . ? N102 C103 C114 C115 -33.6(5) . . . . ? C104 C103 C114 C115 146.0(3) . . . . ? C113 C114 C115 C116 -2.2(5) . . . . ? C103 C114 C115 C116 178.3(3) . . . . ? C112 N111 C116 C115 2.7(5) . . . . ? C114 C115 C116 N111 -0.1(5) . . . . ? N101 B1 N121 C125 127.5(3) . . . . ? N141 B1 N121 C125 -110.9(3) . . . . ? N101 B1 N121 N122 -56.9(4) . . . . ? N141 B1 N121 N122 64.6(4) . . . . ? C125 N121 N122 C123 -0.3(3) . . . . ? B1 N121 N122 C123 -176.6(3) . . . . ? C125 N121 N122 Cu1 174.5(2) . . . . ? B1 N121 N122 Cu1 -1.8(3) . . . . ? N151 Cu1 N122 C123 11.8(4) 3_677 . . . ? N102 Cu1 N122 C123 -140.5(3) . . . . ? N142 Cu1 N122 C123 128.1(3) . . . . ? N151 Cu1 N122 N121 -160.15(17) 3_677 . . . ? N102 Cu1 N122 N121 47.5(2) . . . . ? N142 Cu1 N122 N121 -43.82(19) . . . . ? N121 N122 C123 C124 0.2(3) . . . . ? Cu1 N122 C123 C124 -172.1(3) . . . . ? N121 N122 C123 C134 179.4(3) . . . . ? Cu1 N122 C123 C134 7.1(5) . . . . ? N122 C123 C124 C125 0.0(4) . . . . ? C134 C123 C124 C125 -179.2(3) . . . . ? N122 N121 C125 C124 0.3(4) . . . . ? B1 N121 C125 C124 176.3(3) . . . . ? C123 C124 C125 N121 -0.2(4) . . . . ? C136 N131 C132 C133 -0.3(5) . . . . ? N131 C132 C133 C134 2.3(6) . . . . ? C132 C133 C134 C135 -2.1(5) . . . . ? C132 C133 C134 C123 178.6(3) . . . . ? N122 C123 C134 C135 27.2(5) . . . . ? C124 C123 C134 C135 -153.8(3) . . . . ? N122 C123 C134 C133 -153.6(3) . . . . ? C124 C123 C134 C133 25.5(5) . . . . ? C133 C134 C135 C136 0.3(5) . . . . ? C123 C134 C135 C136 179.5(3) . . . . ? C132 N131 C136 C135 -1.7(5) . . . . ? C134 C135 C136 N131 1.8(5) . . . . ? N121 B1 N141 C145 100.0(4) . . . . ? N101 B1 N141 C145 -139.0(3) . . . . ? N121 B1 N141 N142 -64.7(4) . . . . ? N101 B1 N141 N142 56.3(4) . . . . ? C145 N141 N142 C143 0.4(3) . . . . ? B1 N141 N142 C143 167.6(3) . . . . ? C145 N141 N142 Cu1 -163.1(2) . . . . ? B1 N141 N142 Cu1 4.1(3) . . . . ? N151 Cu1 N142 C143 18.5(3) 3_677 . . . ? N102 Cu1 N142 C143 157.4(3) . . . . ? N122 Cu1 N142 C143 -112.1(3) . . . . ? N151 Cu1 N142 N141 173.78(19) 3_677 . . . ? N102 Cu1 N142 N141 -47.4(2) . . . . ? N122 Cu1 N142 N141 43.2(2) . . . . ? N141 N142 C143 C144 -0.2(4) . . . . ? Cu1 N142 C143 C144 156.1(3) . . . . ? N141 N142 C143 C154 -179.7(3) . . . . ? Cu1 N142 C143 C154 -23.4(5) . . . . ? N142 C143 C144 C145 0.0(4) . . . . ? C154 C143 C144 C145 179.4(3) . . . . ? N142 N141 C145 C144 -0.4(4) . . . . ? B1 N141 C145 C144 -166.2(3) . . . . ? C143 C144 C145 N141 0.2(4) . . . . ? C156 N151 C152 C153 -0.5(5) . . . . ? Cu1 N151 C152 C153 168.7(3) 3_677 . . . ? N151 C152 C153 C154 -2.5(5) . . . . ? C152 C153 C154 C155 2.3(5) . . . . ? C152 C153 C154 C143 -177.8(3) . . . . ? N142 C143 C154 C155 -56.2(4) . . . . ? C144 C143 C154 C155 124.4(4) . . . . ? N142 C143 C154 C153 123.9(3) . . . . ? C144 C143 C154 C153 -55.5(5) . . . . ? C153 C154 C155 C156 0.5(5) . . . . ? C143 C154 C155 C156 -179.4(3) . . . . ? C152 N151 C156 C155 3.5(5) . . . . ? Cu1 N151 C156 C155 -165.8(3) 3_677 . . . ? C154 C155 C156 N151 -3.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.521 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.084 #=END data_ReTp4py _database_code_depnum_ccdc_archive 'CCDC 264763' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H19 B N9 O3 Re' _chemical_formula_weight 714.52 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' _cell_length_a 14.468(2) _cell_length_b 14.468(2) _cell_length_c 8.0751(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1463.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 28392 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 4.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3135 _exptl_absorpt_correction_T_max 0.9208 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius KappaCCD' _diffrn_measurement_method '\F & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10655 _diffrn_reflns_av_R_equivalents 0.1957 _diffrn_reflns_av_sigmaI/netI 0.1086 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.20 _reflns_number_total 2173 _reflns_number_gt 1583 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0549P)^2^+5.8492P] 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 constr _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 0.05(4) _refine_ls_number_reflns 2173 _refine_ls_number_parameters 124 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0995 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.1715 _refine_ls_wR_factor_gt 0.1587 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.050 _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 C1 C 0.4752(11) 0.1668(10) 0.7193(17) 0.058(3) Uani 1 1 d . . . H1 H 0.4694 0.1621 0.6020 0.069 Uiso 1 1 calc R . . C2 C 0.3993(12) 0.0996(12) 0.8297(15) 0.053(3) Uani 1 1 d . . . H2 H 0.3308 0.0406 0.8060 0.064 Uiso 1 1 calc R . . C3 C 0.4450(11) 0.1370(11) 0.9833(16) 0.052(3) Uani 1 1 d . . . C4 C 0.3962(9) 0.0917(10) 1.149(3) 0.060(3) Uani 1 1 d . . . C5 C 0.3359(15) 0.122(2) 1.231(3) 0.105(7) Uani 1 1 d . . . H5 H 0.3254 0.1772 1.1857 0.126 Uiso 1 1 calc R . . C6 C 0.2891(17) 0.076(2) 1.377(3) 0.116(8) Uani 1 1 d . . . H6 H 0.2469 0.1003 1.4314 0.140 Uiso 1 1 calc R . . C7 C 0.355(2) -0.0310(16) 1.374(2) 0.114(9) Uani 1 1 d . . . H7 H 0.3640 -0.0857 1.4226 0.136 Uiso 1 1 calc R . . C8 C 0.4066(19) 0.0121(15) 1.219(2) 0.106(7) Uani 1 1 d . . . H8 H 0.4473 -0.0145 1.1658 0.127 Uiso 1 1 calc R . . C9 C 0.6543(11) 0.2194(11) 1.2950(17) 0.054(3) Uani 1 1 d . . . B1 B 0.6667 0.3333 0.762(4) 0.048(7) Uani 1 3 d S . . H1A H 0.6667 0.3333 0.6387 0.058 Uiso 1 3 calc SR . . N1 N 0.5585(9) 0.2398(9) 0.8046(12) 0.048(3) Uani 1 1 d . . . N2 N 0.5396(11) 0.2214(10) 0.9710(13) 0.057(3) Uani 1 1 d . . . N3 N 0.2998(14) -0.0028(14) 1.4484(18) 0.102(6) Uani 1 1 d . . . O1 O 0.6432(12) 0.1555(9) 1.3804(15) 0.100(4) Uani 1 1 d . . . Re1 Re 0.6667 0.3333 1.1452(3) 0.0534(3) Uani 1 3 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.079(9) 0.057(8) 0.039(6) -0.005(6) -0.011(7) 0.036(8) C2 0.061(9) 0.060(8) 0.033(6) 0.000(6) -0.002(6) 0.026(7) C3 0.053(8) 0.050(8) 0.038(6) 0.001(6) -0.005(6) 0.015(7) C4 0.059(7) 0.072(7) 0.036(6) 0.011(12) -0.011(11) 0.023(6) C5 0.089(13) 0.156(19) 0.096(15) 0.057(14) 0.038(11) 0.081(15) C6 0.120(16) 0.18(2) 0.070(14) 0.063(17) 0.036(13) 0.088(17) C7 0.19(3) 0.078(12) 0.043(11) 0.009(9) -0.041(14) 0.046(15) C8 0.16(2) 0.074(12) 0.064(11) 0.008(9) -0.015(12) 0.046(13) C9 0.078(10) 0.044(7) 0.039(7) -0.022(6) -0.025(7) 0.030(7) B1 0.026(6) 0.026(6) 0.09(2) 0.000 0.000 0.013(3) N1 0.055(6) 0.064(7) 0.020(4) -0.004(5) -0.009(5) 0.026(6) N2 0.083(9) 0.074(8) 0.032(5) -0.003(5) -0.006(6) 0.051(8) N3 0.100(12) 0.088(12) 0.042(8) 0.008(8) 0.012(8) -0.010(9) O1 0.182(13) 0.079(7) 0.057(7) -0.001(7) -0.035(9) 0.080(8) Re1 0.0652(4) 0.0652(4) 0.0297(3) 0.000 0.000 0.03262(18) _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 C1 N1 1.330(16) . ? C1 C2 1.371(19) . ? C1 H1 0.9500 . ? C2 C3 1.383(17) . ? C2 H2 0.9500 . ? C3 N2 1.305(17) . ? C3 C4 1.50(2) . ? C4 C5 1.33(2) . ? C4 C8 1.35(2) . ? C5 C6 1.36(2) . ? C5 H5 0.9500 . ? C6 N3 1.36(3) . ? C6 H6 0.9500 . ? C7 N3 1.22(3) . ? C7 C8 1.43(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 O1 1.099(16) . ? C9 Re1 1.979(15) . ? B1 N1 1.509(14) 2_655 ? B1 N1 1.509(14) . ? B1 N1 1.509(14) 3_665 ? B1 H1A 1.0000 . ? N1 N2 1.370(13) . ? N2 Re1 2.237(12) . ? Re1 C9 1.979(15) 2_655 ? Re1 C9 1.979(15) 3_665 ? Re1 N2 2.237(12) 2_655 ? Re1 N2 2.237(12) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 108.2(12) . . ? N1 C1 H1 125.9 . . ? C2 C1 H1 125.9 . . ? C1 C2 C3 104.4(12) . . ? C1 C2 H2 127.8 . . ? C3 C2 H2 127.8 . . ? N2 C3 C2 111.7(13) . . ? N2 C3 C4 121.3(12) . . ? C2 C3 C4 126.9(12) . . ? C5 C4 C8 117(2) . . ? C5 C4 C3 122.4(14) . . ? C8 C4 C3 120.8(17) . . ? C4 C5 C6 121(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? N3 C6 C5 123(2) . . ? N3 C6 H6 118.4 . . ? C5 C6 H6 118.4 . . ? N3 C7 C8 125(2) . . ? N3 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C4 C8 C7 118(2) . . ? C4 C8 H8 120.8 . . ? C7 C8 H8 120.8 . . ? O1 C9 Re1 176.8(15) . . ? N1 B1 N1 115.1(10) 2_655 . ? N1 B1 N1 115.1(10) 2_655 3_665 ? N1 B1 N1 115.1(10) . 3_665 ? N1 B1 H1A 103.0 2_655 . ? N1 B1 H1A 103.0 . . ? N1 B1 H1A 103.0 3_665 . ? C1 N1 N2 109.9(12) . . ? C1 N1 B1 135.8(16) . . ? N2 N1 B1 114.3(16) . . ? C3 N2 N1 105.7(11) . . ? C3 N2 Re1 136.6(10) . . ? N1 N2 Re1 117.7(10) . . ? C7 N3 C6 116.1(17) . . ? C9 Re1 C9 86.6(5) . 2_655 ? C9 Re1 C9 86.6(5) . 3_665 ? C9 Re1 C9 86.6(5) 2_655 3_665 ? C9 Re1 N2 94.1(5) . 2_655 ? C9 Re1 N2 94.7(4) 2_655 2_655 ? C9 Re1 N2 178.6(5) 3_665 2_655 ? C9 Re1 N2 94.7(4) . . ? C9 Re1 N2 178.6(5) 2_655 . ? C9 Re1 N2 94.1(5) 3_665 . ? N2 Re1 N2 84.6(5) 2_655 . ? C9 Re1 N2 178.6(5) . 3_665 ? C9 Re1 N2 94.1(5) 2_655 3_665 ? C9 Re1 N2 94.7(4) 3_665 3_665 ? N2 Re1 N2 84.6(5) 2_655 3_665 ? N2 Re1 N2 84.6(5) . 3_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.213 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.129 #=END data_ReTp2py _database_code_depnum_ccdc_archive 'CCDC 264764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H20 B N9 O3.50 Re' _chemical_formula_weight 723.53 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' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 11.364(3) _cell_length_b 11.364(3) _cell_length_c 11.951(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1336.6(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 ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 4.597 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4600 _exptl_absorpt_correction_T_max 0.6564 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8660 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2049 _reflns_number_gt 1722 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0346P)^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 2049 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0617 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _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 Re1 Re 0.3333 0.6667 0.19950(2) 0.02075(10) Uani 1 3 d S . . C1 C 0.4788(5) 0.6878(5) 0.2933(4) 0.0356(10) Uani 1 1 d . . . O1 O 0.5680(4) 0.7077(4) 0.3521(3) 0.0499(9) Uani 1 1 d . . . B1 B 0.3333 0.6667 -0.0742(7) 0.0247(16) Uani 1 3 d S . . H1 H 0.3333 0.6667 -0.179(5) 0.020(17) Uiso 1 3 d S . . N11 N 0.3356(3) 0.5411(3) -0.0306(3) 0.0256(7) Uani 1 1 d . . . N12 N 0.3375(3) 0.5182(3) 0.0816(3) 0.0254(7) Uani 1 1 d . . . C13 C 0.3264(4) 0.3949(4) 0.0918(3) 0.0272(9) Uani 1 1 d . . . C14 C 0.3198(4) 0.3399(4) -0.0136(4) 0.0305(9) Uani 1 1 d . . . H14 H 0.3125 0.2548 -0.0303 0.037 Uiso 1 1 calc R . . C15 C 0.3260(4) 0.4348(4) -0.0883(4) 0.0305(9) Uani 1 1 d . . . H15 H 0.3239 0.4268 -0.1675 0.037 Uiso 1 1 calc R . . N21 N 0.4174(4) 0.3983(4) 0.2777(3) 0.0464(10) Uani 1 1 d . . . C22 C 0.3212(4) 0.3270(4) 0.1988(3) 0.0297(9) Uani 1 1 d . . . C23 C 0.2258(4) 0.1932(4) 0.2114(4) 0.0328(10) Uani 1 1 d . . . H23 H 0.1598 0.1465 0.1549 0.039 Uiso 1 1 calc R . . C24 C 0.2270(5) 0.1273(5) 0.3075(4) 0.0438(12) Uani 1 1 d . . . H24 H 0.1627 0.0336 0.3169 0.053 Uiso 1 1 calc R . . C25 C 0.3203(6) 0.1957(6) 0.3897(4) 0.0535(14) Uani 1 1 d . . . H25 H 0.3204 0.1513 0.4570 0.064 Uiso 1 1 calc R . . C26 C 0.4146(6) 0.3315(6) 0.3724(4) 0.0505(13) Uani 1 1 d . . . H26 H 0.4798 0.3796 0.4291 0.061 Uiso 1 1 calc R . . O100 O 0.0000 0.0000 0.0000 0.141(6) Uani 1 6 d S . . 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 Re1 0.02237(11) 0.02237(11) 0.01750(13) 0.000 0.000 0.01118(6) C1 0.041(3) 0.036(3) 0.029(2) 0.0016(19) -0.001(2) 0.019(2) O1 0.047(2) 0.056(2) 0.048(2) -0.0001(17) -0.0218(18) 0.0273(18) B1 0.025(2) 0.025(2) 0.024(4) 0.000 0.000 0.0126(12) N11 0.0260(18) 0.0266(18) 0.0224(17) -0.0013(14) 0.0001(14) 0.0119(15) N12 0.0263(18) 0.0276(18) 0.0210(16) 0.0000(14) 0.0000(14) 0.0125(15) C13 0.024(2) 0.025(2) 0.034(2) 0.0006(17) 0.0009(17) 0.0140(18) C14 0.031(2) 0.026(2) 0.035(2) -0.0051(18) -0.0002(19) 0.0147(19) C15 0.027(2) 0.030(2) 0.034(2) -0.0054(18) -0.0011(18) 0.0143(19) N21 0.047(2) 0.047(3) 0.042(2) -0.0003(19) -0.004(2) 0.021(2) C22 0.030(2) 0.030(2) 0.033(2) -0.0001(18) 0.0030(18) 0.018(2) C23 0.027(2) 0.027(2) 0.040(3) -0.0004(19) 0.0034(19) 0.0105(19) C24 0.048(3) 0.031(3) 0.048(3) 0.013(2) 0.019(2) 0.016(2) C25 0.068(4) 0.060(4) 0.040(3) 0.019(3) 0.007(3) 0.038(3) C26 0.051(3) 0.061(4) 0.036(3) 0.002(2) -0.005(2) 0.026(3) O100 0.096(7) 0.096(7) 0.23(2) 0.000 0.000 0.048(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 Re1 C1 1.911(5) 2_665 ? Re1 C1 1.911(5) 3_565 ? Re1 C1 1.911(5) . ? Re1 N12 2.217(3) 3_565 ? Re1 N12 2.217(3) 2_665 ? Re1 N12 2.217(3) . ? C1 O1 1.159(5) . ? B1 N11 1.532(4) 3_565 ? B1 N11 1.532(4) 2_665 ? B1 N11 1.532(4) . ? N11 C15 1.347(5) . ? N11 N12 1.367(4) . ? N12 C13 1.349(5) . ? C13 C14 1.390(6) . ? C13 C22 1.480(6) . ? C14 C15 1.374(6) . ? N21 C26 1.354(6) . ? N21 C22 1.362(6) . ? C22 C23 1.365(6) . ? C23 C24 1.375(6) . ? C24 C25 1.366(7) . ? C25 C26 1.385(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 C1 Re1 C1 89.04(19) 2_665 3_565 ? C1 Re1 C1 89.04(19) 2_665 . ? C1 Re1 C1 89.04(19) 3_565 . ? C1 Re1 N12 90.14(16) 2_665 3_565 ? C1 Re1 N12 97.05(16) 3_565 3_565 ? C1 Re1 N12 173.84(16) . 3_565 ? C1 Re1 N12 97.05(16) 2_665 2_665 ? C1 Re1 N12 173.84(16) 3_565 2_665 ? C1 Re1 N12 90.14(16) . 2_665 ? N12 Re1 N12 83.89(13) 3_565 2_665 ? C1 Re1 N12 173.84(16) 2_665 . ? C1 Re1 N12 90.14(16) 3_565 . ? C1 Re1 N12 97.05(16) . . ? N12 Re1 N12 83.89(13) 3_565 . ? N12 Re1 N12 83.89(13) 2_665 . ? O1 C1 Re1 176.1(4) . . ? N11 B1 N11 109.0(3) 3_565 2_665 ? N11 B1 N11 109.0(3) 3_565 . ? N11 B1 N11 109.0(3) 2_665 . ? C15 N11 N12 109.5(3) . . ? C15 N11 B1 129.0(4) . . ? N12 N11 B1 121.3(4) . . ? C13 N12 N11 106.5(3) . . ? C13 N12 Re1 135.0(3) . . ? N11 N12 Re1 118.1(2) . . ? N12 C13 C14 110.0(4) . . ? N12 C13 C22 125.3(4) . . ? C14 C13 C22 124.7(4) . . ? C15 C14 C13 105.4(4) . . ? N11 C15 C14 108.7(4) . . ? C26 N21 C22 117.3(4) . . ? N21 C22 C23 122.7(4) . . ? N21 C22 C13 118.5(4) . . ? C23 C22 C13 118.6(4) . . ? C22 C23 C24 118.7(4) . . ? C25 C24 C23 120.4(4) . . ? C24 C25 C26 118.3(5) . . ? N21 C26 C25 122.5(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.922 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.122 #=END data_CdTp3py _database_code_depnum_ccdc_archive 'CCDC 264765' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30.50 H32.50 B Cd N10.50 O3.50' _chemical_formula_sum 'C30.50 H32.50 B Cd N10.50 O3.50' _chemical_formula_weight 725.38 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' Cd Cd -0.8075 1.2024 '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' _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 9.5334(13) _cell_length_b 13.7358(18) _cell_length_c 13.8959(19) _cell_angle_alpha 70.983(2) _cell_angle_beta 84.410(2) _cell_angle_gamma 70.248(2) _cell_volume 1619.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4351 _cell_measurement_theta_min 4.671 _cell_measurement_theta_max 50.665 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.8116 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18642 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.59 _reflns_number_total 7263 _reflns_number_gt 4861 _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^)+(0.0658P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7263 _refine_ls_number_parameters 422 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 Cd1 Cd 0.20513(4) 0.07558(3) 0.25712(2) 0.03180(12) Uani 1 1 d . . . B1 B 0.4289(6) 0.2029(5) 0.2873(4) 0.0384(13) Uani 1 1 d . . . H1 H 0.493(4) 0.245(3) 0.295(2) 0.011(9) Uiso 1 1 d . . . N101 N 0.5167(4) 0.1197(3) 0.2344(3) 0.0386(9) Uani 1 1 d . . . N102 N 0.4645(4) 0.0451(3) 0.2172(3) 0.0358(9) Uani 1 1 d . . . C103 C 0.5739(5) -0.0134(4) 0.1694(3) 0.0411(12) Uani 1 1 d . . . C104 C 0.6939(5) 0.0260(4) 0.1538(4) 0.0510(14) Uani 1 1 d . . . H104 H 0.7841 0.0012 0.1202 0.061 Uiso 1 1 calc R . . C105 C 0.6551(5) 0.1079(4) 0.1970(4) 0.0494(14) Uani 1 1 d . . . H105 H 0.7157 0.1494 0.2000 0.059 Uiso 1 1 calc R . . N111 N 0.4914(5) -0.2678(4) 0.1921(4) 0.0593(13) Uani 1 1 d . . . C112 C 0.4970(5) -0.1792(4) 0.2087(4) 0.0463(13) Uani 1 1 d . . . H112 H 0.4517 -0.1637 0.2684 0.056 Uiso 1 1 calc R . . C113 C 0.5652(5) -0.1077(4) 0.1443(3) 0.0427(12) Uani 1 1 d . . . C114 C 0.6317(6) -0.1310(5) 0.0573(4) 0.0626(17) Uani 1 1 d . . . H114 H 0.6806 -0.0849 0.0114 0.075 Uiso 1 1 calc R . . C115 C 0.6252(7) -0.2230(5) 0.0388(5) 0.071(2) Uani 1 1 d . . . H115 H 0.6682 -0.2407 -0.0205 0.085 Uiso 1 1 calc R . . C116 C 0.5549(7) -0.2880(5) 0.1087(5) 0.0660(18) Uani 1 1 d . . . H116 H 0.5520 -0.3512 0.0961 0.079 Uiso 1 1 calc R . . N121 N 0.2947(4) 0.2879(3) 0.2199(3) 0.0338(9) Uani 1 1 d . . . N122 N 0.1798(4) 0.2597(3) 0.1963(3) 0.0298(8) Uani 1 1 d . . . C123 C 0.0738(5) 0.3547(4) 0.1494(3) 0.0347(10) Uani 1 1 d . . . C124 C 0.1223(6) 0.4418(4) 0.1425(4) 0.0466(13) Uani 1 1 d . . . H124 H 0.0704 0.5172 0.1129 0.056 Uiso 1 1 calc R . . C125 C 0.2609(6) 0.3952(4) 0.1875(4) 0.0462(13) Uani 1 1 d . . . H125 H 0.3233 0.4339 0.1943 0.055 Uiso 1 1 calc R . . N131 N -0.3377(5) 0.4475(4) 0.1060(4) 0.0662(14) Uani 1 1 d . . . C132 C -0.2015(6) 0.4345(4) 0.1352(4) 0.0565(15) Uani 1 1 d . . . H132 H -0.1928 0.4797 0.1718 0.068 Uiso 1 1 calc R . . C133 C -0.0708(5) 0.3588(3) 0.1153(3) 0.0352(10) Uani 1 1 d . . . C134 C -0.0850(6) 0.2927(4) 0.0633(4) 0.0408(12) Uani 1 1 d . . . H134 H -0.0002 0.2385 0.0493 0.049 Uiso 1 1 calc R . . C135 C -0.2253(6) 0.3071(4) 0.0322(4) 0.0456(12) Uani 1 1 d . . . H135 H -0.2383 0.2634 -0.0047 0.055 Uiso 1 1 calc R . . C136 C -0.3464(6) 0.3849(4) 0.0546(4) 0.0498(13) Uani 1 1 d . . . H136 H -0.4419 0.3939 0.0315 0.060 Uiso 1 1 calc R . . N141 N 0.3730(4) 0.1476(3) 0.3913(3) 0.0312(8) Uani 1 1 d . . . N142 N 0.3069(4) 0.0698(3) 0.4045(3) 0.0303(8) Uani 1 1 d . . . C143 C 0.2702(4) 0.0411(3) 0.5027(3) 0.0290(9) Uani 1 1 d . . . C144 C 0.3101(5) 0.1010(3) 0.5531(3) 0.0336(10) Uani 1 1 d . . . H144 H 0.2958 0.0969 0.6228 0.040 Uiso 1 1 calc R . . C145 C 0.3741(5) 0.1664(4) 0.4807(4) 0.0372(11) Uani 1 1 d . . . H145 H 0.4132 0.2172 0.4914 0.045 Uiso 1 1 calc R . . N151 N 0.0249(4) -0.1154(3) 0.6554(3) 0.0294(8) Uani 1 1 d . . . C152 C 0.0933(4) -0.0402(3) 0.6171(3) 0.0280(9) Uani 1 1 d . . . C153 C 0.2012(4) -0.0454(3) 0.5425(3) 0.0286(9) Uani 1 1 d . . . C154 C 0.2376(5) -0.1336(3) 0.5060(3) 0.0316(10) Uani 1 1 d . . . H154 H 0.3098 -0.1402 0.4542 0.038 Uiso 1 1 calc R . . C155 C 0.1691(5) -0.2114(4) 0.5446(3) 0.0349(10) Uani 1 1 d . . . H155 H 0.1942 -0.2725 0.5207 0.042 Uiso 1 1 calc R . . C156 C 0.0633(5) -0.1990(4) 0.6187(3) 0.0334(10) Uani 1 1 d . . . H156 H 0.0156 -0.2527 0.6448 0.040 Uiso 1 1 calc R . . H152 H 0.0658 0.0189 0.6429 0.040 Uiso 1 1 d R . . O1 O 0.1389(4) 0.0400(3) 0.1167(3) 0.0469(8) Uani 1 1 d . . . O2 O 0.1654(4) -0.0852(3) 0.2665(3) 0.0452(8) Uani 1 1 d . . . C3 C 0.1382(5) -0.0529(4) 0.1737(4) 0.0397(11) Uani 1 1 d . . . C4 C 0.1095(6) -0.1284(4) 0.1261(5) 0.0651(17) Uani 1 1 d . . . H4B H 0.1996 -0.1915 0.1320 0.098 Uiso 1 1 calc R . . H4A H 0.0826 -0.0899 0.0541 0.098 Uiso 1 1 calc R . . H4C H 0.0275 -0.1530 0.1613 0.098 Uiso 1 1 calc R . . N1S N 0.0102(7) 0.5718(5) 0.3506(4) 0.0814(17) Uani 1 1 d D . . O1S O -0.0981(9) 0.4440(5) 0.3854(5) 0.126(2) Uani 1 1 d . . . C1S C 0.0130(12) 0.4731(7) 0.3869(6) 0.107(3) Uani 1 1 d D . . H1S H 0.1035 0.4189 0.4164 0.128 Uiso 1 1 calc R . . C2S C 0.1464(11) 0.6007(8) 0.3497(8) 0.146(4) Uani 1 1 d . . . H2SA H 0.1229 0.6797 0.3203 0.220 Uiso 1 1 calc R . . H2SC H 0.2224 0.5643 0.3088 0.220 Uiso 1 1 calc R . . H2SB H 0.1841 0.5772 0.4196 0.220 Uiso 1 1 calc R . . C3S C -0.1222(10) 0.6610(7) 0.2990(8) 0.142(4) Uani 1 1 d . . . H3SA H -0.1010 0.7299 0.2775 0.214 Uiso 1 1 calc R . . H3SB H -0.2061 0.6653 0.3459 0.214 Uiso 1 1 calc R . . H3SC H -0.1476 0.6470 0.2392 0.214 Uiso 1 1 calc R . . N2S N 0.5107(9) 0.4937(6) 0.4546(6) 0.045(2) Uiso 0.50 1 d PD A -1 O2S O 0.4675(9) 0.3359(7) 0.5342(6) 0.072(2) Uiso 0.50 1 d P A -1 C4S C 0.4688(19) 0.4262(12) 0.5287(12) 0.056(5) Uiso 0.50 1 d PD A -1 H4SA H 0.4344 0.4490 0.5868 0.068 Uiso 0.50 1 calc PR A -1 C5S C 0.5124(19) 0.5958(13) 0.4543(13) 0.052(5) Uiso 0.50 1 d P A -1 H5SA H 0.4873 0.6035 0.5221 0.077 Uiso 0.50 1 calc PR A -1 H5SB H 0.4391 0.6536 0.4043 0.077 Uiso 0.50 1 calc PR A -1 H5SC H 0.6119 0.6015 0.4361 0.077 Uiso 0.50 1 calc PR A -1 C6S C 0.5455(14) 0.4753(10) 0.3548(9) 0.065(3) Uiso 0.50 1 d P A -1 H6SA H 0.5412 0.4035 0.3597 0.097 Uiso 0.50 1 calc PR A -1 H6SB H 0.6457 0.4783 0.3347 0.097 Uiso 0.50 1 calc PR A -1 H6SC H 0.4726 0.5317 0.3037 0.097 Uiso 0.50 1 calc PR A -1 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 Cd1 0.02829(19) 0.0339(2) 0.03186(19) -0.00999(14) -0.00084(13) -0.00838(14) B1 0.035(3) 0.040(3) 0.038(3) -0.003(2) -0.004(2) -0.017(3) N101 0.029(2) 0.045(2) 0.033(2) -0.0019(18) -0.0010(17) -0.0109(18) N102 0.029(2) 0.041(2) 0.029(2) -0.0078(17) 0.0005(16) -0.0050(17) C103 0.030(3) 0.047(3) 0.027(2) 0.000(2) -0.0022(19) 0.001(2) C104 0.031(3) 0.060(4) 0.038(3) 0.000(3) 0.007(2) -0.001(2) C105 0.031(3) 0.057(3) 0.042(3) 0.008(3) -0.001(2) -0.014(2) N111 0.050(3) 0.052(3) 0.070(3) -0.028(3) -0.008(2) 0.003(2) C112 0.038(3) 0.044(3) 0.045(3) -0.019(3) -0.004(2) 0.006(2) C113 0.030(3) 0.049(3) 0.027(2) -0.007(2) -0.001(2) 0.011(2) C114 0.055(4) 0.069(4) 0.033(3) -0.011(3) 0.001(3) 0.014(3) C115 0.064(4) 0.074(4) 0.044(4) -0.031(3) -0.016(3) 0.032(3) C116 0.056(4) 0.064(4) 0.063(4) -0.032(3) -0.024(3) 0.017(3) N121 0.035(2) 0.034(2) 0.030(2) -0.0032(16) -0.0010(16) -0.0139(17) N122 0.032(2) 0.0279(19) 0.0273(19) -0.0067(15) -0.0020(15) -0.0075(16) C123 0.044(3) 0.033(3) 0.023(2) -0.0072(19) -0.0021(19) -0.007(2) C124 0.063(3) 0.027(3) 0.042(3) -0.003(2) -0.014(3) -0.008(2) C125 0.058(3) 0.039(3) 0.042(3) -0.002(2) -0.009(2) -0.025(3) N131 0.042(3) 0.064(3) 0.087(4) -0.040(3) -0.021(3) 0.012(2) C132 0.050(3) 0.048(3) 0.062(4) -0.024(3) -0.022(3) 0.009(3) C133 0.038(3) 0.029(2) 0.029(2) -0.0050(19) -0.005(2) -0.003(2) C134 0.046(3) 0.025(2) 0.043(3) -0.003(2) 0.000(2) -0.008(2) C135 0.050(3) 0.041(3) 0.051(3) -0.016(2) -0.006(2) -0.018(2) C136 0.046(3) 0.040(3) 0.059(3) -0.016(3) -0.016(3) -0.004(2) N141 0.0254(19) 0.036(2) 0.033(2) -0.0067(16) -0.0038(15) -0.0132(16) N142 0.0250(18) 0.038(2) 0.0266(19) -0.0075(16) 0.0003(15) -0.0110(16) C143 0.018(2) 0.031(2) 0.034(2) -0.0069(19) -0.0029(17) -0.0051(18) C144 0.032(2) 0.038(3) 0.029(2) -0.008(2) -0.0018(19) -0.010(2) C145 0.031(2) 0.037(3) 0.043(3) -0.012(2) -0.005(2) -0.011(2) N151 0.0264(19) 0.033(2) 0.0259(19) -0.0067(16) -0.0021(15) -0.0070(16) C152 0.022(2) 0.029(2) 0.031(2) -0.0087(19) -0.0047(17) -0.0053(18) C153 0.019(2) 0.033(2) 0.028(2) -0.0046(19) -0.0050(17) -0.0034(18) C154 0.025(2) 0.033(2) 0.032(2) -0.009(2) 0.0008(18) -0.0053(19) C155 0.036(3) 0.030(2) 0.038(3) -0.013(2) 0.001(2) -0.007(2) C156 0.029(2) 0.034(3) 0.035(3) -0.009(2) -0.0015(19) -0.009(2) O1 0.052(2) 0.041(2) 0.047(2) -0.0154(17) -0.0021(17) -0.0117(17) O2 0.047(2) 0.0387(19) 0.048(2) -0.0148(16) 0.0088(17) -0.0128(16) C3 0.031(3) 0.042(3) 0.048(3) -0.020(2) 0.010(2) -0.010(2) C4 0.062(4) 0.048(3) 0.095(5) -0.039(3) -0.007(3) -0.011(3) N1S 0.089(4) 0.071(4) 0.078(4) -0.021(3) -0.028(3) -0.012(3) O1S 0.185(7) 0.092(4) 0.125(5) -0.044(4) 0.011(5) -0.068(5) C1S 0.156(10) 0.076(6) 0.087(6) -0.026(5) 0.000(6) -0.034(6) C2S 0.140(9) 0.165(10) 0.144(9) -0.032(7) -0.047(7) -0.063(8) C3S 0.105(7) 0.090(7) 0.191(11) -0.031(7) -0.011(7) 0.011(5) _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 Cd1 N142 2.317(3) . ? Cd1 N122 2.324(3) . ? Cd1 O2 2.325(3) . ? Cd1 O1 2.349(3) . ? Cd1 N151 2.385(3) 2_556 ? Cd1 N102 2.405(4) . ? Cd1 C3 2.665(5) . ? B1 N101 1.526(7) . ? B1 N141 1.536(6) . ? B1 N121 1.546(6) . ? B1 H1 1.00(3) . ? N101 C105 1.347(6) . ? N101 N102 1.372(5) . ? N102 C103 1.349(6) . ? C103 C104 1.394(7) . ? C103 C113 1.476(7) . ? C104 C105 1.370(7) . ? C104 H104 0.9500 . ? C105 H105 0.9500 . ? N111 C116 1.322(7) . ? N111 C112 1.330(6) . ? C112 C113 1.390(7) . ? C112 H112 0.9500 . ? C113 C114 1.389(7) . ? C114 C115 1.392(9) . ? C114 H114 0.9500 . ? C115 C116 1.379(9) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.324(6) . ? N121 N122 1.378(5) . ? N122 C123 1.353(5) . ? C123 C124 1.395(6) . ? C123 C133 1.478(6) . ? C124 C125 1.369(7) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? N131 C136 1.311(6) . ? N131 C132 1.334(7) . ? C132 C133 1.398(7) . ? C132 H132 0.9500 . ? C133 C134 1.377(6) . ? C134 C135 1.376(7) . ? C134 H134 0.9500 . ? C135 C136 1.373(7) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.350(5) . ? N141 N142 1.370(5) . ? N142 C143 1.338(5) . ? C143 C144 1.397(6) . ? C143 C153 1.476(6) . ? C144 C145 1.361(6) . ? C144 H144 0.9500 . ? C145 H145 0.9500 . ? N151 C156 1.333(5) . ? N151 C152 1.344(5) . ? N151 Cd1 2.385(3) 2_556 ? C152 C153 1.389(6) . ? C152 H152 0.9401 . ? C153 C154 1.389(6) . ? C154 C155 1.372(6) . ? C154 H154 0.9500 . ? C155 C156 1.379(6) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? O1 C3 1.265(6) . ? O2 C3 1.242(6) . ? C3 C4 1.504(7) . ? C4 H4B 0.9800 . ? C4 H4A 0.9800 . ? C4 H4C 0.9800 . ? N1S C1S 1.276(8) . ? N1S C3S 1.472(9) . ? N1S C2S 1.478(10) . ? O1S C1S 1.256(11) . ? C1S H1S 0.9500 . ? C2S H2SA 0.9800 . ? C2S H2SC 0.9800 . ? C2S H2SB 0.9800 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? N2S C4S 1.276(8) . ? N2S C5S 1.407(18) . ? N2S C6S 1.476(13) . ? O2S C4S 1.222(17) . ? C4S H4SA 0.9500 . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? 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 N142 Cd1 N122 87.34(12) . . ? N142 Cd1 O2 113.84(12) . . ? N122 Cd1 O2 157.81(12) . . ? N142 Cd1 O1 166.82(12) . . ? N122 Cd1 O1 103.88(12) . . ? O2 Cd1 O1 56.11(12) . . ? N142 Cd1 N151 84.10(12) . 2_556 ? N122 Cd1 N151 90.32(12) . 2_556 ? O2 Cd1 N151 85.62(11) . 2_556 ? O1 Cd1 N151 102.47(12) . 2_556 ? N142 Cd1 N102 76.85(12) . . ? N122 Cd1 N102 85.61(12) . . ? O2 Cd1 N102 104.95(12) . . ? O1 Cd1 N102 96.85(12) . . ? N151 Cd1 N102 160.67(12) 2_556 . ? N142 Cd1 C3 140.98(14) . . ? N122 Cd1 C3 131.68(14) . . ? O2 Cd1 C3 27.77(13) . . ? O1 Cd1 C3 28.35(13) . . ? N151 Cd1 C3 94.68(13) 2_556 . ? N102 Cd1 C3 102.14(13) . . ? N101 B1 N141 111.3(4) . . ? N101 B1 N121 110.0(4) . . ? N141 B1 N121 109.5(4) . . ? N101 B1 H1 109(2) . . ? N141 B1 H1 111(2) . . ? N121 B1 H1 106(2) . . ? C105 N101 N102 109.5(4) . . ? C105 N101 B1 126.1(4) . . ? N102 N101 B1 124.4(4) . . ? C103 N102 N101 106.6(4) . . ? C103 N102 Cd1 140.0(3) . . ? N101 N102 Cd1 112.6(3) . . ? N102 C103 C104 109.4(5) . . ? N102 C103 C113 123.3(4) . . ? C104 C103 C113 127.2(5) . . ? C105 C104 C103 106.0(4) . . ? C105 C104 H104 127.0 . . ? C103 C104 H104 127.0 . . ? N101 C105 C104 108.5(5) . . ? N101 C105 H105 125.7 . . ? C104 C105 H105 125.7 . . ? C116 N111 C112 117.1(6) . . ? N111 C112 C113 124.2(5) . . ? N111 C112 H112 117.9 . . ? C113 C112 H112 117.9 . . ? C114 C113 C112 117.6(5) . . ? C114 C113 C103 120.8(5) . . ? C112 C113 C103 121.5(4) . . ? C113 C114 C115 118.7(6) . . ? C113 C114 H114 120.7 . . ? C115 C114 H114 120.7 . . ? C116 C115 C114 118.4(5) . . ? C116 C115 H115 120.8 . . ? C114 C115 H115 120.8 . . ? N111 C116 C115 124.1(6) . . ? N111 C116 H116 117.9 . . ? C115 C116 H116 117.9 . . ? C125 N121 N122 109.7(4) . . ? C125 N121 B1 127.9(4) . . ? N122 N121 B1 121.9(4) . . ? C123 N122 N121 105.8(3) . . ? C123 N122 Cd1 137.7(3) . . ? N121 N122 Cd1 116.1(2) . . ? N122 C123 C124 109.7(4) . . ? N122 C123 C133 122.3(4) . . ? C124 C123 C133 128.0(4) . . ? C125 C124 C123 105.2(4) . . ? C125 C124 H124 127.4 . . ? C123 C124 H124 127.4 . . ? N121 C125 C124 109.5(4) . . ? N121 C125 H125 125.2 . . ? C124 C125 H125 125.2 . . ? C136 N131 C132 116.5(5) . . ? N131 C132 C133 124.4(5) . . ? N131 C132 H132 117.8 . . ? C133 C132 H132 117.8 . . ? C134 C133 C132 117.3(5) . . ? C134 C133 C123 123.7(4) . . ? C132 C133 C123 119.1(4) . . ? C133 C134 C135 118.3(5) . . ? C133 C134 H134 120.9 . . ? C135 C134 H134 120.9 . . ? C136 C135 C134 119.8(5) . . ? C136 C135 H135 120.1 . . ? C134 C135 H135 120.1 . . ? N131 C136 C135 123.7(5) . . ? N131 C136 H136 118.2 . . ? C135 C136 H136 118.2 . . ? C145 N141 N142 109.2(3) . . ? C145 N141 B1 128.7(4) . . ? N142 N141 B1 122.1(4) . . ? C143 N142 N141 106.2(3) . . ? C143 N142 Cd1 133.3(3) . . ? N141 N142 Cd1 114.4(2) . . ? N142 C143 C144 110.5(4) . . ? N142 C143 C153 119.6(4) . . ? C144 C143 C153 129.9(4) . . ? C145 C144 C143 105.0(4) . . ? C145 C144 H144 127.5 . . ? C143 C144 H144 127.5 . . ? N141 C145 C144 109.2(4) . . ? N141 C145 H145 125.4 . . ? C144 C145 H145 125.4 . . ? C156 N151 C152 117.5(4) . . ? C156 N151 Cd1 118.7(3) . 2_556 ? C152 N151 Cd1 121.0(3) . 2_556 ? N151 C152 C153 123.7(4) . . ? N151 C152 H152 117.3 . . ? C153 C152 H152 119.0 . . ? C154 C153 C152 117.0(4) . . ? C154 C153 C143 122.2(4) . . ? C152 C153 C143 120.8(4) . . ? C155 C154 C153 120.0(4) . . ? C155 C154 H154 120.0 . . ? C153 C154 H154 120.0 . . ? C154 C155 C156 118.7(4) . . ? C154 C155 H155 120.6 . . ? C156 C155 H155 120.6 . . ? N151 C156 C155 123.1(4) . . ? N151 C156 H156 118.4 . . ? C155 C156 H156 118.4 . . ? C3 O1 Cd1 89.8(3) . . ? C3 O2 Cd1 91.5(3) . . ? O2 C3 O1 122.5(5) . . ? O2 C3 C4 119.0(5) . . ? O1 C3 C4 118.5(5) . . ? O2 C3 Cd1 60.7(3) . . ? O1 C3 Cd1 61.8(2) . . ? C4 C3 Cd1 176.8(3) . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? C3 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? C1S N1S C3S 122.6(8) . . ? C1S N1S C2S 120.8(8) . . ? C3S N1S C2S 116.3(7) . . ? O1S C1S N1S 123.1(9) . . ? O1S C1S H1S 118.4 . . ? N1S C1S H1S 118.4 . . ? N1S C2S H2SA 109.5 . . ? N1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? N1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? H2SC C2S H2SB 109.5 . . ? N1S C3S H3SA 109.5 . . ? N1S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? N1S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? C4S N2S C5S 125.1(14) . . ? C4S N2S C6S 121.1(12) . . ? C5S N2S C6S 113.4(9) . . ? O2S C4S N2S 128.1(16) . . ? O2S C4S H4SA 115.9 . . ? N2S C4S H4SA 115.9 . . ? N2S C5S H5SA 109.5 . . ? N2S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? N2S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? N2S C6S H6SA 109.5 . . ? N2S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? N2S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.232 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.104 #=END data_NiTp3py2 _database_code_depnum_ccdc_archive 'CCDC 264766' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ni(Tp3py)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H38 B2 N18 Ni' _chemical_formula_weight 947.29 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 10.401(2) _cell_length_b 19.256(4) _cell_length_c 10.599(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.23(3) _cell_angle_gamma 90.00 _cell_volume 2122.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 61597 _cell_measurement_theta_min 3.71 _cell_measurement_theta_max 28.18 _exptl_crystal_description Prismatic _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 0.519 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector CCD _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61597 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 28.18 _reflns_number_total 5185 _reflns_number_gt 4312 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0262P)^2^+1.3644P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5185 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0678 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 Ni1 Ni 0.5000 0.0000 0.0000 0.00972(7) Uani 1 2 d S . . N121 N 0.34555(10) -0.06132(6) 0.19752(11) 0.0123(2) Uani 1 1 d . . . N101 N 0.22649(10) 0.02579(6) 0.06356(11) 0.0132(2) Uani 1 1 d . . . N141 N 0.27439(10) -0.09322(6) -0.02337(11) 0.0129(2) Uani 1 1 d . . . C143 C 0.38384(13) -0.13332(7) -0.17944(13) 0.0135(3) Uani 1 1 d . . . C113 C 0.36266(13) 0.19437(7) -0.00153(13) 0.0140(3) Uani 1 1 d . . . C133 C 0.67917(13) -0.04859(7) 0.29890(13) 0.0143(3) Uani 1 1 d . . . C125 C 0.33450(14) -0.08544(8) 0.31581(13) 0.0182(3) Uani 1 1 d . . . H125 H 0.2575 -0.1011 0.3531 0.022 Uiso 1 1 calc R . . C123 C 0.53744(13) -0.05689(7) 0.28303(13) 0.0138(3) Uani 1 1 d . . . C155 C 0.68020(13) -0.12783(8) -0.38370(13) 0.0174(3) Uani 1 1 d . . . H155 H 0.7526 -0.0997 -0.4016 0.021 Uiso 1 1 calc R . . C114 C 0.46274(13) 0.19916(7) -0.08611(13) 0.0161(3) Uani 1 1 d . . . H114 H 0.4947 0.1586 -0.1257 0.019 Uiso 1 1 calc R . . C153 C 0.48616(13) -0.14851(7) -0.27040(13) 0.0141(3) Uani 1 1 d . . . C103 C 0.28733(13) 0.13137(7) 0.02663(13) 0.0136(3) Uani 1 1 d . . . C145 C 0.20297(13) -0.14416(7) -0.07573(14) 0.0170(3) Uani 1 1 d . . . H145 H 0.1212 -0.1591 -0.0481 0.020 Uiso 1 1 calc R . . C156 C 0.66282(14) -0.19106(8) -0.44366(15) 0.0224(3) Uani 1 1 d . . . H156 H 0.7247 -0.2056 -0.5027 0.027 Uiso 1 1 calc R . . C105 C 0.12373(13) 0.06637(7) 0.08433(14) 0.0172(3) Uani 1 1 d . . . H105 H 0.0418 0.0509 0.1106 0.021 Uiso 1 1 calc R . . C115 C 0.51548(14) 0.26348(7) -0.11222(14) 0.0186(3) Uani 1 1 d . . . H115 H 0.5833 0.2675 -0.1704 0.022 Uiso 1 1 calc R . . N131 N 0.85949(13) 0.01641(7) 0.38429(15) 0.0296(3) Uani 1 1 d . . . C144 C 0.26781(14) -0.17075(8) -0.17545(14) 0.0183(3) Uani 1 1 d . . . H144 H 0.2403 -0.2070 -0.2306 0.022 Uiso 1 1 calc R . . N151 N 0.56243(13) -0.23269(7) -0.42200(14) 0.0283(3) Uani 1 1 d . . . N111 N 0.37654(13) 0.31870(7) 0.03336(14) 0.0281(3) Uani 1 1 d . . . C152 C 0.47845(15) -0.21130(8) -0.33701(16) 0.0234(3) Uani 1 1 d . . . H152 H 0.4078 -0.2410 -0.3203 0.028 Uiso 1 1 calc R . . C104 C 0.15767(13) 0.13396(8) 0.06110(14) 0.0184(3) Uani 1 1 d . . . H104 H 0.1048 0.1740 0.0671 0.022 Uiso 1 1 calc R . . C134 C 0.76247(14) -0.10163(8) 0.26607(14) 0.0209(3) Uani 1 1 d . . . H134 H 0.7299 -0.1427 0.2274 0.025 Uiso 1 1 calc R . . C116 C 0.46845(15) 0.32177(8) -0.05271(16) 0.0227(3) Uani 1 1 d . . . H116 H 0.5029 0.3659 -0.0738 0.027 Uiso 1 1 calc R . . C154 C 0.59052(13) -0.10604(7) -0.29716(13) 0.0151(3) Uani 1 1 d . . . H154 H 0.6002 -0.0624 -0.2563 0.018 Uiso 1 1 calc R . . C132 C 0.73330(14) 0.00890(8) 0.35826(15) 0.0218(3) Uani 1 1 d . . . H132 H 0.6774 0.0454 0.3821 0.026 Uiso 1 1 calc R . . C124 C 0.45444(14) -0.08337(8) 0.37333(14) 0.0216(3) Uani 1 1 d . . . H124 H 0.4763 -0.0971 0.4572 0.026 Uiso 1 1 calc R . . C112 C 0.32646(15) 0.25616(8) 0.05707(15) 0.0225(3) Uani 1 1 d . . . H112 H 0.2613 0.2536 0.1184 0.027 Uiso 1 1 calc R . . B1 B 0.23937(14) -0.05195(8) 0.09460(15) 0.0131(3) Uani 1 1 d . . . H1 H 0.1559 -0.0695 0.1271 0.016 Uiso 1 1 calc R . . C136 C 0.93652(14) -0.03523(9) 0.34914(15) 0.0255(3) Uani 1 1 d . . . H136 H 1.0262 -0.0308 0.3661 0.031 Uiso 1 1 calc R . . C135 C 0.89340(15) -0.09431(9) 0.28993(15) 0.0255(3) Uani 1 1 d . . . H135 H 0.9519 -0.1295 0.2657 0.031 Uiso 1 1 calc R . . N142 N 0.38699(10) -0.08477(6) -0.08630(10) 0.0119(2) Uani 1 1 d . . . N122 N 0.47040(10) -0.04322(6) 0.17549(10) 0.0110(2) Uani 1 1 d . . . N102 N 0.32917(10) 0.06471(6) 0.02635(10) 0.0118(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 Ni1 0.00891(11) 0.01031(12) 0.00996(11) 0.00120(9) 0.00095(8) -0.00066(9) N121 0.0098(5) 0.0129(6) 0.0143(6) 0.0016(4) 0.0030(4) -0.0003(4) N101 0.0092(5) 0.0146(6) 0.0160(6) 0.0023(5) 0.0010(4) -0.0005(4) N141 0.0096(5) 0.0141(6) 0.0152(6) 0.0014(4) 0.0015(4) -0.0021(4) C143 0.0145(6) 0.0136(6) 0.0122(6) 0.0016(5) -0.0016(5) -0.0002(5) C113 0.0137(6) 0.0130(6) 0.0153(7) 0.0022(5) -0.0028(5) 0.0008(5) C133 0.0134(6) 0.0194(7) 0.0103(6) 0.0030(5) -0.0008(5) 0.0011(5) C125 0.0160(7) 0.0231(8) 0.0157(7) 0.0068(6) 0.0060(5) 0.0011(6) C123 0.0147(6) 0.0148(7) 0.0118(6) 0.0002(5) 0.0008(5) 0.0027(5) C155 0.0146(7) 0.0210(7) 0.0166(7) -0.0005(6) 0.0003(5) 0.0012(5) C114 0.0145(6) 0.0146(7) 0.0191(7) -0.0015(5) -0.0004(5) 0.0014(5) C153 0.0156(6) 0.0147(7) 0.0119(6) 0.0009(5) -0.0013(5) 0.0029(5) C103 0.0137(6) 0.0127(6) 0.0144(6) 0.0012(5) -0.0003(5) 0.0010(5) C145 0.0121(6) 0.0176(7) 0.0212(7) 0.0001(6) -0.0007(5) -0.0047(5) C156 0.0200(7) 0.0250(8) 0.0222(8) -0.0054(6) 0.0044(6) 0.0041(6) C105 0.0095(6) 0.0185(7) 0.0237(7) 0.0028(6) 0.0016(5) 0.0022(5) C115 0.0165(7) 0.0190(7) 0.0204(7) 0.0001(6) 0.0024(5) -0.0017(6) N131 0.0240(7) 0.0238(7) 0.0404(9) -0.0006(6) -0.0109(6) -0.0024(5) C144 0.0173(7) 0.0171(7) 0.0204(7) -0.0036(6) -0.0009(5) -0.0033(5) N151 0.0270(7) 0.0225(7) 0.0357(8) -0.0119(6) 0.0091(6) -0.0007(6) N111 0.0281(7) 0.0160(6) 0.0409(8) -0.0059(6) 0.0127(6) -0.0022(5) C152 0.0233(8) 0.0178(7) 0.0295(8) -0.0052(6) 0.0066(6) -0.0027(6) C104 0.0138(7) 0.0153(7) 0.0260(8) 0.0013(6) 0.0002(6) 0.0036(5) C134 0.0179(7) 0.0252(8) 0.0194(7) -0.0067(6) -0.0025(6) 0.0018(6) C116 0.0224(7) 0.0142(7) 0.0317(9) 0.0005(6) 0.0042(6) -0.0031(6) C154 0.0163(7) 0.0150(7) 0.0140(6) -0.0012(5) -0.0023(5) 0.0011(5) C132 0.0200(7) 0.0193(8) 0.0260(8) 0.0001(6) -0.0052(6) 0.0036(6) C124 0.0187(7) 0.0322(9) 0.0140(7) 0.0079(6) 0.0013(5) 0.0025(6) C112 0.0228(7) 0.0187(7) 0.0265(8) -0.0033(6) 0.0099(6) -0.0015(6) B1 0.0088(7) 0.0143(7) 0.0162(7) 0.0015(6) 0.0025(5) -0.0007(5) C136 0.0154(7) 0.0325(9) 0.0283(8) 0.0011(7) -0.0047(6) -0.0015(6) C135 0.0172(7) 0.0349(9) 0.0244(8) -0.0060(7) -0.0016(6) 0.0065(6) N142 0.0094(5) 0.0134(5) 0.0131(5) 0.0015(4) 0.0012(4) -0.0007(4) N122 0.0095(5) 0.0107(5) 0.0127(5) 0.0008(4) 0.0016(4) -0.0002(4) N102 0.0098(5) 0.0131(5) 0.0126(5) 0.0020(4) 0.0006(4) -0.0015(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 Ni1 N122 2.0668(12) . ? Ni1 N122 2.0668(12) 3_655 ? Ni1 N102 2.1930(11) . ? Ni1 N102 2.1930(11) 3_655 ? Ni1 N142 2.1992(12) 3_655 ? Ni1 N142 2.1992(12) . ? N121 C125 1.3442(18) . ? N121 N122 1.3694(15) . ? N121 B1 1.5461(19) . ? N101 C105 1.3459(18) . ? N101 N102 1.3696(15) . ? N101 B1 1.538(2) . ? N141 C145 1.3433(18) . ? N141 N142 1.3698(16) . ? N141 B1 1.5321(19) . ? C143 N142 1.3595(18) . ? C143 C144 1.4071(19) . ? C143 C153 1.4804(19) . ? C113 C114 1.391(2) . ? C113 C112 1.398(2) . ? C113 C103 1.4781(19) . ? C133 C132 1.387(2) . ? C133 C134 1.388(2) . ? C133 C123 1.4887(19) . ? C125 C124 1.377(2) . ? C123 N122 1.3493(18) . ? C123 C124 1.399(2) . ? C155 C156 1.384(2) . ? C155 C154 1.387(2) . ? C114 C115 1.385(2) . ? C153 C154 1.393(2) . ? C153 C152 1.402(2) . ? C103 N102 1.3553(17) . ? C103 C104 1.4056(19) . ? C145 C144 1.366(2) . ? C156 N151 1.340(2) . ? C105 C104 1.372(2) . ? C115 C116 1.382(2) . ? N131 C136 1.335(2) . ? N131 C132 1.343(2) . ? N151 C152 1.333(2) . ? N111 C116 1.337(2) . ? N111 C112 1.338(2) . ? C134 C135 1.387(2) . ? C136 C135 1.370(2) . ? 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 N122 Ni1 N122 180.00(8) . 3_655 ? N122 Ni1 N102 88.71(5) . . ? N122 Ni1 N102 91.29(5) 3_655 . ? N122 Ni1 N102 91.29(5) . 3_655 ? N122 Ni1 N102 88.71(5) 3_655 3_655 ? N102 Ni1 N102 180.00(8) . 3_655 ? N122 Ni1 N142 90.76(4) . 3_655 ? N122 Ni1 N142 89.24(4) 3_655 3_655 ? N102 Ni1 N142 87.28(4) . 3_655 ? N102 Ni1 N142 92.72(4) 3_655 3_655 ? N122 Ni1 N142 89.24(4) . . ? N122 Ni1 N142 90.76(4) 3_655 . ? N102 Ni1 N142 92.72(4) . . ? N102 Ni1 N142 87.28(4) 3_655 . ? N142 Ni1 N142 180.00(7) 3_655 . ? C125 N121 N122 110.33(11) . . ? C125 N121 B1 128.63(11) . . ? N122 N121 B1 121.04(11) . . ? C105 N101 N102 110.87(11) . . ? C105 N101 B1 126.58(11) . . ? N102 N101 B1 121.96(10) . . ? C145 N141 N142 110.89(11) . . ? C145 N141 B1 125.23(11) . . ? N142 N141 B1 123.81(11) . . ? N142 C143 C144 109.74(12) . . ? N142 C143 C153 127.03(12) . . ? C144 C143 C153 123.18(13) . . ? C114 C113 C112 116.26(13) . . ? C114 C113 C103 126.27(13) . . ? C112 C113 C103 117.39(12) . . ? C132 C133 C134 116.84(13) . . ? C132 C133 C123 121.89(13) . . ? C134 C133 C123 120.96(13) . . ? N121 C125 C124 107.94(12) . . ? N122 C123 C124 109.50(12) . . ? N122 C123 C133 124.54(12) . . ? C124 C123 C133 125.88(13) . . ? C156 C155 C154 119.14(13) . . ? C115 C114 C113 119.54(13) . . ? C154 C153 C152 116.12(13) . . ? C154 C153 C143 126.21(13) . . ? C152 C153 C143 117.67(13) . . ? N102 C103 C104 110.13(12) . . ? N102 C103 C113 127.25(12) . . ? C104 C103 C113 122.62(12) . . ? N141 C145 C144 108.40(12) . . ? N151 C156 C155 122.84(14) . . ? N101 C105 C104 108.24(12) . . ? C116 C115 C114 119.31(13) . . ? C136 N131 C132 116.88(14) . . ? C145 C144 C143 105.62(13) . . ? C152 N151 C156 117.08(13) . . ? C116 N111 C112 117.06(13) . . ? N151 C152 C153 125.14(14) . . ? C105 C104 C103 105.36(12) . . ? C135 C134 C133 119.67(14) . . ? N111 C116 C115 122.73(14) . . ? C155 C154 C153 119.66(13) . . ? N131 C132 C133 124.36(14) . . ? C125 C124 C123 105.91(13) . . ? N111 C112 C113 124.97(14) . . ? N141 B1 N101 110.57(11) . . ? N141 B1 N121 109.67(11) . . ? N101 B1 N121 108.80(11) . . ? N131 C136 C135 123.62(14) . . ? C136 C135 C134 118.59(15) . . ? C143 N142 N141 105.33(11) . . ? C143 N142 Ni1 144.76(9) . . ? N141 N142 Ni1 109.91(8) . . ? C123 N122 N121 106.32(11) . . ? C123 N122 Ni1 138.98(9) . . ? N121 N122 Ni1 114.59(8) . . ? C103 N102 N101 105.38(10) . . ? C103 N102 Ni1 143.08(9) . . ? N101 N102 Ni1 111.39(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.311 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.052 #=END data_AgTkp4py _database_code_depnum_ccdc_archive 'CCDC 264767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AgTkp4py.3DMF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H45 Ag B N15 O3' _chemical_formula_weight 914.60 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' Ag Ag -0.8971 1.1015 '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 13.2535(2) _cell_length_b 14.0184(3) _cell_length_c 14.1607(3) _cell_angle_alpha 87.643(1) _cell_angle_beta 68.305(1) _cell_angle_gamma 62.109(1) _cell_volume 2132.62(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 24166 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 25.69 _exptl_crystal_description Needle _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.8433 _exptl_absorpt_correction_T_max 0.9778 _exptl_absorpt_process_details 'XPREP (Siemens, 1994)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_detector CCD _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24150 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 25.69 _reflns_number_total 7921 _reflns_number_gt 6635 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0972P)^2^+4.6117P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7921 _refine_ls_number_parameters 564 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1691 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Ag1 Ag 0.07142(3) 0.09121(3) 0.18831(2) 0.03072(14) Uani 1 1 d . . . O1 O 0.3048(7) 0.4486(6) 0.3583(6) 0.123(3) Uani 1 1 d . . . O2 O 0.4091(8) 0.5993(7) -0.0563(5) 0.118(2) Uani 1 1 d . . . O3 O 0.5609(6) 0.3014(5) 0.7368(5) 0.101(2) Uani 1 1 d . . . N101 N 0.0217(3) 0.3363(3) 0.1454(3) 0.0235(7) Uani 1 1 d . . . N102 N -0.0034(3) 0.2608(3) 0.1185(3) 0.0238(7) Uani 1 1 d . . . N111 N -0.0412(4) 0.0429(3) -0.1286(3) 0.0293(8) Uani 1 1 d . . . N141 N 0.1642(3) 0.2705(3) 0.2396(3) 0.0253(8) Uani 1 1 d . . . N142 N 0.2624(3) 0.2458(3) 0.1477(3) 0.0267(8) Uani 1 1 d . . . N151 N 0.7187(3) 0.0001(3) -0.0861(3) 0.0311(8) Uani 1 1 d . . . N121 N -0.0566(3) 0.3157(3) 0.3365(3) 0.0256(8) Uani 1 1 d . . . N122 N -0.0416(3) 0.2127(3) 0.3345(3) 0.0262(8) Uani 1 1 d . . . N131 N -0.1325(5) -0.0865(4) 0.4938(4) 0.0500(12) Uani 1 1 d . . . N161 N -0.0080(3) 0.4661(3) 0.2815(3) 0.0262(8) Uani 1 1 d . . . N162 N -0.1144(3) 0.5472(3) 0.2759(3) 0.0259(8) Uani 1 1 d . . . N171 N -0.4496(4) 0.9452(3) 0.3435(4) 0.0441(11) Uani 1 1 d . . . N13 N 0.4840(6) 0.2872(6) 0.3204(5) 0.0820(19) Uani 1 1 d . . . N14 N 0.2840(7) 0.6044(7) 0.1110(6) 0.091(2) Uani 1 1 d . . . N15 N 0.4202(7) 0.4566(6) 0.7133(7) 0.093(2) Uani 1 1 d . . . C105 C 0.0584(4) 0.3829(4) 0.0639(3) 0.0297(10) Uani 1 1 d . . . H105 H 0.0814 0.4376 0.0641 0.036 Uiso 1 1 calc R . . C104 C 0.0567(4) 0.3378(3) -0.0196(3) 0.0294(9) Uani 1 1 d . . . H104 H 0.0780 0.3542 -0.0876 0.035 Uiso 1 1 calc R . . C103 C 0.0168(4) 0.2624(3) 0.0183(3) 0.0240(9) Uani 1 1 d . . . C114 C -0.0040(4) 0.1887(3) -0.0337(3) 0.0251(9) Uani 1 1 d . . . C113 C 0.0746(4) 0.1349(4) -0.1340(3) 0.0292(9) Uani 1 1 d . . . H113 H 0.1420 0.1475 -0.1721 0.035 Uiso 1 1 calc R . . C112 C 0.0539(4) 0.0632(4) -0.1777(3) 0.0308(10) Uani 1 1 d . . . H112 H 0.1095 0.0262 -0.2459 0.037 Uiso 1 1 calc R . . C116 C -0.1178(4) 0.0963(4) -0.0321(4) 0.0315(10) Uani 1 1 d . . . H116 H -0.1860 0.0842 0.0037 0.038 Uiso 1 1 calc R . . C115 C -0.1023(4) 0.1680(4) 0.0175(3) 0.0291(9) Uani 1 1 d . . . H115 H -0.1583 0.2030 0.0862 0.035 Uiso 1 1 calc R . . C145 C 0.2037(4) 0.2147(4) 0.3103(3) 0.0305(10) Uani 1 1 d . . . H145 H 0.1525 0.2187 0.3795 0.037 Uiso 1 1 calc R . . C144 C 0.3292(4) 0.1521(4) 0.2653(4) 0.0298(9) Uani 1 1 d . . . H144 H 0.3831 0.1043 0.2957 0.036 Uiso 1 1 calc R . . C143 C 0.3621(4) 0.1736(3) 0.1637(3) 0.0272(9) Uani 1 1 d . . . C154 C 0.4845(4) 0.1188(4) 0.0777(3) 0.0276(9) Uani 1 1 d . . . C155 C 0.5770(4) 0.0192(4) 0.0861(4) 0.0322(10) Uani 1 1 d . . . H155 H 0.5626 -0.0096 0.1487 0.039 Uiso 1 1 calc R . . C156 C 0.6895(4) -0.0368(4) 0.0030(4) 0.0332(10) Uani 1 1 d . . . H156 H 0.7496 -0.1056 0.0096 0.040 Uiso 1 1 calc R . . C152 C 0.6303(4) 0.0967(4) -0.0939(4) 0.0322(10) Uani 1 1 d . . . H152 H 0.6491 0.1248 -0.1565 0.039 Uiso 1 1 calc R . . C153 C 0.5136(4) 0.1573(4) -0.0156(4) 0.0322(10) Uani 1 1 d . . . H153 H 0.4541 0.2243 -0.0255 0.039 Uiso 1 1 calc R . . C125 C -0.1456(4) 0.3772(4) 0.4294(3) 0.0323(10) Uani 1 1 d . . . H125 H -0.1723 0.4515 0.4507 0.039 Uiso 1 1 calc R . . C124 C -0.1898(4) 0.3136(4) 0.4864(4) 0.0350(11) Uani 1 1 d . . . H124 H -0.2533 0.3348 0.5538 0.042 Uiso 1 1 calc R . . C123 C -0.1220(4) 0.2107(4) 0.4247(3) 0.0282(9) Uani 1 1 d . . . C134 C -0.1260(4) 0.1096(4) 0.4471(4) 0.0325(10) Uani 1 1 d . . . C133 C -0.0273(5) 0.0076(4) 0.3960(3) 0.0341(10) Uani 1 1 d . . . H133 H 0.0458 0.0020 0.3434 0.041 Uiso 1 1 calc R . . C132 C -0.0339(6) -0.0872(4) 0.4209(4) 0.0400(12) Uani 1 1 d . . . H132 H 0.0355 -0.1558 0.3839 0.048 Uiso 1 1 calc R . . C136 C -0.2261(6) 0.0099(5) 0.5432(5) 0.0552(16) Uani 1 1 d . . . H136 H -0.2974 0.0122 0.5957 0.066 Uiso 1 1 calc R . . C135 C -0.2288(5) 0.1099(5) 0.5242(5) 0.0474(13) Uani 1 1 d . . . H135 H -0.2996 0.1769 0.5633 0.057 Uiso 1 1 calc R . . C165 C 0.0349(4) 0.5061(4) 0.3340(4) 0.0334(10) Uani 1 1 d . . . H165 H 0.1071 0.4650 0.3480 0.040 Uiso 1 1 calc R . . C164 C -0.0442(5) 0.6163(4) 0.3632(4) 0.0363(11) Uani 1 1 d . . . H164 H -0.0388 0.6667 0.4012 0.044 Uiso 1 1 calc R . . C163 C -0.1359(4) 0.6385(3) 0.3245(3) 0.0261(9) Uani 1 1 d . . . C174 C -0.2435(4) 0.7430(4) 0.3307(3) 0.0279(9) Uani 1 1 d . . . C175 C -0.3217(5) 0.7510(4) 0.2836(4) 0.0345(10) Uani 1 1 d . . . H175 H -0.3061 0.6881 0.2453 0.041 Uiso 1 1 calc R . . C176 C -0.4221(5) 0.8513(4) 0.2932(4) 0.0438(12) Uani 1 1 d . . . H176 H -0.4757 0.8543 0.2621 0.053 Uiso 1 1 calc R . . C172 C -0.3738(5) 0.9363(4) 0.3884(4) 0.0415(12) Uani 1 1 d . . . H172 H -0.3906 1.0010 0.4249 0.050 Uiso 1 1 calc R . . C173 C -0.2726(5) 0.8394(4) 0.3856(4) 0.0339(10) Uani 1 1 d . . . H173 H -0.2232 0.8382 0.4205 0.041 Uiso 1 1 calc R . . C33 C 0.4105(8) 0.3775(7) 0.2955(8) 0.091(3) Uani 1 1 d . . . H33 H 0.4388 0.3897 0.2264 0.110 Uiso 1 1 calc R . . C34 C 0.4403(12) 0.2624(10) 0.4221(8) 0.145(6) Uani 1 1 d . . . H34A H 0.4865 0.2685 0.4598 0.217 Uiso 1 1 calc R . . H34B H 0.4530 0.1878 0.4174 0.217 Uiso 1 1 calc R . . H34C H 0.3514 0.3140 0.4586 0.217 Uiso 1 1 calc R . . C35 C 0.5991(8) 0.2032(7) 0.2461(9) 0.099(3) Uani 1 1 d . . . H35A H 0.6167 0.2282 0.1792 0.148 Uiso 1 1 calc R . . H35B H 0.5927 0.1370 0.2398 0.148 Uiso 1 1 calc R . . H35C H 0.6664 0.1869 0.2683 0.148 Uiso 1 1 calc R . . C36 C 0.3569(9) 0.6369(8) 0.0361(7) 0.089(3) Uani 1 1 d . . . H36 H 0.3681 0.6934 0.0574 0.107 Uiso 1 1 calc R . . C37 C 0.2288(9) 0.6604(7) 0.2082(7) 0.092(3) Uani 1 1 d . . . H37A H 0.2806 0.6881 0.2176 0.137 Uiso 1 1 calc R . . H37B H 0.2193 0.6116 0.2582 0.137 Uiso 1 1 calc R . . H37C H 0.1468 0.7219 0.2188 0.137 Uiso 1 1 calc R . . C38 C 0.2573(10) 0.5243(8) 0.0791(8) 0.099(3) Uani 1 1 d . . . H38A H 0.2584 0.4734 0.1287 0.149 Uiso 1 1 calc R . . H38B H 0.3205 0.4837 0.0108 0.149 Uiso 1 1 calc R . . H38C H 0.1751 0.5620 0.0762 0.149 Uiso 1 1 calc R . . C39 C 0.4872(8) 0.3906(7) 0.7644(8) 0.089(3) Uani 1 1 d . . . H39 H 0.4709 0.4220 0.8301 0.106 Uiso 1 1 calc R . . C40 C 0.4497(12) 0.4125(10) 0.6090(8) 0.121(4) Uani 1 1 d . . . H40A H 0.5142 0.3355 0.5923 0.181 Uiso 1 1 calc R . . H40B H 0.4800 0.4540 0.5600 0.181 Uiso 1 1 calc R . . H40C H 0.3748 0.4186 0.6049 0.181 Uiso 1 1 calc R . . C41A C 0.3178(12) 0.5664(9) 0.7555(12) 0.064(4) Uani 0.50 1 d P . . B1 B 0.0309(4) 0.3461(4) 0.2497(4) 0.0242(10) Uani 1 1 d . . . C41B C 0.2818(13) 0.4929(12) 0.7925(15) 0.079(5) Uani 0.50 1 d P . . 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 Ag1 0.0332(2) 0.02347(19) 0.0264(2) 0.00258(13) -0.00405(14) -0.01264(15) O1 0.084(5) 0.113(5) 0.121(6) -0.007(5) -0.016(4) -0.026(4) O2 0.137(6) 0.140(6) 0.076(4) 0.013(4) -0.023(4) -0.079(5) O3 0.102(5) 0.054(3) 0.128(5) -0.009(3) -0.057(4) -0.014(3) N101 0.0222(18) 0.0184(16) 0.0256(18) 0.0036(14) -0.0074(14) -0.0083(14) N102 0.0231(18) 0.0192(16) 0.0261(18) 0.0054(14) -0.0086(14) -0.0091(14) N111 0.034(2) 0.0253(18) 0.0262(18) 0.0040(15) -0.0105(16) -0.0135(16) N141 0.0238(18) 0.0250(17) 0.0237(17) 0.0072(15) -0.0059(15) -0.0121(15) N142 0.0227(18) 0.0250(17) 0.0253(18) 0.0038(15) -0.0038(15) -0.0106(15) N151 0.0250(19) 0.0289(19) 0.037(2) 0.0050(17) -0.0089(16) -0.0139(16) N121 0.0240(18) 0.0236(17) 0.0234(17) 0.0028(14) -0.0063(15) -0.0095(15) N122 0.0267(19) 0.0264(18) 0.0260(18) 0.0064(15) -0.0083(15) -0.0150(15) N131 0.064(3) 0.060(3) 0.058(3) 0.030(3) -0.036(3) -0.047(3) N161 0.0229(18) 0.0231(17) 0.0268(18) 0.0016(15) -0.0072(15) -0.0086(15) N162 0.0251(19) 0.0216(17) 0.0278(18) 0.0030(15) -0.0092(15) -0.0097(15) N171 0.041(2) 0.030(2) 0.048(3) 0.0053(19) -0.016(2) -0.0076(19) N13 0.071(4) 0.072(4) 0.071(4) 0.012(3) -0.011(3) -0.024(3) N14 0.071(4) 0.128(6) 0.083(5) 0.003(4) -0.017(4) -0.065(5) N15 0.080(5) 0.076(4) 0.131(7) 0.005(4) -0.049(5) -0.036(4) C105 0.035(2) 0.025(2) 0.031(2) 0.0094(18) -0.0118(19) -0.0174(19) C104 0.032(2) 0.026(2) 0.027(2) 0.0059(18) -0.0088(18) -0.0135(19) C103 0.023(2) 0.0203(19) 0.024(2) 0.0044(16) -0.0080(17) -0.0079(16) C114 0.027(2) 0.0207(19) 0.025(2) 0.0070(17) -0.0114(18) -0.0097(17) C113 0.032(2) 0.034(2) 0.023(2) 0.0071(18) -0.0090(18) -0.019(2) C112 0.034(2) 0.036(2) 0.022(2) 0.0052(19) -0.0077(18) -0.019(2) C116 0.031(2) 0.031(2) 0.030(2) 0.0033(19) -0.0072(19) -0.017(2) C115 0.025(2) 0.029(2) 0.024(2) -0.0019(18) -0.0026(17) -0.0112(18) C145 0.030(2) 0.030(2) 0.027(2) 0.0070(18) -0.0102(19) -0.0123(19) C144 0.026(2) 0.029(2) 0.035(2) 0.0081(19) -0.0151(19) -0.0109(18) C143 0.024(2) 0.025(2) 0.031(2) 0.0050(18) -0.0107(18) -0.0112(18) C154 0.024(2) 0.027(2) 0.033(2) 0.0052(18) -0.0102(18) -0.0142(18) C155 0.027(2) 0.029(2) 0.037(2) 0.009(2) -0.010(2) -0.0148(19) C156 0.024(2) 0.028(2) 0.042(3) 0.008(2) -0.010(2) -0.0116(19) C152 0.029(2) 0.033(2) 0.035(2) 0.011(2) -0.011(2) -0.018(2) C153 0.029(2) 0.028(2) 0.037(2) 0.008(2) -0.013(2) -0.0122(19) C125 0.030(2) 0.027(2) 0.027(2) 0.0010(18) -0.0049(19) -0.0089(19) C124 0.029(2) 0.036(2) 0.027(2) 0.002(2) -0.0012(19) -0.013(2) C123 0.025(2) 0.035(2) 0.025(2) 0.0077(19) -0.0092(18) -0.0162(19) C134 0.036(3) 0.043(3) 0.029(2) 0.016(2) -0.018(2) -0.024(2) C133 0.050(3) 0.039(3) 0.026(2) 0.012(2) -0.020(2) -0.029(2) C132 0.062(3) 0.043(3) 0.035(3) 0.017(2) -0.030(3) -0.034(3) C136 0.051(4) 0.067(4) 0.066(4) 0.037(3) -0.026(3) -0.043(3) C135 0.037(3) 0.052(3) 0.053(3) 0.022(3) -0.013(2) -0.026(3) C165 0.028(2) 0.032(2) 0.042(3) 0.004(2) -0.016(2) -0.015(2) C164 0.035(3) 0.030(2) 0.047(3) 0.001(2) -0.017(2) -0.017(2) C163 0.028(2) 0.025(2) 0.025(2) 0.0043(17) -0.0072(17) -0.0148(18) C174 0.029(2) 0.027(2) 0.024(2) 0.0059(18) -0.0058(18) -0.0144(19) C175 0.038(3) 0.029(2) 0.034(2) 0.006(2) -0.014(2) -0.015(2) C176 0.041(3) 0.039(3) 0.047(3) 0.010(2) -0.023(2) -0.012(2) C172 0.046(3) 0.028(2) 0.037(3) 0.000(2) -0.009(2) -0.013(2) C173 0.034(3) 0.029(2) 0.033(2) 0.0017(19) -0.009(2) -0.015(2) C33 0.070(5) 0.074(5) 0.097(6) 0.009(5) -0.023(5) -0.018(5) C34 0.130(10) 0.119(9) 0.086(7) 0.028(7) 0.001(7) -0.021(8) C35 0.069(5) 0.075(5) 0.131(8) -0.014(5) -0.023(5) -0.031(4) C36 0.095(6) 0.100(6) 0.077(6) 0.012(5) -0.023(5) -0.059(6) C37 0.093(6) 0.080(5) 0.087(6) 0.019(5) -0.026(5) -0.038(5) C38 0.104(7) 0.087(6) 0.111(7) 0.020(5) -0.028(6) -0.061(6) C39 0.067(5) 0.072(5) 0.117(7) 0.011(5) -0.050(5) -0.016(4) C40 0.148(11) 0.142(10) 0.088(7) 0.028(7) -0.050(7) -0.080(9) C41A 0.049(7) 0.033(6) 0.088(10) -0.023(6) -0.040(7) 0.008(5) B1 0.021(2) 0.020(2) 0.025(2) 0.0009(18) -0.0044(19) -0.0083(18) C41B 0.048(8) 0.057(8) 0.130(15) -0.007(9) -0.032(9) -0.024(7) _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 Ag1 N122 2.246(4) . ? Ag1 N151 2.306(4) 2_655 ? Ag1 N111 2.343(4) 2 ? Ag1 N102 2.437(3) . ? O1 C33 1.262(10) . ? O2 C36 1.231(10) . ? O3 C39 1.133(9) . ? N101 C105 1.347(6) . ? N101 N102 1.353(5) . ? N101 B1 1.543(6) . ? N102 C103 1.345(5) . ? N111 C116 1.343(6) . ? N111 C112 1.352(6) . ? N111 Ag1 2.343(4) 2 ? N141 C145 1.351(6) . ? N141 N142 1.368(5) . ? N141 B1 1.530(6) . ? N142 C143 1.332(6) . ? N151 C156 1.334(6) . ? N151 C152 1.349(6) . ? N151 Ag1 2.306(4) 2_655 ? N121 N122 1.362(5) . ? N121 C125 1.363(6) . ? N121 B1 1.551(6) . ? N122 C123 1.336(6) . ? N131 C136 1.312(8) . ? N131 C132 1.328(7) . ? N161 C165 1.354(6) . ? N161 N162 1.365(5) . ? N161 B1 1.542(6) . ? N162 C163 1.334(6) . ? N171 C172 1.333(7) . ? N171 C176 1.346(7) . ? N13 C33 1.319(10) . ? N13 C35 1.433(10) . ? N13 C34 1.435(12) . ? N14 C37 1.361(11) . ? N14 C36 1.371(11) . ? N14 C38 1.457(11) . ? N15 C39 1.349(11) . ? N15 C41A 1.446(13) . ? N15 C40 1.461(12) . ? N15 C41B 1.592(17) . ? C105 C104 1.375(7) . ? C104 C103 1.397(6) . ? C103 C114 1.472(6) . ? C114 C113 1.389(6) . ? C114 C115 1.395(6) . ? C113 C112 1.380(7) . ? C116 C115 1.379(7) . ? C145 C144 1.356(7) . ? C144 C143 1.404(6) . ? C143 C154 1.468(6) . ? C154 C153 1.394(6) . ? C154 C155 1.400(6) . ? C155 C156 1.381(7) . ? C152 C153 1.387(7) . ? C125 C124 1.368(7) . ? C124 C123 1.401(7) . ? C123 C134 1.460(6) . ? C134 C133 1.384(7) . ? C134 C135 1.393(7) . ? C133 C132 1.395(7) . ? C136 C135 1.403(8) . ? C165 C164 1.368(7) . ? C164 C163 1.413(7) . ? C163 C174 1.466(6) . ? C174 C175 1.388(7) . ? C174 C173 1.398(6) . ? C175 C176 1.378(7) . ? C172 C173 1.381(7) . ? C41A C41B 1.34(2) . ? 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 N122 Ag1 N151 132.69(14) . 2_655 ? N122 Ag1 N111 130.42(13) . 2 ? N151 Ag1 N111 92.01(13) 2_655 2 ? N122 Ag1 N102 79.97(12) . . ? N151 Ag1 N102 102.93(13) 2_655 . ? N111 Ag1 N102 114.39(12) 2 . ? C105 N101 N102 110.7(3) . . ? C105 N101 B1 126.6(4) . . ? N102 N101 B1 121.6(3) . . ? C103 N102 N101 105.6(3) . . ? C103 N102 Ag1 122.5(3) . . ? N101 N102 Ag1 115.5(2) . . ? C116 N111 C112 116.7(4) . . ? C116 N111 Ag1 116.9(3) . 2 ? C112 N111 Ag1 126.0(3) . 2 ? C145 N141 N142 110.7(4) . . ? C145 N141 B1 128.7(4) . . ? N142 N141 B1 120.4(3) . . ? C143 N142 N141 104.9(3) . . ? C156 N151 C152 116.6(4) . . ? C156 N151 Ag1 113.3(3) . 2_655 ? C152 N151 Ag1 128.3(3) . 2_655 ? N122 N121 C125 109.2(3) . . ? N122 N121 B1 122.1(3) . . ? C125 N121 B1 128.1(4) . . ? C123 N122 N121 107.2(3) . . ? C123 N122 Ag1 130.0(3) . . ? N121 N122 Ag1 121.6(3) . . ? C136 N131 C132 116.3(5) . . ? C165 N161 N162 110.9(3) . . ? C165 N161 B1 129.0(4) . . ? N162 N161 B1 118.9(3) . . ? C163 N162 N161 105.5(4) . . ? C172 N171 C176 115.5(4) . . ? C33 N13 C35 122.7(8) . . ? C33 N13 C34 119.4(8) . . ? C35 N13 C34 117.1(8) . . ? C37 N14 C36 116.7(8) . . ? C37 N14 C38 124.6(8) . . ? C36 N14 C38 118.0(8) . . ? C39 N15 C41A 124.8(9) . . ? C39 N15 C40 117.7(9) . . ? C41A N15 C40 117.4(9) . . ? C39 N15 C41B 101.6(10) . . ? C41A N15 C41B 52.1(9) . . ? C40 N15 C41B 114.4(9) . . ? N101 C105 C104 108.4(4) . . ? C105 C104 C103 104.4(4) . . ? N102 C103 C104 111.0(4) . . ? N102 C103 C114 118.6(4) . . ? C104 C103 C114 130.5(4) . . ? C113 C114 C115 117.5(4) . . ? C113 C114 C103 121.7(4) . . ? C115 C114 C103 120.8(4) . . ? C112 C113 C114 119.4(4) . . ? N111 C112 C113 123.4(4) . . ? N111 C116 C115 123.4(4) . . ? C116 C115 C114 119.6(4) . . ? N141 C145 C144 108.2(4) . . ? C145 C144 C143 104.9(4) . . ? N142 C143 C144 111.3(4) . . ? N142 C143 C154 120.3(4) . . ? C144 C143 C154 128.0(4) . . ? C153 C154 C155 116.9(4) . . ? C153 C154 C143 123.9(4) . . ? C155 C154 C143 119.2(4) . . ? C156 C155 C154 119.6(4) . . ? N151 C156 C155 123.9(4) . . ? N151 C152 C153 123.6(4) . . ? C152 C153 C154 119.4(4) . . ? N121 C125 C124 108.2(4) . . ? C125 C124 C123 105.6(4) . . ? N122 C123 C124 109.7(4) . . ? N122 C123 C134 120.3(4) . . ? C124 C123 C134 130.0(4) . . ? C133 C134 C135 115.7(5) . . ? C133 C134 C123 122.5(4) . . ? C135 C134 C123 121.7(5) . . ? C134 C133 C132 120.8(5) . . ? N131 C132 C133 123.2(5) . . ? N131 C136 C135 124.9(5) . . ? C134 C135 C136 119.0(5) . . ? N161 C165 C164 107.9(4) . . ? C165 C164 C163 104.9(4) . . ? N162 C163 C164 110.9(4) . . ? N162 C163 C174 119.6(4) . . ? C164 C163 C174 129.5(4) . . ? C175 C174 C173 116.9(4) . . ? C175 C174 C163 121.9(4) . . ? C173 C174 C163 121.2(4) . . ? C176 C175 C174 119.3(5) . . ? N171 C176 C175 124.6(5) . . ? N171 C172 C173 124.4(5) . . ? C172 C173 C174 119.4(5) . . ? O1 C33 N13 123.7(9) . . ? O2 C36 N14 125.7(9) . . ? O3 C39 N15 126.6(10) . . ? C41B C41A N15 69.6(9) . . ? N141 B1 N161 110.3(4) . . ? N141 B1 N101 110.0(3) . . ? N161 B1 N101 108.1(3) . . ? N141 B1 N121 108.1(3) . . ? N161 B1 N121 107.6(3) . . ? N101 B1 N121 112.7(4) . . ? C41A C41B N15 58.3(8) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C145 H145 N131 0.95 2.56 3.326(6) 137.7 2_556 C144 H144 N171 0.95 2.59 3.524(6) 167.9 1_645 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 0.00 0.0300 -1.00 0.00 0.00 0.0150 0.00 1.00 0.00 0.2290 0.00 -1.00 0.00 0.2400 -2.00 -3.00 13.00 0.0480 0.00 0.00 -1.00 0.0940 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.062 _refine_diff_density_min -0.823 _refine_diff_density_rms 0.118 #=END