Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Thurston, John H.' ; Department of Chemistry MS-60 Rice University 6100 Main St. Houtson Tx. 77005 United States of America ; 'Marlier, Elodie E.' ; Department of Chemistry MS-60 Rice University 6100 Main St. Houtson Tx. 77005 United States of America ; 'Whitmire, Kenton H.' ; Department of Chemistry MS-60 Rice University 6100 Main St. Houtson Tx. 77005 United States of America ; _publ_contact_author_name 'Dr Kenton Whitmire' _publ_contact_author_address ; Dr. Kenton H. Whitmire Department of Chemistry MS-60 Rice University Houtson Tx. 77251-1892 United States of America ; _publ_contact_author_phone '713 348 5650' _publ_contact_author_fax '713 348 5652' _publ_contact_author_email 'whitmir@rice.edu' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; Supplementary publication for Chemical Communications. ; _publ_section_title ; Towards a molecular model for Bismuth(III) subsalicylate. Synthesis and solid-state structure of [Bi(Hsal)3(bipy)*C7H8]2 and [Bi(Hsal)(sal)(1,10-phenanthroline)*C7H8]2 ; #============================================================================ data_2 _database_code_CSD 194668 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 159 _chemical_formula_moiety Bi2(Hsal)6(bipy)2(tol)2 _chemical_formula_sum 'C76 H62 Bi2 N4 O18' _chemical_formula_weight 1737.26 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.830(2) _cell_length_b 12.489(3) _cell_length_c 14.319(3) _cell_angle_alpha 87.22(3) _cell_angle_beta 81.65(3) _cell_angle_gamma 64.33(3) _cell_volume 1727.0(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 972 _cell_measurement_theta_min 6.846 _cell_measurement_theta_max 46.413 _exptl_crystal_description 'thin-plate' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 5.164 _exptl_absorpt_correction_type 'empirical with SADABS' _exptl_absorpt_correction_T_min 0.671013 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1k; CCD' _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 7438 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4920 _reflns_number_gt 4349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL 6.10 (Bruker, 2001)' _computing_cell_refinement 'SHELXTL 6.10 (Bruker, 2001)' _computing_data_reduction 'SHELXTL 6.10 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4920 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0328 _refine_ls_R_factor_gt 0.0272 _refine_ls_wR_factor_ref 0.0644 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.051 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.469114(18) 1.162897(15) 0.467089(13) 0.03618(8) Uani 1 1 d . . . N1 N 0.6703(4) 1.2100(4) 0.4687(3) 0.0413(10) Uani 1 1 d . . . C1 C 0.7825(5) 1.1391(5) 0.5077(4) 0.0493(13) Uani 1 1 d . . . H1A H 0.7888 1.0663 0.5308 0.059 Uiso 1 1 calc R . . N2 N 0.4346(4) 1.3507(3) 0.4005(3) 0.0365(9) Uani 1 1 d . . . C2 C 0.8892(6) 1.1690(6) 0.5151(4) 0.0583(15) Uani 1 1 d . . . H2A H 0.9647 1.1189 0.5443 0.070 Uiso 1 1 calc R . . C3 C 0.8808(6) 1.2742(6) 0.4784(5) 0.0686(18) Uani 1 1 d . . . H3A H 0.9520 1.2962 0.4810 0.082 Uiso 1 1 calc R . . C4 C 0.7665(6) 1.3478(5) 0.4373(4) 0.0598(16) Uani 1 1 d . . . H4A H 0.7599 1.4199 0.4122 0.072 Uiso 1 1 calc R . . C5 C 0.6620(5) 1.3136(5) 0.4339(3) 0.0418(12) Uani 1 1 d . . . C6 C 0.5330(5) 1.3902(4) 0.3943(3) 0.0433(12) Uani 1 1 d . . . C7 C 0.5121(6) 1.4975(5) 0.3536(4) 0.0553(15) Uani 1 1 d . . . H7A H 0.5820 1.5227 0.3469 0.066 Uiso 1 1 calc R . . C8 C 0.3876(7) 1.5677(5) 0.3225(4) 0.0609(16) Uani 1 1 d . . . H8A H 0.3725 1.6411 0.2960 0.073 Uiso 1 1 calc R . . C9 C 0.2861(6) 1.5285(5) 0.3311(4) 0.0565(15) Uani 1 1 d . . . H9A H 0.2013 1.5749 0.3107 0.068 Uiso 1 1 calc R . . C10 C 0.3121(5) 1.4187(4) 0.3706(3) 0.0431(12) Uani 1 1 d . . . H10A H 0.2440 1.3914 0.3766 0.052 Uiso 1 1 calc R . . O21 O 0.3440(4) 0.8626(3) 0.2722(3) 0.0641(11) Uani 1 1 d . . . H21A H 0.3910 0.8732 0.3075 0.096 Uiso 1 1 calc R . . C21 C 0.2356(6) 0.9667(5) 0.2593(4) 0.0502(14) Uani 1 1 d . . . O22 O 0.4069(3) 0.9922(3) 0.3815(2) 0.0447(8) Uani 1 1 d . . . C22 C 0.1411(7) 0.9608(6) 0.2064(4) 0.0677(17) Uani 1 1 d . . . H22A H 0.1546 0.8881 0.1824 0.081 Uiso 1 1 calc R . . O23 O 0.2926(4) 1.1892(3) 0.3780(3) 0.0512(9) Uani 1 1 d . . . C23 C 0.0286(7) 1.0613(7) 0.1895(4) 0.074(2) Uani 1 1 d . . . H23A H -0.0344 1.0563 0.1542 0.089 Uiso 1 1 calc R . . C24 C 0.0062(7) 1.1704(7) 0.2235(5) 0.0734(19) Uani 1 1 d . . . H24A H -0.0703 1.2387 0.2106 0.088 Uiso 1 1 calc R . . C25 C 0.1000(6) 1.1770(5) 0.2776(4) 0.0585(15) Uani 1 1 d . . . H25A H 0.0853 1.2501 0.3016 0.070 Uiso 1 1 calc R . . C26 C 0.2153(5) 1.0753(5) 0.2960(3) 0.0410(12) Uani 1 1 d . . . C27 C 0.3131(5) 1.0843(4) 0.3547(3) 0.0386(12) Uani 1 1 d . . . O31 O 0.0111(4) 1.4846(4) 0.6274(3) 0.0698(12) Uani 1 1 d . . . H31A H 0.0673 1.4386 0.5863 0.105 Uiso 1 1 calc R . . C31 C 0.0689(6) 1.4692(5) 0.7079(4) 0.0569(15) Uani 1 1 d . . . O32 O 0.2440(3) 1.3197(3) 0.5545(2) 0.0471(9) Uani 1 1 d . . . C32 C -0.0115(7) 1.5318(6) 0.7882(5) 0.076(2) Uani 1 1 d . . . H32A H -0.1045 1.5818 0.7867 0.091 Uiso 1 1 calc R . . O33 O 0.4271(3) 1.2720(3) 0.6246(2) 0.0496(9) Uani 1 1 d . . . C33 C 0.0436(9) 1.5214(7) 0.8696(6) 0.089(2) Uani 1 1 d . . . H33A H -0.0125 1.5650 0.9228 0.107 Uiso 1 1 calc R . . C34 C 0.1814(9) 1.4472(7) 0.8751(5) 0.081(2) Uani 1 1 d . . . H34A H 0.2179 1.4399 0.9312 0.097 Uiso 1 1 calc R . . C35 C 0.2624(6) 1.3848(6) 0.7954(4) 0.0594(15) Uani 1 1 d . . . H35A H 0.3554 1.3354 0.7976 0.071 Uiso 1 1 calc R . . C36 C 0.2080(5) 1.3940(5) 0.7107(4) 0.0442(13) Uani 1 1 d . . . C37 C 0.2988(5) 1.3241(4) 0.6266(4) 0.0408(12) Uani 1 1 d . . . O41 O 0.9318(4) 0.7874(3) 0.3217(3) 0.0573(10) Uani 1 1 d . . . H41A H 0.8743 0.8259 0.3657 0.086 Uiso 1 1 calc R . . C41 C 0.8893(5) 0.8370(5) 0.2386(4) 0.0474(13) Uani 1 1 d . . . O42 O 0.7038(4) 0.9571(3) 0.4026(2) 0.0492(9) Uani 1 1 d . . . C42 C 0.9686(6) 0.7804(5) 0.1557(4) 0.0617(16) Uani 1 1 d . . . H42A H 1.0472 0.7093 0.1579 0.074 Uiso 1 1 calc R . . O43 O 0.5899(3) 1.1127(3) 0.3169(2) 0.0468(9) Uani 1 1 d . . . C43 C 0.9324(7) 0.8280(6) 0.0707(5) 0.0728(19) Uani 1 1 d . . . H43A H 0.9868 0.7892 0.0153 0.087 Uiso 1 1 calc R . . C44 C 0.8141(7) 0.9348(7) 0.0657(4) 0.075(2) Uani 1 1 d . . . H44A H 0.7891 0.9670 0.0077 0.090 Uiso 1 1 calc R . . C45 C 0.7362(6) 0.9906(6) 0.1479(4) 0.0590(16) Uani 1 1 d . . . H45A H 0.6578 1.0618 0.1451 0.071 Uiso 1 1 calc R . . C46 C 0.7712(5) 0.9435(4) 0.2368(4) 0.0413(12) Uani 1 1 d . . . C47 C 0.6841(5) 1.0067(5) 0.3237(4) 0.0447(13) Uani 1 1 d . . . C51 C 0.4429(14) 0.7005(17) -0.0362(17) 0.245(13) Uani 1 1 d . . . C52 C 0.4474(14) 0.7556(16) 0.0415(9) 0.171(8) Uani 1 1 d . . . H52A H 0.3957 0.7605 0.1003 0.205 Uiso 1 1 calc R . . C53 C 0.5532(19) 0.8094(13) 0.0164(11) 0.193(8) Uani 1 1 d . . . H53A H 0.5690 0.8501 0.0625 0.231 Uiso 1 1 calc R . . C54 C 0.6215(12) 0.7977(11) -0.0705(11) 0.138(4) Uani 1 1 d . . . H54A H 0.6847 0.8299 -0.0863 0.165 Uiso 1 1 calc R . . C55 C 0.5950(16) 0.7360(14) -0.1365(8) 0.174(7) Uani 1 1 d . . . H55A H 0.6412 0.7261 -0.1978 0.209 Uiso 1 1 calc R . . C56 C 0.5049(13) 0.6908(11) -0.1136(10) 0.139(5) Uani 1 1 d . . . H56A H 0.4892 0.6499 -0.1597 0.166 Uiso 1 1 calc R . . C57 C 0.3434(12) 0.6501(12) -0.0090(14) 0.247(10) Uani 1 1 d . . . H57A H 0.3373 0.6100 -0.0624 0.370 Uiso 1 1 calc R . . H57B H 0.2541 0.7127 0.0124 0.370 Uiso 1 1 calc R . . H57C H 0.3735 0.5945 0.0409 0.370 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 Bi1 0.03974(12) 0.02867(11) 0.04067(13) 0.00276(8) -0.00746(8) -0.01490(8) N1 0.039(2) 0.045(3) 0.041(2) 0.002(2) -0.008(2) -0.018(2) C1 0.048(3) 0.049(3) 0.052(3) 0.003(3) -0.004(3) -0.022(3) N2 0.040(2) 0.032(2) 0.040(2) -0.0031(18) -0.0029(19) -0.0179(19) C2 0.044(3) 0.069(4) 0.064(4) -0.002(3) -0.012(3) -0.025(3) C3 0.054(4) 0.075(5) 0.088(5) -0.008(4) -0.007(3) -0.038(4) C4 0.059(4) 0.056(4) 0.075(4) 0.006(3) -0.009(3) -0.036(3) C5 0.043(3) 0.046(3) 0.038(3) -0.003(2) 0.005(2) -0.023(3) C6 0.055(3) 0.040(3) 0.039(3) 0.000(2) -0.005(2) -0.024(3) C7 0.067(4) 0.045(3) 0.062(4) 0.009(3) -0.008(3) -0.033(3) C8 0.084(5) 0.038(3) 0.061(4) 0.010(3) -0.010(3) -0.028(3) C9 0.073(4) 0.038(3) 0.051(3) 0.006(3) -0.011(3) -0.016(3) C10 0.044(3) 0.041(3) 0.038(3) 0.004(2) -0.002(2) -0.014(2) O21 0.078(3) 0.048(2) 0.069(3) -0.010(2) -0.026(2) -0.023(2) C21 0.058(4) 0.057(4) 0.042(3) 0.002(3) -0.007(3) -0.030(3) O22 0.049(2) 0.037(2) 0.048(2) 0.0050(16) -0.0132(17) -0.0178(17) C22 0.078(4) 0.075(5) 0.068(4) -0.003(3) -0.027(4) -0.043(4) O23 0.052(2) 0.038(2) 0.064(2) -0.0019(18) -0.0217(19) -0.0160(18) C23 0.074(5) 0.109(6) 0.064(4) 0.004(4) -0.025(4) -0.056(5) C24 0.061(4) 0.082(5) 0.080(5) 0.014(4) -0.032(4) -0.027(4) C25 0.057(4) 0.058(4) 0.064(4) 0.004(3) -0.016(3) -0.026(3) C26 0.046(3) 0.043(3) 0.038(3) 0.006(2) -0.010(2) -0.022(3) C27 0.042(3) 0.037(3) 0.037(3) 0.002(2) -0.002(2) -0.018(2) O31 0.053(2) 0.061(3) 0.078(3) 0.004(2) -0.011(2) -0.008(2) C31 0.057(4) 0.035(3) 0.070(4) -0.001(3) 0.009(3) -0.017(3) O32 0.047(2) 0.049(2) 0.045(2) 0.0048(17) -0.0064(18) -0.0212(18) C32 0.071(5) 0.053(4) 0.082(5) -0.008(4) 0.020(4) -0.016(3) O33 0.039(2) 0.046(2) 0.060(2) -0.0110(18) -0.0002(18) -0.0157(17) C33 0.111(7) 0.062(5) 0.073(5) -0.021(4) 0.041(5) -0.033(5) C34 0.112(6) 0.082(5) 0.051(4) -0.014(4) 0.004(4) -0.047(5) C35 0.066(4) 0.066(4) 0.052(4) -0.002(3) -0.005(3) -0.034(3) C36 0.047(3) 0.039(3) 0.046(3) 0.000(2) 0.007(3) -0.023(3) C37 0.042(3) 0.030(3) 0.050(3) 0.002(2) 0.003(3) -0.019(2) O41 0.051(2) 0.051(2) 0.062(2) 0.010(2) -0.0077(19) -0.0153(19) C41 0.049(3) 0.046(3) 0.054(4) 0.001(3) -0.003(3) -0.029(3) O42 0.058(2) 0.046(2) 0.040(2) 0.0025(17) -0.0064(18) -0.0191(18) C42 0.060(4) 0.053(4) 0.067(4) -0.005(3) 0.005(3) -0.023(3) O43 0.052(2) 0.040(2) 0.041(2) -0.0003(16) -0.0035(17) -0.0144(18) C43 0.078(5) 0.075(5) 0.059(4) -0.021(4) 0.014(4) -0.032(4) C44 0.081(5) 0.090(5) 0.041(4) -0.006(3) -0.009(3) -0.023(4) C45 0.055(4) 0.067(4) 0.045(3) -0.001(3) -0.006(3) -0.017(3) C46 0.039(3) 0.037(3) 0.049(3) -0.001(2) -0.003(2) -0.019(2) C47 0.048(3) 0.047(3) 0.048(3) 0.000(3) -0.011(3) -0.027(3) C51 0.121(12) 0.186(16) 0.24(2) 0.114(16) 0.092(14) 0.063(11) C52 0.124(11) 0.209(17) 0.074(7) -0.007(9) 0.022(7) 0.017(10) C53 0.218(18) 0.178(15) 0.112(11) -0.022(10) -0.062(12) -0.005(13) C54 0.130(9) 0.144(11) 0.119(9) 0.028(9) -0.030(8) -0.040(8) C55 0.153(12) 0.160(13) 0.082(8) -0.005(9) -0.018(9) 0.052(10) C56 0.104(9) 0.123(9) 0.138(12) 0.015(8) 0.023(8) -0.016(7) C57 0.098(9) 0.164(13) 0.44(3) 0.081(15) 0.040(13) -0.049(8) _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 Bi1 O43 2.310(3) . ? Bi1 O23 2.348(3) . ? Bi1 N2 2.383(4) . ? Bi1 N1 2.494(4) . ? Bi1 O32 2.561(4) . ? Bi1 O33 2.572(4) . ? N1 C5 1.335(6) . ? N1 C1 1.338(6) . ? C1 C2 1.379(7) . ? N2 C6 1.345(6) . ? N2 C10 1.348(6) . ? C2 C3 1.361(8) . ? C3 C4 1.377(8) . ? C4 C5 1.381(7) . ? C5 C6 1.485(7) . ? C6 C7 1.374(7) . ? C7 C8 1.376(8) . ? C8 C9 1.373(8) . ? C9 C10 1.384(7) . ? O21 C21 1.349(7) . ? C21 C22 1.388(8) . ? C21 C26 1.393(7) . ? O22 C27 1.249(5) . ? C22 C23 1.360(9) . ? O23 C27 1.283(6) . ? C23 C24 1.377(9) . ? C24 C25 1.395(8) . ? C25 C26 1.389(7) . ? C26 C27 1.487(7) . ? O31 C31 1.357(7) . ? C31 C32 1.378(9) . ? C31 C36 1.394(7) . ? O32 C37 1.278(6) . ? C32 C33 1.361(10) . ? O33 C37 1.249(6) . ? C33 C34 1.386(10) . ? C34 C35 1.372(8) . ? C35 C36 1.402(7) . ? C36 C37 1.481(7) . ? O41 C41 1.361(6) . ? C41 C42 1.380(8) . ? C41 C46 1.392(7) . ? O42 C47 1.262(6) . ? C42 C43 1.363(8) . ? O43 C47 1.284(6) . ? C43 C44 1.400(9) . ? C44 C45 1.365(8) . ? C45 C46 1.410(7) . ? C46 C47 1.473(7) . ? C51 C56 1.192(16) . ? C51 C52 1.35(3) . ? C51 C57 1.47(2) . ? C52 C53 1.55(2) . ? C53 C54 1.332(16) . ? C54 C55 1.382(17) . ? C55 C56 1.320(19) . ? 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 O43 Bi1 O23 78.30(13) . . ? O43 Bi1 N2 76.95(13) . . ? O23 Bi1 N2 80.96(13) . . ? O43 Bi1 N1 75.57(13) . . ? O23 Bi1 N1 142.18(13) . . ? N2 Bi1 N1 66.88(13) . . ? O43 Bi1 O32 140.74(11) . . ? O23 Bi1 O32 73.16(12) . . ? N2 Bi1 O32 72.46(12) . . ? N1 Bi1 O32 112.82(13) . . ? O43 Bi1 O33 148.15(12) . . ? O23 Bi1 O33 123.60(12) . . ? N2 Bi1 O33 83.76(12) . . ? N1 Bi1 O33 73.61(12) . . ? O32 Bi1 O33 50.47(11) . . ? C5 N1 C1 118.7(4) . . ? C5 N1 Bi1 118.3(3) . . ? C1 N1 Bi1 122.9(3) . . ? N1 C1 C2 123.0(5) . . ? C6 N2 C10 120.2(4) . . ? C6 N2 Bi1 121.4(3) . . ? C10 N2 Bi1 118.4(3) . . ? C3 C2 C1 118.0(5) . . ? C2 C3 C4 119.9(6) . . ? C3 C4 C5 119.3(5) . . ? N1 C5 C4 121.2(5) . . ? N1 C5 C6 116.2(4) . . ? C4 C5 C6 122.5(5) . . ? N2 C6 C7 120.4(5) . . ? N2 C6 C5 117.1(4) . . ? C7 C6 C5 122.5(5) . . ? C6 C7 C8 120.0(5) . . ? C9 C8 C7 119.5(5) . . ? C8 C9 C10 118.8(5) . . ? N2 C10 C9 121.1(5) . . ? O21 C21 C22 115.8(5) . . ? O21 C21 C26 123.9(5) . . ? C22 C21 C26 120.2(6) . . ? C23 C22 C21 120.1(6) . . ? C27 O23 Bi1 105.7(3) . . ? C22 C23 C24 121.3(6) . . ? C23 C24 C25 119.0(6) . . ? C26 C25 C24 120.6(6) . . ? C25 C26 C21 118.8(5) . . ? C25 C26 C27 119.7(5) . . ? C21 C26 C27 121.5(5) . . ? O22 C27 O23 123.1(5) . . ? O22 C27 C26 120.0(5) . . ? O23 C27 C26 116.8(4) . . ? O31 C31 C32 119.0(6) . . ? O31 C31 C36 121.7(5) . . ? C32 C31 C36 119.3(6) . . ? C37 O32 Bi1 94.3(3) . . ? C33 C32 C31 120.8(7) . . ? C37 O33 Bi1 94.5(3) . . ? C32 C33 C34 121.5(7) . . ? C35 C34 C33 118.2(7) . . ? C34 C35 C36 121.4(6) . . ? C31 C36 C35 118.9(5) . . ? C31 C36 C37 121.5(5) . . ? C35 C36 C37 119.6(5) . . ? O33 C37 O32 120.0(5) . . ? O33 C37 C36 121.2(5) . . ? O32 C37 C36 118.8(5) . . ? O41 C41 C42 118.1(5) . . ? O41 C41 C46 121.1(5) . . ? C42 C41 C46 120.7(5) . . ? C43 C42 C41 120.4(6) . . ? C47 O43 Bi1 104.9(3) . . ? C42 C43 C44 120.7(6) . . ? C45 C44 C43 118.7(6) . . ? C44 C45 C46 121.9(6) . . ? C41 C46 C45 117.6(5) . . ? C41 C46 C47 122.3(5) . . ? C45 C46 C47 120.0(5) . . ? O42 C47 O43 121.5(5) . . ? O42 C47 C46 120.1(5) . . ? O43 C47 C46 118.4(4) . . ? C56 C51 C52 130(3) . . ? C56 C51 C57 123(3) . . ? C52 C51 C57 107.0(17) . . ? C51 C52 C53 108.9(14) . . ? C54 C53 C52 120.7(14) . . ? C53 C54 C55 117.5(14) . . ? C56 C55 C54 120.9(14) . . ? C51 C56 C55 122(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.800 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.087 #====END data_3 _database_code_CSD 194669 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Bi2(sal)2(salH)2(1,10-phenanthroline)2(tol)2' _chemical_formula_sum 'C66 H48 Bi2 N4 O12' _chemical_formula_weight 1507.04 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 '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 10.022(2) _cell_length_b 24.530(5) _cell_length_c 12.195(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.167(4) _cell_angle_gamma 90.00 _cell_volume 2864.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 865 _cell_measurement_theta_min 4.822 _cell_measurement_theta_max 46.328 _exptl_crystal_description 'thin plate' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.747 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 6.204 _exptl_absorpt_correction_type 'empirical with SADABS' _exptl_absorpt_correction_T_min 0.829181 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K; CCD' _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 12698 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4113 _reflns_number_gt 3167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_cell_refinement 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_data_reduction 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker AXS, 2001)' _computing_publication_material 'SHELXTL 6.10 (Bruker AXS, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4113 _refine_ls_number_parameters 344 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0652 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 0.973 _refine_ls_restrained_S_all 0.973 _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 Bi1 Bi -0.92349(2) 0.528156(8) -0.330547(18) 0.05090(10) Uani 1 1 d . . . N1 N -0.6775(4) 0.48398(17) -0.2840(4) 0.0498(11) Uani 1 1 d . . . C1 C -0.6535(6) 0.4402(3) -0.3377(5) 0.0641(16) Uani 1 1 d . . . H1A H -0.7281 0.4245 -0.3931 0.077 Uiso 1 1 calc R . . N2 N -0.7248(4) 0.57381(19) -0.1684(4) 0.0537(12) Uani 1 1 d . . . C2 C -0.5217(7) 0.4160(3) -0.3157(6) 0.0791(19) Uani 1 1 d . . . H2A H -0.5095 0.3853 -0.3565 0.095 Uiso 1 1 calc R . . C3 C -0.4113(7) 0.4381(3) -0.2337(6) 0.0723(18) Uani 1 1 d . . . H3A H -0.3230 0.4226 -0.2182 0.087 Uiso 1 1 calc R . . C4 C -0.4323(6) 0.4841(2) -0.1735(5) 0.0570(16) Uani 1 1 d . . . C5 C -0.3233(6) 0.5101(3) -0.0835(6) 0.0702(19) Uani 1 1 d . . . H5A H -0.2331 0.4961 -0.0648 0.084 Uiso 1 1 calc R . . C6 C -0.3476(6) 0.5526(3) -0.0279(5) 0.0705(18) Uani 1 1 d . . . H6A H -0.2753 0.5676 0.0306 0.085 Uiso 1 1 calc R . . C7 C -0.4832(5) 0.5762(3) -0.0553(5) 0.0578(15) Uani 1 1 d . . . C8 C -0.5114(7) 0.6230(3) -0.0006(5) 0.0777(19) Uani 1 1 d . . . H8A H -0.4402 0.6394 0.0568 0.093 Uiso 1 1 calc R . . C9 C -0.6419(7) 0.6447(3) -0.0305(6) 0.083(2) Uani 1 1 d . . . H9A H -0.6612 0.6761 0.0048 0.100 Uiso 1 1 calc R . . C10 C -0.7454(6) 0.6186(3) -0.1155(5) 0.0686(17) Uani 1 1 d . . . H10A H -0.8347 0.6335 -0.1364 0.082 Uiso 1 1 calc R . . C11 C -0.5939(5) 0.5529(2) -0.1400(5) 0.0517(14) Uani 1 1 d . . . C12 C -0.5688(5) 0.5059(2) -0.2009(5) 0.0497(14) Uani 1 1 d . . . O21 O -1.2311(6) 0.6625(2) -0.1852(6) 0.127(2) Uani 1 1 d . . . O22 O -1.0687(5) 0.59171(18) -0.2407(4) 0.0843(13) Uani 1 1 d . . . O23 O -1.1712(4) 0.53162(19) -0.3700(4) 0.0742(12) Uani 1 1 d . . . C21 C -1.3348(6) 0.6400(2) -0.2600(4) 0.107(3) Uani 1 1 d G . . C22 C -1.4659(7) 0.6633(2) -0.2775(5) 0.115(3) Uani 1 1 d G . . H22A H -1.4759 0.6942 -0.2364 0.138 Uiso 1 1 calc R . . C23 C -1.5819(5) 0.6405(3) -0.3564(6) 0.128(4) Uani 1 1 d G . . H23A H -1.6696 0.6561 -0.3681 0.154 Uiso 1 1 calc R . . C24 C -1.5669(4) 0.5943(3) -0.4178(5) 0.123(3) Uani 1 1 d G . . H24A H -1.6446 0.5791 -0.4706 0.147 Uiso 1 1 calc R . . C25 C -1.4359(5) 0.5710(2) -0.4004(4) 0.089(3) Uani 1 1 d G . . H25A H -1.4259 0.5401 -0.4415 0.106 Uiso 1 1 calc R . . C26 C -1.3198(4) 0.5938(2) -0.3214(4) 0.080(2) Uani 1 1 d G . . C27 C -1.1793(6) 0.5709(3) -0.3094(6) 0.0690(18) Uani 1 1 d . . . O31 O -0.9352(4) 0.47371(16) -0.1990(3) 0.0632(10) Uani 1 1 d . . . O32 O -0.9823(4) 0.45302(16) -0.4373(3) 0.0583(10) Uani 1 1 d . . . O33 O -1.0911(5) 0.37915(19) -0.5048(4) 0.0925(15) Uani 1 1 d . . . C31 C -1.0014(3) 0.42530(13) -0.2078(3) 0.0545(15) Uani 1 1 d G . . C32 C -1.0106(4) 0.40584(18) -0.1033(3) 0.0638(16) Uani 1 1 d G . . H32A H -0.9734 0.4260 -0.0367 0.077 Uiso 1 1 calc R . . C33 C -1.0756(4) 0.35622(19) -0.0982(3) 0.082(2) Uani 1 1 d G . . H33A H -1.0818 0.3432 -0.0283 0.098 Uiso 1 1 calc R . . C34 C -1.1313(4) 0.32607(14) -0.1978(4) 0.088(2) Uani 1 1 d G . . H34A H -1.1748 0.2929 -0.1944 0.106 Uiso 1 1 calc R . . C35 C -1.1221(4) 0.34553(15) -0.3023(3) 0.0744(18) Uani 1 1 d G . . H35A H -1.1594 0.3254 -0.3689 0.089 Uiso 1 1 calc R . . C36 C -1.0571(4) 0.39515(16) -0.3074(3) 0.0532(14) Uani 1 1 d G . . C37 C -1.0451(5) 0.4091(3) -0.4224(5) 0.0560(15) Uani 1 1 d . . . C41 C -0.9561(9) 0.7495(3) -0.2438(14) 0.192(8) Uani 1 1 d GD . . H41A H -1.0312 0.7327 -0.2967 0.231 Uiso 1 1 calc R . . C42 C -0.9618(11) 0.7604(4) -0.1334(16) 0.209(9) Uani 1 1 d G . . H42A H -1.0407 0.7509 -0.1124 0.251 Uiso 1 1 calc R . . C43 C -0.8495(18) 0.7854(5) -0.0544(9) 0.183(5) Uani 1 1 d G . . H43A H -0.8533 0.7927 0.0194 0.219 Uiso 1 1 calc R . . C44 C -0.7316(12) 0.7996(3) -0.0858(11) 0.280(16) Uani 1 1 d G . . H44A H -0.6564 0.8164 -0.0330 0.335 Uiso 1 1 calc R . . C45 C -0.7259(8) 0.7888(4) -0.1962(14) 0.210(10) Uani 1 1 d GD . . H45A H -0.6470 0.7983 -0.2173 0.253 Uiso 1 1 calc R . . C46 C -0.8382(15) 0.7637(5) -0.2753(9) 0.39(3) Uani 1 1 d GD . . C47 C -0.832(3) 0.7547(9) -0.356(3) 0.54(3) Uani 1 1 d D . . H47A H -0.7433 0.7668 -0.3624 0.808 Uiso 1 1 calc R . . H47B H -0.9058 0.7729 -0.4123 0.808 Uiso 1 1 calc R . . H47C H -0.8402 0.7161 -0.3681 0.808 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 Bi1 0.04339(13) 0.05458(15) 0.04576(14) -0.00147(12) -0.00068(9) 0.00002(11) N1 0.044(3) 0.053(3) 0.050(3) -0.004(2) 0.010(2) 0.002(2) C1 0.054(4) 0.066(4) 0.067(4) -0.008(3) 0.009(3) 0.004(3) N2 0.041(3) 0.066(3) 0.049(3) -0.007(3) 0.004(2) 0.003(2) C2 0.087(5) 0.064(4) 0.085(5) -0.002(4) 0.024(4) 0.026(4) C3 0.059(4) 0.079(5) 0.075(5) 0.016(4) 0.014(4) 0.021(4) C4 0.047(3) 0.063(4) 0.055(4) 0.022(3) 0.006(3) 0.006(3) C5 0.040(3) 0.088(5) 0.074(5) 0.029(4) 0.003(3) 0.008(3) C6 0.055(4) 0.086(5) 0.057(4) 0.003(4) -0.004(3) -0.014(4) C7 0.043(3) 0.079(4) 0.044(3) 0.008(3) 0.001(3) -0.008(3) C8 0.064(5) 0.100(5) 0.057(4) -0.020(4) -0.001(4) -0.029(4) C9 0.081(5) 0.081(5) 0.083(5) -0.036(4) 0.017(4) -0.019(4) C10 0.063(4) 0.072(4) 0.062(4) -0.014(4) 0.006(3) 0.001(3) C11 0.047(3) 0.061(4) 0.044(3) 0.004(3) 0.010(3) -0.006(3) C12 0.043(3) 0.056(4) 0.046(3) 0.012(3) 0.006(3) -0.001(3) O21 0.107(4) 0.113(5) 0.156(6) -0.018(4) 0.033(4) -0.003(4) O22 0.075(3) 0.080(3) 0.091(3) -0.012(3) 0.014(3) 0.004(3) O23 0.051(2) 0.084(3) 0.081(3) -0.007(3) 0.010(2) 0.002(2) C21 0.087(6) 0.112(7) 0.129(8) 0.048(7) 0.042(6) -0.003(6) C22 0.106(6) 0.109(7) 0.148(9) 0.051(6) 0.063(7) 0.036(6) C23 0.098(7) 0.138(9) 0.169(10) 0.069(8) 0.070(7) 0.039(6) C24 0.084(6) 0.153(9) 0.131(8) 0.071(7) 0.031(5) 0.018(6) C25 0.021(3) 0.153(7) 0.085(5) 0.061(5) 0.005(3) 0.008(4) C26 0.089(5) 0.072(5) 0.089(5) 0.034(4) 0.043(5) 0.022(4) C27 0.051(4) 0.082(5) 0.071(5) 0.018(4) 0.014(4) 0.007(4) O31 0.058(2) 0.076(3) 0.047(2) 0.003(2) 0.0025(19) -0.003(2) O32 0.064(2) 0.057(2) 0.049(2) -0.0023(19) 0.010(2) -0.012(2) O33 0.117(4) 0.083(3) 0.077(3) -0.020(3) 0.028(3) -0.042(3) C31 0.034(3) 0.066(4) 0.060(4) 0.017(3) 0.009(3) 0.008(3) C32 0.043(3) 0.083(5) 0.063(4) 0.011(4) 0.012(3) 0.002(3) C33 0.070(4) 0.105(6) 0.078(5) 0.021(5) 0.032(4) 0.012(4) C34 0.087(5) 0.072(5) 0.114(6) 0.018(5) 0.043(5) -0.007(4) C35 0.076(4) 0.063(4) 0.084(5) 0.002(4) 0.023(4) -0.004(3) C36 0.044(3) 0.054(4) 0.056(4) 0.005(3) 0.006(3) 0.009(3) C37 0.042(3) 0.057(4) 0.062(4) -0.005(3) 0.005(3) 0.002(3) C41 0.120(10) 0.094(8) 0.34(2) 0.064(12) 0.026(12) 0.032(8) C42 0.160(13) 0.095(10) 0.32(3) 0.093(13) -0.017(13) -0.007(8) C43 0.203(15) 0.097(10) 0.227(15) 0.029(10) 0.032(16) 0.044(10) C44 0.144(15) 0.075(8) 0.55(5) 0.075(16) -0.004(16) 0.005(9) C45 0.106(11) 0.130(13) 0.39(3) 0.069(15) 0.067(13) 0.016(9) C46 0.24(3) 0.126(18) 0.84(10) 0.20(3) 0.20(4) 0.108(18) C47 0.71(7) 0.33(3) 0.44(4) 0.01(3) -0.04(4) 0.41(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 Bi1 O31 2.117(4) . ? Bi1 O32 2.233(4) . ? Bi1 O23 2.387(4) . ? Bi1 O22 2.587(4) . ? Bi1 N1 2.598(4) . ? Bi1 N2 2.609(4) . ? Bi1 O32 2.747(4) 3_364 ? Bi1 C27 2.851(6) . ? N1 C1 1.317(7) . ? N1 C12 1.360(6) . ? C1 C2 1.400(8) . ? N2 C10 1.321(7) . ? N2 C11 1.355(6) . ? C2 C3 1.366(8) . ? C3 C4 1.396(8) . ? C4 C12 1.414(7) . ? C4 C5 1.448(8) . ? C5 C6 1.305(9) . ? C6 C7 1.423(8) . ? C7 C11 1.396(7) . ? C7 C8 1.398(8) . ? C8 C9 1.359(8) . ? C9 C10 1.388(8) . ? C11 C12 1.434(8) . ? O21 C21 1.287(7) . ? O22 C27 1.282(7) . ? O23 C27 1.231(8) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C26 C27 1.484(7) . ? O31 C31 1.349(5) . ? O32 C37 1.287(6) . ? O32 Bi1 2.747(4) 3_364 ? O33 C37 1.219(6) . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.484(7) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.03(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 O31 Bi1 O32 81.77(14) . . ? O31 Bi1 O23 83.60(15) . . ? O32 Bi1 O23 80.31(15) . . ? O31 Bi1 O22 83.98(15) . . ? O32 Bi1 O22 131.26(14) . . ? O23 Bi1 O22 51.84(15) . . ? O31 Bi1 N1 80.36(14) . . ? O32 Bi1 N1 81.57(13) . . ? O23 Bi1 N1 157.29(14) . . ? O22 Bi1 N1 140.82(15) . . ? O31 Bi1 N2 84.09(14) . . ? O32 Bi1 N2 143.84(14) . . ? O23 Bi1 N2 130.81(15) . . ? O22 Bi1 N2 79.60(14) . . ? N1 Bi1 N2 63.28(14) . . ? O31 Bi1 O32 143.93(13) . 3_364 ? O32 Bi1 O32 65.59(15) . 3_364 ? O23 Bi1 O32 76.44(14) . 3_364 ? O22 Bi1 O32 105.68(13) . 3_364 ? N1 Bi1 O32 108.10(13) . 3_364 ? N2 Bi1 O32 131.48(13) . 3_364 ? O31 Bi1 C27 84.89(16) . . ? O32 Bi1 C27 105.4(2) . . ? O23 Bi1 C27 25.24(16) . . ? O22 Bi1 C27 26.72(17) . . ? N1 Bi1 C27 162.62(17) . . ? N2 Bi1 C27 106.2(2) . . ? O32 Bi1 C27 89.24(16) 3_364 . ? C1 N1 C12 118.0(5) . . ? C1 N1 Bi1 122.1(3) . . ? C12 N1 Bi1 119.9(3) . . ? N1 C1 C2 123.4(6) . . ? C10 N2 C11 118.0(5) . . ? C10 N2 Bi1 122.2(4) . . ? C11 N2 Bi1 119.8(4) . . ? C3 C2 C1 119.1(6) . . ? C2 C3 C4 119.4(6) . . ? C3 C4 C12 117.8(5) . . ? C3 C4 C5 123.9(6) . . ? C12 C4 C5 118.2(6) . . ? C6 C5 C4 122.1(6) . . ? C5 C6 C7 121.0(6) . . ? C11 C7 C8 117.5(5) . . ? C11 C7 C6 120.1(6) . . ? C8 C7 C6 122.4(6) . . ? C9 C8 C7 120.5(6) . . ? C8 C9 C10 117.9(6) . . ? N2 C10 C9 123.9(6) . . ? N2 C11 C7 122.2(6) . . ? N2 C11 C12 118.5(5) . . ? C7 C11 C12 119.4(5) . . ? N1 C12 C4 122.2(6) . . ? N1 C12 C11 118.6(5) . . ? C4 C12 C11 119.2(5) . . ? C27 O22 Bi1 88.2(4) . . ? C27 O23 Bi1 99.0(4) . . ? O21 C21 C22 117.5(5) . . ? O21 C21 C26 122.5(5) . . ? C22 C21 C26 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C27 119.4(5) . . ? C21 C26 C27 120.5(5) . . ? O23 C27 O22 120.5(6) . . ? O23 C27 C26 117.8(6) . . ? O22 C27 C26 121.7(7) . . ? O23 C27 Bi1 55.8(3) . . ? O22 C27 Bi1 65.1(3) . . ? C26 C27 Bi1 169.6(5) . . ? C31 O31 Bi1 129.1(3) . . ? C37 O32 Bi1 131.7(4) . . ? C37 O32 Bi1 104.6(3) . 3_364 ? Bi1 O32 Bi1 114.41(15) . 3_364 ? O31 C31 C32 113.2(3) . . ? O31 C31 C36 126.8(3) . . ? C32 C31 C36 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 C37 114.4(4) . . ? C31 C36 C37 125.4(4) . . ? O33 C37 O32 118.1(6) . . ? O33 C37 C36 121.5(5) . . ? O32 C37 C36 120.4(5) . . ? C42 C41 C46 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C44 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C47 C46 C45 119.4(7) . . ? C47 C46 C41 120.5(7) . . ? C45 C46 C41 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.601 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.082 #====END # End of Crystallographic Information File