#------------------------------------------------------------------------------ #$Date: 2015-12-31 12:29:25 +0000 (Thu, 31 Dec 2015) $ #$Revision: 171772 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112127.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7112127 loop_ _publ_author_name 'Tyler D. Boyd' 'Ish Kumar' 'Eric E. Wagner' 'Kenton H. Whitmire' _publ_section_title ; Synthesis and structural studies of the simplest bismuth(III) oxo-salicylate complex: [Bi4(mu3-O)2(HO-2-C6H4CO2)8].2Solv (Solv = MeCN or MeNO2) ; _journal_name_full Chem.Commun. _journal_page_first 3556 _journal_paper_doi 10.1039/C4CC00056K _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C56 H40 Bi4 O26, 2(C2 H3 N)' _chemical_formula_sum 'C60 H46 Bi4 N2 O26' _chemical_formula_weight 2046.91 _chemical_name_systematic ; tetrakis(salicylato)dioxotetrabismuth acetonitrile solvate ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _cell_angle_alpha 69.9520(10) _cell_angle_beta 68.4760(10) _cell_angle_gamma 77.0260(10) _cell_formula_units_Z 1 _cell_length_a 11.0416(9) _cell_length_b 11.4113(10) _cell_length_c 14.0227(12) _cell_measurement_reflns_used 7279 _cell_measurement_temperature 298(2) _cell_volume 1534.2(2) _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.949 _diffrn_measurement_device_type BRUKERSMART1000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_laue_measured_fraction_full 0.998 _diffrn_reflns_laue_measured_fraction_max 0.949 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 19036 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.949 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.341 _diffrn_reflns_theta_min 1.912 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 11.524 _exptl_absorpt_correction_T_max 0.056 _exptl_absorpt_correction_T_min 0.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 5.1,1997' _exptl_crystal_colour Brown _exptl_crystal_density_diffrn 2.216 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 960 _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _refine_diff_density_max 1.741 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.158 _refine_ls_extinction_coef 0.00434(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.221 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 420 _refine_ls_number_reflns 7278 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.221 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0256 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.0573 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5930 _reflns_number_total 7278 _reflns_threshold_expression 'I > 2\s(I)' _[local]_cod_data_source_file c4cc00056k.cif _[local]_cod_data_source_block abs _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_database_code 7112127 #BEGIN Tags that were not found in dictionaries: _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-2 _shelx_res_file ; TITL 1 in P-1 CELL 0.71073 11.0416 11.4113 14.0227 69.952 68.476 77.026 ZERR 1.00 0.0009 0.0010 0.0012 0.001 0.001 0.001 LATT 1 SFAC C H O BI N UNIT 60 46 26 4 2 TEMP 25.0 L.S. 100 BOND FMAP 2 PLAN 10 ACTA BOND $H BIND BI2 N1 EQIV_$1 -x+1, -y+2, -z MPLA 3 BI1 BI2 BI2_$1 O1 O1_$1 MPLA 4 BI1 BI2 BI1_$1 BI2_$1 O1 O1_$1 OMIT 0 0 1 WGHT 0.000000 EXTI 0.004340 FVAR 0.34704 1.85000 BI1 4 0.797648 0.869170 0.014234 11.00000 0.01705 0.02545 = 0.02999 -0.00702 -0.01100 0.00007 BI2 4 0.449214 0.986114 0.139867 11.00000 0.01822 0.03218 = 0.02907 -0.01077 -0.01123 -0.00022 O1 3 0.611688 0.934121 -0.001439 11.00000 0.01618 0.03205 = 0.03228 -0.01010 -0.01495 0.00438 O111 3 -0.080653 0.853688 0.187474 11.00000 0.03563 0.06312 = 0.05594 0.01112 -0.02584 -0.01280 AFIX 143 H111 2 -0.023771 0.897413 0.142986 11.00000 -1.50000 AFIX 0 O112 3 0.300449 0.833016 0.185451 11.00000 0.03917 0.04019 = 0.06072 0.00221 -0.02672 -0.01506 O113 3 0.132655 0.945569 0.131546 11.00000 0.03501 0.03042 = 0.04330 0.00270 -0.01547 -0.00477 O121 3 0.907901 1.162690 0.068334 11.00000 0.03295 0.03495 = 0.07727 -0.01692 -0.03052 0.00246 AFIX 147 H121 2 0.858903 1.107419 0.096067 11.00000 -1.50000 AFIX 0 O122 3 0.706358 1.057452 0.105575 11.00000 0.03732 0.03109 = 0.04092 -0.01008 -0.01794 -0.00663 O123 3 0.527599 1.176368 0.076572 11.00000 0.02593 0.03500 = 0.06269 -0.01737 -0.02056 -0.00231 O131 3 0.468134 0.665853 0.386716 11.00000 0.06048 0.08604 = 0.03890 -0.01199 -0.00232 -0.00157 AFIX 147 H131 2 0.512529 0.721466 0.342815 11.00000 -1.50000 AFIX 0 O132 3 0.628079 0.775756 0.202399 11.00000 0.03745 0.03309 = 0.04055 -0.01157 -0.01519 -0.00167 O133 3 0.731768 0.669415 0.085375 11.00000 0.04144 0.02880 = 0.04059 -0.01060 -0.00371 -0.00968 O141 3 0.811089 0.881440 -0.424037 11.00000 0.06123 0.11328 = 0.05483 -0.04186 -0.03043 0.03195 AFIX 147 H141 2 0.758826 0.898564 -0.370174 11.00000 -1.50000 AFIX 0 O142 3 0.871334 0.797600 -0.129185 11.00000 0.03483 0.03746 = 0.03270 -0.01334 -0.01384 0.00050 O143 3 0.742005 0.900026 -0.229182 11.00000 0.03142 0.06867 = 0.04149 -0.03124 -0.01596 0.01601 N1 5 0.476980 0.989347 0.347206 11.00000 0.07048 0.14842 = 0.07195 -0.04691 -0.03349 -0.00410 C1 1 0.571931 0.985362 0.360776 11.00000 0.06344 0.07446 = 0.04076 -0.01989 -0.02115 0.00179 C2 1 0.693622 0.982531 0.375766 11.00000 0.06670 0.16110 = 0.07363 -0.02843 -0.03273 -0.01478 AFIX 133 H2A 2 0.731736 0.897077 0.395799 11.00000 -1.50000 H2B 2 0.678955 1.020123 0.431285 11.00000 -1.50000 H2C 2 0.752095 1.028489 0.310304 11.00000 -1.50000 AFIX 0 C111 1 0.105286 0.738908 0.244095 11.00000 0.03353 0.03236 = 0.02822 -0.00315 -0.01271 -0.00821 C112 1 -0.024146 0.748568 0.245061 11.00000 0.03913 0.04660 = 0.03487 -0.00589 -0.01715 -0.01289 C113 1 -0.095009 0.646908 0.304094 11.00000 0.04491 0.07872 = 0.05259 0.00311 -0.01603 -0.03665 AFIX 43 H11A 2 -0.180834 0.652781 0.305117 11.00000 -1.20000 AFIX 0 C114 1 -0.041435 0.538678 0.360580 11.00000 0.07309 0.06084 = 0.05777 0.00905 -0.02146 -0.04081 AFIX 43 H11B 2 -0.090802 0.471587 0.399985 11.00000 -1.20000 AFIX 0 C115 1 0.084880 0.528107 0.359662 11.00000 0.06867 0.04027 = 0.05854 0.00941 -0.02578 -0.01618 AFIX 43 H11C 2 0.121472 0.453890 0.398162 11.00000 -1.20000 AFIX 0 C116 1 0.156733 0.626477 0.302270 11.00000 0.04102 0.03820 = 0.04875 -0.00128 -0.02001 -0.00694 AFIX 43 H11D 2 0.242591 0.618259 0.301962 11.00000 -1.20000 AFIX 0 C117 1 0.186377 0.845244 0.183593 11.00000 0.03462 0.02957 = 0.03030 -0.00984 -0.01558 -0.00108 C121 1 0.716951 1.276143 0.018748 11.00000 0.02430 0.02944 = 0.04010 -0.01394 -0.01368 0.00137 C122 1 0.844790 1.271084 0.020574 11.00000 0.03176 0.02793 = 0.04405 -0.01842 -0.01044 -0.00153 C123 1 0.907258 1.379047 -0.026429 11.00000 0.03471 0.04562 = 0.07587 -0.02961 -0.01099 -0.00918 AFIX 43 H12A 2 0.990350 1.376943 -0.023136 11.00000 -1.20000 AFIX 0 C124 1 0.848526 1.487684 -0.077153 11.00000 0.05034 0.03228 = 0.06860 -0.01674 -0.00218 -0.01358 AFIX 43 H12B 2 0.892662 1.558800 -0.109062 11.00000 -1.20000 AFIX 0 C125 1 0.724828 1.494972 -0.082435 11.00000 0.06430 0.02950 = 0.06376 -0.00911 -0.02316 -0.00138 AFIX 43 H12C 2 0.685849 1.569955 -0.117923 11.00000 -1.20000 AFIX 0 C126 1 0.659652 1.389257 -0.034238 11.00000 0.03985 0.03710 = 0.05830 -0.01328 -0.02594 0.00116 AFIX 43 H12D 2 0.575923 1.393627 -0.037194 11.00000 -1.20000 AFIX 0 C127 1 0.647162 1.164266 0.069222 11.00000 0.02599 0.03034 = 0.03587 -0.01631 -0.01057 -0.00281 C131 1 0.575822 0.567266 0.246177 11.00000 0.03336 0.03887 = 0.03841 -0.00072 -0.01461 -0.00731 C132 1 0.490182 0.568746 0.346260 11.00000 0.03639 0.05257 = 0.04230 -0.00046 -0.01811 -0.00117 C133 1 0.419545 0.466351 0.411077 11.00000 0.04234 0.07978 = 0.05143 0.01816 -0.01002 -0.01127 AFIX 43 H13A 2 0.362084 0.466310 0.478939 11.00000 -1.20000 AFIX 0 C134 1 0.436484 0.366023 0.372831 11.00000 0.07394 0.06396 = 0.07786 0.02394 -0.02864 -0.03434 AFIX 43 H13B 2 0.389088 0.298184 0.415287 11.00000 -1.20000 AFIX 0 C135 1 0.521468 0.363531 0.273714 11.00000 0.10306 0.05764 = 0.07055 -0.00263 -0.03415 -0.03446 AFIX 43 H13C 2 0.531370 0.294669 0.249309 11.00000 -1.20000 AFIX 0 C136 1 0.592509 0.463671 0.210023 11.00000 0.06636 0.04157 = 0.05500 -0.00041 -0.01547 -0.02209 AFIX 43 H13D 2 0.651425 0.461810 0.143045 11.00000 -1.20000 AFIX 0 C137 1 0.648495 0.675480 0.175064 11.00000 0.03153 0.03101 = 0.03678 -0.00550 -0.01910 -0.00235 C141 1 0.953004 0.813975 -0.313557 11.00000 0.02917 0.03086 = 0.03273 -0.01110 -0.00666 -0.00162 C142 1 0.929086 0.840050 -0.410061 11.00000 0.04365 0.04696 = 0.04117 -0.01739 -0.01117 0.00344 C143 1 1.030447 0.821384 -0.499946 11.00000 0.07001 0.07483 = 0.03219 -0.02140 -0.00417 0.00095 AFIX 43 H14A 2 1.014575 0.838975 -0.564438 11.00000 -1.20000 AFIX 0 C144 1 1.153911 0.776941 -0.493170 11.00000 0.05210 0.06755 = 0.05633 -0.02885 0.01194 -0.00642 AFIX 43 H14B 2 1.221271 0.764585 -0.553680 11.00000 -1.20000 AFIX 0 C145 1 1.180702 0.750129 -0.399000 11.00000 0.02513 0.07012 = 0.07910 -0.03350 -0.00274 0.00028 AFIX 43 H14C 2 1.265342 0.720954 -0.396086 11.00000 -1.20000 AFIX 0 C146 1 1.079798 0.767187 -0.308454 11.00000 0.02845 0.05490 = 0.05256 -0.02387 -0.00910 -0.00103 AFIX 43 H14D 2 1.096451 0.747442 -0.244011 11.00000 -1.20000 AFIX 0 C147 1 0.848324 0.837813 -0.217604 11.00000 0.02471 0.02933 = 0.03502 -0.01216 -0.00679 -0.00435 HKLF 4 REM 1 in P-1 REM R1 = 0.0256 for 5930 Fo > 4sig(Fo) and 0.0371 for all 7278 data REM 420 parameters refined using 0 restraints END WGHT 0.0267 1.0031 REM Highest difference peak 1.741, deepest hole -1.398, 1-sigma level 0.158 Q1 1 0.7771 0.8310 -0.0293 11.00000 0.05 1.74 Q2 1 0.4629 1.0248 0.1826 11.00000 0.05 1.66 Q3 1 0.8176 0.9059 0.0562 11.00000 0.05 1.63 Q4 1 0.4235 0.9554 0.1004 11.00000 0.05 1.59 Q5 1 0.8550 1.2447 0.1131 11.00000 0.05 1.45 Q6 1 0.0433 0.7246 0.1701 11.00000 0.05 1.36 Q7 1 0.3757 0.9745 0.1979 11.00000 0.05 1.30 Q8 1 0.7234 0.8644 0.0763 11.00000 0.05 1.29 Q9 1 0.8683 0.8756 -0.0419 11.00000 0.05 1.28 Q10 1 0.5195 0.9949 0.0807 11.00000 0.05 1.16 ; _shelx_res_checksum 96029 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Bi1 Bi 0.79765(2) 0.86917(2) 0.01423(2) 0.02379(6) Uani 1 1 d . . Bi2 Bi 0.44921(2) 0.98611(2) 0.13987(2) 0.02530(6) Uani 1 1 d . . O1 O 0.6117(2) 0.9341(3) -0.0014(2) 0.0257(6) Uani 1 1 d . . O111 O -0.0807(3) 0.8537(3) 0.1875(3) 0.0547(10) Uani 1 1 d . . H111 H -0.0238 0.8974 0.1430 0.082 Uiso 1 1 calc R U O112 O 0.3004(3) 0.8330(3) 0.1855(3) 0.0462(9) Uani 1 1 d . . O113 O 0.1327(3) 0.9456(3) 0.1315(2) 0.0388(7) Uani 1 1 d . . O121 O 0.9079(3) 1.1627(3) 0.0683(3) 0.0454(9) Uani 1 1 d . . H121 H 0.8589 1.1074 0.0961 0.068 Uiso 1 1 calc R U O122 O 0.7064(3) 1.0575(3) 0.1056(2) 0.0344(7) Uani 1 1 d . . O123 O 0.5276(3) 1.1764(3) 0.0766(3) 0.0386(8) Uani 1 1 d . . O131 O 0.4681(4) 0.6659(4) 0.3867(3) 0.0686(12) Uani 1 1 d . . H131 H 0.5125 0.7215 0.3428 0.103 Uiso 1 1 calc R U O132 O 0.6281(3) 0.7758(3) 0.2024(2) 0.0363(7) Uani 1 1 d . . O133 O 0.7318(3) 0.6694(3) 0.0854(2) 0.0385(7) Uani 1 1 d . . O141 O 0.8111(4) 0.8814(5) -0.4240(3) 0.0753(14) Uani 1 1 d . . H141 H 0.7588 0.8986 -0.3702 0.113 Uiso 1 1 calc R U O142 O 0.8713(3) 0.7976(3) -0.1292(2) 0.0340(7) Uani 1 1 d . . O143 O 0.7420(3) 0.9000(3) -0.2292(3) 0.0454(9) Uani 1 1 d . . N1 N 0.4770(6) 0.9893(7) 0.3472(5) 0.091(2) Uani 1 1 d . . C1 C 0.5719(6) 0.9854(6) 0.3608(4) 0.0589(16) Uani 1 1 d . . C2 C 0.6936(6) 0.9825(8) 0.3758(6) 0.098(3) Uani 1 1 d . . H2A H 0.7317 0.8971 0.3958 0.148 Uiso 1 1 calc R U H2B H 0.6790 1.0201 0.4313 0.148 Uiso 1 1 calc R U H2C H 0.7521 1.0285 0.3103 0.148 Uiso 1 1 calc R U C111 C 0.1053(4) 0.7389(4) 0.2441(3) 0.0312(9) Uani 1 1 d . . C112 C -0.0241(4) 0.7486(5) 0.2451(4) 0.0388(11) Uani 1 1 d . . C113 C -0.0950(5) 0.6469(6) 0.3041(4) 0.0595(16) Uani 1 1 d . . H11A H -0.1808 0.6528 0.3051 0.071 Uiso 1 1 calc R U C114 C -0.0414(6) 0.5387(6) 0.3606(5) 0.0651(17) Uani 1 1 d . . H11B H -0.0908 0.4716 0.4000 0.078 Uiso 1 1 calc R U C115 C 0.0849(6) 0.5281(5) 0.3597(4) 0.0589(15) Uani 1 1 d . . H11C H 0.1215 0.4539 0.3982 0.071 Uiso 1 1 calc R U C116 C 0.1567(5) 0.6265(5) 0.3023(4) 0.0436(12) Uani 1 1 d . . H11D H 0.2426 0.6183 0.3020 0.052 Uiso 1 1 calc R U C117 C 0.1864(4) 0.8452(4) 0.1836(3) 0.0300(9) Uani 1 1 d . . C121 C 0.7170(4) 1.2761(4) 0.0187(3) 0.0299(9) Uani 1 1 d . . C122 C 0.8448(4) 1.2711(4) 0.0206(4) 0.0331(10) Uani 1 1 d . . C123 C 0.9073(5) 1.3790(5) -0.0264(5) 0.0499(14) Uani 1 1 d . . H12A H 0.9904 1.3769 -0.0231 0.060 Uiso 1 1 calc R U C124 C 0.8485(5) 1.4877(5) -0.0772(4) 0.0532(14) Uani 1 1 d . . H12B H 0.8927 1.5588 -0.1091 0.064 Uiso 1 1 calc R U C125 C 0.7248(6) 1.4950(5) -0.0824(5) 0.0535(14) Uani 1 1 d . . H12C H 0.6858 1.5700 -0.1179 0.064 Uiso 1 1 calc R U C126 C 0.6597(5) 1.3893(5) -0.0342(4) 0.0431(12) Uani 1 1 d . . H12D H 0.5759 1.3936 -0.0372 0.052 Uiso 1 1 calc R U C127 C 0.6472(4) 1.1643(4) 0.0692(3) 0.0287(9) Uani 1 1 d . . C131 C 0.5758(4) 0.5673(4) 0.2462(4) 0.0382(11) Uani 1 1 d . . C132 C 0.4902(5) 0.5687(5) 0.3463(4) 0.0464(12) Uani 1 1 d . . C133 C 0.4195(5) 0.4664(7) 0.4111(5) 0.0687(19) Uani 1 1 d . . H13A H 0.3621 0.4663 0.4789 0.082 Uiso 1 1 calc R U C134 C 0.4365(6) 0.3660(7) 0.3728(6) 0.078(2) Uani 1 1 d . . H13B H 0.3891 0.2982 0.4153 0.094 Uiso 1 1 calc R U C135 C 0.5215(7) 0.3635(6) 0.2737(5) 0.0750(19) Uani 1 1 d . . H13C H 0.5314 0.2947 0.2493 0.090 Uiso 1 1 calc R U C136 C 0.5925(6) 0.4637(5) 0.2100(5) 0.0564(15) Uani 1 1 d . . H13D H 0.6514 0.4618 0.1430 0.068 Uiso 1 1 calc R U C137 C 0.6485(4) 0.6755(4) 0.1751(4) 0.0320(10) Uani 1 1 d . . C141 C 0.9530(4) 0.8140(4) -0.3136(3) 0.0316(10) Uani 1 1 d . . C142 C 0.9291(5) 0.8400(5) -0.4101(4) 0.0448(12) Uani 1 1 d . . C143 C 1.0304(6) 0.8214(6) -0.4999(4) 0.0625(16) Uani 1 1 d . . H14A H 1.0146 0.8390 -0.5644 0.075 Uiso 1 1 calc R U C144 C 1.1539(6) 0.7769(6) -0.4932(5) 0.0643(17) Uani 1 1 d . . H14B H 1.2213 0.7646 -0.5537 0.077 Uiso 1 1 calc R U C145 C 1.1807(5) 0.7501(6) -0.3990(5) 0.0599(16) Uani 1 1 d . . H14C H 1.2653 0.7210 -0.3961 0.072 Uiso 1 1 calc R U C146 C 1.0798(4) 0.7672(5) -0.3085(4) 0.0447(12) Uani 1 1 d . . H14D H 1.0965 0.7474 -0.2440 0.054 Uiso 1 1 calc R U C147 C 0.8483(4) 0.8378(4) -0.2176(3) 0.0295(9) 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 Bi1 0.01705(8) 0.02545(9) 0.02999(9) -0.00702(7) -0.01100(7) 0.00007(6) Bi2 0.01822(8) 0.03218(10) 0.02907(9) -0.01077(7) -0.01123(7) -0.00022(6) O1 0.0162(13) 0.0321(16) 0.0323(15) -0.0101(13) -0.0149(12) 0.0044(11) O111 0.0356(18) 0.063(2) 0.056(2) 0.0111(19) -0.0258(17) -0.0128(17) O112 0.0392(19) 0.040(2) 0.061(2) 0.0022(17) -0.0267(17) -0.0151(15) O113 0.0350(17) 0.0304(17) 0.0433(18) 0.0027(14) -0.0155(15) -0.0048(14) O121 0.0330(17) 0.0349(19) 0.077(3) -0.0169(18) -0.0305(18) 0.0025(14) O122 0.0373(17) 0.0311(17) 0.0409(17) -0.0101(14) -0.0179(14) -0.0066(14) O123 0.0259(15) 0.0350(18) 0.063(2) -0.0174(16) -0.0206(15) -0.0023(13) O131 0.060(3) 0.086(3) 0.039(2) -0.012(2) -0.0023(19) -0.002(2) O132 0.0374(17) 0.0331(18) 0.0406(18) -0.0116(15) -0.0152(15) -0.0017(14) O133 0.0414(18) 0.0288(17) 0.0406(18) -0.0106(14) -0.0037(15) -0.0097(14) O141 0.061(3) 0.113(4) 0.055(3) -0.042(3) -0.030(2) 0.032(3) O142 0.0348(16) 0.0375(18) 0.0327(16) -0.0133(14) -0.0138(14) 0.0005(14) O143 0.0314(17) 0.069(2) 0.0415(19) -0.0312(18) -0.0160(15) 0.0160(16) N1 0.070(4) 0.148(6) 0.072(4) -0.047(4) -0.033(3) -0.004(4) C1 0.063(4) 0.074(4) 0.041(3) -0.020(3) -0.021(3) 0.002(3) C2 0.067(4) 0.161(8) 0.074(5) -0.028(5) -0.033(4) -0.015(5) C111 0.034(2) 0.032(2) 0.028(2) -0.0032(19) -0.0127(19) -0.0082(19) C112 0.039(3) 0.047(3) 0.035(3) -0.006(2) -0.017(2) -0.013(2) C113 0.045(3) 0.079(4) 0.053(3) 0.003(3) -0.016(3) -0.037(3) C114 0.073(4) 0.061(4) 0.058(4) 0.009(3) -0.021(3) -0.041(3) C115 0.069(4) 0.040(3) 0.059(4) 0.009(3) -0.026(3) -0.016(3) C116 0.041(3) 0.038(3) 0.049(3) -0.001(2) -0.020(2) -0.007(2) C117 0.035(2) 0.030(2) 0.030(2) -0.0098(19) -0.0156(19) -0.0011(19) C121 0.024(2) 0.029(2) 0.040(2) -0.014(2) -0.0137(19) 0.0014(17) C122 0.032(2) 0.028(2) 0.044(3) -0.018(2) -0.010(2) -0.0015(18) C123 0.035(3) 0.046(3) 0.076(4) -0.030(3) -0.011(3) -0.009(2) C124 0.050(3) 0.032(3) 0.069(4) -0.017(3) -0.002(3) -0.014(2) C125 0.064(4) 0.029(3) 0.064(4) -0.009(3) -0.023(3) -0.001(3) C126 0.040(3) 0.037(3) 0.058(3) -0.013(2) -0.026(2) 0.001(2) C127 0.026(2) 0.030(2) 0.036(2) -0.0163(19) -0.0106(18) -0.0028(17) C131 0.033(2) 0.039(3) 0.038(3) -0.001(2) -0.015(2) -0.007(2) C132 0.036(3) 0.053(3) 0.042(3) 0.000(3) -0.018(2) -0.001(2) C133 0.042(3) 0.080(5) 0.051(4) 0.018(3) -0.010(3) -0.011(3) C134 0.074(5) 0.064(5) 0.078(5) 0.024(4) -0.029(4) -0.034(4) C135 0.103(5) 0.058(4) 0.071(4) -0.003(3) -0.034(4) -0.034(4) C136 0.066(4) 0.042(3) 0.055(3) 0.000(3) -0.015(3) -0.022(3) C137 0.032(2) 0.031(2) 0.037(2) -0.005(2) -0.019(2) -0.0024(19) C141 0.029(2) 0.031(2) 0.033(2) -0.0111(19) -0.0067(19) -0.0016(18) C142 0.044(3) 0.047(3) 0.041(3) -0.017(2) -0.011(2) 0.003(2) C143 0.070(4) 0.075(4) 0.032(3) -0.021(3) -0.004(3) 0.001(3) C144 0.052(4) 0.068(4) 0.056(4) -0.029(3) 0.012(3) -0.006(3) C145 0.025(3) 0.070(4) 0.079(4) -0.033(4) -0.003(3) 0.000(3) C146 0.028(2) 0.055(3) 0.053(3) -0.024(3) -0.009(2) -0.001(2) C147 0.025(2) 0.029(2) 0.035(2) -0.0122(19) -0.0068(19) -0.0043(18) 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O1 Bi1 O142 93.96(10) . . O1 Bi1 O133 87.07(11) . . O142 Bi1 O133 77.67(11) . . O1 Bi1 O113 85.58(10) . 2_675 O142 Bi1 O113 77.27(11) . 2_675 O133 Bi1 O113 153.28(11) . 2_675 O1 Bi1 O132 73.42(10) . . O142 Bi1 O132 128.21(10) . . O133 Bi1 O132 52.25(10) . . O113 Bi1 O132 147.08(9) 2_675 . O1 Bi1 O122 74.47(9) . . O142 Bi1 O122 151.49(10) . . O133 Bi1 O122 126.37(10) . . O113 Bi1 O122 75.94(10) 2_675 . O132 Bi1 O122 74.17(9) . . O1 Bi1 C137 78.72(11) . . O142 Bi1 C137 102.57(12) . . O133 Bi1 C137 25.80(11) . . O113 Bi1 C137 164.27(11) 2_675 . O132 Bi1 C137 26.46(10) . . O122 Bi1 C137 100.57(11) . . O1 Bi2 O123 79.95(11) 2_675 . O1 Bi2 O1 71.46(10) 2_675 . O123 Bi2 O1 86.98(10) . . O1 Bi2 O143 87.00(10) 2_675 2_675 O123 Bi2 O143 82.30(12) . 2_675 O1 Bi2 O143 157.35(10) . 2_675 O1 Bi2 O112 83.60(11) 2_675 . O123 Bi2 O112 158.89(11) . . O1 Bi2 O112 100.27(11) . . O143 Bi2 O112 83.72(12) 2_675 . O1 Bi2 N1 153.81(15) 2_675 . O123 Bi2 N1 82.58(16) . . O1 Bi2 N1 126.97(13) . . O143 Bi2 N1 71.38(14) 2_675 . O112 Bi2 N1 107.74(15) . . O1 Bi2 Bi2 37.21(7) 2_675 2_675 O123 Bi2 Bi2 82.11(8) . 2_675 O1 Bi2 Bi2 34.26(6) . 2_675 O143 Bi2 Bi2 123.88(8) 2_675 2_675 O112 Bi2 Bi2 92.73(8) . 2_675 N1 Bi2 Bi2 156.39(12) . 2_675 Bi1 O1 Bi2 130.93(13) . 2_675 Bi1 O1 Bi2 117.87(11) . . Bi2 O1 Bi2 108.54(10) 2_675 . C112 O111 H111 109.5 . . C117 O112 Bi2 131.8(3) . . C117 O113 Bi1 137.5(3) . 2_675 C122 O121 H121 109.5 . . C127 O122 Bi1 127.1(3) . . C127 O123 Bi2 111.4(3) . . C132 O131 H131 109.5 . . C137 O132 Bi1 86.6(3) . . C137 O133 Bi1 101.6(3) . . C142 O141 H141 109.5 . . C147 O142 Bi1 131.9(3) . . C147 O143 Bi2 141.1(3) . 2_675 C1 N1 Bi2 125.3(5) . . N1 C1 C2 178.7(8) . . C1 C2 H2A 109.5 . . C1 C2 H2B 109.5 . . H2A C2 H2B 109.5 . . C1 C2 H2C 109.5 . . H2A C2 H2C 109.5 . . H2B C2 H2C 109.5 . . C116 C111 C112 118.0(4) . . C116 C111 C117 120.2(4) . . C112 C111 C117 121.8(4) . . O111 C112 C113 119.1(4) . . O111 C112 C111 121.9(4) . . C113 C112 C111 119.0(5) . . C114 C113 C112 121.2(5) . . C114 C113 H11A 119.4 . . C112 C113 H11A 119.4 . . C113 C114 C115 120.2(5) . . C113 C114 H11B 119.9 . . C115 C114 H11B 119.9 . . C116 C115 C114 119.8(5) . . C116 C115 H11C 120.1 . . C114 C115 H11C 120.1 . . C115 C116 C111 121.7(5) . . C115 C116 H11D 119.1 . . C111 C116 H11D 119.1 . . O112 C117 O113 123.6(4) . . O112 C117 C111 119.7(4) . . O113 C117 C111 116.6(4) . . C126 C121 C122 118.4(4) . . C126 C121 C127 120.8(4) . . C122 C121 C127 120.8(4) . . O121 C122 C123 119.2(4) . . O121 C122 C121 121.5(4) . . C123 C122 C121 119.3(4) . . C124 C123 C122 120.7(5) . . C124 C123 H12A 119.7 . . C122 C123 H12A 119.7 . . C123 C124 C125 121.4(5) . . C123 C124 H12B 119.3 . . C125 C124 H12B 119.3 . . C124 C125 C126 118.9(5) . . C124 C125 H12C 120.5 . . C126 C125 H12C 120.5 . . C125 C126 C121 121.2(5) . . C125 C126 H12D 119.4 . . C121 C126 H12D 119.4 . . O123 C127 O122 121.2(4) . . O123 C127 C121 118.5(4) . . O122 C127 C121 120.3(4) . . C132 C131 C136 119.9(5) . . C132 C131 C137 121.1(5) . . C136 C131 C137 119.0(4) . . O131 C132 C131 123.4(5) . . O131 C132 C133 116.6(5) . . C131 C132 C133 120.0(6) . . C134 C133 C132 118.9(6) . . C134 C133 H13A 120.5 . . C132 C133 H13A 120.5 . . C135 C134 C133 121.5(6) . . C135 C134 H13B 119.2 . . C133 C134 H13B 119.2 . . C134 C135 C136 119.7(6) . . C134 C135 H13C 120.1 . . C136 C135 H13C 120.1 . . C135 C136 C131 119.9(6) . . C135 C136 H13D 120.0 . . C131 C136 H13D 120.0 . . O133 C137 O132 119.5(4) . . O133 C137 C131 119.9(4) . . O132 C137 C131 120.7(4) . . O133 C137 Bi1 52.6(2) . . O132 C137 Bi1 67.0(2) . . C131 C137 Bi1 172.0(3) . . C142 C141 C146 119.0(4) . . C142 C141 C147 121.4(4) . . C146 C141 C147 119.5(4) . . O141 C142 C143 115.3(5) . . O141 C142 C141 124.5(4) . . C143 C142 C141 120.1(5) . . C144 C143 C142 119.7(5) . . C144 C143 H14A 120.2 . . C142 C143 H14A 120.2 . . C143 C144 C145 121.6(5) . . C143 C144 H14B 119.2 . . C145 C144 H14B 119.2 . . C144 C145 C146 119.1(5) . . C144 C145 H14C 120.4 . . C146 C145 H14C 120.4 . . C145 C146 C141 120.4(5) . . C145 C146 H14D 119.8 . . C141 C146 H14D 119.8 . . O143 C147 O142 123.7(4) . . O143 C147 C141 118.0(4) . . O142 C147 C141 118.3(4) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Bi1 O1 2.086(2) . Bi1 O142 2.236(3) . Bi1 O133 2.318(3) . Bi1 O113 2.419(3) 2_675 Bi1 O132 2.636(3) . Bi1 O122 2.691(3) . Bi1 C137 2.859(4) . Bi2 O1 2.126(3) 2_675 Bi2 O123 2.282(3) . Bi2 O1 2.284(3) . Bi2 O143 2.379(3) 2_675 Bi2 O112 2.431(3) . Bi2 N1 3.047(5) . Bi2 Bi2 3.5811(4) 2_675 O1 Bi2 2.126(3) 2_675 O111 C112 1.360(5) . O111 H111 0.8200 . O112 C117 1.245(5) . O113 C117 1.279(5) . O113 Bi1 2.419(3) 2_675 O121 C122 1.361(5) . O121 H121 0.8200 . O122 C127 1.278(5) . O123 C127 1.265(5) . O131 C132 1.348(6) . O131 H131 0.8200 . O132 C137 1.276(5) . O133 C137 1.271(5) . O141 C142 1.344(6) . O141 H141 0.8200 . O142 C147 1.265(5) . O143 C147 1.263(5) . O143 Bi2 2.379(3) 2_675 N1 C1 1.121(7) . C1 C2 1.426(8) . C2 H2A 0.9600 . C2 H2B 0.9600 . C2 H2C 0.9600 . C111 C116 1.389(6) . C111 C112 1.404(6) . C111 C117 1.489(6) . C112 C113 1.385(7) . C113 C114 1.359(8) . C113 H11A 0.9300 . C114 C115 1.368(8) . C114 H11B 0.9300 . C115 C116 1.360(7) . C115 H11C 0.9300 . C116 H11D 0.9300 . C121 C126 1.393(6) . C121 C122 1.409(6) . C121 C127 1.465(6) . C122 C123 1.385(6) . C123 C124 1.355(7) . C123 H12A 0.9300 . C124 C125 1.377(7) . C124 H12B 0.9300 . C125 C126 1.380(7) . C125 H12C 0.9300 . C126 H12D 0.9300 . C131 C132 1.378(7) . C131 C136 1.390(7) . C131 C137 1.475(6) . C132 C133 1.400(8) . C133 C134 1.373(9) . C133 H13A 0.9300 . C134 C135 1.368(9) . C134 H13B 0.9300 . C135 C136 1.381(8) . C135 H13C 0.9300 . C136 H13D 0.9300 . C141 C142 1.393(6) . C141 C146 1.401(6) . C141 C147 1.480(6) . C142 C143 1.389(7) . C143 C144 1.370(8) . C143 H14A 0.9300 . C144 C145 1.376(8) . C144 H14B 0.9300 . C145 C146 1.388(7) . C145 H14C 0.9300 . C146 H14D 0.9300 .