#------------------------------------------------------------------------------ #$Date: 2020-07-06 06:52:44 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253998 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240351.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_7240351 loop_ _publ_author_name 'Fritzsche, Ana-Maria' 'Scholz, Sebastian' 'Krasowska, Ma\/lgorzata' 'Bhattacharyya, Kalishankar' 'Toma, Ana Maria' 'Silvestru, Cristian' 'Korb, Marcus' 'R\"uffer, Tobias' 'Lang, Heinrich' 'Auer, Alexander A.' 'Mehring, Michael' _publ_section_title ; Evaluation of bismuth-based dispersion energy donors - synthesis, structure and theoretical study of 2-biphenylbismuth(iii) derivatives. ; _journal_issue 18 _journal_name_full 'Physical chemistry chemical physics : PCCP' _journal_page_first 10189 _journal_page_last 10211 _journal_paper_doi 10.1039/c9cp06924k _journal_volume 22 _journal_year 2020 _chemical_formula_moiety 'C25 H21 Bi' _chemical_formula_sum 'C25 H21 Bi' _chemical_formula_weight 530.40 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2013 _audit_update_record ; 2020-04-16 deposited with the CCDC. 2020-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.773(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.1772(5) _cell_length_b 6.7889(3) _cell_length_c 19.2090(7) _cell_measurement_reflns_used 10804 _cell_measurement_temperature 100 _cell_measurement_theta_max 67.5560 _cell_measurement_theta_min 4.0090 _cell_volume 1950.51(13) _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.970 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_device_type 'rigaku oxford gemini s' _diffrn_measurement_method 'w\ scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_unetI/netI 0.0413 _diffrn_reflns_Laue_measured_fraction_full 0.970 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 28460 _diffrn_reflns_point_group_measured_fraction_full 0.900 _diffrn_reflns_point_group_measured_fraction_max 0.899 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 67.800 _diffrn_reflns_theta_min 2.954 _exptl_absorpt_coefficient_mu 17.710 _exptl_absorpt_correction_T_max 0.673 _exptl_absorpt_correction_T_min 0.023 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.806 _exptl_crystal_description needle _exptl_crystal_F_000 1016 _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _refine_diff_density_max 4.754 _refine_diff_density_min -1.543 _refine_diff_density_rms 0.227 _refine_ls_abs_structure_details ; Flack x determined using 2097 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.059(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 469 _refine_ls_number_reflns 6360 _refine_ls_number_restraints 37 _refine_ls_restrained_S_all 1.089 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0533 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+5.1701P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1422 _refine_ls_wR_factor_ref 0.1489 _reflns_Friedel_coverage 0.699 _reflns_Friedel_fraction_full 0.816 _reflns_Friedel_fraction_max 0.814 _reflns_number_gt 5599 _reflns_number_total 6360 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cp06924k2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7240350--7240358.cif.' _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 7240351 _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. ; _oxdiff_exptl_absorpt_empirical_full_min 0.600 _oxdiff_exptl_absorpt_empirical_full_max 2.197 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelxl_version_number 2013-4 _shelx_res_file ; TITL ss062 P 21 CELL 1.54184 15.1772 6.7889 19.2090 90.000 99.773 90.000 ZERR 4.00 0.0005 0.0003 0.0007 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H BI UNIT 100 84 4 MERG 2 OMIT -10 -3 19 OMIT -11 -3 18 OMIT -12 -3 17 OMIT -10 -4 17 OMIT -17 0 10 OMIT -6 1 15 RIGU C44 C45 C46 C47 C48 C49 OMIT -11 -4 2 OMIT -11 -6 2 OMIT -10 5 6 OMIT 0 0 22 FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 10 WGHT 0.099300 5.170100 FVAR 2.34572 C1 1 0.905099 -0.411886 0.188713 11.00000 0.04268 0.04055 = 0.05311 -0.00702 0.01226 0.00654 AFIX 33 H1A 2 0.906525 -0.498756 0.149486 11.00000 -1.50000 H1B 2 0.852413 -0.331362 0.179446 11.00000 -1.50000 H1C 2 0.904260 -0.488119 0.230688 11.00000 -1.50000 AFIX 0 C2 1 0.967205 0.013163 0.125230 11.00000 0.02851 0.03819 = 0.03701 0.00055 0.00944 0.01069 C3 1 0.879705 -0.006702 0.088706 11.00000 0.01966 0.04177 = 0.03506 0.00048 0.00400 0.00882 AFIX 43 H3 2 0.843668 -0.106936 0.101242 11.00000 -1.20000 AFIX 0 C4 1 0.845724 0.120158 0.034204 11.00000 0.02278 0.03500 = 0.05430 -0.00428 -0.00975 0.00901 AFIX 43 H4 2 0.787059 0.106200 0.011071 11.00000 -1.20000 AFIX 0 C5 1 0.899462 0.268210 0.014194 11.00000 0.04918 0.03749 = 0.03745 -0.00841 0.00587 0.00706 AFIX 43 H5 2 0.877085 0.350651 -0.023325 11.00000 -1.20000 AFIX 0 C6 1 0.984776 0.293751 0.049093 11.00000 0.04811 0.02416 = 0.04099 -0.01119 0.01224 -0.00869 AFIX 43 H6 2 1.019727 0.394682 0.035589 11.00000 -1.20000 AFIX 0 C7 1 1.020411 0.168734 0.105367 11.00000 0.03168 0.02934 = 0.04117 -0.00510 0.01241 0.00579 C8 1 1.112954 0.202149 0.142664 11.00000 0.02910 0.02812 = 0.04971 0.00643 0.00623 -0.01028 C9 1 1.130194 0.230018 0.211928 11.00000 0.01160 0.05719 = 0.03760 -0.03125 0.00937 -0.01634 AFIX 43 H9 2 1.082537 0.243186 0.236282 11.00000 -1.20000 AFIX 0 C10 1 1.219063 0.240593 0.250558 11.00000 0.04271 0.04836 = 0.04891 -0.00612 0.01095 -0.00697 AFIX 43 H10 2 1.230139 0.238062 0.299676 11.00000 -1.20000 AFIX 0 C11 1 1.287645 0.254652 0.212472 11.00000 0.03528 0.07572 = 0.05608 -0.01367 0.00886 -0.01233 AFIX 43 H11 2 1.345530 0.279139 0.235650 11.00000 -1.20000 AFIX 0 C12 1 1.271266 0.232806 0.140527 11.00000 0.04065 0.03449 = 0.05551 -0.00616 0.02190 -0.00901 AFIX 43 H12 2 1.318479 0.230920 0.115361 11.00000 -1.20000 AFIX 0 C13 1 1.183593 0.213425 0.105207 11.00000 0.03309 0.05110 = 0.04605 -0.00668 0.01057 -0.00336 AFIX 43 H13 2 1.172199 0.207977 0.056123 11.00000 -1.20000 AFIX 0 C14 1 0.980401 -0.072302 0.296278 11.00000 0.02546 0.01482 = 0.03172 -0.00578 0.00653 -0.00203 C15 1 0.913582 0.073375 0.286173 11.00000 0.02154 0.02970 = 0.02871 -0.00581 0.00569 -0.00558 AFIX 43 H15 2 0.892993 0.118238 0.240568 11.00000 -1.20000 AFIX 0 C16 1 0.876970 0.153227 0.341658 11.00000 0.02074 0.02278 = 0.05453 -0.00358 0.00639 -0.00539 AFIX 43 H16 2 0.834389 0.252744 0.333177 11.00000 -1.20000 AFIX 0 C17 1 0.904988 0.081974 0.410704 11.00000 0.02494 0.02752 = 0.05007 -0.00751 0.01282 -0.00578 AFIX 43 H17 2 0.879199 0.128596 0.448102 11.00000 -1.20000 AFIX 0 C18 1 0.972144 -0.059795 0.421722 11.00000 0.03205 0.03985 = 0.03244 0.00297 0.00413 -0.00464 AFIX 43 H18 2 0.993440 -0.103422 0.467372 11.00000 -1.20000 AFIX 0 C19 1 1.008582 -0.138710 0.364519 11.00000 0.02253 0.02185 = 0.04769 0.00328 -0.00247 -0.00640 C20 1 1.078629 -0.295931 0.382629 11.00000 0.02141 0.02865 = 0.03481 -0.00367 -0.00345 -0.00301 C21 1 1.056352 -0.484569 0.394825 11.00000 0.02935 0.02493 = 0.04709 -0.00197 0.00709 -0.00428 AFIX 43 H21 2 0.996115 -0.517620 0.389506 11.00000 -1.20000 AFIX 0 C22 1 1.120356 -0.632402 0.415166 11.00000 0.04074 0.02948 = 0.04568 0.00024 0.00348 0.00425 AFIX 43 H22 2 1.103429 -0.761140 0.422903 11.00000 -1.20000 AFIX 0 C23 1 1.211034 -0.578257 0.423386 11.00000 0.03869 0.04061 = 0.03967 0.00818 0.00481 0.00976 AFIX 43 H23 2 1.255421 -0.670110 0.439118 11.00000 -1.20000 AFIX 0 C24 1 1.233479 -0.391245 0.408244 11.00000 0.02900 0.03827 = 0.05395 -0.00690 0.00110 -0.00086 AFIX 43 H24 2 1.293519 -0.357967 0.411814 11.00000 -1.20000 AFIX 0 C25 1 1.169482 -0.250507 0.387809 11.00000 0.03064 0.02942 = 0.05382 0.00373 0.01055 -0.00838 AFIX 43 H25 2 1.186579 -0.123872 0.377309 11.00000 -1.20000 AFIX 0 C31 1 0.676446 0.091184 0.191983 11.00000 0.03594 0.05140 = 0.04765 0.00397 -0.00114 -0.00001 AFIX 33 H31A 2 0.658029 0.004060 0.152854 11.00000 -1.50000 H31B 2 0.696084 0.015216 0.233898 11.00000 -1.50000 H31C 2 0.724658 0.172596 0.182307 11.00000 -1.50000 AFIX 0 C32 1 0.585265 0.516790 0.128329 11.00000 0.02291 0.03750 = 0.03854 0.00731 -0.00359 -0.00487 C33 1 0.656231 0.497253 0.090384 11.00000 0.02767 0.03946 = 0.04522 0.00429 0.00323 0.00053 AFIX 43 H33 2 0.697880 0.397172 0.102388 11.00000 -1.20000 AFIX 0 C34 1 0.665473 0.623010 0.035819 11.00000 0.04121 0.05372 = 0.04539 -0.00524 0.01137 -0.00591 AFIX 43 H34 2 0.712858 0.608582 0.011244 11.00000 -1.20000 AFIX 0 C35 1 0.603924 0.769148 0.018423 11.00000 0.04324 0.03451 = 0.03638 0.00337 0.00191 -0.02119 AFIX 43 H35 2 0.609908 0.854046 -0.018484 11.00000 -1.20000 AFIX 0 C36 1 0.532563 0.794692 0.054293 11.00000 0.03236 0.01850 = 0.04471 -0.00065 -0.00540 -0.00364 AFIX 43 H36 2 0.491189 0.894740 0.041272 11.00000 -1.20000 AFIX 0 C37 1 0.523526 0.667027 0.110770 11.00000 0.03846 0.02241 = 0.04188 -0.00351 -0.00714 -0.00943 C38 1 0.448025 0.697427 0.149073 11.00000 0.03217 0.01998 = 0.05332 -0.00528 0.00569 0.00155 C39 1 0.359999 0.714291 0.112893 11.00000 0.02792 0.03586 = 0.04520 -0.00831 -0.00847 0.00693 AFIX 43 H39 2 0.348831 0.713030 0.063770 11.00000 -1.20000 AFIX 0 C40 1 0.289936 0.732713 0.149586 11.00000 0.04138 0.03170 = 0.04595 -0.00621 0.00016 0.00833 AFIX 43 H40 2 0.231719 0.738521 0.124897 11.00000 -1.20000 AFIX 0 C41 1 0.304432 0.742470 0.220808 11.00000 0.03680 0.05103 = 0.05683 -0.01423 0.00529 0.00783 AFIX 43 H41 2 0.256299 0.754235 0.244718 11.00000 -1.20000 AFIX 0 C42 1 0.390536 0.735041 0.258321 11.00000 0.04693 0.04137 = 0.04187 -0.00083 0.00205 0.01412 AFIX 43 H42 2 0.401204 0.738900 0.307429 11.00000 -1.20000 AFIX 0 C43 1 0.461311 0.721525 0.220251 11.00000 0.02139 0.04945 = 0.02867 -0.01655 -0.00823 0.00640 AFIX 43 H43 2 0.519609 0.729362 0.244676 11.00000 -1.20000 AFIX 0 C44 1 0.650889 0.425824 0.300283 11.00000 0.01723 0.01645 = 0.04741 -0.00604 0.00545 0.00262 C45 1 0.711494 0.575163 0.286975 11.00000 0.02449 0.02497 = 0.04340 -0.00637 0.00618 -0.00062 AFIX 43 H45 2 0.709876 0.621972 0.241275 11.00000 -1.20000 AFIX 0 C46 1 0.771859 0.649717 0.340992 11.00000 0.02640 0.02453 = 0.05035 -0.00700 0.00704 -0.00599 AFIX 43 H46 2 0.810844 0.747513 0.331124 11.00000 -1.20000 AFIX 0 C47 1 0.777541 0.586955 0.408974 11.00000 0.02714 0.02035 = 0.04788 -0.00625 0.00753 0.00533 AFIX 43 H47 2 0.819641 0.639629 0.444998 11.00000 -1.20000 AFIX 0 C48 1 0.717236 0.438916 0.422949 11.00000 0.03005 0.02946 = 0.04395 -0.00033 0.00282 0.00132 AFIX 43 H48 2 0.719914 0.392151 0.468767 11.00000 -1.20000 AFIX 0 C49 1 0.654434 0.363357 0.369065 11.00000 0.02117 0.02096 = 0.04527 -0.00296 0.00462 0.00356 C50 1 0.593618 0.201490 0.389187 11.00000 0.02792 0.02609 = 0.04742 -0.00095 -0.00356 -0.00042 C51 1 0.499938 0.247355 0.381591 11.00000 0.03279 0.06077 = 0.04953 -0.00991 0.00577 -0.00384 AFIX 43 H51 2 0.477207 0.366506 0.362498 11.00000 -1.20000 AFIX 0 C52 1 0.445375 0.106813 0.403875 11.00000 0.01990 0.05659 = 0.05285 -0.01227 0.01197 -0.00673 AFIX 43 H52 2 0.384238 0.130479 0.398491 11.00000 -1.20000 AFIX 0 C53 1 0.479550 -0.070779 0.434425 11.00000 0.04300 0.06316 = 0.04670 0.00497 0.00418 -0.02746 AFIX 43 H53 2 0.441955 -0.160129 0.451516 11.00000 -1.20000 AFIX 0 C54 1 0.569433 -0.112230 0.438983 11.00000 0.04896 0.04387 = 0.06891 0.01697 -0.00255 -0.02158 AFIX 43 H54 2 0.592151 -0.233179 0.456308 11.00000 -1.20000 AFIX 0 C55 1 0.625001 0.027027 0.417663 11.00000 0.03012 0.02943 = 0.05295 0.00507 0.00642 0.00094 AFIX 43 H55 2 0.685919 0.000853 0.422918 11.00000 -1.20000 AFIX 0 BI1 3 1.027417 -0.218005 0.204019 11.00000 0.02300 0.02721 = 0.03551 0.00170 0.00428 0.00300 BI2 3 0.561594 0.280959 0.207993 11.00000 0.02154 0.02704 = 0.03616 0.00092 0.00096 -0.00198 HKLF 4 REM ss062 P 21 REM R1 = 0.0533 for 5599 Fo > 4sig(Fo) and 0.0591 for all 6360 data REM 469 parameters refined using 37 restraints END WGHT 0.0988 4.9947 REM Highest difference peak 4.754, deepest hole -1.543, 1-sigma level 0.227 Q1 1 0.5571 0.2815 0.1580 11.00000 0.05 4.75 Q2 1 1.0366 -0.2187 0.2542 11.00000 0.05 4.55 Q3 1 1.0219 -0.2193 0.1525 11.00000 0.05 4.54 Q4 1 0.5690 0.2809 0.2590 11.00000 0.05 3.91 Q5 1 0.5999 0.7807 0.2079 11.00000 0.05 3.83 Q6 1 0.9946 0.2794 0.2050 11.00000 0.05 2.46 Q7 1 0.1667 0.7809 0.2065 11.00000 0.05 1.93 Q8 1 0.6956 0.2799 0.2041 11.00000 0.05 1.93 Q9 1 1.1325 0.2814 0.2083 11.00000 0.05 1.61 Q10 1 0.4635 0.7796 0.2059 11.00000 0.05 1.55 Q11 1 0.8974 -0.2205 0.2080 11.00000 0.05 1.38 Q12 1 0.8529 0.7825 0.3826 11.00000 0.05 1.28 Q13 1 0.5058 0.2720 0.2074 11.00000 0.05 1.23 Q14 1 1.4243 0.2799 0.2056 11.00000 0.05 1.13 Q15 1 0.9561 -0.2218 0.1132 11.00000 0.05 1.13 Q16 1 0.3942 0.2815 0.3887 11.00000 0.05 1.11 Q17 1 1.0904 -0.2501 0.2080 11.00000 0.05 1.09 Q18 1 1.0546 -0.3252 0.2332 11.00000 0.05 1.05 Q19 1 1.0565 -0.1108 0.2339 11.00000 0.05 1.04 Q20 1 1.0980 -0.2199 0.2963 11.00000 0.05 1.00 Q21 1 0.5591 0.1192 0.2033 11.00000 0.05 0.95 Q22 1 1.0368 -0.3587 0.2150 11.00000 0.05 0.94 Q23 1 0.6375 0.2867 0.2991 11.00000 0.05 0.93 Q24 1 1.0403 -0.0799 0.2182 11.00000 0.05 0.93 Q25 1 0.4960 0.2819 0.1084 11.00000 0.05 0.92 ; _shelx_res_checksum 25751 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9051(14) -0.412(3) 0.1887(10) 0.045(5) Uani 1 1 d . . . . . H1A H 0.9065 -0.4988 0.1495 0.067 Uiso 1 1 calc R U . . . H1B H 0.8524 -0.3314 0.1794 0.067 Uiso 1 1 calc R U . . . H1C H 0.9043 -0.4881 0.2307 0.067 Uiso 1 1 calc R U . . . C2 C 0.9672(11) 0.013(3) 0.1252(9) 0.034(4) Uani 1 1 d . . . . . C3 C 0.8797(10) -0.007(3) 0.0887(8) 0.032(4) Uani 1 1 d . . . . . H3 H 0.8437 -0.1069 0.1012 0.039 Uiso 1 1 calc R U . . . C4 C 0.8457(11) 0.120(3) 0.0342(10) 0.039(4) Uani 1 1 d . . . . . H4 H 0.7871 0.1062 0.0111 0.047 Uiso 1 1 calc R U . . . C5 C 0.8995(11) 0.268(5) 0.0142(8) 0.042(4) Uani 1 1 d . . . . . H5 H 0.8771 0.3507 -0.0233 0.050 Uiso 1 1 calc R U . . . C6 C 0.9848(11) 0.294(5) 0.0491(8) 0.037(4) Uani 1 1 d . . . . . H6 H 1.0197 0.3947 0.0356 0.045 Uiso 1 1 calc R U . . . C7 C 1.0204(11) 0.169(3) 0.1054(9) 0.033(4) Uani 1 1 d . . . . . C8 C 1.1130(11) 0.202(3) 0.1427(10) 0.036(4) Uani 1 1 d . . . . . C9 C 1.1302(9) 0.230(3) 0.2119(8) 0.035(6) Uani 1 1 d . . . . . H9 H 1.0825 0.2432 0.2363 0.042 Uiso 1 1 calc R U . . . C10 C 1.2191(13) 0.241(4) 0.2506(10) 0.046(7) Uani 1 1 d . . . . . H10 H 1.2301 0.2381 0.2997 0.056 Uiso 1 1 calc R U . . . C11 C 1.2876(13) 0.255(5) 0.2125(10) 0.056(7) Uani 1 1 d . . . . . H11 H 1.3455 0.2791 0.2357 0.067 Uiso 1 1 calc R U . . . C12 C 1.2713(13) 0.233(3) 0.1405(10) 0.042(6) Uani 1 1 d . . . . . H12 H 1.3185 0.2309 0.1154 0.050 Uiso 1 1 calc R U . . . C13 C 1.1836(12) 0.213(3) 0.1052(10) 0.043(5) Uani 1 1 d . . . . . H13 H 1.1722 0.2080 0.0561 0.052 Uiso 1 1 calc R U . . . C14 C 0.9804(10) -0.072(2) 0.2963(7) 0.024(3) Uani 1 1 d . . . . . C15 C 0.9136(10) 0.073(3) 0.2862(8) 0.026(3) Uani 1 1 d . . . . . H15 H 0.8930 0.1182 0.2406 0.032 Uiso 1 1 calc R U . . . C16 C 0.8770(11) 0.153(3) 0.3417(9) 0.033(4) Uani 1 1 d . . . . . H16 H 0.8344 0.2527 0.3332 0.039 Uiso 1 1 calc R U . . . C17 C 0.9050(11) 0.082(3) 0.4107(9) 0.033(4) Uani 1 1 d . . . . . H17 H 0.8792 0.1286 0.4481 0.040 Uiso 1 1 calc R U . . . C18 C 0.9721(11) -0.060(3) 0.4217(9) 0.035(4) Uani 1 1 d . . . . . H18 H 0.9934 -0.1034 0.4674 0.042 Uiso 1 1 calc R U . . . C19 C 1.0086(11) -0.139(2) 0.3645(9) 0.032(4) Uani 1 1 d . . . . . C20 C 1.0786(11) -0.296(3) 0.3826(9) 0.029(4) Uani 1 1 d . . . . . C21 C 1.0564(11) -0.485(3) 0.3948(9) 0.034(4) Uani 1 1 d . . . . . H21 H 0.9961 -0.5176 0.3895 0.040 Uiso 1 1 calc R U . . . C22 C 1.1204(13) -0.632(3) 0.4152(9) 0.039(4) Uani 1 1 d . . . . . H22 H 1.1034 -0.7611 0.4229 0.047 Uiso 1 1 calc R U . . . C23 C 1.2110(12) -0.578(3) 0.4234(9) 0.040(4) Uani 1 1 d . . . . . H23 H 1.2554 -0.6701 0.4391 0.048 Uiso 1 1 calc R U . . . C24 C 1.2335(12) -0.391(3) 0.4082(10) 0.041(4) Uani 1 1 d . . . . . H24 H 1.2935 -0.3580 0.4118 0.049 Uiso 1 1 calc R U . . . C25 C 1.1695(11) -0.251(4) 0.3878(9) 0.038(5) Uani 1 1 d . . . . . H25 H 1.1866 -0.1239 0.3773 0.045 Uiso 1 1 calc R U . . . C31 C 0.6764(13) 0.091(3) 0.1920(10) 0.046(5) Uani 1 1 d . . . . . H31A H 0.6580 0.0041 0.1529 0.069 Uiso 1 1 calc R U . . . H31B H 0.6961 0.0152 0.2339 0.069 Uiso 1 1 calc R U . . . H31C H 0.7247 0.1726 0.1823 0.069 Uiso 1 1 calc R U . . . C32 C 0.5853(11) 0.517(3) 0.1283(9) 0.034(4) Uani 1 1 d . . . . . C33 C 0.6562(11) 0.497(3) 0.0904(9) 0.038(4) Uani 1 1 d . . . . . H33 H 0.6979 0.3972 0.1024 0.045 Uiso 1 1 calc R U . . . C34 C 0.6655(14) 0.623(3) 0.0358(10) 0.046(5) Uani 1 1 d . . . . . H34 H 0.7129 0.6086 0.0112 0.056 Uiso 1 1 calc R U . . . C35 C 0.6039(11) 0.769(4) 0.0184(8) 0.039(4) Uani 1 1 d . . . . . H35 H 0.6099 0.8540 -0.0185 0.046 Uiso 1 1 calc R U . . . C36 C 0.5326(9) 0.795(5) 0.0543(8) 0.033(4) Uani 1 1 d . . . . . H36 H 0.4912 0.8947 0.0413 0.040 Uiso 1 1 calc R U . . . C37 C 0.5235(12) 0.667(3) 0.1108(9) 0.036(4) Uani 1 1 d . . . . . C38 C 0.4480(12) 0.697(3) 0.1491(10) 0.035(4) Uani 1 1 d . . . . . C39 C 0.3600(11) 0.714(3) 0.1129(10) 0.038(5) Uani 1 1 d . . . . . H39 H 0.3488 0.7130 0.0638 0.046 Uiso 1 1 calc R U . . . C40 C 0.2899(13) 0.733(3) 0.1496(9) 0.041(5) Uani 1 1 d . . . . . H40 H 0.2317 0.7385 0.1249 0.049 Uiso 1 1 calc R U . . . C41 C 0.3044(13) 0.742(4) 0.2208(10) 0.049(7) Uani 1 1 d . . . . . H41 H 0.2563 0.7542 0.2447 0.058 Uiso 1 1 calc R U . . . C42 C 0.3905(13) 0.735(3) 0.2583(10) 0.044(6) Uani 1 1 d . . . . . H42 H 0.4012 0.7389 0.3074 0.053 Uiso 1 1 calc R U . . . C43 C 0.4613(11) 0.722(3) 0.2203(8) 0.035(5) Uani 1 1 d . . . . . H43 H 0.5196 0.7294 0.2447 0.042 Uiso 1 1 calc R U . . . C44 C 0.6509(10) 0.426(2) 0.3003(8) 0.027(3) Uani 1 1 d . U . . . C45 C 0.7115(10) 0.575(3) 0.2870(9) 0.031(3) Uani 1 1 d . U . . . H45 H 0.7099 0.6220 0.2413 0.037 Uiso 1 1 calc R U . . . C46 C 0.7719(11) 0.650(3) 0.3410(9) 0.034(3) Uani 1 1 d . U . . . H46 H 0.8108 0.7475 0.3311 0.040 Uiso 1 1 calc R U . . . C47 C 0.7775(11) 0.587(2) 0.4090(9) 0.032(3) Uani 1 1 d . U . . . H47 H 0.8196 0.6396 0.4450 0.038 Uiso 1 1 calc R U . . . C48 C 0.7172(11) 0.439(3) 0.4229(9) 0.035(4) Uani 1 1 d . U . . . H48 H 0.7199 0.3922 0.4688 0.042 Uiso 1 1 calc R U . . . C49 C 0.6544(11) 0.363(2) 0.3691(9) 0.029(3) Uani 1 1 d . U . . . C50 C 0.5936(12) 0.201(3) 0.3892(10) 0.035(4) Uani 1 1 d . . . . . C51 C 0.4999(12) 0.247(4) 0.3816(10) 0.048(7) Uani 1 1 d . . . . . H51 H 0.4772 0.3665 0.3625 0.057 Uiso 1 1 calc R U . . . C52 C 0.4454(12) 0.107(3) 0.4039(10) 0.042(5) Uani 1 1 d . . . . . H52 H 0.3842 0.1305 0.3985 0.051 Uiso 1 1 calc R U . . . C53 C 0.4796(14) -0.071(4) 0.4344(10) 0.051(6) Uani 1 1 d . . . . . H53 H 0.4420 -0.1601 0.4515 0.062 Uiso 1 1 calc R U . . . C54 C 0.5694(14) -0.112(3) 0.4390(11) 0.055(6) Uani 1 1 d . . . . . H54 H 0.5922 -0.2332 0.4563 0.066 Uiso 1 1 calc R U . . . C55 C 0.6250(12) 0.027(3) 0.4177(10) 0.038(4) Uani 1 1 d . . . . . H55 H 0.6859 0.0009 0.4229 0.045 Uiso 1 1 calc R U . . . Bi1 Bi 1.02742(3) -0.21801(13) 0.20402(2) 0.0287(2) Uani 1 1 d . . . . . Bi2 Bi 0.56159(3) 0.28096(13) 0.20799(2) 0.0287(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 C1 0.043(11) 0.041(14) 0.053(11) -0.007(9) 0.012(9) 0.007(9) C2 0.029(8) 0.038(12) 0.037(9) 0.001(7) 0.009(7) 0.011(8) C3 0.020(7) 0.042(12) 0.035(8) 0.000(7) 0.004(6) 0.009(7) C4 0.023(8) 0.035(12) 0.054(11) -0.004(8) -0.010(7) 0.009(8) C5 0.049(9) 0.037(11) 0.037(7) -0.008(12) 0.006(6) 0.007(14) C6 0.048(9) 0.024(11) 0.041(7) -0.011(12) 0.012(6) -0.009(14) C7 0.032(9) 0.029(11) 0.041(9) -0.005(7) 0.012(7) 0.006(7) C8 0.029(9) 0.028(10) 0.050(10) 0.006(7) 0.006(8) -0.010(7) C9 0.012(6) 0.057(18) 0.038(8) -0.031(8) 0.009(6) -0.016(7) C10 0.043(10) 0.05(2) 0.049(10) -0.006(9) 0.011(8) -0.007(9) C11 0.035(9) 0.08(2) 0.056(10) -0.014(14) 0.009(8) -0.012(13) C12 0.041(9) 0.034(17) 0.056(10) -0.006(7) 0.022(8) -0.009(8) C13 0.033(9) 0.051(15) 0.046(10) -0.007(7) 0.011(8) -0.003(8) C14 0.025(8) 0.015(9) 0.032(8) -0.006(5) 0.007(6) -0.002(6) C15 0.022(7) 0.030(11) 0.029(8) -0.006(6) 0.006(6) -0.006(7) C16 0.021(8) 0.023(11) 0.055(10) -0.004(7) 0.006(7) -0.005(7) C17 0.025(8) 0.028(11) 0.050(10) -0.008(7) 0.013(7) -0.006(7) C18 0.032(9) 0.040(12) 0.032(8) 0.003(7) 0.004(7) -0.005(8) C19 0.023(8) 0.022(9) 0.048(9) 0.003(7) -0.002(7) -0.006(6) C20 0.021(8) 0.029(10) 0.035(8) -0.004(6) -0.003(7) -0.003(6) C21 0.029(8) 0.025(11) 0.047(10) -0.002(7) 0.007(7) -0.004(7) C22 0.041(10) 0.029(10) 0.046(10) 0.000(7) 0.003(8) 0.004(8) C23 0.039(10) 0.041(13) 0.040(9) 0.008(8) 0.005(8) 0.010(9) C24 0.029(9) 0.038(13) 0.054(11) -0.007(8) 0.001(8) -0.001(8) C25 0.031(8) 0.029(16) 0.054(9) 0.004(8) 0.011(7) -0.008(8) C31 0.036(10) 0.051(15) 0.048(11) 0.004(9) -0.001(8) 0.000(9) C32 0.023(8) 0.038(12) 0.039(9) 0.007(7) -0.004(6) -0.005(7) C33 0.028(8) 0.039(12) 0.045(9) 0.004(8) 0.003(7) 0.001(8) C34 0.041(11) 0.054(14) 0.045(11) -0.005(9) 0.011(8) -0.006(10) C35 0.043(8) 0.035(11) 0.036(7) 0.003(11) 0.002(6) -0.021(13) C36 0.032(7) 0.019(10) 0.045(7) -0.001(11) -0.005(6) -0.004(12) C37 0.038(10) 0.022(11) 0.042(9) -0.004(7) -0.007(7) -0.009(8) C38 0.032(9) 0.020(9) 0.053(10) -0.005(7) 0.006(8) 0.002(7) C39 0.028(8) 0.036(13) 0.045(9) -0.008(7) -0.008(7) 0.007(7) C40 0.041(9) 0.032(17) 0.046(9) -0.006(7) 0.000(8) 0.008(7) C41 0.037(9) 0.05(2) 0.057(10) -0.014(10) 0.005(8) 0.008(9) C42 0.047(10) 0.04(2) 0.042(9) -0.001(7) 0.002(8) 0.014(8) C43 0.021(7) 0.049(16) 0.029(7) -0.017(6) -0.008(6) 0.006(7) C44 0.017(6) 0.016(7) 0.047(6) -0.006(5) 0.005(5) 0.003(5) C45 0.024(6) 0.025(8) 0.043(7) -0.006(5) 0.006(5) -0.001(6) C46 0.026(7) 0.025(9) 0.050(7) -0.007(5) 0.007(5) -0.006(6) C47 0.027(7) 0.020(8) 0.048(7) -0.006(5) 0.008(5) 0.005(6) C48 0.030(7) 0.029(9) 0.044(7) 0.000(6) 0.003(5) 0.001(6) C49 0.021(7) 0.021(8) 0.045(6) -0.003(5) 0.005(5) 0.004(5) C50 0.028(9) 0.026(10) 0.047(10) -0.001(7) -0.004(8) 0.000(7) C51 0.033(8) 0.06(2) 0.050(9) -0.010(10) 0.006(7) -0.004(10) C52 0.020(8) 0.057(14) 0.053(11) -0.012(9) 0.012(8) -0.007(8) C53 0.043(11) 0.063(16) 0.047(11) 0.005(9) 0.004(9) -0.027(11) C54 0.049(12) 0.044(15) 0.069(14) 0.017(11) -0.003(10) -0.022(10) C55 0.030(9) 0.029(11) 0.053(10) 0.005(8) 0.006(7) 0.001(8) Bi1 0.0230(3) 0.0272(4) 0.0355(3) 0.0017(5) 0.00428(19) 0.0030(5) Bi2 0.0215(3) 0.0270(4) 0.0362(3) 0.0009(5) 0.00096(19) -0.0020(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Bi Bi -4.0111 8.9310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -5 0.0085 -6 0 11 0.0163 -6 0 -8 0.0979 0 0 0 0.0292 0 0 0 0.0485 0 0 0 1.2236 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 Bi1 C1 H1A 109.5 . . ? Bi1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Bi1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 118.1(16) . . ? C3 C2 Bi1 120.6(14) . . ? C7 C2 Bi1 120.8(12) . . ? C4 C3 C2 121.2(17) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.9(16) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 121(2) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 121(3) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C6 C7 C2 119.5(17) . . ? C6 C7 C8 119.2(17) . . ? C2 C7 C8 121.3(16) . . ? C9 C8 C13 118.2(16) . . ? C9 C8 C7 121.1(15) . . ? C13 C8 C7 120.6(16) . . ? C8 C9 C10 122.5(15) . . ? C8 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C11 C10 C9 117.5(17) . . ? C11 C10 H10 121.3 . . ? C9 C10 H10 121.3 . . ? C12 C11 C10 120.4(19) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 119.7(17) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C8 C13 C12 120.6(17) . . ? C8 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C19 C14 C15 117.4(14) . . ? C19 C14 Bi1 121.0(12) . . ? C15 C14 Bi1 121.2(10) . . ? C16 C15 C14 122.7(15) . . ? C16 C15 H15 118.7 . . ? C14 C15 H15 118.7 . . ? C15 C16 C17 119.4(16) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 118.5(16) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C19 121.1(16) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C14 C19 C18 120.9(16) . . ? C14 C19 C20 122.9(15) . . ? C18 C19 C20 116.3(15) . . ? C21 C20 C25 117.9(18) . . ? C21 C20 C19 121.5(15) . . ? C25 C20 C19 120.6(17) . . ? C20 C21 C22 122.8(16) . . ? C20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C23 C22 C21 117.5(18) . . ? C23 C22 H22 121.3 . . ? C21 C22 H22 121.3 . . ? C24 C23 C22 119.7(18) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C25 121.4(18) . . ? C23 C24 H24 119.3 . . ? C25 C24 H24 119.3 . . ? C24 C25 C20 121(2) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? Bi2 C31 H31A 109.5 . . ? Bi2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Bi2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C37 C32 C33 119.3(16) . . ? C37 C32 Bi2 120.1(13) . . ? C33 C32 Bi2 120.2(13) . . ? C34 C33 C32 121.5(18) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C35 C34 C33 118.9(18) . . ? C35 C34 H34 120.6 . . ? C33 C34 H34 120.6 . . ? C34 C35 C36 122(2) . . ? C34 C35 H35 119.1 . . ? C36 C35 H35 119.1 . . ? C35 C36 C37 119(2) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C32 C37 C36 119.2(18) . . ? C32 C37 C38 122.0(16) . . ? C36 C37 C38 118.8(18) . . ? C43 C38 C39 117.1(16) . . ? C43 C38 C37 121.5(15) . . ? C39 C38 C37 121.3(16) . . ? C40 C39 C38 120.5(17) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 121.1(18) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C42 120.2(19) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C43 118.1(16) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C38 C43 C42 122.5(15) . . ? C38 C43 H43 118.7 . . ? C42 C43 H43 118.7 . . ? C49 C44 C45 118.1(15) . . ? C49 C44 Bi2 122.5(12) . . ? C45 C44 Bi2 119.2(12) . . ? C46 C45 C44 120.1(16) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C47 122.7(17) . . ? C45 C46 H46 118.7 . . ? C47 C46 H46 118.7 . . ? C46 C47 C48 117.8(16) . . ? C46 C47 H47 121.1 . . ? C48 C47 H47 121.1 . . ? C49 C48 C47 120.5(17) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C48 C49 C44 120.9(16) . . ? C48 C49 C50 116.6(15) . . ? C44 C49 C50 122.5(15) . . ? C55 C50 C51 120(2) . . ? C55 C50 C49 123.0(16) . . ? C51 C50 C49 116.6(18) . . ? C52 C51 C50 117(2) . . ? C52 C51 H51 121.5 . . ? C50 C51 H51 121.5 . . ? C51 C52 C53 121.8(18) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 119.6(19) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 119(2) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C50 C55 C54 122.0(19) . . ? C50 C55 H55 119.0 . . ? C54 C55 H55 119.0 . . ? C14 Bi1 C1 89.7(6) . . ? C14 Bi1 C2 94.4(6) . . ? C1 Bi1 C2 95.0(7) . . ? C31 Bi2 C44 88.9(6) . . ? C31 Bi2 C32 95.6(7) . . ? C44 Bi2 C32 94.5(6) . . ? 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 Bi1 2.25(2) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.40(2) . ? C2 C7 1.42(3) . ? C2 Bi1 2.263(18) . ? C3 C4 1.39(2) . ? C3 H3 0.9300 . ? C4 C5 1.39(3) . ? C4 H4 0.9300 . ? C5 C6 1.36(2) . ? C5 H5 0.9300 . ? C6 C7 1.41(3) . ? C6 H6 0.9300 . ? C7 C8 1.48(2) . ? C8 C9 1.33(2) . ? C8 C13 1.39(2) . ? C9 C10 1.43(2) . ? C9 H9 0.9300 . ? C10 C11 1.37(3) . ? C10 H10 0.9300 . ? C11 C12 1.37(3) . ? C11 H11 0.9300 . ? C12 C13 1.39(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.38(2) . ? C14 C15 1.41(2) . ? C14 Bi1 2.249(14) . ? C15 C16 1.39(2) . ? C15 H15 0.9300 . ? C16 C17 1.41(2) . ? C16 H16 0.9300 . ? C17 C18 1.39(3) . ? C17 H17 0.9300 . ? C18 C19 1.42(2) . ? C18 H18 0.9300 . ? C19 C20 1.50(2) . ? C20 C21 1.36(3) . ? C20 C25 1.40(2) . ? C21 C22 1.41(3) . ? C21 H21 0.9300 . ? C22 C23 1.41(3) . ? C22 H22 0.9300 . ? C23 C24 1.36(3) . ? C23 H23 0.9300 . ? C24 C25 1.37(3) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C31 Bi2 2.23(2) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C37 1.39(3) . ? C32 C33 1.41(2) . ? C32 Bi2 2.285(17) . ? C33 C34 1.38(3) . ? C33 H33 0.9300 . ? C34 C35 1.36(3) . ? C34 H34 0.9300 . ? C35 C36 1.39(2) . ? C35 H35 0.9300 . ? C36 C37 1.41(3) . ? C36 H36 0.9300 . ? C37 C38 1.48(3) . ? C38 C43 1.36(2) . ? C38 C39 1.40(2) . ? C39 C40 1.38(3) . ? C39 H39 0.9300 . ? C40 C41 1.35(3) . ? C40 H40 0.9300 . ? C41 C42 1.38(3) . ? C41 H41 0.9300 . ? C42 C43 1.40(2) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 C49 1.38(2) . ? C44 C45 1.42(2) . ? C44 Bi2 2.265(16) . ? C45 C46 1.36(2) . ? C45 H45 0.9300 . ? C46 C47 1.36(2) . ? C46 H46 0.9300 . ? C47 C48 1.42(3) . ? C47 H47 0.9300 . ? C48 C49 1.38(2) . ? C48 H48 0.9300 . ? C49 C50 1.53(2) . ? C50 C55 1.36(3) . ? C50 C51 1.44(2) . ? C51 C52 1.38(3) . ? C51 H51 0.9300 . ? C52 C53 1.40(3) . ? C52 H52 0.9300 . ? C53 C54 1.38(3) . ? C53 H53 0.9300 . ? C54 C55 1.37(3) . ? C54 H54 0.9300 . ? C55 H55 0.9300 . ? 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 C7 C2 C3 C4 1(3) . . . . ? Bi1 C2 C3 C4 -171.9(13) . . . . ? C2 C3 C4 C5 1(3) . . . . ? C3 C4 C5 C6 -2(3) . . . . ? C4 C5 C6 C7 1(3) . . . . ? C5 C6 C7 C2 1(3) . . . . ? C5 C6 C7 C8 -179.3(19) . . . . ? C3 C2 C7 C6 -2(3) . . . . ? Bi1 C2 C7 C6 171.0(14) . . . . ? C3 C2 C7 C8 178.5(16) . . . . ? Bi1 C2 C7 C8 -9(2) . . . . ? C6 C7 C8 C9 124(2) . . . . ? C2 C7 C8 C9 -56(3) . . . . ? C6 C7 C8 C13 -53(3) . . . . ? C2 C7 C8 C13 126.6(19) . . . . ? C13 C8 C9 C10 -10(3) . . . . ? C7 C8 C9 C10 172.8(19) . . . . ? C8 C9 C10 C11 11(4) . . . . ? C9 C10 C11 C12 -8(4) . . . . ? C10 C11 C12 C13 6(4) . . . . ? C9 C8 C13 C12 7(3) . . . . ? C7 C8 C13 C12 -176.1(18) . . . . ? C11 C12 C13 C8 -5(3) . . . . ? C19 C14 C15 C16 1(2) . . . . ? Bi1 C14 C15 C16 173.8(12) . . . . ? C14 C15 C16 C17 -2(2) . . . . ? C15 C16 C17 C18 3(2) . . . . ? C16 C17 C18 C19 -3(3) . . . . ? C15 C14 C19 C18 -1(2) . . . . ? Bi1 C14 C19 C18 -173.7(12) . . . . ? C15 C14 C19 C20 179.1(15) . . . . ? Bi1 C14 C19 C20 6(2) . . . . ? C17 C18 C19 C14 2(3) . . . . ? C17 C18 C19 C20 -178.0(16) . . . . ? C14 C19 C20 C21 -101(2) . . . . ? C18 C19 C20 C21 79(2) . . . . ? C14 C19 C20 C25 79(2) . . . . ? C18 C19 C20 C25 -100.9(19) . . . . ? C25 C20 C21 C22 3(3) . . . . ? C19 C20 C21 C22 -176.8(16) . . . . ? C20 C21 C22 C23 0(3) . . . . ? C21 C22 C23 C24 -3(3) . . . . ? C22 C23 C24 C25 3(3) . . . . ? C23 C24 C25 C20 1(3) . . . . ? C21 C20 C25 C24 -3(3) . . . . ? C19 C20 C25 C24 176.3(16) . . . . ? C37 C32 C33 C34 0(3) . . . . ? Bi2 C32 C33 C34 171.6(14) . . . . ? C32 C33 C34 C35 0(3) . . . . ? C33 C34 C35 C36 0(3) . . . . ? C34 C35 C36 C37 0(3) . . . . ? C33 C32 C37 C36 1(3) . . . . ? Bi2 C32 C37 C36 -171.0(14) . . . . ? C33 C32 C37 C38 -179.2(16) . . . . ? Bi2 C32 C37 C38 9(2) . . . . ? C35 C36 C37 C32 -1(3) . . . . ? C35 C36 C37 C38 179.2(18) . . . . ? C32 C37 C38 C43 55(3) . . . . ? C36 C37 C38 C43 -125(2) . . . . ? C32 C37 C38 C39 -128.7(19) . . . . ? C36 C37 C38 C39 51(3) . . . . ? C43 C38 C39 C40 -7(3) . . . . ? C37 C38 C39 C40 176.7(17) . . . . ? C38 C39 C40 C41 3(3) . . . . ? C39 C40 C41 C42 0(4) . . . . ? C40 C41 C42 C43 1(4) . . . . ? C39 C38 C43 C42 9(3) . . . . ? C37 C38 C43 C42 -174.9(18) . . . . ? C41 C42 C43 C38 -6(3) . . . . ? C49 C44 C45 C46 1(2) . . . . ? Bi2 C44 C45 C46 -173.3(12) . . . . ? C44 C45 C46 C47 0(3) . . . . ? C45 C46 C47 C48 0(3) . . . . ? C46 C47 C48 C49 -1(3) . . . . ? C47 C48 C49 C44 2(3) . . . . ? C47 C48 C49 C50 178.9(15) . . . . ? C45 C44 C49 C48 -2(2) . . . . ? Bi2 C44 C49 C48 172.1(12) . . . . ? C45 C44 C49 C50 -178.9(15) . . . . ? Bi2 C44 C49 C50 -5(2) . . . . ? C48 C49 C50 C55 -60(2) . . . . ? C44 C49 C50 C55 117(2) . . . . ? C48 C49 C50 C51 115.1(19) . . . . ? C44 C49 C50 C51 -68(2) . . . . ? C55 C50 C51 C52 0(3) . . . . ? C49 C50 C51 C52 -176.0(17) . . . . ? C50 C51 C52 C53 2(3) . . . . ? C51 C52 C53 C54 -4(3) . . . . ? C52 C53 C54 C55 4(3) . . . . ? C51 C50 C55 C54 1(3) . . . . ? C49 C50 C55 C54 176.3(18) . . . . ? C53 C54 C55 C50 -3(3) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0101 0.0052 -5.0006 -0.3951 0.0147 -0.0966 -5.7432 -0.0972 11.2202 0.8022 0.5551 0.2199 -6.3802 0.1595 -7.9839 -0.7106 0.6731 -0.2050 0.2071 0.0023 -0.0016 0.0029 -0.0211 0.0000 0.1567 0.0039 -0.1973 -0.0132 -0.0154 -0.0042 0.1451 0.2508 -0.1754 0.0016 -0.0139 -0.0582