#------------------------------------------------------------------------------ #$Date: 2024-07-05 17:14:44 +0300 (Fri, 05 Jul 2024) $ #$Revision: 292880 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571707.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_1571707 loop_ _publ_author_name 'Prajapati, Bibek' 'Kwenda, Tendai' 'Lis, Tadeusz' 'Chmielewski, Piotr J.' 'G\'omez-Garc\'ia, Carlos J.' 'Majewski, Marcin A.' 'St\;epie\'n, Marcin' _publ_section_title ; Difluorenoheteroles: topological control of \p conjugation in diradicaloids and mixed-valence radical ions ; _journal_issue 26 _journal_name_full 'Chemical Science' _journal_page_first 10101 _journal_page_last 10109 _journal_paper_doi 10.1039/D4SC02459A _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C56 H58 S, 1.5(C7 D8)' _chemical_formula_sum 'C66.5 H58 D12 S' _chemical_formula_weight 913.35 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_method SHELXL-2013 _audit_update_record ; 2023-10-22 deposited with the CCDC. 2024-05-21 downloaded from the CCDC. ; _cell_angle_alpha 104.66(2) _cell_angle_beta 97.26(2) _cell_angle_gamma 102.40(2) _cell_formula_units_Z 2 _cell_length_a 9.2015(19) _cell_length_b 15.281(4) _cell_length_c 20.007(3) _cell_measurement_reflns_used 19930 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 60 _cell_measurement_theta_min 2.3 _cell_volume 2609.0(10) _computing_cell_refinement 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 150' _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.952 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix-Arc 150' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0552 _diffrn_reflns_av_unetI/netI 0.0388 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.952 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 39794 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.952 _diffrn_reflns_theta_full 67.000 _diffrn_reflns_theta_max 73.983 _diffrn_reflns_theta_min 2.326 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.843 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.741 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light pink' _exptl_crystal_density_diffrn 1.163 _exptl_crystal_description plate _exptl_crystal_F_000 970 _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.020 _refine_diff_density_max 0.603 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.057 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 665 _refine_ls_number_reflns 10083 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.087 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0575 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+0.3112P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1654 _refine_ls_wR_factor_ref 0.1725 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8290 _reflns_number_total 10083 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02459a3.cif _cod_data_source_block tw19ca _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_primary' value 'direct methods' was changed to 'direct'. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 1571707--1571709.cif. ; _cod_original_formula_sum 'C66.50 H58 D12 S' _cod_database_code 1571707 _shelxl_version_number 2013-2 _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. ; _shelx_estimated_absorpt_t_max 0.983 _shelx_estimated_absorpt_t_min 0.735 _olex2_refinement_description ; 1. Others Fixed Sof: D1C(0.5) C7C(0.5) D7CA(0.5) D7CB(0.5) D7CC(0.5) C1D(0.5) C2D(0.5) D2D(0.5) C3D(0.5) D3D(0.5) C4D(0.5) D4D(0.5) C5D(0.5) D5D(0.5) C6D(0.5) D6D(0.5) C7D(0.5) D7DA(0.5) D7DB(0.5) D7DC(0.5) C1E(0.5) C2E(0.5) D2E(0.5) C3E(0.5) D3E(0.5) C4E(0.5) D4E(0.5) C5E(0.5) D5E(0.5) C6E(0.5) D6E(0.5) C7E(0.5) D7EA(0.5) D7EB(0.5) D7EC(0.5) Fixed Uiso: H3A(0.029) H6(0.029) H8A(0.036) H9A(0.044) H10A(0.045) H11A(0.04) H16A(0.036) H18A(0.038) H20A(0.035) H21A(0.051) H21B(0.051) H21C(0.051) H22A(0.056) H22B(0.056) H22C(0.056) H25(0.042) H24A(0.058) H24B(0.058) H24C(0.058) H25A(0.069) H25B(0.069) H25C(0.069) H26A(0.043) H27A(0.065) H27B(0.065) H27C(0.065) H28A(0.068) H28B(0.068) H28C(0.068) H3B(0.029) H6B(0.03) H8B(0.034) H9B(0.038) H10B(0.04) H11B(0.035) H16B(0.031) H18B(0.032) H20B(0.038) H21D(0.06) H21E(0.06) H21F(0.06) H22D(0.069) H22E(0.069) H22F(0.069) H23B(0.034) H24D(0.053) H24E(0.053) H24F(0.053) H25D(0.054) H25E(0.054) H25F(0.054) H26B(0.042) H27D(0.071) H27E(0.071) H27F(0.071) H28D(0.077) H28E(0.077) H28F(0.077) D1C(0.063) D2C(0.057) D3C(0.061) D7CA(0.098) D7CB(0.098) D7CC(0.098) D2D(0.071) D3D(0.141) D4D(0.175) D5D(0.134) D6D(0.107) D7DA(0.135) D7DB(0.135) D7DC(0.135) D2E(0.094) D3E(0.129) D4E(0.083) D5E(0.085) D6E(0.071) D7EA(0.163) D7EB(0.163) D7EC(0.163) Fixed X: H3A(0.4045) H6(0.478) H8A(0.1861) H9A(-0.0011) H10A(-0.0714) H11A(0.0424) H16A(0.439) H18A(0.1286) H20A(0.403) H21A(0.6643) H21B(0.6717) H21C(0.613) H22A(0.3443) H22B(0.4977) H22C(0.5049) H25(0.2175) H24A(0.538) H24B(0.4487) H24C(0.4581) H25A(0.2989) H25B(0.206) H25C(0.3873) H26A(0.0877) H27A(-0.1215) H27B(-0.1671) H27C(-0.1063) H28A(0.1885) H28B(0.0139) H28C(0.062) H3B(0.5648) H6B(0.851) H8B(0.6432) H9B(0.7444) H10B(0.9109) H11B(0.9848) H16B(1.0024) H18B(1.3423) H20B(0.7292) H21D(0.8235) H21E(0.6504) H21F(0.7813) H22D(0.7223) H22E(0.5763) H22F(0.6951) H23B(1.2946) H24D(1.222) H24E(1.2878) H24F(1.1213) H25D(1.4986) H25E(1.5131) H25F(1.4548) H26B(1.1244) H27D(1.4288) H27E(1.3706) H27F(1.3194) H28D(1.152) H28E(1.2749) H28F(1.324) D1C(0.7582) D2C(0.8071) D3C(0.9561) D7CA(0.6374) D7CB(0.7009) D7CC(0.6549) D2D(0.879) D3D(0.6942) D4D(0.6762) D5D(0.843) D6D(1.0279) D7DA(1.1591) D7DB(1.1372) D7DC(1.034) D2E(0.851) D3E(0.6484) D4E(0.5937) D5E(0.7416) D6E(0.9442) D7EA(1.0859) D7EB(1.0121) D7EC(1.1272) Fixed Y: H3A(0.1933) H6(0.5044) H8A(0.1674) H9A(0.1819) H10A(0.3211) H11A(0.4506) H16A(0.7628) H18A(0.6897) H20A(0.5269) H21A(0.6614) H21B(0.5825) H21C(0.5533) H22A(0.6476) H22B(0.6248) H22C(0.716) H25(0.849) H24A(0.882) H24B(0.8518) H24C(0.9526) H25A(0.969) H25B(0.8781) H25C(0.9078) H26A(0.4411) H27A(0.556) H27B(0.4458) H27C(0.4842) H28A(0.5183) H28B(0.4648) H28C(0.5758) H3B(0.1087) H6B(0.3014) H8B(-0.0578) H9B(-0.1857) H10B(-0.1816) H11B(-0.048) H16B(0.1669) H18B(0.2637) H20B(0.0539) H21D(-0.0196) H21E(-0.0167) H21F(0.0562) H22D(0.1975) H22E(0.1305) H22F(0.2058) H23B(0.2056) H24D(0.3819) H24E(0.3455) H24F(0.294) H25D(0.2665) H25E(0.3295) H25F(0.3645) H26B(0.1695) H27D(0.2066) H27E(0.1656) H27F(0.1034) H28D(0.3321) H28E(0.3115) H28F(0.3464) D1C(0.4351) D2C(0.5738) D3C(0.3621) D7CA(0.3848) D7CB(0.3835) D7CC(0.4742) D2D(-0.0073) D3D(0.048) D4D(0.2012) D5D(0.299) D6D(0.2437) D7DA(0.1306) D7DB(0.0445) D7DC(0.035) D2E(-0.0127) D3E(0.0137) D4E(0.1598) D5E(0.2794) D6E(0.2529) D7EA(0.0563) D7EB(0.0928) D7EC(0.1657) Fixed Z: H3A(0.1101) H6(0.2585) H8A(-0.0061) H9A(-0.0912) H10A(-0.0788) H11A(0.0198) H16A(0.157) H18A(0.2714) H20A(0.0536) H21A(0.1433) H21B(0.0748) H21C(0.1399) H22A(0.0089) H22B(-0.0113) H22C(0.051) H25(0.2834) H24A(0.2914) H24B(0.349) H24C(0.3374) H25A(0.2343) H25B(0.172) H25C(0.1854) H26A(0.2049) H27A(0.2132) H27B(0.2037) H27C(0.1423) H28A(0.3249) H28B(0.3146) H28C(0.3282) H3B(0.1649) H6B(0.39) H8B(0.1376) H9B(0.1406) H10B(0.2402) H11B(0.3384) H16B(0.5829) H18B(0.4906) H20B(0.4235) H21D(0.5074) H21E(0.5063) H21F(0.5679) H22D(0.5457) H22E(0.4896) H22F(0.4672) H23B(0.6395) H24D(0.6569) H24E(0.7197) H24F(0.6742) H25D(0.5905) H25E(0.6694) H25F(0.6044) H26B(0.3142) H27D(0.3869) H27E(0.3035) H27F(0.354) H28D(0.3573) H28E(0.3097) H28F(0.3936) D1C(0.5178) D2C(0.4855) D3C(0.5333) D7CA(0.4731) D7CB(0.551) D7CC(0.5387) D2D(0.0351) D3D(- 0.0208) D4D(0.0259) D5D(0.1286) D6D(0.1846) D7DA(0.1877) D7DB(0.119) D7DC(0.1768) D2E(0.027) D3E(-0.0414) D4E(-0.012) D5E(0.086) D6E(0.1544) D7EA(0.1195) D7EB(0.1861) D7EC(0.16) ; _shelx_res_file ; TITL tw19c in P-1 CELL 1.54184 9.2015 15.281 20.007 104.66 97.26 102.40 ZERR 2 0.0019 0.004 0.003 0.02 0.02 0.02 LATT 1 SFAC C H S D UNIT 133 116 2 24 acta 134 size 0.02 0.04 0.39 L.S. 10 PLAN 20 TEMP -173 fmap 2 WGHT 0.116100 0.311200 FVAR 2.60158 S 3 0.666747 0.408003 0.328200 11.00000 0.02548 0.02738 = 0.02239 0.00862 -0.00323 0.00782 C1A 1 0.539315 0.382143 0.248854 11.00000 0.02073 0.02754 = 0.01887 0.00782 -0.00032 0.00372 C2A 1 0.520496 0.288532 0.205758 11.00000 0.01904 0.02677 = 0.02322 0.01093 0.00146 0.00493 C3A 1 0.417906 0.254981 0.139686 11.00000 0.02179 0.02805 = 0.02382 0.01098 0.00222 0.00679 AFIX 43 H3A 2 0.404473 0.193307 0.110134 11.00000 -1.20000 AFIX 0 C4A 1 0.339439 0.313628 0.119914 11.00000 0.01919 0.02816 = 0.02151 0.00941 0.00115 0.00390 C5A 1 0.361623 0.408318 0.163570 11.00000 0.02129 0.02880 = 0.02378 0.01191 0.00129 0.00577 C6A 1 0.463162 0.442411 0.229225 11.00000 0.02227 0.02630 = 0.02386 0.01007 0.00065 0.00593 AFIX 43 H6 2 0.477976 0.504415 0.258476 11.00000 -1.20000 AFIX 0 C7A 1 0.224481 0.300439 0.057594 11.00000 0.02037 0.03327 = 0.02297 0.01265 0.00009 0.00578 C8A 1 0.157432 0.224547 -0.000560 11.00000 0.02683 0.03459 = 0.02785 0.00827 -0.00158 0.00872 AFIX 43 H8A 2 0.186138 0.167381 -0.006147 11.00000 -1.20000 AFIX 0 C9A 1 0.046266 0.233693 -0.051084 11.00000 0.02991 0.04772 = 0.02779 0.00702 -0.00547 0.00931 AFIX 43 H9A 2 -0.001106 0.181902 -0.091204 11.00000 -1.20000 AFIX 0 C10A 1 0.004186 0.316531 -0.043714 11.00000 0.03054 0.05124 = 0.02916 0.01258 -0.00732 0.01393 AFIX 43 H10A 2 -0.071411 0.321057 -0.078771 11.00000 -1.20000 AFIX 0 C11A 1 0.071505 0.393616 0.014655 11.00000 0.03080 0.04086 = 0.03135 0.01477 -0.00342 0.01449 AFIX 43 H11A 2 0.042392 0.450602 0.019786 11.00000 -1.20000 AFIX 0 C12A 1 0.182455 0.385431 0.065378 11.00000 0.02234 0.03435 = 0.02435 0.01253 0.00061 0.00734 C13A 1 0.269875 0.453168 0.130523 11.00000 0.02191 0.03110 = 0.02543 0.01261 0.00157 0.00770 C14A 1 0.267818 0.552693 0.158417 11.00000 0.02094 0.03209 = 0.02556 0.01131 -0.00237 0.01003 C15A 1 0.361927 0.621782 0.137208 11.00000 0.02325 0.03279 = 0.02778 0.01210 -0.00008 0.01015 C16A 1 0.372357 0.715834 0.169913 11.00000 0.02518 0.03230 = 0.03369 0.01298 0.00295 0.00860 AFIX 43 H16A 2 0.439045 0.762813 0.157045 11.00000 -1.20000 AFIX 0 C17A 1 0.287375 0.742739 0.221057 11.00000 0.02386 0.03411 = 0.03273 0.00887 -0.00135 0.01076 C18A 1 0.189831 0.672618 0.237999 11.00000 0.02403 0.04127 = 0.03158 0.01033 0.00297 0.01453 AFIX 43 H18A 2 0.128602 0.689717 0.271410 11.00000 -1.20000 AFIX 0 C19A 1 0.177892 0.577584 0.207855 11.00000 0.02445 0.03778 = 0.03080 0.01472 0.00105 0.01178 C20A 1 0.452661 0.593769 0.080369 11.00000 0.02957 0.03076 = 0.02952 0.01158 0.00475 0.00831 AFIX 13 H20A 2 0.403012 0.526922 0.053578 11.00000 -1.20000 AFIX 0 C21A 1 0.615011 0.598142 0.112471 11.00000 0.03125 0.03802 = 0.03726 0.01456 0.00833 0.01346 AFIX 137 H21A 2 0.664255 0.661445 0.143285 11.00000 -1.50000 H21B 2 0.671735 0.582529 0.074763 11.00000 -1.50000 H21C 2 0.613019 0.553254 0.139925 11.00000 -1.50000 AFIX 0 C22A 1 0.449636 0.650655 0.027496 11.00000 0.03934 0.04269 = 0.03483 0.01829 0.00831 0.01269 AFIX 137 H22A 2 0.344344 0.647642 0.008887 11.00000 -1.50000 H22B 2 0.497718 0.624753 -0.011267 11.00000 -1.50000 H22C 2 0.504911 0.715983 0.051022 11.00000 -1.50000 AFIX 0 C23A 1 0.304425 0.845552 0.258365 11.00000 0.02700 0.03392 = 0.04051 0.00521 0.00162 0.00989 AFIX 13 H25 2 0.217450 0.848999 0.283392 11.00000 -1.20000 AFIX 0 C24A 1 0.450469 0.886682 0.314074 11.00000 0.04029 0.03667 = 0.03378 0.00592 -0.00289 0.01056 AFIX 137 H24A 2 0.538045 0.882008 0.291426 11.00000 -1.50000 H24B 2 0.448694 0.851776 0.348987 11.00000 -1.50000 H24C 2 0.458087 0.952571 0.337445 11.00000 -1.50000 AFIX 0 C25A 1 0.298639 0.905498 0.208008 11.00000 0.04575 0.03319 = 0.05072 0.00663 -0.01511 0.01356 AFIX 137 H25A 2 0.298863 0.969046 0.234334 11.00000 -1.50000 H25B 2 0.206017 0.878115 0.171956 11.00000 -1.50000 H25C 2 0.387322 0.907806 0.185415 11.00000 -1.50000 AFIX 0 C26A 1 0.066237 0.502465 0.226350 11.00000 0.03223 0.03914 = 0.03961 0.01519 0.01072 0.01086 AFIX 13 H26A 2 0.087723 0.441092 0.204920 11.00000 -1.20000 AFIX 0 C27A 1 -0.096910 0.496570 0.193385 11.00000 0.03132 0.05773 = 0.03664 0.01307 0.00576 0.00483 AFIX 137 H27A 2 -0.121476 0.555969 0.213153 11.00000 -1.50000 H27B 2 -0.167101 0.445797 0.203658 11.00000 -1.50000 H27C 2 -0.106267 0.484181 0.142307 11.00000 -1.50000 AFIX 0 C28A 1 0.084281 0.516642 0.305588 11.00000 0.03665 0.06321 = 0.04411 0.02997 0.00825 0.01343 AFIX 137 H28A 2 0.188538 0.518343 0.324863 11.00000 -1.50000 H28B 2 0.013868 0.464839 0.314599 11.00000 -1.50000 H28C 2 0.062017 0.575842 0.328155 11.00000 -1.50000 AFIX 0 C1B 1 0.698050 0.295976 0.304975 11.00000 0.02270 0.02653 = 0.02330 0.01027 0.00142 0.00558 C2B 1 0.610655 0.240079 0.237235 11.00000 0.02023 0.03046 = 0.02286 0.01264 0.00072 0.00547 C3B 1 0.621396 0.146603 0.209814 11.00000 0.02195 0.02901 = 0.02242 0.01072 -0.00038 0.00530 AFIX 43 H3B 2 0.564783 0.108664 0.164927 11.00000 -1.20000 AFIX 0 C4B 1 0.715097 0.112676 0.249580 11.00000 0.02235 0.02894 = 0.02321 0.01077 0.00168 0.00536 C5B 1 0.801016 0.169687 0.318416 11.00000 0.02075 0.03095 = 0.02279 0.01263 -0.00035 0.00571 C6B 1 0.793041 0.262958 0.345507 11.00000 0.02252 0.02855 = 0.02316 0.01067 -0.00212 0.00532 AFIX 43 H6B 2 0.851008 0.301412 0.389988 11.00000 -1.20000 AFIX 0 C7B 1 0.753728 0.022612 0.235905 11.00000 0.02148 0.02974 = 0.02645 0.01425 0.00230 0.00611 C8B 1 0.711728 -0.055683 0.178020 11.00000 0.02754 0.02980 = 0.02566 0.00993 -0.00034 0.00519 AFIX 43 H8B 2 0.643171 -0.057820 0.137577 11.00000 -1.20000 AFIX 0 C9B 1 0.771957 -0.131605 0.180092 11.00000 0.03089 0.03055 = 0.03136 0.00852 0.00276 0.00750 AFIX 43 H9B 2 0.744439 -0.185744 0.140551 11.00000 -1.20000 AFIX 0 C10B 1 0.872139 -0.128921 0.239572 11.00000 0.03404 0.02993 = 0.03736 0.01233 0.00195 0.01230 AFIX 43 H10B 2 0.910937 -0.181576 0.240222 11.00000 -1.20000 AFIX 0 C11B 1 0.916055 -0.049804 0.298140 11.00000 0.02960 0.02952 = 0.03005 0.01319 -0.00038 0.00853 AFIX 43 H11B 2 0.984832 -0.047981 0.338406 11.00000 -1.20000 AFIX 0 C12B 1 0.857047 0.026225 0.296298 11.00000 0.02181 0.03162 = 0.02538 0.01210 -0.00021 0.00529 C13B 1 0.886093 0.117610 0.347223 11.00000 0.02124 0.02855 = 0.02614 0.01296 0.00175 0.00591 C14B 1 0.991257 0.151398 0.416481 11.00000 0.02316 0.02433 = 0.02300 0.00959 0.00002 0.00866 C15B 1 0.938123 0.139151 0.477490 11.00000 0.02395 0.02975 = 0.02671 0.01302 0.00328 0.00873 C16B 1 1.038197 0.175112 0.541825 11.00000 0.02748 0.03130 = 0.02319 0.01321 0.00384 0.00990 AFIX 43 H16B 2 1.002416 0.166949 0.582916 11.00000 -1.20000 AFIX 0 C17B 1 1.188992 0.222684 0.548433 11.00000 0.02524 0.02835 = 0.02488 0.01080 -0.00016 0.01072 C18B 1 1.239604 0.232193 0.487351 11.00000 0.01944 0.03252 = 0.02953 0.01179 0.00203 0.00593 AFIX 43 H18B 2 1.342286 0.263732 0.490564 11.00000 -1.20000 AFIX 0 C19B 1 1.143521 0.196617 0.421371 11.00000 0.02534 0.03289 = 0.02558 0.01364 0.00389 0.00923 C20B 1 0.773352 0.090174 0.473698 11.00000 0.02391 0.04060 = 0.02912 0.01382 0.00154 0.00230 AFIX 13 H20B 2 0.729152 0.053901 0.423484 11.00000 -1.20000 AFIX 0 C21B 1 0.755526 0.021319 0.517790 11.00000 0.03153 0.03639 = 0.05758 0.02271 0.01220 0.00675 AFIX 137 H21D 2 0.823489 -0.019594 0.507350 11.00000 -1.50000 H21E 2 0.650424 -0.016679 0.506337 11.00000 -1.50000 H21F 2 0.781254 0.056160 0.567902 11.00000 -1.50000 AFIX 0 C22B 1 0.683746 0.162475 0.496053 11.00000 0.02473 0.05538 = 0.07229 0.03894 0.01209 0.01490 AFIX 137 H22D 2 0.722313 0.197519 0.545731 11.00000 -1.50000 H22E 2 0.576331 0.130514 0.489558 11.00000 -1.50000 H22F 2 0.695123 0.205765 0.467206 11.00000 -1.50000 AFIX 0 C23B 1 1.290999 0.260365 0.621156 11.00000 0.02638 0.03499 = 0.02465 0.01031 -0.00206 0.01050 AFIX 13 H23B 2 1.294615 0.205617 0.639500 11.00000 -1.20000 AFIX 0 C24B 1 1.224518 0.326399 0.672638 11.00000 0.03399 0.04040 = 0.02688 0.00656 0.00127 0.00816 AFIX 137 H24D 2 1.221963 0.381905 0.656927 11.00000 -1.50000 H24E 2 1.287766 0.345472 0.719714 11.00000 -1.50000 H24F 2 1.121341 0.294021 0.674173 11.00000 -1.50000 AFIX 0 C25B 1 1.453934 0.309625 0.621384 11.00000 0.02745 0.04439 = 0.03167 0.00649 -0.00531 0.00971 AFIX 137 H25D 2 1.498586 0.266472 0.590467 11.00000 -1.50000 H25E 2 1.513114 0.329537 0.669392 11.00000 -1.50000 H25F 2 1.454792 0.364518 0.604439 11.00000 -1.50000 AFIX 0 C26B 1 1.205404 0.206828 0.356018 11.00000 0.02750 0.04849 = 0.02739 0.01542 0.00405 0.00226 AFIX 13 H26B 2 1.124360 0.169514 0.314177 11.00000 -1.20000 AFIX 0 C27B 1 1.343427 0.167030 0.349546 11.00000 0.04861 0.05990 = 0.04307 0.01982 0.02144 0.01954 AFIX 137 H27D 2 1.428836 0.206611 0.386891 11.00000 -1.50000 H27E 2 1.370649 0.165578 0.303550 11.00000 -1.50000 H27F 2 1.319355 0.103367 0.354045 11.00000 -1.50000 AFIX 0 C28B 1 1.242409 0.308302 0.353968 11.00000 0.05613 0.06294 = 0.05360 0.03799 0.02579 0.02000 AFIX 137 H28D 2 1.152013 0.332108 0.357320 11.00000 -1.50000 H28E 2 1.274921 0.311493 0.309659 11.00000 -1.50000 H28F 2 1.324047 0.346439 0.393611 11.00000 -1.50000 AFIX 0 C1C 1 1.143662 0.538655 0.489255 11.00000 0.05636 0.06107 = 0.02790 0.00214 -0.00179 0.00685 part 1 AFIX 43 D1C 4 1.241797 0.564943 0.482152 10.50000 -1.20000 AFIX 0 part 0 C2C 1 1.114041 0.456420 0.508704 11.00000 0.05941 0.05041 = 0.02652 0.00303 -0.00486 0.01808 AFIX 43 D2C 4 1.192920 0.426241 0.514509 11.00000 -1.20000 AFIX 0 C3C 1 1.026204 0.581937 0.480349 11.00000 0.06600 0.04846 = 0.03024 0.00653 -0.00367 0.01317 AFIX 43 D3C 4 1.043852 0.637924 0.466710 11.00000 -1.20000 AFIX 0 part 2 C7C 1 1.301067 0.577332 0.480930 10.50000 0.07197 0.07264 = 0.04315 0.02142 0.00643 -0.00193 AFIX 137 D7CA 4 1.362563 0.615184 0.526940 10.50000 -1.50000 D7CB 4 1.299066 0.616499 0.449048 10.50000 -1.50000 D7CC 4 1.345150 0.525764 0.461323 10.50000 -1.50000 AFIX 66 part 3 C1D 1 0.970872 0.113001 0.115098 10.50000 0.07821 0.07862 = 0.05468 0.03418 0.02181 -0.00377 C2D 1 0.871735 0.054892 0.054103 10.50000 0.08595 0.04031 = 0.04398 0.01657 -0.00456 0.00641 AFIX 43 D2D 4 0.879041 -0.007276 0.035122 10.50000 -1.20000 AFIX 65 C3D 1 0.761910 0.087745 0.020880 10.50000 0.12612 0.16570 = 0.11565 0.10444 0.05261 0.05922 AFIX 43 D3D 4 0.694155 0.048030 -0.020807 10.50000 -1.20000 AFIX 65 C4D 1 0.751219 0.178707 0.048652 10.50000 0.16142 0.15143 = 0.25727 0.17514 0.15346 0.11358 AFIX 43 D4D 4 0.676158 0.201160 0.025945 10.50000 -1.20000 AFIX 65 C5D 1 0.850355 0.236817 0.109647 10.50000 0.11324 0.07756 = 0.17195 0.04609 0.09837 0.02981 AFIX 43 D5D 4 0.843048 0.298985 0.128628 10.50000 -1.20000 AFIX 65 C6D 1 0.960181 0.203966 0.142871 10.50000 0.09051 0.05570 = 0.14765 0.04230 0.09100 0.01762 AFIX 43 D6D 4 1.027936 0.243681 0.184558 10.50000 -1.20000 AFIX 0 C7D 1 1.085050 0.077810 0.152908 10.50000 0.08470 0.12833 = 0.05987 0.04598 0.01282 0.01007 AFIX 3 D7DA 4 1.159079 0.130635 0.187740 10.50000 -1.50000 D7DB 4 1.137223 0.044547 0.119050 10.50000 -1.50000 D7DC 4 1.034010 0.034971 0.176790 10.50000 -1.50000 AFIX 66 part 4 C1E 1 0.916652 0.117586 0.097178 10.50000 0.06128 0.10959 = 0.05200 0.04601 0.00584 -0.01211 C2E 1 0.828820 0.046555 0.039001 10.50000 0.09780 0.05116 = 0.09258 0.04103 -0.00187 0.02199 AFIX 43 D2E 4 0.851041 -0.012750 0.027042 10.50000 -1.20000 AFIX 65 C3E 1 0.708477 0.062295 -0.001676 10.50000 0.14450 0.05516 = 0.09817 0.01796 -0.02256 0.00716 AFIX 43 D3E 4 0.648449 0.013749 -0.041437 10.50000 -1.20000 AFIX 65 C4E 1 0.675965 0.149067 0.015822 10.50000 0.08251 0.06786 = 0.07017 0.04332 0.01038 0.02115 AFIX 43 D4E 4 0.593715 0.159824 -0.011979 10.50000 -1.20000 AFIX 65 C5E 1 0.763795 0.220098 0.073999 10.50000 0.09810 0.05616 = 0.06623 0.02312 0.04197 0.01426 AFIX 43 D5E 4 0.741573 0.279402 0.085958 10.50000 -1.20000 AFIX 65 C6E 1 0.884138 0.204359 0.114677 10.50000 0.06269 0.06228 = 0.05438 0.00954 0.03702 0.01340 AFIX 43 D6E 4 0.944166 0.252906 0.154438 10.50000 -1.20000 AFIX 0 C7E 1 1.046710 0.107237 0.144817 10.50000 0.05573 0.20141 = 0.09430 0.11604 0.01278 0.00121 AFIX 3 D7EA 4 1.085908 0.056260 0.119513 10.50000 -1.50000 D7EB 4 1.012143 0.092769 0.186088 10.50000 -1.50000 D7EC 4 1.127206 0.165692 0.160038 10.50000 -1.50000 dfix 1.5 0.005 c1d c7d c1e c7e c1c c7c AFIX 0 HKLF 4 REM tw19c in P-1 REM R1 = 0.0575 for 8290 Fo > 4sig(Fo) and 0.0666 for all 10083 data REM 665 parameters refined using 3 restraints END WGHT 0.1143 0.3267 REM Highest difference peak 0.603, deepest hole -0.547, 1-sigma level 0.057 Q1 1 0.6924 0.3525 0.3197 11.00000 0.05 0.60 Q2 1 0.9781 0.0448 0.0910 11.00000 0.05 0.51 Q3 1 0.7492 0.4617 0.3309 11.00000 0.05 0.50 Q4 1 0.5930 0.3552 0.3294 11.00000 0.05 0.42 Q5 1 0.7961 0.1417 0.0529 11.00000 0.05 0.36 Q6 1 0.1303 0.5404 0.2191 11.00000 0.05 0.34 Q7 1 0.6364 0.4630 0.3348 11.00000 0.05 0.31 Q8 1 0.7278 0.0649 0.2376 11.00000 0.05 0.29 Q9 1 0.2688 0.5089 0.1462 11.00000 0.05 0.29 Q10 1 1.0968 0.2135 0.5421 11.00000 0.05 0.28 Q11 1 1.0626 0.1737 0.4203 11.00000 0.05 0.27 Q12 1 0.2584 0.7112 0.2311 11.00000 0.05 0.27 Q13 1 0.9057 -0.0059 0.2981 11.00000 0.05 0.26 Q14 1 0.1700 0.6319 0.2190 11.00000 0.05 0.26 Q15 1 0.3389 0.5858 0.1524 11.00000 0.05 0.26 Q16 1 0.8220 0.3955 0.3475 11.00000 0.05 0.26 Q17 1 0.7391 0.4927 0.3880 11.00000 0.05 0.26 Q18 1 1.1867 0.5977 0.4785 11.00000 0.05 0.25 Q19 1 1.3644 0.2936 0.6129 11.00000 0.05 0.25 Q20 1 0.8637 0.1174 0.4760 11.00000 0.05 0.25 ; _shelx_res_checksum 98167 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.801 _oxdiff_exptl_absorpt_empirical_full_min 0.655 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S S 0.66675(4) 0.40800(3) 0.32820(2) 0.02537(13) Uani 1 1 d . . . . . C1A C 0.53931(18) 0.38214(12) 0.24885(8) 0.0229(3) Uani 1 1 d . . . . . C2A C 0.52050(17) 0.28853(12) 0.20576(9) 0.0227(3) Uani 1 1 d . . . . . C3A C 0.41791(18) 0.25498(12) 0.13969(9) 0.0240(3) Uani 1 1 d . . . . . H3A H 0.4045 0.1933 0.1101 0.029 Uiso 1 1 calc R U . . . C4A C 0.33944(17) 0.31363(12) 0.11991(9) 0.0231(3) Uani 1 1 d . . . . . C5A C 0.36162(18) 0.40832(12) 0.16357(9) 0.0242(3) Uani 1 1 d . . . . . C6A C 0.46316(18) 0.44241(12) 0.22922(9) 0.0240(3) Uani 1 1 d . . . . . H6 H 0.4780 0.5044 0.2585 0.029 Uiso 1 1 calc R U . . . C7A C 0.22448(18) 0.30044(12) 0.05759(9) 0.0252(4) Uani 1 1 d . . . . . C8A C 0.15743(19) 0.22455(13) -0.00056(10) 0.0304(4) Uani 1 1 d . . . . . H8A H 0.1861 0.1674 -0.0061 0.036 Uiso 1 1 calc R U . . . C9A C 0.0463(2) 0.23369(15) -0.05108(10) 0.0370(4) Uani 1 1 d . . . . . H9A H -0.0011 0.1819 -0.0912 0.044 Uiso 1 1 calc R U . . . C10A C 0.0042(2) 0.31653(15) -0.04371(10) 0.0375(4) Uani 1 1 d . . . . . H10A H -0.0714 0.3211 -0.0788 0.045 Uiso 1 1 calc R U . . . C11A C 0.0715(2) 0.39362(14) 0.01465(10) 0.0335(4) Uani 1 1 d . . . . . H11A H 0.0424 0.4506 0.0198 0.040 Uiso 1 1 calc R U . . . C12A C 0.18245(18) 0.38543(13) 0.06538(9) 0.0266(4) Uani 1 1 d . . . . . C13A C 0.26988(18) 0.45317(12) 0.13052(9) 0.0254(4) Uani 1 1 d . . . . . C14A C 0.26782(18) 0.55269(12) 0.15842(9) 0.0258(4) Uani 1 1 d . . . . . C15A C 0.36193(19) 0.62178(12) 0.13721(9) 0.0273(4) Uani 1 1 d . . . . . C16A C 0.37236(19) 0.71583(13) 0.16991(10) 0.0298(4) Uani 1 1 d . . . . . H16A H 0.4390 0.7628 0.1570 0.036 Uiso 1 1 calc R U . . . C17A C 0.28738(19) 0.74274(13) 0.22106(10) 0.0305(4) Uani 1 1 d . . . . . C18A C 0.18983(19) 0.67262(13) 0.23800(10) 0.0316(4) Uani 1 1 d . . . . . H18A H 0.1286 0.6897 0.2714 0.038 Uiso 1 1 calc R U . . . C19A C 0.17789(19) 0.57758(13) 0.20785(10) 0.0299(4) Uani 1 1 d . . . . . C20A C 0.4527(2) 0.59377(13) 0.08037(10) 0.0294(4) Uani 1 1 d . . . . . H20A H 0.4030 0.5269 0.0536 0.035 Uiso 1 1 calc R U . . . C21A C 0.6150(2) 0.59814(14) 0.11247(11) 0.0339(4) Uani 1 1 d . . . . . H21A H 0.6643 0.6614 0.1433 0.051 Uiso 1 1 calc R U . . . H21B H 0.6717 0.5825 0.0748 0.051 Uiso 1 1 calc R U . . . H21C H 0.6130 0.5533 0.1399 0.051 Uiso 1 1 calc R U . . . C22A C 0.4496(2) 0.65065(15) 0.02750(11) 0.0372(4) Uani 1 1 d . . . . . H22A H 0.3443 0.6476 0.0089 0.056 Uiso 1 1 calc R U . . . H22B H 0.4977 0.6248 -0.0113 0.056 Uiso 1 1 calc R U . . . H22C H 0.5049 0.7160 0.0510 0.056 Uiso 1 1 calc R U . . . C23A C 0.3044(2) 0.84555(14) 0.25837(11) 0.0350(4) Uani 1 1 d . . . . . H25 H 0.2175 0.8490 0.2834 0.042 Uiso 1 1 calc R U . . . C24A C 0.4505(2) 0.88668(14) 0.31407(11) 0.0385(4) Uani 1 1 d . . . . . H24A H 0.5380 0.8820 0.2914 0.058 Uiso 1 1 calc R U . . . H24B H 0.4487 0.8518 0.3490 0.058 Uiso 1 1 calc R U . . . H24C H 0.4581 0.9526 0.3374 0.058 Uiso 1 1 calc R U . . . C25A C 0.2986(3) 0.90550(15) 0.20801(12) 0.0460(5) Uani 1 1 d . . . . . H25A H 0.2989 0.9690 0.2343 0.069 Uiso 1 1 calc R U . . . H25B H 0.2060 0.8781 0.1720 0.069 Uiso 1 1 calc R U . . . H25C H 0.3873 0.9078 0.1854 0.069 Uiso 1 1 calc R U . . . C26A C 0.0662(2) 0.50247(14) 0.22635(11) 0.0356(4) Uani 1 1 d . . . . . H26A H 0.0877 0.4411 0.2049 0.043 Uiso 1 1 calc R U . . . C27A C -0.0969(2) 0.49657(17) 0.19338(11) 0.0431(5) Uani 1 1 d . . . . . H27A H -0.1215 0.5560 0.2132 0.065 Uiso 1 1 calc R U . . . H27B H -0.1671 0.4458 0.2037 0.065 Uiso 1 1 calc R U . . . H27C H -0.1063 0.4842 0.1423 0.065 Uiso 1 1 calc R U . . . C28A C 0.0843(2) 0.51664(18) 0.30559(12) 0.0451(5) Uani 1 1 d . . . . . H28A H 0.1885 0.5183 0.3249 0.068 Uiso 1 1 calc R U . . . H28B H 0.0139 0.4648 0.3146 0.068 Uiso 1 1 calc R U . . . H28C H 0.0620 0.5758 0.3282 0.068 Uiso 1 1 calc R U . . . C1B C 0.69805(18) 0.29598(12) 0.30497(9) 0.0240(3) Uani 1 1 d . . . . . C2B C 0.61065(18) 0.24008(12) 0.23724(9) 0.0241(3) Uani 1 1 d . . . . . C3B C 0.62140(18) 0.14660(12) 0.20981(9) 0.0245(3) Uani 1 1 d . . . . . H3B H 0.5648 0.1087 0.1649 0.029 Uiso 1 1 calc R U . . . C4B C 0.71510(18) 0.11268(12) 0.24958(9) 0.0247(3) Uani 1 1 d . . . . . C5B C 0.80102(18) 0.16969(12) 0.31842(9) 0.0245(3) Uani 1 1 d . . . . . C6B C 0.79304(18) 0.26296(12) 0.34551(9) 0.0249(3) Uani 1 1 d . . . . . H6B H 0.8510 0.3014 0.3900 0.030 Uiso 1 1 calc R U . . . C7B C 0.75373(18) 0.02261(12) 0.23590(9) 0.0250(4) Uani 1 1 d . . . . . C8B C 0.71173(19) -0.05568(12) 0.17802(9) 0.0282(4) Uani 1 1 d . . . . . H8B H 0.6432 -0.0578 0.1376 0.034 Uiso 1 1 calc R U . . . C9B C 0.7720(2) -0.13160(13) 0.18009(10) 0.0314(4) Uani 1 1 d . . . . . H9B H 0.7444 -0.1857 0.1406 0.038 Uiso 1 1 calc R U . . . C10B C 0.8721(2) -0.12892(13) 0.23957(10) 0.0331(4) Uani 1 1 d . . . . . H10B H 0.9109 -0.1816 0.2402 0.040 Uiso 1 1 calc R U . . . C11B C 0.9161(2) -0.04980(12) 0.29814(10) 0.0293(4) Uani 1 1 d . . . . . H11B H 0.9848 -0.0480 0.3384 0.035 Uiso 1 1 calc R U . . . C12B C 0.85705(18) 0.02622(12) 0.29630(9) 0.0262(4) Uani 1 1 d . . . . . C13B C 0.88609(18) 0.11761(12) 0.34722(9) 0.0247(3) Uani 1 1 d . . . . . C14B C 0.99126(18) 0.15140(11) 0.41648(9) 0.0230(3) Uani 1 1 d . . . . . C15B C 0.93812(18) 0.13915(12) 0.47749(9) 0.0257(4) Uani 1 1 d . . . . . C16B C 1.03820(19) 0.17511(12) 0.54182(9) 0.0260(4) Uani 1 1 d . . . . . H16B H 1.0024 0.1669 0.5829 0.031 Uiso 1 1 calc R U . . . C17B C 1.18899(19) 0.22268(12) 0.54843(9) 0.0254(4) Uani 1 1 d . . . . . C18B C 1.23960(18) 0.23219(12) 0.48735(9) 0.0270(4) Uani 1 1 d . . . . . H18B H 1.3423 0.2637 0.4906 0.032 Uiso 1 1 calc R U . . . C19B C 1.14352(19) 0.19662(12) 0.42137(9) 0.0268(4) Uani 1 1 d . . . . . C20B C 0.77335(19) 0.09017(14) 0.47370(10) 0.0318(4) Uani 1 1 d . . . . . H20B H 0.7292 0.0539 0.4235 0.038 Uiso 1 1 calc R U . . . C21B C 0.7555(2) 0.02132(14) 0.51779(13) 0.0401(5) Uani 1 1 d . . . . . H21D H 0.8235 -0.0196 0.5074 0.060 Uiso 1 1 calc R U . . . H21E H 0.6504 -0.0167 0.5063 0.060 Uiso 1 1 calc R U . . . H21F H 0.7813 0.0562 0.5679 0.060 Uiso 1 1 calc R U . . . C22B C 0.6837(2) 0.16248(16) 0.49605(14) 0.0459(6) Uani 1 1 d . . . . . H22D H 0.7223 0.1975 0.5457 0.069 Uiso 1 1 calc R U . . . H22E H 0.5763 0.1305 0.4896 0.069 Uiso 1 1 calc R U . . . H22F H 0.6951 0.2058 0.4672 0.069 Uiso 1 1 calc R U . . . C23B C 1.29100(19) 0.26037(13) 0.62116(9) 0.0286(4) Uani 1 1 d . . . . . H23B H 1.2946 0.2056 0.6395 0.034 Uiso 1 1 calc R U . . . C24B C 1.2245(2) 0.32640(14) 0.67264(10) 0.0350(4) Uani 1 1 d . . . . . H24D H 1.2220 0.3819 0.6569 0.053 Uiso 1 1 calc R U . . . H24E H 1.2878 0.3455 0.7197 0.053 Uiso 1 1 calc R U . . . H24F H 1.1213 0.2940 0.6742 0.053 Uiso 1 1 calc R U . . . C25B C 1.4539(2) 0.30963(15) 0.62138(10) 0.0363(4) Uani 1 1 d . . . . . H25D H 1.4986 0.2665 0.5905 0.054 Uiso 1 1 calc R U . . . H25E H 1.5131 0.3295 0.6694 0.054 Uiso 1 1 calc R U . . . H25F H 1.4548 0.3645 0.6044 0.054 Uiso 1 1 calc R U . . . C26B C 1.2054(2) 0.20683(15) 0.35602(10) 0.0349(4) Uani 1 1 d . . . . . H26B H 1.1244 0.1695 0.3142 0.042 Uiso 1 1 calc R U . . . C27B C 1.3434(3) 0.16703(18) 0.34955(12) 0.0475(5) Uani 1 1 d . . . . . H27D H 1.4288 0.2066 0.3869 0.071 Uiso 1 1 calc R U . . . H27E H 1.3706 0.1656 0.3035 0.071 Uiso 1 1 calc R U . . . H27F H 1.3194 0.1034 0.3540 0.071 Uiso 1 1 calc R U . . . C28B C 1.2424(3) 0.30830(18) 0.35397(14) 0.0514(6) Uani 1 1 d . . . . . H28D H 1.1520 0.3321 0.3573 0.077 Uiso 1 1 calc R U . . . H28E H 1.2749 0.3115 0.3097 0.077 Uiso 1 1 calc R U . . . H28F H 1.3240 0.3464 0.3936 0.077 Uiso 1 1 calc R U . . . C1C C 1.1437(3) 0.53866(18) 0.48926(12) 0.0527(6) Uani 1 1 d D . . . . D1C D 1.2418 0.5649 0.4822 0.063 Uiso 0.5 1 calc R U P A 1 C2C C 1.1140(3) 0.45642(17) 0.50870(11) 0.0476(5) Uani 1 1 d . . . . . D2C D 1.1929 0.4262 0.5145 0.057 Uiso 1 1 calc R U . . . C3C C 1.0262(3) 0.58194(17) 0.48035(12) 0.0506(6) Uani 1 1 d . . . . . D3C D 1.0439 0.6379 0.4667 0.061 Uiso 1 1 calc R U . . . C7C C 1.3011(5) 0.5773(4) 0.4809(3) 0.0654(14) Uani 0.5 1 d D . P B 2 D7CA D 1.3626 0.6152 0.5269 0.098 Uiso 0.5 1 calc R U P B 2 D7CB D 1.2991 0.6165 0.4490 0.098 Uiso 0.5 1 calc R U P B 2 D7CC D 1.3451 0.5258 0.4613 0.098 Uiso 0.5 1 calc R U P B 2 C1D C 0.9709(8) 0.1130(4) 0.1151(4) 0.071(2) Uani 0.5 1 d DG . P C 3 C2D C 0.8717(9) 0.0549(4) 0.0541(4) 0.059(2) Uani 0.5 1 d G . P C 3 D2D D 0.8790 -0.0073 0.0351 0.071 Uiso 0.5 1 calc R U P C 3 C3D C 0.7619(9) 0.0877(6) 0.0209(4) 0.118(4) Uani 0.5 1 d G . P C 3 D3D D 0.6942 0.0480 -0.0208 0.141 Uiso 0.5 1 calc R U P C 3 C4D C 0.7512(9) 0.1787(6) 0.0487(5) 0.146(7) Uani 0.5 1 d G . P C 3 D4D D 0.6762 0.2012 0.0259 0.175 Uiso 0.5 1 calc R U P C 3 C5D C 0.8504(10) 0.2368(4) 0.1096(5) 0.112(5) Uani 0.5 1 d G . P C 3 D5D D 0.8430 0.2990 0.1286 0.134 Uiso 0.5 1 calc R U P C 3 C6D C 0.9602(8) 0.2040(4) 0.1429(4) 0.089(3) Uani 0.5 1 d G . P C 3 D6D D 1.0279 0.2437 0.1846 0.107 Uiso 0.5 1 calc R U P C 3 C7D C 1.0850(12) 0.0778(9) 0.1529(6) 0.090(3) Uani 0.5 1 d D . P C 3 D7DA D 1.1591 0.1306 0.1877 0.135 Uiso 0.5 1 d R U P C 3 D7DB D 1.1372 0.0445 0.1190 0.135 Uiso 0.5 1 d R U P C 3 D7DC D 1.0340 0.0350 0.1768 0.135 Uiso 0.5 1 d R U P C 3 C1E C 0.9167(8) 0.1176(5) 0.0972(4) 0.076(3) Uani 0.5 1 d DG . P D 4 C2E C 0.8288(10) 0.0466(4) 0.0390(5) 0.078(3) Uani 0.5 1 d G . P D 4 D2E D 0.8510 -0.0127 0.0270 0.094 Uiso 0.5 1 calc R U P D 4 C3E C 0.7085(10) 0.0623(4) -0.0017(4) 0.107(4) Uani 0.5 1 d G . P D 4 D3E D 0.6484 0.0137 -0.0414 0.129 Uiso 0.5 1 calc R U P D 4 C4E C 0.6760(7) 0.1491(4) 0.0158(3) 0.069(2) Uani 0.5 1 d G . P D 4 D4E D 0.5937 0.1598 -0.0120 0.083 Uiso 0.5 1 calc R U P D 4 C5E C 0.7638(7) 0.2201(4) 0.0740(3) 0.071(2) Uani 0.5 1 d G . P D 4 D5E D 0.7416 0.2794 0.0860 0.085 Uiso 0.5 1 calc R U P D 4 C6E C 0.8841(6) 0.2044(4) 0.1147(3) 0.059(2) Uani 0.5 1 d G . P D 4 D6E D 0.9442 0.2529 0.1544 0.071 Uiso 0.5 1 calc R U P D 4 C7E C 1.0467(9) 0.1072(11) 0.1448(6) 0.108(5) Uani 0.5 1 d D . P D 4 D7EA D 1.0859 0.0563 0.1195 0.163 Uiso 0.5 1 d R U P D 4 D7EB D 1.0121 0.0928 0.1861 0.163 Uiso 0.5 1 d R U P D 4 D7EC D 1.1272 0.1657 0.1600 0.163 Uiso 0.5 1 d R U P D 4 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 S 0.0255(2) 0.0274(2) 0.0224(2) 0.00862(16) -0.00323(16) 0.00782(16) C1A 0.0207(7) 0.0275(8) 0.0189(7) 0.0078(6) -0.0003(6) 0.0037(6) C2A 0.0190(7) 0.0268(8) 0.0232(8) 0.0109(7) 0.0015(6) 0.0049(6) C3A 0.0218(8) 0.0280(8) 0.0238(8) 0.0110(7) 0.0022(6) 0.0068(6) C4A 0.0192(7) 0.0282(8) 0.0215(8) 0.0094(7) 0.0011(6) 0.0039(6) C5A 0.0213(8) 0.0288(8) 0.0238(8) 0.0119(7) 0.0013(6) 0.0058(6) C6A 0.0223(8) 0.0263(8) 0.0239(8) 0.0101(7) 0.0006(6) 0.0059(6) C7A 0.0204(8) 0.0333(9) 0.0230(8) 0.0127(7) 0.0001(6) 0.0058(7) C8A 0.0268(9) 0.0346(9) 0.0279(9) 0.0083(7) -0.0016(7) 0.0087(7) C9A 0.0299(9) 0.0477(11) 0.0278(9) 0.0070(8) -0.0055(8) 0.0093(8) C10A 0.0305(9) 0.0512(12) 0.0292(10) 0.0126(9) -0.0073(8) 0.0139(8) C11A 0.0308(9) 0.0409(10) 0.0313(9) 0.0148(8) -0.0034(7) 0.0145(8) C12A 0.0223(8) 0.0344(9) 0.0243(8) 0.0125(7) 0.0006(7) 0.0073(7) C13A 0.0219(8) 0.0311(9) 0.0254(8) 0.0126(7) 0.0016(6) 0.0077(7) C14A 0.0209(8) 0.0321(9) 0.0256(8) 0.0113(7) -0.0024(6) 0.0100(7) C15A 0.0233(8) 0.0328(9) 0.0278(9) 0.0121(7) -0.0001(7) 0.0102(7) C16A 0.0252(8) 0.0323(9) 0.0337(9) 0.0130(8) 0.0030(7) 0.0086(7) C17A 0.0239(8) 0.0341(10) 0.0327(9) 0.0089(8) -0.0013(7) 0.0108(7) C18A 0.0240(8) 0.0413(10) 0.0316(9) 0.0103(8) 0.0030(7) 0.0145(8) C19A 0.0245(8) 0.0378(10) 0.0308(9) 0.0147(8) 0.0011(7) 0.0118(7) C20A 0.0296(9) 0.0308(9) 0.0295(9) 0.0116(7) 0.0047(7) 0.0083(7) C21A 0.0313(9) 0.0380(10) 0.0373(10) 0.0146(8) 0.0083(8) 0.0135(8) C22A 0.0393(10) 0.0427(11) 0.0348(10) 0.0183(9) 0.0083(8) 0.0127(9) C23A 0.0270(9) 0.0339(10) 0.0405(11) 0.0052(8) 0.0016(8) 0.0099(8) C24A 0.0403(11) 0.0367(10) 0.0338(10) 0.0059(8) -0.0029(8) 0.0106(8) C25A 0.0458(12) 0.0332(10) 0.0507(13) 0.0066(9) -0.0151(10) 0.0136(9) C26A 0.0322(10) 0.0391(10) 0.0396(11) 0.0152(9) 0.0107(8) 0.0109(8) C27A 0.0313(10) 0.0577(13) 0.0366(11) 0.0131(10) 0.0058(8) 0.0048(9) C28A 0.0366(11) 0.0632(14) 0.0441(12) 0.0300(11) 0.0083(9) 0.0134(10) C1B 0.0227(8) 0.0265(8) 0.0233(8) 0.0103(7) 0.0014(6) 0.0056(6) C2B 0.0202(8) 0.0305(9) 0.0229(8) 0.0126(7) 0.0007(6) 0.0055(7) C3B 0.0219(8) 0.0290(8) 0.0224(8) 0.0107(7) -0.0004(6) 0.0053(6) C4B 0.0224(8) 0.0289(9) 0.0232(8) 0.0108(7) 0.0017(6) 0.0054(7) C5B 0.0207(8) 0.0310(9) 0.0228(8) 0.0126(7) -0.0004(6) 0.0057(7) C6B 0.0225(8) 0.0285(8) 0.0232(8) 0.0107(7) -0.0021(6) 0.0053(7) C7B 0.0215(8) 0.0297(9) 0.0265(9) 0.0142(7) 0.0023(6) 0.0061(7) C8B 0.0275(8) 0.0298(9) 0.0257(9) 0.0099(7) -0.0003(7) 0.0052(7) C9B 0.0309(9) 0.0306(9) 0.0314(9) 0.0085(8) 0.0028(7) 0.0075(7) C10B 0.0340(10) 0.0299(9) 0.0374(10) 0.0123(8) 0.0020(8) 0.0123(8) C11B 0.0296(9) 0.0295(9) 0.0301(9) 0.0132(7) -0.0004(7) 0.0085(7) C12B 0.0218(8) 0.0316(9) 0.0254(8) 0.0121(7) -0.0002(7) 0.0053(7) C13B 0.0212(8) 0.0286(8) 0.0261(9) 0.0130(7) 0.0018(7) 0.0059(6) C14B 0.0232(8) 0.0243(8) 0.0230(8) 0.0096(6) 0.0000(6) 0.0087(6) C15B 0.0240(8) 0.0298(9) 0.0267(9) 0.0130(7) 0.0033(7) 0.0087(7) C16B 0.0275(8) 0.0313(9) 0.0232(8) 0.0132(7) 0.0038(7) 0.0099(7) C17B 0.0252(8) 0.0284(8) 0.0249(8) 0.0108(7) -0.0002(7) 0.0107(7) C18B 0.0194(8) 0.0325(9) 0.0295(9) 0.0118(7) 0.0020(7) 0.0059(7) C19B 0.0253(8) 0.0329(9) 0.0256(9) 0.0136(7) 0.0039(7) 0.0092(7) C20B 0.0239(8) 0.0406(10) 0.0291(9) 0.0138(8) 0.0015(7) 0.0023(7) C21B 0.0315(10) 0.0364(10) 0.0576(13) 0.0227(10) 0.0122(9) 0.0068(8) C22B 0.0247(9) 0.0554(13) 0.0723(16) 0.0389(12) 0.0121(10) 0.0149(9) C23B 0.0264(9) 0.0350(9) 0.0247(9) 0.0103(7) -0.0021(7) 0.0105(7) C24B 0.0340(10) 0.0404(10) 0.0269(9) 0.0066(8) 0.0013(8) 0.0082(8) C25B 0.0275(9) 0.0444(11) 0.0317(10) 0.0065(8) -0.0053(7) 0.0097(8) C26B 0.0275(9) 0.0485(11) 0.0274(9) 0.0154(8) 0.0041(7) 0.0023(8) C27B 0.0486(12) 0.0599(14) 0.0431(12) 0.0198(11) 0.0214(10) 0.0195(11) C28B 0.0561(13) 0.0629(15) 0.0536(14) 0.0380(12) 0.0258(11) 0.0200(11) C1C 0.0564(13) 0.0611(15) 0.0279(10) 0.0021(10) -0.0018(10) 0.0069(11) C2C 0.0594(14) 0.0504(13) 0.0265(10) 0.0030(9) -0.0049(9) 0.0181(11) C3C 0.0660(15) 0.0485(13) 0.0302(11) 0.0065(9) -0.0037(10) 0.0132(11) C7C 0.072(3) 0.073(4) 0.043(3) 0.021(3) 0.006(2) -0.002(3) C1D 0.078(7) 0.079(5) 0.055(5) 0.034(4) 0.022(5) -0.004(4) C2D 0.086(5) 0.040(3) 0.044(3) 0.017(3) -0.005(4) 0.006(3) C3D 0.126(8) 0.166(11) 0.116(8) 0.104(9) 0.053(7) 0.059(8) C4D 0.161(14) 0.151(12) 0.257(19) 0.175(13) 0.153(14) 0.114(11) C5D 0.113(9) 0.078(7) 0.172(13) 0.046(8) 0.098(9) 0.030(7) C6D 0.091(6) 0.056(4) 0.148(9) 0.042(5) 0.091(6) 0.018(4) C7D 0.085(6) 0.128(8) 0.060(5) 0.046(5) 0.013(4) 0.010(5) C1E 0.061(5) 0.110(7) 0.052(5) 0.046(5) 0.006(4) -0.012(4) C2E 0.098(6) 0.051(4) 0.093(7) 0.041(4) -0.002(5) 0.022(4) C3E 0.144(9) 0.055(4) 0.098(7) 0.018(4) -0.023(6) 0.007(5) C4E 0.083(5) 0.068(4) 0.070(4) 0.043(3) 0.010(4) 0.021(4) C5E 0.098(6) 0.056(4) 0.066(4) 0.023(4) 0.042(4) 0.014(4) C6E 0.063(4) 0.062(5) 0.054(4) 0.010(3) 0.037(3) 0.013(4) C7E 0.056(6) 0.201(13) 0.094(7) 0.116(8) 0.013(5) 0.001(6) 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' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' D D 0.0000 0.0000 '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 _geom_angle_publ_flag C1A S C1B 91.41(8) . . ? C2A C1A S 111.99(12) . . ? C6A C1A S 125.22(13) . . ? C6A C1A C2A 122.79(15) . . ? C3A C2A C1A 119.48(15) . . ? C2B C2A C1A 112.35(15) . . ? C2B C2A C3A 128.17(16) . . ? C4A C3A C2A 118.43(16) . . ? C3A C4A C5A 121.31(15) . . ? C3A C4A C7A 132.02(16) . . ? C5A C4A C7A 106.66(14) . . ? C6A C5A C4A 120.75(15) . . ? C13A C5A C4A 109.52(15) . . ? C13A C5A C6A 129.73(16) . . ? C1A C6A C5A 117.22(15) . . ? C8A C7A C4A 132.38(16) . . ? C8A C7A C12A 120.53(15) . . ? C12A C7A C4A 107.08(15) . . ? C7A C8A C9A 118.56(17) . . ? C10A C9A C8A 121.24(18) . . ? C9A C10A C11A 120.65(17) . . ? C10A C11A C12A 118.68(18) . . ? C7A C12A C13A 109.27(14) . . ? C11A C12A C7A 120.34(17) . . ? C11A C12A C13A 130.39(17) . . ? C5A C13A C12A 107.43(15) . . ? C5A C13A C14A 124.69(15) . . ? C12A C13A C14A 127.88(14) . . ? C15A C14A C13A 119.44(16) . . ? C19A C14A C13A 120.12(16) . . ? C19A C14A C15A 120.38(17) . . ? C14A C15A C20A 120.05(16) . . ? C16A C15A C14A 118.86(16) . . ? C16A C15A C20A 121.08(16) . . ? C15A C16A C17A 121.83(17) . . ? C16A C17A C23A 121.28(17) . . ? C18A C17A C16A 117.68(17) . . ? C18A C17A C23A 121.02(17) . . ? C17A C18A C19A 122.57(17) . . ? C14A C19A C26A 120.42(17) . . ? C18A C19A C14A 118.52(17) . . ? C18A C19A C26A 121.03(17) . . ? C15A C20A C21A 111.37(15) . . ? C15A C20A C22A 112.50(15) . . ? C21A C20A C22A 111.61(15) . . ? C17A C23A C24A 111.22(15) . . ? C17A C23A C25A 113.25(17) . . ? C25A C23A C24A 109.88(17) . . ? C19A C26A C27A 110.37(16) . . ? C19A C26A C28A 112.64(17) . . ? C28A C26A C27A 111.37(16) . . ? C2B C1B S 111.76(12) . . ? C6B C1B S 125.63(14) . . ? C6B C1B C2B 122.61(16) . . ? C2A C2B C1B 112.48(15) . . ? C2A C2B C3B 127.94(15) . . ? C3B C2B C1B 119.58(15) . . ? C4B C3B C2B 118.51(15) . . ? C3B C4B C5B 121.21(16) . . ? C3B C4B C7B 131.72(16) . . ? C5B C4B C7B 107.06(14) . . ? C6B C5B C4B 120.66(15) . . ? C13B C5B C4B 109.09(15) . . ? C13B C5B C6B 130.24(16) . . ? C1B C6B C5B 117.42(16) . . ? C8B C7B C4B 132.13(15) . . ? C8B C7B C12B 120.74(16) . . ? C12B C7B C4B 107.10(15) . . ? C7B C8B C9B 118.74(16) . . ? C10B C9B C8B 120.80(17) . . ? C9B C10B C11B 120.85(17) . . ? C12B C11B C10B 118.65(16) . . ? C7B C12B C13B 108.92(15) . . ? C11B C12B C7B 120.22(17) . . ? C11B C12B C13B 130.82(16) . . ? C5B C13B C12B 107.81(15) . . ? C5B C13B C14B 125.87(16) . . ? C12B C13B C14B 126.29(14) . . ? C15B C14B C13B 120.28(15) . . ? C19B C14B C13B 119.85(15) . . ? C19B C14B C15B 119.86(15) . . ? C14B C15B C20B 120.97(15) . . ? C16B C15B C14B 118.69(15) . . ? C16B C15B C20B 120.31(15) . . ? C15B C16B C17B 122.59(16) . . ? C16B C17B C23B 119.20(15) . . ? C18B C17B C16B 117.67(15) . . ? C18B C17B C23B 123.13(15) . . ? C17B C18B C19B 121.83(16) . . ? C14B C19B C26B 120.93(15) . . ? C18B C19B C14B 119.32(16) . . ? C18B C19B C26B 119.75(15) . . ? C15B C20B C21B 113.09(15) . . ? C15B C20B C22B 110.11(16) . . ? C22B C20B C21B 110.16(16) . . ? C17B C23B C24B 111.21(14) . . ? C25B C23B C17B 114.26(15) . . ? C25B C23B C24B 109.25(16) . . ? C19B C26B C27B 111.54(16) . . ? C19B C26B C28B 111.81(18) . . ? C28B C26B C27B 110.77(17) . . ? C2C C1C C3C 118.7(2) . . ? C2C C1C C7C 117.8(3) . . ? C3C C1C C7C 123.5(3) . . ? C3C C2C C1C 121.4(2) 2_766 . ? C2C C3C C1C 119.9(2) 2_766 . ? C2D C1D C6D 120.0 . . ? C2D C1D C7D 120.7(6) . . ? C6D C1D C7D 119.2(6) . . ? C1D C2D C3D 120.0 . . ? C4D C3D C2D 120.0 . . ? C3D C4D C5D 120.0 . . ? C6D C5D C4D 120.0 . . ? C5D C6D C1D 120.0 . . ? C2E C1E C6E 120.0 . . ? C2E C1E C7E 124.1(8) . . ? C6E C1E C7E 115.9(8) . . ? C1E C2E C3E 120.0 . . ? C4E C3E C2E 120.0 . . ? C3E C4E C5E 120.0 . . ? C4E C5E C6E 120.0 . . ? C5E C6E C1E 120.0 . . ? 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 S C1A 1.7505(17) . ? S C1B 1.7528(18) . ? C1A C2A 1.432(2) . ? C1A C6A 1.373(2) . ? C2A C3A 1.427(2) . ? C2A C2B 1.414(2) . ? C3A C4A 1.366(2) . ? C4A C5A 1.445(2) . ? C4A C7A 1.470(2) . ? C5A C6A 1.416(2) . ? C5A C13A 1.399(2) . ? C7A C8A 1.381(3) . ? C7A C12A 1.410(2) . ? C8A C9A 1.400(2) . ? C9A C10A 1.380(3) . ? C10A C11A 1.394(3) . ? C11A C12A 1.395(2) . ? C12A C13A 1.453(2) . ? C13A C14A 1.487(2) . ? C14A C15A 1.404(2) . ? C14A C19A 1.400(3) . ? C15A C16A 1.397(3) . ? C15A C20A 1.523(3) . ? C16A C17A 1.398(3) . ? C17A C18A 1.384(3) . ? C17A C23A 1.523(3) . ? C18A C19A 1.399(3) . ? C19A C26A 1.521(3) . ? C20A C21A 1.530(2) . ? C20A C22A 1.531(2) . ? C23A C24A 1.532(3) . ? C23A C25A 1.527(3) . ? C26A C27A 1.536(3) . ? C26A C28A 1.527(3) . ? C1B C2B 1.434(2) . ? C1B C6B 1.376(2) . ? C2B C3B 1.424(2) . ? C3B C4B 1.368(2) . ? C4B C5B 1.450(2) . ? C4B C7B 1.463(2) . ? C5B C6B 1.412(2) . ? C5B C13B 1.401(2) . ? C7B C8B 1.382(3) . ? C7B C12B 1.421(2) . ? C8B C9B 1.396(2) . ? C9B C10B 1.396(3) . ? C10B C11B 1.397(3) . ? C11B C12B 1.390(2) . ? C12B C13B 1.453(3) . ? C13B C14B 1.486(2) . ? C14B C15B 1.411(2) . ? C14B C19B 1.402(2) . ? C15B C16B 1.390(2) . ? C15B C20B 1.523(2) . ? C16B C17B 1.394(2) . ? C17B C18B 1.391(2) . ? C17B C23B 1.526(2) . ? C18B C19B 1.398(2) . ? C19B C26B 1.520(2) . ? C20B C21B 1.531(3) . ? C20B C22B 1.528(3) . ? C23B C24B 1.533(3) . ? C23B C25B 1.525(3) . ? C26B C27B 1.527(3) . ? C26B C28B 1.527(3) . ? C1C C2C 1.390(4) . ? C1C C3C 1.398(3) . ? C1C C7C 1.489(4) . ? C2C C3C 1.367(4) 2_766 ? C3C C2C 1.367(4) 2_766 ? C1D C2D 1.3900 . ? C1D C6D 1.3900 . ? C1D C7D 1.488(5) . ? C2D C3D 1.3900 . ? C3D C4D 1.3900 . ? C4D C5D 1.3900 . ? C5D C6D 1.3900 . ? C1E C2E 1.3900 . ? C1E C6E 1.3900 . ? C1E C7E 1.495(5) . ? C2E C3E 1.3900 . ? C3E C4E 1.3900 . ? C4E C5E 1.3900 . ? C5E C6E 1.3900 . ?