#------------------------------------------------------------------------------ #$Date: 2025-02-21 10:25:04 +0200 (Fri, 21 Feb 2025) $ #$Revision: 297825 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/35/08/4350836.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_4350836 loop_ _publ_author_name 'Satabdi Roy' 'Michael B\"ohme' 'Subhashree P. Dash' 'Monalisa Mohanty' 'Axel Buchholz' 'Winfried Plass' 'Sudarshana Majumder' 'Senthilguru Kulanthaivel' 'Indranil Banerjee' 'Hans Reuter' 'Werner Kaminsky' 'Rupam Dinda' _publ_contact_author 'Rupam Dinda' _publ_contact_author_email rupamdinda@nitrkl.ac.in _publ_section_title ; Anionic Dinuclear Oxidovanadium(IV) Complexes with Azo Functionalized Tridentate Ligands and \m-Ethoxido Bridge Leading to an Unsymmetric Twisted Arrangement: Synthesis, X-ray Structure, Magnetic Properties, and Cytotoxicity ; _journal_coden_ASTM INOCAJ _journal_issue 10 _journal_name_full 'Inorganic Chemistry' _journal_page_first 5767 _journal_page_last 5781 _journal_paper_doi 10.1021/acs.inorgchem.8b00035 _journal_volume 57 _journal_year 2018 _chemical_formula_moiety 'C36 H23 Br2 N4 O9 V2, C6 H16 N' _chemical_formula_sum 'C42 H39 Br2 N5 O9 V2' _chemical_formula_weight 1019.48 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_creation_date 2013-10-24T13:30:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 93.516(2) _cell_angle_beta 107.485(3) _cell_angle_gamma 95.750(2) _cell_formula_units_Z 2 _cell_length_a 11.0675(5) _cell_length_b 12.2101(6) _cell_length_c 16.9540(8) _cell_measurement_reflns_used 448 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 20 _cell_measurement_theta_min 3 _cell_volume 2164.12(18) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection KappaCCD _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_unetI/netI 0.1172 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16045 _diffrn_reflns_theta_full 25 _diffrn_reflns_theta_max 25.35 _diffrn_reflns_theta_min 2.2 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 2.338 _exptl_absorpt_correction_T_max 0.6521 _exptl_absorpt_correction_T_min 0.3877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details HKL2008 _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1028 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.677 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.087 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 586 _refine_ls_number_reflns 7824 _refine_ls_number_restraints 57 _refine_ls_restrained_S_all 0.986 _refine_ls_R_factor_all 0.1419 _refine_ls_R_factor_gt 0.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0674P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1207 _refine_ls_wR_factor_ref 0.1535 _reflns_number_gt 3968 _reflns_number_total 7824 _reflns_threshold_expression >2\s(I) _iucr_refine_instructions_details ; TITL SA_7 in P -1 dark red prism by R Dinda, Str. Kaminsky CELL 0.71070 11.0675 12.2101 16.9540 93.516 107.485 95.750 ZERR 2.00 0.0005 0.0006 0.0008 0.002 0.003 0.002 LATT 1 SFAC C H N O BR V UNIT 84 78 10 18 4 4 MERG 2 OMIT -3.00 180.00 OMIT -12 8 5 OMIT 9 -8 11 OMIT -11 -5 3 OMIT -10 -7 2 OMIT 7 10 1 OMIT -9 -8 1 OMIT -10 11 3 OMIT 4 -13 7 OMIT 9 -13 2 OMIT 11 -6 4 OMIT 5 11 3 OMIT -12 -2 4 OMIT 8 -2 10 OMIT 4 13 2 OMIT -4 -5 2 OMIT -11 5 10 OMIT -1 11 14 OMIT 13 -1 3 OMIT -3 14 8 OMIT -7 -2 3 OMIT 1 7 0 OMIT -12 5 0 OMIT 5 2 13 OMIT 8 9 0 OMIT 4 -13 6 OMIT 9 4 6 OMIT -5 -4 1 OMIT 12 4 1 OMIT 9 -2 12 OMIT -3 -9 17 OMIT -5 2 21 OMIT -11 -7 13 OMIT 10 7 5 OMIT -11 4 3 OMIT 6 -13 1 OMIT 5 -13 6 OMIT -8 -6 16 OMIT -8 -12 2 OMIT -5 -3 2 OMIT 9 4 9 OMIT -10 -8 7 OMIT 3 4 16 OMIT -14 -2 2 OMIT -5 4 18 OMIT 9 -9 6 OMIT 0 -9 1 OMIT 5 -14 4 OMIT -7 11 8 OMIT -4 -2 22 OMIT 4 14 2 OMIT 3 -12 10 OMIT -6 4 19 OMIT 5 -13 7 OMIT 1 -13 10 OMIT -12 4 12 OMIT -1 -5 17 OMIT -2 3 18 OMIT -11 -6 1 OMIT 8 -2 12 OMIT -3 -1 21 OMIT -5 14 3 OMIT -9 4 15 OMIT -7 8 13 OMIT -4 4 19 OMIT -8 3 19 OMIT -8 -11 9 OMIT -3 8 17 OMIT -10 -9 5 OMIT 7 -10 7 OMIT -8 12 4 OMIT 1 6 15 OMIT -11 4 15 OMIT 4 -14 5 OMIT 7 -13 4 OMIT -6 -2 1 OMIT 4 4 10 OMIT 0 -1 2 OMIT -4 13 0 OMIT -9 -7 5 OMIT -4 -6 2 OMIT -2 -7 1 OMIT -6 6 18 OMIT 6 9 6 OMIT 7 -11 5 OMIT 5 -13 1 OMIT -5 -4 3 OMIT -7 12 2 OMIT -7 -5 3 OMIT 5 -13 3 OMIT 2 -8 13 OMIT -5 4 20 OMIT -8 -6 15 OMIT -1 -9 3 OMIT -7 -11 2 OMIT 6 -14 3 OMIT 4 -13 5 OMIT 4 -12 8 OMIT -2 10 1 OMIT -6 3 20 OMIT 9 7 3 EADP N5 N5B EADP C38 C38B EADP C39 C39B EADP C40 C40B EADP C35 C35B EADP C36 C36B EADP C37 C37B EADP O6 O6B DELU 0.005 O9 C41 C42 C41B C42B N5 C35 > C40 ISOR 0.015 C42 C42B REM SADI 0.005 N5 C35 N5 C37 N5 C39 SHEL 10 0.83 FMAP 2 PLAN 20 SIZE 0.20 0.30 0.50 ACTA 50.00 BOND $H WPDB -2 L.S. 12 TEMP 22.00 WGHT 0.067400 FVAR 0.48089 0.63760 0.79057 0.79092 C1 1 0.427402 0.312026 0.545286 11.00000 0.04393 0.03677 = 0.02660 0.00518 0.01205 0.00044 C2 1 0.368078 0.381052 0.486247 11.00000 0.04809 0.05070 = 0.04281 0.01358 0.01952 0.02023 AFIX 43 H2 2 0.302491 0.418064 0.494062 11.00000 -1.20000 AFIX 0 C3 1 0.406094 0.394753 0.416340 11.00000 0.04866 0.05775 = 0.04252 0.01858 0.01719 0.02029 AFIX 43 H3 2 0.365985 0.440188 0.377083 11.00000 -1.20000 AFIX 0 C4 1 0.503769 0.340396 0.405726 11.00000 0.04867 0.06190 = 0.02924 0.01202 0.01456 0.01155 C5 1 0.556773 0.266456 0.461013 11.00000 0.04814 0.06473 = 0.03583 0.00586 0.01381 0.02037 AFIX 43 H5 2 0.616989 0.224900 0.450205 11.00000 -1.20000 AFIX 0 C6 1 0.522508 0.253381 0.530850 11.00000 0.03958 0.04471 = 0.02895 0.00615 0.00641 0.01203 C7 1 0.591620 0.173926 0.588044 11.00000 0.04679 0.04792 = 0.04038 0.01375 0.01540 0.01638 C8 1 0.310936 0.356674 0.763276 11.00000 0.04162 0.04057 = 0.04550 0.00723 0.01899 0.00753 C9 1 0.251005 0.381309 0.824027 11.00000 0.05097 0.06684 = 0.03999 0.00637 0.02403 0.01072 AFIX 43 H9 2 0.299120 0.389345 0.879876 11.00000 -1.20000 AFIX 0 C10 1 0.126004 0.393393 0.802911 11.00000 0.05839 0.05635 = 0.06602 0.00573 0.04260 0.00590 AFIX 43 H10 2 0.089947 0.407566 0.844881 11.00000 -1.20000 AFIX 0 C11 1 0.046766 0.385253 0.718466 11.00000 0.04482 0.03549 = 0.05925 0.00456 0.02882 0.00218 C12 1 -0.082186 0.401856 0.695797 11.00000 0.05548 0.05738 = 0.07452 0.01341 0.04186 0.01498 AFIX 43 H12 2 -0.118967 0.417526 0.737164 11.00000 -1.20000 AFIX 0 C13 1 -0.154694 0.395642 0.615031 11.00000 0.03920 0.06266 = 0.07867 0.01533 0.02749 0.01528 AFIX 43 H13 2 -0.240101 0.407030 0.601169 11.00000 -1.20000 AFIX 0 C14 1 -0.100100 0.372205 0.553694 11.00000 0.04421 0.08334 = 0.05980 0.00791 0.01234 0.00795 AFIX 43 H14 2 -0.149909 0.367433 0.498305 11.00000 -1.20000 AFIX 0 C15 1 0.026275 0.355713 0.572476 11.00000 0.04474 0.07342 = 0.05206 0.00450 0.02151 0.01335 AFIX 43 H15 2 0.061159 0.341292 0.529960 11.00000 -1.20000 AFIX 0 C16 1 0.102361 0.360609 0.655429 11.00000 0.04595 0.03235 = 0.05476 0.01234 0.01948 0.01065 C17 1 0.237161 0.345354 0.678720 11.00000 0.03742 0.04117 = 0.04065 0.00415 0.01720 0.00013 C18 1 0.312960 -0.016758 0.841189 11.00000 0.04026 0.03076 = 0.03506 0.00617 0.00962 0.00364 C19 1 0.264447 -0.103107 0.877273 11.00000 0.06187 0.04674 = 0.03960 0.00628 0.01204 0.00480 AFIX 43 H19 2 0.275112 -0.096055 0.933968 11.00000 -1.20000 AFIX 0 C20 1 0.200782 -0.198872 0.829559 11.00000 0.06555 0.04268 = 0.05950 0.01470 0.02558 0.00008 AFIX 43 H20 2 0.169670 -0.257088 0.853817 11.00000 -1.20000 AFIX 0 C21 1 0.183613 -0.207446 0.744811 11.00000 0.05320 0.04379 = 0.05977 0.00394 0.02188 0.00838 C22 1 0.233949 -0.124308 0.708985 11.00000 0.05319 0.04177 = 0.03483 0.00325 0.01476 0.00848 AFIX 43 H22 2 0.222184 -0.131850 0.652161 11.00000 -1.20000 AFIX 0 C23 1 0.302218 -0.029111 0.756671 11.00000 0.04391 0.03696 = 0.03874 0.00869 0.01202 0.00451 C24 1 0.351125 0.059950 0.713986 11.00000 0.05538 0.04856 = 0.03754 0.00483 0.01276 0.00743 C25 1 0.473656 0.269785 1.009860 11.00000 0.05459 0.04881 = 0.03282 0.00948 0.00814 0.00167 C26 1 0.503609 0.366732 1.067281 11.00000 0.07553 0.04791 = 0.04259 -0.00196 0.01636 -0.00663 AFIX 43 H26 2 0.578741 0.413405 1.074797 11.00000 -1.20000 AFIX 0 C27 1 0.424351 0.391162 1.110528 11.00000 0.07580 0.05396 = 0.04578 -0.00488 0.01101 0.00725 AFIX 43 H27 2 0.445133 0.456167 1.145914 11.00000 -1.20000 AFIX 0 C28 1 0.310023 0.321796 1.104464 11.00000 0.06543 0.06120 = 0.03101 0.00001 0.00995 0.01405 C29 1 0.232714 0.348069 1.152216 11.00000 0.08556 0.07069 = 0.05321 0.00408 0.02700 0.02627 AFIX 43 H29 2 0.255748 0.411989 1.188820 11.00000 -1.20000 AFIX 0 C30 1 0.123298 0.280965 1.145916 11.00000 0.07726 0.09269 = 0.06500 0.00358 0.03506 0.02994 AFIX 43 H30 2 0.072674 0.298588 1.178663 11.00000 -1.20000 AFIX 0 C31 1 0.087564 0.185778 1.090170 11.00000 0.06920 0.07769 = 0.06664 0.00139 0.03029 0.00701 AFIX 43 H31 2 0.012713 0.140237 1.085541 11.00000 -1.20000 AFIX 0 C32 1 0.161732 0.159497 1.042709 11.00000 0.07086 0.05628 = 0.04761 0.00330 0.02383 0.00725 AFIX 43 H32 2 0.136997 0.095822 1.005848 11.00000 -1.20000 AFIX 0 C33 1 0.275132 0.226747 1.048284 11.00000 0.06042 0.05023 = 0.03308 0.01092 0.01320 0.01242 C34 1 0.357801 0.201895 0.999251 11.00000 0.05161 0.04807 = 0.02709 0.00684 0.00185 0.00947 PART 1 N5 3 0.799839 0.006002 0.677720 31.00000 0.06787 0.05859 = 0.06505 0.01208 0.00766 0.02498 AFIX 13 H5A 2 0.733754 0.026138 0.636838 31.00000 -1.20000 AFIX 0 C35 1 0.901844 0.104607 0.700211 31.00000 0.08358 0.06860 = 0.10637 0.03332 0.00352 0.01494 AFIX 23 H35A 2 0.925933 0.120570 0.651237 31.00000 -1.20000 H35B 2 0.866506 0.168383 0.716982 31.00000 -1.20000 AFIX 0 C36 1 1.016985 0.088569 0.767366 31.00000 0.07906 0.06548 = 0.17808 0.02679 -0.02061 0.01386 AFIX 33 H36A 2 1.076701 0.154679 0.779594 31.00000 -1.50000 H36B 2 1.055278 0.028012 0.750194 31.00000 -1.50000 H36C 2 0.994117 0.072549 0.816133 31.00000 -1.50000 AFIX 0 SAME C35 C36 C37 1 0.748013 -0.014356 0.749624 31.00000 0.10726 0.05994 = 0.06396 0.01442 0.02058 0.02835 AFIX 23 H37A 2 0.811688 -0.044942 0.792401 31.00000 -1.20000 H37B 2 0.734098 0.055917 0.773184 31.00000 -1.20000 AFIX 0 C38 1 0.629078 -0.089082 0.726394 31.00000 0.14187 0.07484 = 0.11286 -0.00314 0.06479 -0.00386 AFIX 33 H38A 2 0.602025 -0.098612 0.774560 31.00000 -1.50000 H38B 2 0.642268 -0.159437 0.704020 31.00000 -1.50000 H38C 2 0.564597 -0.058419 0.685302 31.00000 -1.50000 AFIX 0 SAME C35 C36 C39 1 0.832749 -0.096949 0.642504 31.00000 0.11018 0.08197 = 0.08877 0.00325 0.02411 0.04665 AFIX 23 H39A 2 0.761419 -0.154520 0.632773 31.00000 -1.20000 H39B 2 0.905348 -0.120184 0.683341 31.00000 -1.20000 AFIX 0 C40 1 0.864219 -0.086931 0.563007 31.00000 0.15181 0.11592 = 0.08511 -0.00200 0.03908 0.04499 AFIX 33 H40A 2 0.883608 -0.156871 0.544185 31.00000 -1.50000 H40B 2 0.936778 -0.032083 0.572272 31.00000 -1.50000 H40C 2 0.792426 -0.065423 0.521647 31.00000 -1.50000 AFIX 0 PART 2 SAME N5 C35 > C40 N5B 3 0.817962 -0.002900 0.657528 -31.00000 0.06787 0.05859 = 0.06505 0.01208 0.00766 0.02498 AFIX 13 H5B 2 0.751765 0.027858 0.624311 -31.00000 -1.20000 AFIX 0 C35B 1 0.895898 0.085615 0.725809 -31.00000 0.08358 0.06860 = 0.10637 0.03332 0.00352 0.01494 AFIX 23 H35C 2 0.925164 0.148214 0.700835 -31.00000 -1.20000 H35D 2 0.841950 0.111041 0.757071 -31.00000 -1.20000 AFIX 0 C36B 1 1.006991 0.044427 0.782889 -31.00000 0.07906 0.06548 = 0.17808 0.02679 -0.02061 0.01386 AFIX 33 H36D 2 1.045191 0.098046 0.829944 -31.00000 -1.50000 H36E 2 1.068335 0.032223 0.754546 -31.00000 -1.50000 H36F 2 0.979848 -0.023832 0.801379 -31.00000 -1.50000 AFIX 0 C37B 1 0.761862 -0.100342 0.692665 -31.00000 0.10726 0.05994 = 0.06396 0.01442 0.02058 0.02835 AFIX 23 H37C 2 0.736253 -0.163093 0.650757 -31.00000 -1.20000 H37D 2 0.827568 -0.120595 0.739862 -31.00000 -1.20000 AFIX 0 C38B 1 0.651445 -0.077632 0.719099 -31.00000 0.14187 0.07484 = 0.11286 -0.00314 0.06479 -0.00386 AFIX 33 H38D 2 0.622103 -0.141288 0.741948 -31.00000 -1.50000 H38E 2 0.584163 -0.061270 0.672126 -31.00000 -1.50000 H38F 2 0.675825 -0.015478 0.760518 -31.00000 -1.50000 AFIX 0 C39B 1 0.892249 -0.044789 0.604366 -31.00000 0.11018 0.08197 = 0.08877 0.00325 0.02411 0.04665 AFIX 23 H39C 2 0.967497 -0.071031 0.640375 -31.00000 -1.20000 H39D 2 0.840694 -0.108259 0.568507 -31.00000 -1.20000 AFIX 0 C40B 1 0.933750 0.031355 0.552360 -31.00000 0.15181 0.11592 = 0.08511 -0.00200 0.03908 0.04499 AFIX 33 H40D 2 1.011146 0.011545 0.544077 -31.00000 -1.50000 H40E 2 0.948829 0.105286 0.579033 -31.00000 -1.50000 H40F 2 0.868697 0.027546 0.499611 -31.00000 -1.50000 AFIX 0 PART 1 C41 1 0.752242 0.334128 0.891295 21.00000 0.05709 0.08125 = 0.04391 0.00473 0.00887 -0.01166 AFIX 23 H41A 2 0.721316 0.371107 0.932344 21.00000 -1.20000 H41B 2 0.777139 0.389383 0.858508 21.00000 -1.20000 AFIX 0 C42 1 0.864023 0.278545 0.933586 21.00000 0.07369 0.13530 = 0.14542 0.01844 -0.03163 0.00435 AFIX 33 H42A 2 0.929812 0.332261 0.969636 21.00000 -1.50000 H42B 2 0.895742 0.243752 0.892799 21.00000 -1.50000 H42C 2 0.838863 0.223648 0.965694 21.00000 -1.50000 AFIX 0 PART 2 SAME C41 C42 O9 C41B 1 0.787097 0.279467 0.879621 -21.00000 0.04889 0.08434 = 0.03968 0.02176 -0.01561 0.01314 AFIX 23 H41C 2 0.829748 0.299159 0.839243 -21.00000 -1.20000 H41D 2 0.820506 0.214489 0.903721 -21.00000 -1.20000 AFIX 0 C42B 1 0.816092 0.371829 0.945940 -21.00000 0.10119 0.09031 = 0.09707 -0.01472 0.00664 -0.02908 AFIX 33 H42D 2 0.906916 0.388462 0.970306 -21.00000 -1.50000 H42E 2 0.778543 0.350959 0.987873 -21.00000 -1.50000 H42F 2 0.781608 0.435926 0.922621 -21.00000 -1.50000 AFIX 0 PART 0 O9 4 0.652108 0.253213 0.837972 11.00000 0.04009 0.05493 = 0.04007 0.01348 0.00891 0.00214 N1 3 0.395860 0.309577 0.621220 11.00000 0.04126 0.03632 = 0.04141 0.00926 0.02050 0.00652 N2 3 0.280751 0.328249 0.612752 11.00000 0.03793 0.04144 = 0.04444 0.00868 0.02254 0.00953 N3 3 0.373256 0.083915 0.891728 11.00000 0.05781 0.04935 = 0.02818 0.00679 0.01682 0.00712 N4 3 0.313560 0.109925 0.943835 11.00000 0.05436 0.04623 = 0.03136 0.00901 0.01211 0.00781 O1 4 0.608303 0.189166 0.665874 11.00000 0.05417 0.05469 = 0.04250 0.01591 0.01946 0.02542 O2 4 0.635482 0.099740 0.557122 11.00000 0.09173 0.07620 = 0.04947 0.00721 0.02292 0.05412 O3 4 0.432455 0.347822 0.789881 11.00000 0.03948 0.05896 = 0.03823 0.00426 0.01336 0.00615 O4 4 0.631547 0.409591 0.724084 11.00000 0.04114 0.04569 = 0.05354 0.01166 0.01704 0.00155 O5 4 0.449903 0.131377 0.758861 11.00000 0.05037 0.04711 = 0.03822 0.01110 0.01214 -0.00261 PART 2 O6B 4 0.268396 0.071326 0.643964 -41.00000 0.07386 0.07235 = 0.03027 0.01381 -0.00008 -0.01829 PART 1 O6 4 0.312087 0.063400 0.638945 41.00000 0.07386 0.07235 = 0.03027 0.01381 -0.00008 -0.01829 PART 0 O7 4 0.552899 0.252021 0.969454 11.00000 0.05601 0.06915 = 0.04231 0.00010 0.01691 -0.00297 O8 4 0.627003 0.051122 0.908206 11.00000 0.07051 0.06050 = 0.05092 0.02630 0.02118 0.02390 BR1 5 0.569481 0.367542 0.317422 11.00000 0.08521 0.09138 = 0.05736 0.02937 0.04451 0.02909 BR2 5 0.084952 -0.334623 0.678621 11.00000 0.09311 0.05061 = 0.08210 -0.01333 0.03624 -0.01387 V1 6 0.545965 0.299053 0.728728 11.00000 0.03883 0.04727 = 0.03482 0.01139 0.01323 0.00950 V2 6 0.543418 0.147726 0.877813 11.00000 0.04834 0.05185 = 0.03130 0.01110 0.01055 0.00691 HKLF 4 REM SA_7 in P -1 dark red prism by R Dinda, Str. Kaminsky REM R1 = 0.0590 for 3968 Fo > 4sig(Fo) and 0.1419 for all 7824 data REM 586 parameters refined using 57 restraints END WGHT 0.0677 0.0000 REM Highest difference peak 0.677, deepest hole -0.653, 1-sigma level 0.087 Q1 1 0.1450 -0.3481 0.7273 11.00000 0.05 0.68 Q2 1 0.5578 0.3427 0.8100 11.00000 0.05 0.47 Q3 1 0.5076 0.2835 0.2948 11.00000 0.05 0.47 Q4 1 0.0999 -0.3062 0.7641 11.00000 0.05 0.41 Q5 1 0.6984 0.3637 0.3200 11.00000 0.05 0.39 Q6 1 0.6427 0.2402 0.8633 11.00000 0.05 0.39 Q7 1 0.5257 0.1135 0.7870 11.00000 0.05 0.37 Q8 1 0.4005 0.3352 0.7076 11.00000 0.05 0.35 Q9 1 0.9043 0.2463 0.7340 11.00000 0.05 0.35 Q10 1 0.9680 0.1516 0.4828 11.00000 0.05 0.35 Q11 1 -0.0607 0.3965 1.1213 11.00000 0.05 0.35 Q12 1 0.1627 -0.2360 0.6659 11.00000 0.05 0.34 Q13 1 0.3834 0.3399 0.7759 11.00000 0.05 0.33 Q14 1 0.8641 -0.1348 0.5290 11.00000 0.05 0.33 Q15 1 0.9368 0.4049 0.9187 11.00000 0.05 0.33 Q16 1 0.0234 -0.3429 0.5847 11.00000 0.05 0.32 Q17 1 0.0891 -0.3024 0.6760 11.00000 0.05 0.32 Q18 1 0.3870 0.3181 0.5659 11.00000 0.05 0.32 Q19 1 0.6266 0.2810 0.7901 11.00000 0.05 0.32 Q20 1 0.2160 -0.3387 0.7060 11.00000 0.05 0.32 ; _cod_data_source_file SA-4.cif _cod_data_source_block shelxs97 _cod_depositor_comments 'removed _chemical_name_systematic and _chemical_name_common' _cod_database_code 4350836 loop_ _symmetry_equiv_pos_as_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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4274(5) 0.3120(4) 0.5453(3) 0.0357(14) Uani 1 1 d . B . C2 C 0.3681(6) 0.3811(5) 0.4862(3) 0.0446(15) Uani 1 1 d . . . H2 H 0.3025 0.4181 0.4941 0.053 Uiso 1 1 calc R . . C3 C 0.4061(6) 0.3948(5) 0.4163(3) 0.0474(16) Uani 1 1 d . . . H3 H 0.366 0.4402 0.3771 0.057 Uiso 1 1 calc R . . C4 C 0.5038(6) 0.3404(5) 0.4057(3) 0.0454(16) Uani 1 1 d . . . C5 C 0.5568(6) 0.2665(5) 0.4610(3) 0.0484(16) Uani 1 1 d . . . H5 H 0.617 0.2249 0.4502 0.058 Uiso 1 1 calc R . . C6 C 0.5225(5) 0.2534(5) 0.5308(3) 0.0381(14) Uani 1 1 d . . . C7 C 0.5916(6) 0.1739(5) 0.5880(3) 0.0434(15) Uani 1 1 d . B . C8 C 0.3109(6) 0.3567(5) 0.7633(3) 0.0410(14) Uani 1 1 d . B . C9 C 0.2510(6) 0.3813(5) 0.8240(3) 0.0501(17) Uani 1 1 d . . . H9 H 0.2991 0.3893 0.8799 0.06 Uiso 1 1 calc R . . C10 C 0.1260(6) 0.3934(5) 0.8029(4) 0.0551(17) Uani 1 1 d . . . H10 H 0.0899 0.4076 0.8449 0.066 Uiso 1 1 calc R . . C11 C 0.0468(6) 0.3853(5) 0.7185(4) 0.0439(15) Uani 1 1 d . . . C12 C -0.0822(6) 0.4019(5) 0.6958(4) 0.0567(18) Uani 1 1 d . . . H12 H -0.119 0.4175 0.7372 0.068 Uiso 1 1 calc R . . C13 C -0.1547(6) 0.3956(6) 0.6150(4) 0.0571(18) Uani 1 1 d . . . H13 H -0.2401 0.407 0.6012 0.069 Uiso 1 1 calc R . . C14 C -0.1001(6) 0.3722(6) 0.5537(4) 0.063(2) Uani 1 1 d . . . H14 H -0.1499 0.3674 0.4983 0.076 Uiso 1 1 calc R . . C15 C 0.0263(6) 0.3557(6) 0.5725(4) 0.0549(18) Uani 1 1 d . . . H15 H 0.0612 0.3413 0.53 0.066 Uiso 1 1 calc R . . C16 C 0.1024(6) 0.3606(5) 0.6554(3) 0.0427(15) Uani 1 1 d . . . C17 C 0.2372(5) 0.3454(5) 0.6787(3) 0.0389(14) Uani 1 1 d . . . C18 C 0.3130(5) -0.0168(4) 0.8412(3) 0.0357(14) Uani 1 1 d . B . C19 C 0.2644(6) -0.1031(5) 0.8773(3) 0.0503(17) Uani 1 1 d . . . H19 H 0.2751 -0.0961 0.934 0.06 Uiso 1 1 calc R . . C20 C 0.2008(6) -0.1989(5) 0.8296(4) 0.0546(17) Uani 1 1 d . . . H20 H 0.1697 -0.2571 0.8538 0.065 Uiso 1 1 calc R . . C21 C 0.1836(6) -0.2074(5) 0.7448(4) 0.0511(16) Uani 1 1 d . . . C22 C 0.2339(6) -0.1243(5) 0.7090(3) 0.0428(15) Uani 1 1 d . . . H22 H 0.2222 -0.1318 0.6522 0.051 Uiso 1 1 calc R . . C23 C 0.3022(5) -0.0291(5) 0.7567(3) 0.0399(14) Uani 1 1 d . B . C24 C 0.3511(6) 0.0600(5) 0.7140(3) 0.0474(16) Uani 1 1 d . . . C25 C 0.4737(6) 0.2698(5) 1.0099(3) 0.0467(16) Uani 1 1 d . B . C26 C 0.5036(7) 0.3667(5) 1.0673(3) 0.0571(18) Uani 1 1 d . . . H26 H 0.5787 0.4134 1.0748 0.068 Uiso 1 1 calc R . . C27 C 0.4244(7) 0.3912(6) 1.1105(4) 0.0607(19) Uani 1 1 d . . . H27 H 0.4451 0.4562 1.1459 0.073 Uiso 1 1 calc R . . C28 C 0.3100(7) 0.3218(6) 1.1045(3) 0.0534(18) Uani 1 1 d . . . C29 C 0.2327(8) 0.3481(7) 1.1522(4) 0.067(2) Uani 1 1 d . . . H29 H 0.2557 0.412 1.1888 0.081 Uiso 1 1 calc R . . C30 C 0.1233(8) 0.2810(7) 1.1459(4) 0.074(2) Uani 1 1 d . . . H30 H 0.0727 0.2986 1.1787 0.089 Uiso 1 1 calc R . . C31 C 0.0876(7) 0.1858(6) 1.0902(4) 0.069(2) Uani 1 1 d . . . H31 H 0.0127 0.1402 1.0855 0.083 Uiso 1 1 calc R . . C32 C 0.1617(7) 0.1595(6) 1.0427(4) 0.0571(18) Uani 1 1 d . . . H32 H 0.137 0.0958 1.0058 0.069 Uiso 1 1 calc R . . C33 C 0.2751(6) 0.2267(5) 1.0483(3) 0.0475(16) Uani 1 1 d . . . C34 C 0.3578(6) 0.2019(5) 0.9993(3) 0.0442(16) Uani 1 1 d . . . N5 N 0.7998(10) 0.0060(7) 0.6777(6) 0.0652(18) Uani 0.791(8) 1 d PDU A 1 H5A H 0.7338 0.0261 0.6368 0.078 Uiso 0.791(8) 1 calc PR A 1 C35 C 0.9018(12) 0.1046(9) 0.7002(7) 0.090(3) Uani 0.791(8) 1 d PDU A 1 H35A H 0.9259 0.1206 0.6512 0.109 Uiso 0.791(8) 1 calc PR A 1 H35B H 0.8665 0.1684 0.717 0.109 Uiso 0.791(8) 1 calc PR A 1 C36 C 1.0170(14) 0.0886(10) 0.7674(11) 0.120(6) Uani 0.791(8) 1 d PDU A 1 H36A H 1.0767 0.1547 0.7796 0.18 Uiso 0.791(8) 1 calc PR A 1 H36B H 1.0553 0.028 0.7502 0.18 Uiso 0.791(8) 1 calc PR A 1 H36C H 0.9941 0.0725 0.8161 0.18 Uiso 0.791(8) 1 calc PR A 1 C37 C 0.7480(10) -0.0144(8) 0.7496(5) 0.077(2) Uani 0.791(8) 1 d PDU A 1 H37A H 0.8117 -0.0449 0.7924 0.092 Uiso 0.791(8) 1 calc PR A 1 H37B H 0.7341 0.0559 0.7732 0.092 Uiso 0.791(8) 1 calc PR A 1 C38 C 0.6291(17) -0.0891(17) 0.7264(18) 0.106(3) Uani 0.791(8) 1 d PDU A 1 H38A H 0.602 -0.0986 0.7746 0.159 Uiso 0.791(8) 1 calc PR A 1 H38B H 0.6423 -0.1594 0.704 0.159 Uiso 0.791(8) 1 calc PR A 1 H38C H 0.5646 -0.0584 0.6853 0.159 Uiso 0.791(8) 1 calc PR A 1 C39 C 0.8327(12) -0.0969(9) 0.6425(6) 0.093(3) Uani 0.791(8) 1 d PDU A 1 H39A H 0.7614 -0.1545 0.6328 0.111 Uiso 0.791(8) 1 calc PR A 1 H39B H 0.9053 -0.1202 0.6833 0.111 Uiso 0.791(8) 1 calc PR A 1 C40 C 0.8642(14) -0.0869(11) 0.5630(7) 0.116(5) Uani 0.791(8) 1 d PDU A 1 H40A H 0.8836 -0.1569 0.5442 0.173 Uiso 0.791(8) 1 calc PR A 1 H40B H 0.9368 -0.0321 0.5723 0.173 Uiso 0.791(8) 1 calc PR A 1 H40C H 0.7924 -0.0654 0.5216 0.173 Uiso 0.791(8) 1 calc PR A 1 N5B N 0.818(4) -0.003(3) 0.658(2) 0.0652(18) Uani 0.209(8) 1 d PD A 2 H5B H 0.7518 0.0279 0.6243 0.078 Uiso 0.209(8) 1 calc PR A 2 C35B C 0.896(4) 0.086(3) 0.726(3) 0.090(3) Uani 0.209(8) 1 d PD A 2 H35C H 0.9252 0.1482 0.7008 0.109 Uiso 0.209(8) 1 calc PR A 2 H35D H 0.842 0.111 0.7571 0.109 Uiso 0.209(8) 1 calc PR A 2 C36B C 1.007(6) 0.044(4) 0.783(5) 0.120(6) Uani 0.209(8) 1 d PD A 2 H36D H 1.0452 0.098 0.8299 0.18 Uiso 0.209(8) 1 calc PR A 2 H36E H 1.0683 0.0322 0.7545 0.18 Uiso 0.209(8) 1 calc PR A 2 H36F H 0.9798 -0.0238 0.8014 0.18 Uiso 0.209(8) 1 calc PR A 2 C37B C 0.762(3) -0.100(3) 0.693(2) 0.077(2) Uani 0.209(8) 1 d PD A 2 H37C H 0.7363 -0.1631 0.6508 0.092 Uiso 0.209(8) 1 calc PR A 2 H37D H 0.8276 -0.1206 0.7399 0.092 Uiso 0.209(8) 1 calc PR A 2 C38B C 0.651(7) -0.078(7) 0.719(7) 0.106(3) Uani 0.209(8) 1 d PD A 2 H38D H 0.6221 -0.1413 0.7419 0.159 Uiso 0.209(8) 1 calc PR A 2 H38E H 0.5842 -0.0613 0.6721 0.159 Uiso 0.209(8) 1 calc PR A 2 H38F H 0.6758 -0.0155 0.7605 0.159 Uiso 0.209(8) 1 calc PR A 2 C39B C 0.892(4) -0.045(3) 0.604(3) 0.093(3) Uani 0.209(8) 1 d PD A 2 H39C H 0.9675 -0.071 0.6404 0.111 Uiso 0.209(8) 1 calc PR A 2 H39D H 0.8407 -0.1083 0.5685 0.111 Uiso 0.209(8) 1 calc PR A 2 C40B C 0.934(4) 0.031(3) 0.552(2) 0.116(5) Uani 0.209(8) 1 d PD A 2 H40D H 1.0111 0.0115 0.5441 0.173 Uiso 0.209(8) 1 calc PR A 2 H40E H 0.9488 0.1053 0.579 0.173 Uiso 0.209(8) 1 calc PR A 2 H40F H 0.8687 0.0275 0.4996 0.173 Uiso 0.209(8) 1 calc PR A 2 C41 C 0.7522(10) 0.3341(11) 0.8913(7) 0.064(4) Uani 0.638(13) 1 d PDU B 1 H41A H 0.7213 0.3711 0.9323 0.077 Uiso 0.638(13) 1 calc PR B 1 H41B H 0.7771 0.3894 0.8585 0.077 Uiso 0.638(13) 1 calc PR B 1 C42 C 0.8640(13) 0.2785(15) 0.9336(11) 0.133(7) Uani 0.638(13) 1 d PDU B 1 H42A H 0.9298 0.3323 0.9696 0.2 Uiso 0.638(13) 1 calc PR B 1 H42B H 0.8957 0.2438 0.8928 0.2 Uiso 0.638(13) 1 calc PR B 1 H42C H 0.8389 0.2236 0.9657 0.2 Uiso 0.638(13) 1 calc PR B 1 C41B C 0.7871(15) 0.2795(18) 0.8796(12) 0.063(6) Uani 0.362(13) 1 d PDU B 2 H41C H 0.8297 0.2992 0.8392 0.076 Uiso 0.362(13) 1 calc PR B 2 H41D H 0.8205 0.2145 0.9037 0.076 Uiso 0.362(13) 1 calc PR B 2 C42B C 0.816(2) 0.372(2) 0.9459(15) 0.105(9) Uani 0.362(13) 1 d PDU B 2 H42D H 0.9069 0.3885 0.9703 0.158 Uiso 0.362(13) 1 calc PR B 2 H42E H 0.7785 0.351 0.9879 0.158 Uiso 0.362(13) 1 calc PR B 2 H42F H 0.7816 0.4359 0.9226 0.158 Uiso 0.362(13) 1 calc PR B 2 O9 O 0.6521(4) 0.2532(3) 0.8380(2) 0.0457(10) Uani 1 1 d DU . . N1 N 0.3959(4) 0.3096(4) 0.6212(3) 0.0376(11) Uani 1 1 d . . . N2 N 0.2808(4) 0.3282(4) 0.6128(3) 0.0386(11) Uani 1 1 d . B . N3 N 0.3733(5) 0.0839(4) 0.8917(2) 0.0442(13) Uani 1 1 d . . . N4 N 0.3136(5) 0.1099(4) 0.9438(3) 0.0439(12) Uani 1 1 d . B . O1 O 0.6083(4) 0.1892(3) 0.6659(2) 0.0476(11) Uani 1 1 d . . . O2 O 0.6355(5) 0.0997(4) 0.5571(2) 0.0691(15) Uani 1 1 d . . . O3 O 0.4325(4) 0.3478(3) 0.7899(2) 0.0453(10) Uani 1 1 d . . . O4 O 0.6315(4) 0.4096(3) 0.7241(2) 0.0462(10) Uani 1 1 d . . . O5 O 0.4499(4) 0.1314(3) 0.7589(2) 0.0459(10) Uani 1 1 d . B . O6B O 0.268(10) 0.071(6) 0.644(4) 0.064(7) Uani 0.21(12) 1 d P C 2 O6 O 0.312(5) 0.0634(15) 0.6389(9) 0.064(7) Uani 0.79(12) 1 d P C 1 O7 O 0.5529(4) 0.2520(4) 0.9695(2) 0.0564(12) Uani 1 1 d . . . O8 O 0.6270(4) 0.0511(4) 0.9082(2) 0.0581(12) Uani 1 1 d . . . Br1 Br 0.56948(8) 0.36754(7) 0.31742(4) 0.0707(3) Uani 1 1 d . . . Br2 Br 0.08495(8) -0.33462(6) 0.67862(5) 0.0757(3) Uani 1 1 d . . . V1 V 0.54596(9) 0.29905(8) 0.72873(5) 0.0393(3) Uani 1 1 d . B . V2 V 0.54342(10) 0.14773(9) 0.87781(5) 0.0439(3) Uani 1 1 d . B . 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 0.044(4) 0.037(3) 0.027(3) 0.005(2) 0.012(3) 0.000(3) C2 0.048(4) 0.051(4) 0.043(3) 0.014(3) 0.020(3) 0.020(3) C3 0.049(4) 0.058(4) 0.043(3) 0.019(3) 0.017(3) 0.020(3) C4 0.049(4) 0.062(4) 0.029(3) 0.012(3) 0.015(3) 0.012(3) C5 0.048(4) 0.065(5) 0.036(3) 0.006(3) 0.014(3) 0.020(3) C6 0.040(3) 0.045(4) 0.029(3) 0.006(2) 0.006(3) 0.012(3) C7 0.047(4) 0.048(4) 0.040(3) 0.014(3) 0.015(3) 0.016(3) C8 0.042(4) 0.041(4) 0.045(3) 0.007(3) 0.019(3) 0.008(3) C9 0.051(4) 0.067(5) 0.040(3) 0.006(3) 0.024(3) 0.011(3) C10 0.058(5) 0.056(5) 0.066(4) 0.006(3) 0.043(4) 0.006(4) C11 0.045(4) 0.035(4) 0.059(4) 0.005(3) 0.029(3) 0.002(3) C12 0.055(4) 0.057(5) 0.075(5) 0.013(3) 0.042(4) 0.015(4) C13 0.039(4) 0.063(5) 0.079(5) 0.015(4) 0.027(4) 0.015(3) C14 0.044(4) 0.083(6) 0.060(4) 0.008(4) 0.012(3) 0.008(4) C15 0.045(4) 0.073(5) 0.052(4) 0.004(3) 0.022(3) 0.013(4) C16 0.046(4) 0.032(4) 0.055(4) 0.012(3) 0.019(3) 0.011(3) C17 0.037(3) 0.041(4) 0.041(3) 0.004(2) 0.017(3) 0.000(3) C18 0.040(3) 0.031(3) 0.035(3) 0.006(2) 0.010(3) 0.004(3) C19 0.062(4) 0.047(4) 0.040(3) 0.006(3) 0.012(3) 0.005(3) C20 0.066(5) 0.043(4) 0.060(4) 0.015(3) 0.026(3) 0.000(3) C21 0.053(4) 0.044(4) 0.060(4) 0.004(3) 0.022(3) 0.008(3) C22 0.053(4) 0.042(4) 0.035(3) 0.003(3) 0.015(3) 0.008(3) C23 0.044(4) 0.037(4) 0.039(3) 0.009(3) 0.012(3) 0.005(3) C24 0.055(4) 0.049(4) 0.038(4) 0.005(3) 0.013(3) 0.007(3) C25 0.055(4) 0.049(4) 0.033(3) 0.009(3) 0.008(3) 0.002(3) C26 0.076(5) 0.048(4) 0.043(3) -0.002(3) 0.016(3) -0.007(4) C27 0.076(5) 0.054(5) 0.046(4) -0.005(3) 0.011(4) 0.007(4) C28 0.065(5) 0.061(5) 0.031(3) 0.000(3) 0.010(3) 0.014(4) C29 0.086(6) 0.071(6) 0.053(4) 0.004(3) 0.027(4) 0.026(5) C30 0.077(6) 0.093(7) 0.065(5) 0.004(4) 0.035(4) 0.030(5) C31 0.069(5) 0.078(6) 0.067(4) 0.001(4) 0.030(4) 0.007(4) C32 0.071(5) 0.056(5) 0.048(4) 0.003(3) 0.024(4) 0.007(4) C33 0.060(4) 0.050(4) 0.033(3) 0.011(3) 0.013(3) 0.012(4) C34 0.052(4) 0.048(4) 0.027(3) 0.007(3) 0.002(3) 0.009(3) N5 0.068(5) 0.059(4) 0.065(5) 0.012(3) 0.008(3) 0.025(3) C35 0.084(6) 0.069(5) 0.106(9) 0.033(5) 0.004(5) 0.015(4) C36 0.079(6) 0.065(11) 0.178(12) 0.027(10) -0.021(7) 0.014(8) C37 0.107(7) 0.060(6) 0.064(5) 0.014(4) 0.021(4) 0.028(5) C38 0.142(10) 0.075(8) 0.113(8) -0.003(6) 0.065(7) -0.004(6) C39 0.110(10) 0.082(6) 0.089(7) 0.003(5) 0.024(6) 0.047(6) C40 0.152(12) 0.116(10) 0.085(7) -0.002(7) 0.039(7) 0.045(9) N5B 0.068(5) 0.059(4) 0.065(5) 0.012(3) 0.008(3) 0.025(3) C35B 0.084(6) 0.069(5) 0.106(9) 0.033(5) 0.004(5) 0.015(4) C36B 0.079(6) 0.065(11) 0.178(12) 0.027(10) -0.021(7) 0.014(8) C37B 0.107(7) 0.060(6) 0.064(5) 0.014(4) 0.021(4) 0.028(5) C38B 0.142(10) 0.075(8) 0.113(8) -0.003(6) 0.065(7) -0.004(6) C39B 0.110(10) 0.082(6) 0.089(7) 0.003(5) 0.024(6) 0.047(6) C40B 0.152(12) 0.116(10) 0.085(7) -0.002(7) 0.039(7) 0.045(9) C41 0.057(8) 0.081(11) 0.044(7) 0.005(6) 0.009(5) -0.012(5) C42 0.074(7) 0.135(12) 0.145(11) 0.018(9) -0.032(7) 0.004(8) C41B 0.049(7) 0.084(17) 0.040(11) 0.022(8) -0.016(10) 0.013(12) C42B 0.101(13) 0.090(13) 0.097(12) -0.015(10) 0.007(9) -0.029(10) O9 0.040(2) 0.055(3) 0.040(2) 0.0135(17) 0.0089(17) 0.0021(19) N1 0.041(3) 0.036(3) 0.041(2) 0.009(2) 0.020(2) 0.007(2) N2 0.038(3) 0.041(3) 0.044(3) 0.009(2) 0.023(2) 0.010(2) N3 0.058(3) 0.049(3) 0.028(2) 0.007(2) 0.017(2) 0.007(3) N4 0.054(3) 0.046(3) 0.031(2) 0.009(2) 0.012(2) 0.008(3) O1 0.054(3) 0.055(3) 0.043(2) 0.0159(18) 0.019(2) 0.025(2) O2 0.092(4) 0.076(3) 0.049(2) 0.007(2) 0.023(2) 0.054(3) O3 0.039(2) 0.059(3) 0.038(2) 0.0043(18) 0.0134(19) 0.006(2) O4 0.041(2) 0.046(3) 0.054(2) 0.0117(18) 0.0170(19) 0.002(2) O5 0.050(3) 0.047(3) 0.038(2) 0.0111(18) 0.012(2) -0.003(2) O6B 0.074(16) 0.072(4) 0.030(3) 0.014(3) 0.000(6) -0.018(7) O6 0.074(16) 0.072(4) 0.030(3) 0.014(3) 0.000(6) -0.018(7) O7 0.056(3) 0.069(3) 0.042(2) 0.000(2) 0.017(2) -0.003(2) O8 0.071(3) 0.061(3) 0.051(2) 0.026(2) 0.021(2) 0.024(2) Br1 0.0852(6) 0.0914(6) 0.0574(4) 0.0294(4) 0.0445(4) 0.0291(5) Br2 0.0931(6) 0.0506(5) 0.0821(5) -0.0133(4) 0.0362(4) -0.0139(4) V1 0.0388(6) 0.0473(7) 0.0348(5) 0.0114(4) 0.0132(4) 0.0095(5) V2 0.0483(7) 0.0518(7) 0.0313(5) 0.0111(4) 0.0106(5) 0.0069(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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 C2 C1 C6 118.9(5) . . C2 C1 N1 119.1(5) . . C6 C1 N1 121.8(4) . . C3 C2 C1 120.7(5) . . C3 C2 H2 119.7 . . C1 C2 H2 119.7 . . C4 C3 C2 119.2(5) . . C4 C3 H3 120.4 . . C2 C3 H3 120.4 . . C3 C4 C5 120.2(5) . . C3 C4 Br1 120.6(4) . . C5 C4 Br1 119.2(4) . . C6 C5 C4 121.3(5) . . C6 C5 H5 119.3 . . C4 C5 H5 119.3 . . C5 C6 C1 119.4(5) . . C5 C6 C7 116.1(5) . . C1 C6 C7 124.4(5) . . O2 C7 O1 122.7(5) . . O2 C7 C6 117.5(5) . . O1 C7 C6 119.7(5) . . O3 C8 C17 124.3(5) . . O3 C8 C9 117.0(5) . . C17 C8 C9 118.7(5) . . C10 C9 C8 121.6(5) . . C10 C9 H9 119.2 . . C8 C9 H9 119.2 . . C9 C10 C11 122.4(6) . . C9 C10 H10 118.8 . . C11 C10 H10 118.8 . . C12 C11 C16 119.1(5) . . C12 C11 C10 122.9(6) . . C16 C11 C10 118.0(5) . . C13 C12 C11 121.6(6) . . C13 C12 H12 119.2 . . C11 C12 H12 119.2 . . C12 C13 C14 119.1(6) . . C12 C13 H13 120.4 . . C14 C13 H13 120.4 . . C15 C14 C13 121.6(6) . . C15 C14 H14 119.2 . . C13 C14 H14 119.2 . . C14 C15 C16 120.1(6) . . C14 C15 H15 119.9 . . C16 C15 H15 119.9 . . C15 C16 C11 118.4(5) . . C15 C16 C17 122.3(5) . . C11 C16 C17 119.3(5) . . N2 C17 C8 126.3(5) . . N2 C17 C16 113.6(5) . . C8 C17 C16 119.9(5) . . C19 C18 C23 119.9(5) . . C19 C18 N3 119.1(5) . . C23 C18 N3 121.0(5) . . C20 C19 C18 120.4(5) . . C20 C19 H19 119.8 . . C18 C19 H19 119.8 . . C19 C20 C21 119.2(6) . . C19 C20 H20 120.4 . . C21 C20 H20 120.4 . . C22 C21 C20 120.9(6) . . C22 C21 Br2 120.3(5) . . C20 C21 Br2 118.8(5) . . C21 C22 C23 120.5(5) . . C21 C22 H22 119.7 . . C23 C22 H22 119.7 . . C22 C23 C18 118.8(5) . . C22 C23 C24 118.2(5) . . C18 C23 C24 122.7(5) . . O6 C24 O6B 24(3) . . O6 C24 O5 119.1(16) . . O6B C24 O5 128(3) . . O6 C24 C23 122.6(13) . . O6B C24 C23 111(4) . . O5 C24 C23 117.9(5) . . O7 C25 C34 124.4(5) . . O7 C25 C26 117.6(6) . . C34 C25 C26 117.9(6) . . C27 C26 C25 120.7(7) . . C27 C26 H26 119.6 . . C25 C26 H26 119.6 . . C26 C27 C28 122.8(6) . . C26 C27 H27 118.6 . . C28 C27 H27 118.6 . . C29 C28 C33 120.1(7) . . C29 C28 C27 121.1(6) . . C33 C28 C27 118.8(6) . . C30 C29 C28 120.6(7) . . C30 C29 H29 119.7 . . C28 C29 H29 119.7 . . C29 C30 C31 119.8(7) . . C29 C30 H30 120.1 . . C31 C30 H30 120.1 . . C32 C31 C30 120.2(8) . . C32 C31 H31 119.9 . . C30 C31 H31 119.9 . . C31 C32 C33 121.2(6) . . C31 C32 H32 119.4 . . C33 C32 H32 119.4 . . C28 C33 C32 118.1(6) . . C28 C33 C34 118.7(6) . . C32 C33 C34 123.2(6) . . N4 C34 C25 124.5(6) . . N4 C34 C33 114.5(6) . . C25 C34 C33 120.9(5) . . C39 N5 C35 116.4(9) . . C39 N5 C37 111.9(8) . . C35 N5 C37 110.9(8) . . C39 N5 H5A 105.6 . . C35 N5 H5A 105.6 . . C37 N5 H5A 105.6 . . C36 C35 N5 113.7(9) . . C36 C35 H35A 108.8 . . N5 C35 H35A 108.8 . . C36 C35 H35B 108.8 . . N5 C35 H35B 108.8 . . H35A C35 H35B 107.7 . . C35 C36 H36A 109.5 . . C35 C36 H36B 109.5 . . H36A C36 H36B 109.5 . . C35 C36 H36C 109.5 . . H36A C36 H36C 109.5 . . H36B C36 H36C 109.5 . . C38 C37 N5 113.8(12) . . C38 C37 H37A 108.8 . . N5 C37 H37A 108.8 . . C38 C37 H37B 108.8 . . N5 C37 H37B 108.8 . . H37A C37 H37B 107.7 . . C37 C38 H38A 109.5 . . C37 C38 H38B 109.5 . . H38A C38 H38B 109.5 . . C37 C38 H38C 109.5 . . H38A C38 H38C 109.5 . . H38B C38 H38C 109.5 . . N5 C39 C40 114.7(10) . . N5 C39 H39A 108.6 . . C40 C39 H39A 108.6 . . N5 C39 H39B 108.6 . . C40 C39 H39B 108.6 . . H39A C39 H39B 107.6 . . C39 C40 H40A 109.5 . . C39 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C39 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C39B N5B C35B 113(2) . . C39B N5B C37B 109(2) . . C35B N5B C37B 112(2) . . C39B N5B H5B 107.7 . . C35B N5B H5B 107.7 . . C37B N5B H5B 107.7 . . C36B C35B N5B 112(3) . . C36B C35B H35C 109.2 . . N5B C35B H35C 109.2 . . C36B C35B H35D 109.2 . . N5B C35B H35D 109.2 . . H35C C35B H35D 107.9 . . C35B C36B H36D 109.5 . . C35B C36B H36E 109.5 . . H36D C36B H36E 109.5 . . C35B C36B H36F 109.5 . . H36D C36B H36F 109.5 . . H36E C36B H36F 109.5 . . C38B C37B N5B 114(3) . . C38B C37B H37C 108.9 . . N5B C37B H37C 108.9 . . C38B C37B H37D 108.9 . . N5B C37B H37D 108.9 . . H37C C37B H37D 107.7 . . C37B C38B H38D 109.5 . . C37B C38B H38E 109.5 . . H38D C38B H38E 109.5 . . C37B C38B H38F 109.5 . . H38D C38B H38F 109.5 . . H38E C38B H38F 109.5 . . C40B C39B N5B 118(2) . . C40B C39B H39C 107.9 . . N5B C39B H39C 107.9 . . C40B C39B H39D 107.9 . . N5B C39B H39D 107.9 . . H39C C39B H39D 107.2 . . C39B C40B H40D 109.5 . . C39B C40B H40E 109.5 . . H40D C40B H40E 109.5 . . C39B C40B H40F 109.5 . . H40D C40B H40F 109.5 . . H40E C40B H40F 109.5 . . O9 C41 C42 109.6(10) . . O9 C41 H41A 109.7 . . C42 C41 H41A 109.7 . . O9 C41 H41B 109.7 . . C42 C41 H41B 109.7 . . H41A C41 H41B 108.2 . . C41 C42 H42A 109.5 . . C41 C42 H42B 109.5 . . H42A C42 H42B 109.5 . . C41 C42 H42C 109.5 . . H42A C42 H42C 109.5 . . H42B C42 H42C 109.5 . . O9 C41B C42B 112.4(16) . . O9 C41B H41C 109.1 . . C42B C41B H41C 109.1 . . O9 C41B H41D 109.1 . . C42B C41B H41D 109.1 . . H41C C41B H41D 107.9 . . C41B C42B H42D 109.5 . . C41B C42B H42E 109.5 . . H42D C42B H42E 109.5 . . C41B C42B H42F 109.5 . . H42D C42B H42F 109.5 . . H42E C42B H42F 109.5 . . C41B O9 C41 34.1(8) . . C41B O9 V2 122.2(10) . . C41 O9 V2 124.4(6) . . C41B O9 V1 129.2(10) . . C41 O9 V1 117.6(6) . . V2 O9 V1 108.30(17) . . N2 N1 C1 112.9(4) . . N2 N1 V1 129.9(3) . . C1 N1 V1 116.5(3) . . N1 N2 C17 122.4(4) . . N4 N3 C18 111.4(5) . . N4 N3 V2 132.6(4) . . C18 N3 V2 115.6(4) . . N3 N4 C34 120.6(5) . . C7 O1 V1 130.0(3) . . C8 O3 V1 129.8(3) . . C24 O5 V2 131.2(4) . . C24 O5 V1 131.9(3) . . V2 O5 V1 96.03(16) . . C25 O7 V2 132.5(4) . . O4 V1 O1 101.8(2) . . O4 V1 O3 104.12(19) . . O1 V1 O3 154.01(18) . . O4 V1 O9 99.86(17) . . O1 V1 O9 91.55(15) . . O3 V1 O9 86.07(15) . . O4 V1 N1 97.16(18) . . O1 V1 N1 88.66(16) . . O3 V1 N1 86.13(16) . . O9 V1 N1 162.56(18) . . O4 V1 O5 169.18(16) . . O1 V1 O5 78.47(16) . . O3 V1 O5 76.48(16) . . O9 V1 O5 69.34(15) . . N1 V1 O5 93.66(16) . . O8 V2 O7 110.90(19) . . O8 V2 O5 114.40(19) . . O7 V2 O5 134.64(17) . . O8 V2 O9 105.3(2) . . O7 V2 O9 90.92(18) . . O5 V2 O9 79.68(16) . . O8 V2 N3 100.3(2) . . O7 V2 N3 84.86(19) . . O5 V2 N3 85.01(17) . . O9 V2 N3 153.84(17) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 C2 1.401(7) . C1 C6 1.402(7) . C1 N1 1.433(6) . C2 C3 1.385(8) . C2 H2 0.93 . C3 C4 1.374(8) . C3 H3 0.93 . C4 C5 1.385(7) . C4 Br1 1.883(6) . C5 C6 1.361(8) . C5 H5 0.93 . C6 C7 1.512(7) . C7 O2 1.230(6) . C7 O1 1.275(6) . C8 O3 1.302(6) . C8 C17 1.411(7) . C8 C9 1.416(8) . C9 C10 1.347(8) . C9 H9 0.93 . C10 C11 1.428(8) . C10 H10 0.93 . C11 C12 1.401(8) . C11 C16 1.416(8) . C12 C13 1.356(8) . C12 H12 0.93 . C13 C14 1.380(9) . C13 H13 0.93 . C14 C15 1.377(8) . C14 H14 0.93 . C15 C16 1.399(8) . C15 H15 0.93 . C16 C17 1.458(8) . C17 N2 1.358(7) . C18 C19 1.392(8) . C18 C23 1.399(7) . C18 N3 1.433(7) . C19 C20 1.376(8) . C19 H19 0.93 . C20 C21 1.387(8) . C20 H20 0.93 . C21 C22 1.369(9) . C21 Br2 1.890(6) . C22 C23 1.385(8) . C22 H22 0.93 . C23 C24 1.488(8) . C24 O6 1.219(14) . C24 O6B 1.29(6) . C24 O5 1.328(7) . C25 O7 1.291(7) . C25 C34 1.412(9) . C25 C26 1.430(8) . C26 C27 1.345(9) . C26 H26 0.93 . C27 C28 1.423(10) . C27 H27 0.93 . C28 C29 1.389(9) . C28 C33 1.399(8) . C29 C30 1.365(11) . C29 H29 0.93 . C30 C31 1.396(10) . C30 H30 0.93 . C31 C32 1.357(9) . C31 H31 0.93 . C32 C33 1.404(9) . C32 H32 0.93 . C33 C34 1.450(8) . C34 N4 1.367(7) . N5 C39 1.483(12) . N5 C35 1.511(11) . N5 C37 1.518(12) . N5 H5A 0.91 . C35 C36 1.471(11) . C35 H35A 0.97 . C35 H35B 0.97 . C36 H36A 0.96 . C36 H36B 0.96 . C36 H36C 0.96 . C37 C38 1.457(16) . C37 H37A 0.97 . C37 H37B 0.97 . C38 H38A 0.96 . C38 H38B 0.96 . C38 H38C 0.96 . C39 C40 1.499(13) . C39 H39A 0.97 . C39 H39B 0.97 . C40 H40A 0.96 . C40 H40B 0.96 . C40 H40C 0.96 . N5B C39B 1.49(2) . N5B C35B 1.52(2) . N5B C37B 1.52(2) . N5B H5B 0.91 . C35B C36B 1.473(18) . C35B H35C 0.97 . C35B H35D 0.97 . C36B H36D 0.96 . C36B H36E 0.96 . C36B H36F 0.96 . C37B C38B 1.467(19) . C37B H37C 0.97 . C37B H37D 0.97 . C38B H38D 0.96 . C38B H38E 0.96 . C38B H38F 0.96 . C39B C40B 1.453(19) . C39B H39C 0.97 . C39B H39D 0.97 . C40B H40D 0.96 . C40B H40E 0.96 . C40B H40F 0.96 . C41 O9 1.446(10) . C41 C42 1.483(14) . C41 H41A 0.97 . C41 H41B 0.97 . C42 H42A 0.96 . C42 H42B 0.96 . C42 H42C 0.96 . C41B O9 1.441(15) . C41B C42B 1.481(18) . C41B H41C 0.97 . C41B H41D 0.97 . C42B H42D 0.96 . C42B H42E 0.96 . C42B H42F 0.96 . O9 V2 1.961(4) . O9 V1 2.019(3) . N1 N2 1.284(6) . N1 V1 2.086(4) . N3 N4 1.295(6) . N3 V2 2.051(5) . O1 V1 1.966(4) . O3 V1 1.966(4) . O4 V1 1.590(4) . O5 V2 1.958(3) . O5 V1 2.367(4) . O7 V2 1.918(4) . O8 V2 1.587(4) .