#------------------------------------------------------------------------------ #$Date: 2016-02-20 00:53:41 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176768 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/53/2105301.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2105301 loop_ _publ_author_name 'Fulford, Mabel V.' 'Lough, Alan John' 'Bender, Timothy P.' _publ_section_title ; The first report of the crystal structure of non-solvated \m-oxo boron subphthalocyanine and the crystal structures of two solvated forms ; _journal_coeditor_code RY5043 _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 636 _journal_page_last 645 _journal_paper_doi 10.1107/S0108768112037184 _journal_volume 68 _journal_year 2012 _chemical_formula_moiety 'C48 H24 B2 N12 O, 2(C6 H4 Cl2)' _chemical_formula_sum 'C60 H32 B2 Cl4 N12 O' _chemical_formula_weight 1100.40 _space_group_IT_number 2 _symmetry_cell_setting triclinic _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_creation_method SHELXL-97 _cell_angle_alpha 78.3470(16) _cell_angle_beta 85.6160(13) _cell_angle_gamma 76.7400(17) _cell_formula_units_Z 2 _cell_length_a 11.3894(3) _cell_length_b 13.2623(3) _cell_length_c 17.6618(6) _cell_measurement_reflns_used 25833 _cell_measurement_temperature 150.0(10) _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 2.6 _cell_volume 2541.89(13) _computing_cell_refinement 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_data_collection 'Collect (Nonius B.V., 1997-2002)' _computing_data_reduction Denzo-SMN _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL V6.1' _computing_structure_refinement 'SHELXTL V6.1 (Sheldrick, 2008)' _computing_structure_solution 'SIR-92 (Altomare et al., 1994)' _diffrn_ambient_temperature 150.0(10) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f scans and \w scans with \k offsets' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.1088 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 26858 _diffrn_reflns_theta_full 25.24 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_theta_min 2.59 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.291 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_correction_T_min 0.808 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1124 _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.826 _refine_diff_density_min -0.495 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 738 _refine_ls_number_reflns 11383 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 1.011 _refine_ls_R_factor_all 0.1671 _refine_ls_R_factor_gt 0.0848 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^2^+4.0961P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1757 _refine_ls_wR_factor_ref 0.2170 _reflns_number_gt 6168 _reflns_number_total 11383 _reflns_threshold_expression I>2\s(I) _iucr_refine_instructions_details ; TITL k11296 in P-1 CELL 0.71073 11.3894 13.2623 17.6618 78.347 85.616 76.740 ZERR 2 0.0003 0.0003 0.0006 0.0016 0.0013 0.0017 LATT 1 SFAC C H B N O Cl DISP C 0.00330 0.00160 DISP H 0.00000 0.00000 DISP B 0.00130 0.00070 DISP N 0.00610 0.00330 DISP O 0.01060 0.00600 DISP Cl 0.14840 0.15850 UNIT 120 64 4 24 2 8 TEMP -123 SIZE 0.34, 0.16, 0.08 ACTA BOND $H FMAP 2 PLAN 20 L.S. 4 DELU 0.002 C7S > C12S WGHT 0.075000 4.096100 FVAR 0.27104 0.75576 0.85272 O1 5 0.069655 0.145281 0.704483 11.00000 0.02866 0.02854 = 0.02517 -0.00602 0.00553 -0.00845 N1 4 -0.108794 0.294782 0.534278 11.00000 0.02201 0.03409 = 0.02808 -0.00416 0.00262 -0.00827 N2 4 0.030188 0.321791 0.617628 11.00000 0.02298 0.02575 = 0.02835 -0.00758 0.00398 -0.00764 N3 4 0.191828 0.392713 0.644359 11.00000 0.03183 0.03302 = 0.02801 -0.00828 0.00468 -0.01140 N4 4 0.228075 0.217061 0.620923 11.00000 0.02485 0.02640 = 0.02656 -0.00516 -0.00027 -0.00697 N5 4 0.280167 0.091549 0.538026 11.00000 0.02771 0.02715 = 0.02901 -0.00525 0.00447 -0.00527 N6 4 0.075294 0.168405 0.563573 11.00000 0.02079 0.02690 = 0.02476 -0.00702 0.00131 -0.00697 N7 4 -0.137460 0.381360 0.780208 11.00000 0.03093 0.02655 = 0.02885 -0.00348 0.00300 -0.00700 N8 4 0.047746 0.255641 0.806393 11.00000 0.02579 0.03171 = 0.02755 -0.00771 0.00308 -0.00947 N9 4 0.187705 0.135939 0.894392 11.00000 0.02472 0.03337 = 0.03139 -0.00900 0.00250 -0.00770 N10 4 0.039078 0.076527 0.839451 11.00000 0.02347 0.02505 = 0.02829 -0.00564 0.00022 -0.00662 N11 4 -0.147283 0.028057 0.837513 11.00000 0.02946 0.02599 = 0.02845 -0.00877 0.00327 -0.00653 N12 4 -0.123142 0.200389 0.777203 11.00000 0.02473 0.02975 = 0.02576 -0.00756 0.00127 -0.00689 C1 1 -0.073689 0.354723 0.578178 11.00000 0.02010 0.03139 = 0.02719 -0.00738 0.00592 -0.00434 C2 1 -0.115555 0.465717 0.580893 11.00000 0.03146 0.02825 = 0.02609 -0.00162 0.00969 -0.00452 C3 1 -0.220280 0.538779 0.556523 11.00000 0.03434 0.03640 = 0.03230 0.00053 0.00428 -0.00379 AFIX 43 H3A 2 -0.279988 0.520102 0.530682 11.00000 -1.20000 AFIX 0 C4 1 -0.234865 0.639228 0.571002 11.00000 0.04292 0.03304 = 0.03920 0.00085 0.00920 0.00188 AFIX 43 H4A 2 -0.307121 0.689773 0.556424 11.00000 -1.20000 AFIX 0 C5 1 -0.146012 0.668401 0.606560 11.00000 0.05047 0.02299 = 0.04376 -0.00494 0.01804 -0.00624 AFIX 43 H5A 2 -0.159570 0.737985 0.616521 11.00000 -1.20000 AFIX 0 C6 1 -0.038583 0.598129 0.627617 11.00000 0.04619 0.03061 = 0.03918 -0.00606 0.01214 -0.01438 AFIX 43 H6A 2 0.023324 0.619562 0.649340 11.00000 -1.20000 AFIX 0 C7 1 -0.023644 0.495420 0.616154 11.00000 0.03423 0.02595 = 0.02724 -0.00544 0.00993 -0.00798 C8 1 0.074487 0.402989 0.632251 11.00000 0.03075 0.02766 = 0.02324 -0.00666 0.00405 -0.00972 C9 1 0.267640 0.302694 0.632510 11.00000 0.02487 0.03061 = 0.02848 -0.00696 0.00151 -0.00879 C10 1 0.394930 0.283790 0.610215 11.00000 0.02747 0.03363 = 0.02978 -0.00380 -0.00288 -0.00881 C11 1 0.480602 0.344626 0.607630 11.00000 0.03363 0.04258 = 0.04107 -0.00576 -0.00505 -0.01699 AFIX 43 H11A 2 0.461478 0.409267 0.625939 11.00000 -1.20000 AFIX 0 C12 1 0.594337 0.307574 0.577490 11.00000 0.03106 0.04743 = 0.05884 -0.00080 -0.00574 -0.01701 AFIX 43 H12A 2 0.654928 0.346528 0.576704 11.00000 -1.20000 AFIX 0 C13 1 0.622318 0.214921 0.548339 11.00000 0.02201 0.04673 = 0.05368 -0.00573 0.00444 -0.00536 AFIX 43 H13A 2 0.701384 0.192215 0.527840 11.00000 -1.20000 AFIX 0 C14 1 0.537707 0.154937 0.548467 11.00000 0.02938 0.04066 = 0.03940 -0.00513 0.00063 -0.00420 AFIX 43 H14A 2 0.557344 0.091884 0.528079 11.00000 -1.20000 AFIX 0 C15 1 0.422815 0.189795 0.579401 11.00000 0.02314 0.03461 = 0.03486 -0.00370 -0.00002 -0.00806 C16 1 0.311365 0.153388 0.581774 11.00000 0.02160 0.02735 = 0.03049 -0.00543 0.00183 -0.00347 C17 1 0.161226 0.106300 0.526182 11.00000 0.02909 0.02002 = 0.02813 -0.00592 0.00628 -0.00780 C18 1 0.101565 0.086660 0.462454 11.00000 0.03353 0.02748 = 0.02881 -0.00493 0.00209 -0.01344 C19 1 0.145956 0.029145 0.403923 11.00000 0.04115 0.03094 = 0.03495 -0.01084 0.00332 -0.01035 AFIX 43 H19A 2 0.227141 -0.009593 0.402905 11.00000 -1.20000 AFIX 0 C20 1 0.067114 0.031074 0.347965 11.00000 0.05477 0.04360 = 0.03207 -0.01609 0.00156 -0.01557 AFIX 43 H20A 2 0.093493 -0.009929 0.309061 11.00000 -1.20000 AFIX 0 C21 1 -0.050040 0.091535 0.347055 11.00000 0.05218 0.05140 = 0.03477 -0.01630 -0.00665 -0.01906 AFIX 43 H21A 2 -0.101296 0.091048 0.307208 11.00000 -1.20000 AFIX 0 C22 1 -0.094418 0.152301 0.402152 11.00000 0.03920 0.03657 = 0.03627 -0.00408 -0.00718 -0.01310 AFIX 43 H22A 2 -0.173733 0.195262 0.399997 11.00000 -1.20000 AFIX 0 C23 1 -0.016995 0.147704 0.461497 11.00000 0.02985 0.02944 = 0.02788 -0.00529 0.00045 -0.01433 C24 1 -0.029361 0.206068 0.524323 11.00000 0.02460 0.02910 = 0.02685 -0.00285 0.00256 -0.00958 C25 1 -0.022681 0.355754 0.801411 11.00000 0.02898 0.02533 = 0.02813 -0.00381 0.00586 -0.00643 C26 1 0.041616 0.410941 0.842084 11.00000 0.03250 0.03118 = 0.03126 -0.00786 0.00753 -0.01060 C27 1 0.014276 0.513663 0.855806 11.00000 0.04188 0.03298 = 0.04427 -0.01096 0.00096 -0.00976 AFIX 43 H27A 2 -0.052741 0.564382 0.832725 11.00000 -1.20000 AFIX 0 C28 1 0.088228 0.539242 0.904279 11.00000 0.05367 0.03567 = 0.06011 -0.02048 0.00275 -0.01607 AFIX 43 H28A 2 0.072046 0.609150 0.913866 11.00000 -1.20000 AFIX 0 C29 1 0.185563 0.465367 0.939317 11.00000 0.05341 0.04460 = 0.05238 -0.02326 -0.00235 -0.01750 AFIX 43 H29A 2 0.234180 0.485840 0.972326 11.00000 -1.20000 AFIX 0 C30 1 0.212933 0.362929 0.927095 11.00000 0.03274 0.04279 = 0.04061 -0.00982 -0.00169 -0.01155 AFIX 43 H30A 2 0.278916 0.312490 0.951662 11.00000 -1.20000 AFIX 0 C31 1 0.140501 0.335596 0.877387 11.00000 0.03164 0.03394 = 0.03242 -0.00860 0.00469 -0.01234 C32 1 0.137803 0.234485 0.857925 11.00000 0.02252 0.03506 = 0.02997 -0.00815 0.00666 -0.00869 C33 1 0.132178 0.059426 0.887753 11.00000 0.02286 0.03018 = 0.02921 -0.00913 0.00343 -0.00393 C34 1 0.135357 -0.044714 0.935821 11.00000 0.02931 0.02773 = 0.02554 -0.00807 0.00372 -0.00238 C35 1 0.213967 -0.107065 0.991835 11.00000 0.03388 0.03484 = 0.02981 -0.01202 0.00000 -0.00382 AFIX 43 H35A 2 0.281058 -0.083881 1.005490 11.00000 -1.20000 AFIX 0 C36 1 0.191176 -0.204373 1.027174 11.00000 0.04057 0.03917 = 0.02714 -0.00672 -0.00181 0.00083 AFIX 43 H36A 2 0.245303 -0.249431 1.064344 11.00000 -1.20000 AFIX 0 C37 1 0.090677 -0.237535 1.009388 11.00000 0.05060 0.02791 = 0.02745 -0.00400 0.00826 -0.00718 AFIX 43 H37A 2 0.078274 -0.304903 1.034424 11.00000 -1.20000 AFIX 0 C38 1 0.008120 -0.174284 0.955833 11.00000 0.03903 0.03057 = 0.03148 -0.00775 0.00530 -0.00891 AFIX 43 H38A 2 -0.062205 -0.195800 0.945690 11.00000 -1.20000 AFIX 0 C39 1 0.032370 -0.078488 0.917744 11.00000 0.02972 0.02719 = 0.02717 -0.00959 0.00437 -0.00540 C40 1 -0.033007 0.005980 0.859608 11.00000 0.02504 0.02773 = 0.02765 -0.01018 0.00323 -0.00716 C41 1 -0.193556 0.127810 0.802117 11.00000 0.02899 0.03449 = 0.02370 -0.01027 0.00225 -0.00850 C42 1 -0.317968 0.187280 0.798750 11.00000 0.02854 0.03770 = 0.02706 -0.01103 -0.00026 -0.00729 C43 1 -0.426573 0.156268 0.816469 11.00000 0.03007 0.04704 = 0.03576 -0.00784 0.00139 -0.01245 AFIX 43 H43A 2 -0.428909 0.083630 0.829030 11.00000 -1.20000 AFIX 0 C44 1 -0.530720 0.232951 0.815450 11.00000 0.02856 0.05928 = 0.04785 -0.00927 -0.00092 -0.01246 AFIX 43 H44A 2 -0.605974 0.212832 0.826611 11.00000 -1.20000 AFIX 0 C45 1 -0.528207 0.340791 0.798198 11.00000 0.03004 0.05490 = 0.03929 -0.00972 0.00254 -0.00053 AFIX 43 H45A 2 -0.601717 0.392093 0.798174 11.00000 -1.20000 AFIX 0 C46 1 -0.421018 0.373295 0.781338 11.00000 0.03233 0.04227 = 0.03433 -0.00796 -0.00490 -0.00217 AFIX 43 H46A 2 -0.419380 0.446106 0.770469 11.00000 -1.20000 AFIX 0 C47 1 -0.314831 0.295777 0.780737 11.00000 0.02708 0.03775 = 0.02739 -0.01035 0.00117 -0.00522 C48 1 -0.188126 0.301803 0.772600 11.00000 0.03025 0.03008 = 0.02376 -0.00621 0.00256 -0.00684 B1 3 0.097758 0.207917 0.633860 11.00000 0.01962 0.02582 = 0.03151 -0.01048 0.00401 -0.00694 B2 3 0.012870 0.170220 0.774275 11.00000 0.03081 0.02465 = 0.02956 -0.00402 0.00037 -0.01011 PART 1 CL1 6 0.564127 -0.119520 0.962648 31.00000 0.07449 0.05696 = 0.06597 -0.02566 -0.00588 -0.00337 CL2 6 0.482928 -0.337141 0.982253 31.00000 0.06317 0.08378 = 0.08201 -0.02002 0.01761 -0.02620 AFIX 66 C1S 1 0.619613 -0.206991 0.901833 31.00000 0.04458 0.04635 = 0.04612 -0.01362 -0.01098 0.00794 C2S 1 0.581885 -0.301164 0.909452 31.00000 0.04588 0.05170 = 0.05274 -0.00776 -0.01956 0.00003 C3S 1 0.626795 -0.369214 0.858495 31.00000 0.04723 0.05522 = 0.05712 -0.02921 -0.00650 -0.00257 AFIX 43 H3S 2 0.601009 -0.433577 0.863702 31.00000 -1.20000 AFIX 65 C4S 1 0.709434 -0.343092 0.799920 31.00000 0.05645 0.06025 = 0.04495 -0.01349 -0.00666 -0.00413 AFIX 43 H4S 2 0.740127 -0.389602 0.765094 31.00000 -1.20000 AFIX 65 C5S 1 0.747163 -0.248920 0.792301 31.00000 0.04337 0.06858 = 0.05468 -0.00153 -0.00111 -0.00211 AFIX 43 H5S 2 0.803642 -0.231067 0.752268 31.00000 -1.20000 AFIX 65 C6S 1 0.702253 -0.180868 0.843257 31.00000 0.04580 0.05748 = 0.04642 0.00418 -0.01332 -0.00613 AFIX 43 H6S 2 0.728039 -0.116505 0.838050 31.00000 -1.20000 AFIX 0 PART 2 SAME 0.005 Cl1 > C6S CL1B 6 0.811965 -0.219477 0.794854 -31.00000 10.15000 CL2B 6 0.672361 -0.400677 0.831361 -31.00000 10.15000 C1B 1 0.691189 -0.213057 0.859727 -31.00000 10.15000 C2B 1 0.632806 -0.296678 0.878636 -31.00000 10.15000 C3B 1 0.536932 -0.292741 0.932279 -31.00000 10.15000 AFIX 43 H3B 2 0.489733 -0.344668 0.940020 -31.00000 -1.20000 AFIX 0 C4B 1 0.510653 -0.211994 0.974590 -31.00000 10.15000 AFIX 43 H4B 2 0.456591 -0.215757 1.018262 -31.00000 -1.20000 AFIX 0 C5B 1 0.564198 -0.125627 0.952435 -31.00000 10.15000 AFIX 43 H5B 2 0.532586 -0.062602 0.971719 -31.00000 -1.20000 AFIX 0 C6B 1 0.664324 -0.132310 0.901854 -31.00000 10.15000 AFIX 43 H6B 2 0.713711 -0.082278 0.896192 -31.00000 -1.20000 AFIX 0 PART 1 CL3 6 0.543566 0.875265 0.632705 21.00000 0.05877 0.06196 = 0.06767 -0.00775 0.00278 -0.00989 CL4 6 0.388230 0.958324 0.773436 21.00000 0.10702 0.14092 = 0.08792 -0.06579 -0.03647 0.05605 AFIX 66 C7S 1 0.447432 0.806479 0.688590 21.00000 0.03484 0.07898 = 0.04335 -0.00754 -0.00635 0.01176 C8S 1 0.381456 0.841740 0.751330 21.00000 0.05193 0.12972 = 0.03920 -0.00345 -0.00721 0.04343 C9S 1 0.304808 0.782893 0.794978 21.00000 0.06637 0.18898 = 0.06128 0.03713 0.01613 0.04374 AFIX 43 H9S 2 0.259716 0.806992 0.837859 21.00000 -1.20000 AFIX 65 C10S 1 0.294136 0.688784 0.775886 21.00000 0.12828 0.18896 = 0.12766 0.06095 0.04628 -0.02999 AFIX 43 H10S 2 0.241751 0.648565 0.805718 21.00000 -1.20000 AFIX 65 C11S 1 0.360112 0.653522 0.713146 21.00000 0.06011 0.08986 = 0.12691 0.05651 -0.00607 -0.00695 AFIX 43 H11S 2 0.352818 0.589204 0.700097 21.00000 -1.20000 AFIX 65 C12S 1 0.436760 0.712369 0.669497 21.00000 0.06196 0.07650 = 0.06680 0.00897 -0.00569 -0.01758 AFIX 43 H12S 2 0.481851 0.688269 0.626616 21.00000 -1.20000 AFIX 0 PART 2 SAME 0.005 Cl3 > C12S CL3A 6 0.461898 0.651909 0.647367 -21.00000 10.10000 CL4A 6 0.280688 0.667241 0.786926 -21.00000 10.10000 C7A 1 0.427915 0.762405 0.687946 -21.00000 10.10000 C8A 1 0.350673 0.767090 0.752942 -21.00000 10.10000 C9A 1 0.329293 0.854692 0.787784 -21.00000 10.10000 AFIX 43 H9A 2 0.280859 0.856279 0.833953 -21.00000 -1.20000 AFIX 0 C10A 1 0.379441 0.940168 0.754483 -21.00000 10.10000 AFIX 43 H10A 2 0.349555 1.007083 0.768534 -21.00000 -1.20000 AFIX 0 C11A 1 0.474158 0.926132 0.700214 -21.00000 10.10000 AFIX 43 H11B 2 0.523482 0.976368 0.687150 -21.00000 -1.20000 AFIX 0 C12A 1 0.496350 0.838206 0.665146 -21.00000 10.10000 AFIX 43 H12B 2 0.557820 0.830156 0.625940 -21.00000 -1.20000 PART 0 HKLF 4 REM k11296 in P-1 REM R1 = 0.0848 for 6168 Fo > 4sig(Fo) and 0.1671 for all 11383 data REM 738 parameters refined using 48 restraints END WGHT 0.0738 4.1154 REM Highest difference peak 0.826, deepest hole -0.495, 1-sigma level 0.070 Q1 1 0.2835 0.5825 0.5936 11.00000 0.05 0.83 Q2 1 0.4946 -0.4054 0.9395 11.00000 0.05 0.79 Q3 1 0.5627 -0.4334 0.8908 11.00000 0.05 0.55 Q4 1 0.3536 0.8818 0.7808 11.00000 0.05 0.53 Q5 1 0.6261 -0.1357 0.9197 11.00000 0.05 0.50 Q6 1 0.7118 -0.1207 0.8618 11.00000 0.05 0.48 Q7 1 0.6530 -0.2874 0.8613 11.00000 0.05 0.47 Q8 1 0.2410 0.7436 0.8232 11.00000 0.05 0.42 Q9 1 0.4623 0.9844 0.7411 11.00000 0.05 0.39 Q10 1 0.3316 0.6000 0.6854 11.00000 0.05 0.33 Q11 1 0.4423 0.7288 0.6850 11.00000 0.05 0.30 Q12 1 0.0726 0.2734 0.6121 11.00000 0.05 0.30 Q13 1 0.7474 -0.2155 0.8328 11.00000 0.05 0.30 Q14 1 0.1611 0.2228 0.6239 11.00000 0.05 0.29 Q15 1 0.1753 0.2671 0.8623 11.00000 0.05 0.28 Q16 1 0.3324 0.0287 0.5271 11.00000 0.05 0.28 Q17 1 -0.0059 -0.1194 0.9400 11.00000 0.05 0.27 Q18 1 0.4032 -0.3575 0.8833 11.00000 0.05 0.27 Q19 1 0.5823 -0.2366 0.9158 11.00000 0.05 0.26 Q20 1 -0.0760 0.4796 0.5931 11.00000 0.05 0.26 ; _cod_data_source_file ry5043.cif _cod_data_source_block DCB-m-oxo-BsubPc _cod_original_cell_volume 2541.89(12) _cod_database_code 2105301 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.0697(2) 0.14528(18) 0.70448(14) 0.0273(6) Uani d . 1 1 . . N N1 -0.1088(3) 0.2948(2) 0.53428(17) 0.0281(7) Uani d . 1 1 . . N N2 0.0302(3) 0.3218(2) 0.61763(17) 0.0252(7) Uani d . 1 1 . . N N3 0.1918(3) 0.3927(2) 0.64436(17) 0.0302(7) Uani d . 1 1 . . N N4 0.2281(3) 0.2171(2) 0.62092(17) 0.0257(7) Uani d . 1 1 . . N N5 0.2802(3) 0.0915(2) 0.53803(17) 0.0284(7) Uani d . 1 1 . . N N6 0.0753(3) 0.1684(2) 0.56357(16) 0.0237(6) Uani d . 1 1 . . N N7 -0.1375(3) 0.3814(2) 0.78021(17) 0.0291(7) Uani d . 1 1 . . N N8 0.0477(3) 0.2556(2) 0.80639(17) 0.0277(7) Uani d . 1 1 . . N N9 0.1877(3) 0.1359(2) 0.89439(18) 0.0294(7) Uani d . 1 1 . . N N10 0.0391(3) 0.0765(2) 0.83945(17) 0.0254(7) Uani d . 1 1 . . N N11 -0.1473(3) 0.0281(2) 0.83751(17) 0.0276(7) Uani d . 1 1 . . N N12 -0.1231(3) 0.2004(2) 0.77720(17) 0.0264(7) Uani d . 1 1 . . C C1 -0.0737(3) 0.3547(3) 0.5782(2) 0.0265(8) Uani d . 1 1 . . C C2 -0.1156(3) 0.4657(3) 0.5809(2) 0.0300(9) Uani d . 1 1 . . C C3 -0.2203(4) 0.5388(3) 0.5565(2) 0.0363(9) Uani d . 1 1 . . H H3A -0.2800 0.5201 0.5307 0.044 Uiso calc R 1 1 . . C C4 -0.2349(4) 0.6392(3) 0.5710(2) 0.0417(10) Uani d . 1 1 . . H H4A -0.3071 0.6898 0.5564 0.050 Uiso calc R 1 1 . . C C5 -0.1460(4) 0.6684(3) 0.6066(2) 0.0406(10) Uani d . 1 1 . . H H5A -0.1596 0.7380 0.6165 0.049 Uiso calc R 1 1 . . C C6 -0.0386(4) 0.5981(3) 0.6276(2) 0.0385(10) Uani d . 1 1 . . H H6A 0.0233 0.6196 0.6493 0.046 Uiso calc R 1 1 . . C C7 -0.0236(3) 0.4954(3) 0.6162(2) 0.0294(8) Uani d . 1 1 . . C C8 0.0745(3) 0.4030(3) 0.6323(2) 0.0267(8) Uani d . 1 1 . . C C9 0.2676(3) 0.3027(3) 0.6325(2) 0.0275(8) Uani d . 1 1 . . C C10 0.3949(3) 0.2838(3) 0.6102(2) 0.0302(8) Uani d . 1 1 . . C C11 0.4806(4) 0.3446(3) 0.6076(2) 0.0378(10) Uani d . 1 1 . . H H11A 0.4615 0.4093 0.6259 0.045 Uiso calc R 1 1 . . C C12 0.5943(4) 0.3076(3) 0.5775(3) 0.0455(11) Uani d . 1 1 . . H H12A 0.6549 0.3465 0.5767 0.055 Uiso calc R 1 1 . . C C13 0.6223(4) 0.2149(3) 0.5483(3) 0.0420(10) Uani d . 1 1 . . H H13A 0.7014 0.1922 0.5278 0.050 Uiso calc R 1 1 . . C C14 0.5377(4) 0.1549(3) 0.5485(2) 0.0375(10) Uani d . 1 1 . . H H14A 0.5573 0.0919 0.5281 0.045 Uiso calc R 1 1 . . C C15 0.4228(3) 0.1898(3) 0.5794(2) 0.0311(9) Uani d . 1 1 . . C C16 0.3114(3) 0.1534(3) 0.5818(2) 0.0269(8) Uani d . 1 1 . . C C17 0.1612(3) 0.1063(3) 0.5262(2) 0.0255(8) Uani d . 1 1 . . C C18 0.1016(3) 0.0867(3) 0.4625(2) 0.0291(8) Uani d . 1 1 . . C C19 0.1460(4) 0.0291(3) 0.4039(2) 0.0349(9) Uani d . 1 1 . . H H19A 0.2271 -0.0096 0.4029 0.042 Uiso calc R 1 1 . . C C20 0.0671(4) 0.0311(3) 0.3480(2) 0.0416(10) Uani d . 1 1 . . H H20A 0.0935 -0.0099 0.3091 0.050 Uiso calc R 1 1 . . C C21 -0.0500(4) 0.0915(3) 0.3471(2) 0.0434(11) Uani d . 1 1 . . H H21A -0.1013 0.0910 0.3072 0.052 Uiso calc R 1 1 . . C C22 -0.0944(4) 0.1523(3) 0.4022(2) 0.0366(10) Uani d . 1 1 . . H H22A -0.1737 0.1953 0.4000 0.044 Uiso calc R 1 1 . . C C23 -0.0170(3) 0.1477(3) 0.4615(2) 0.0279(8) Uani d . 1 1 . . C C24 -0.0294(3) 0.2061(3) 0.5243(2) 0.0268(8) Uani d . 1 1 . . C C25 -0.0227(3) 0.3558(3) 0.8014(2) 0.0279(8) Uani d . 1 1 . . C C26 0.0416(3) 0.4109(3) 0.8421(2) 0.0312(9) Uani d . 1 1 . . C C27 0.0143(4) 0.5137(3) 0.8558(2) 0.0391(10) Uani d . 1 1 . . H H27A -0.0527 0.5644 0.8327 0.047 Uiso calc R 1 1 . . C C28 0.0882(4) 0.5392(3) 0.9043(3) 0.0474(11) Uani d . 1 1 . . H H28A 0.0720 0.6092 0.9139 0.057 Uiso calc R 1 1 . . C C29 0.1856(4) 0.4654(3) 0.9393(3) 0.0470(11) Uani d . 1 1 . . H H29A 0.2342 0.4858 0.9723 0.056 Uiso calc R 1 1 . . C C30 0.2129(4) 0.3629(3) 0.9271(2) 0.0379(10) Uani d . 1 1 . . H H30A 0.2789 0.3125 0.9517 0.045 Uiso calc R 1 1 . . C C31 0.1405(3) 0.3356(3) 0.8774(2) 0.0318(9) Uani d . 1 1 . . C C32 0.1378(3) 0.2345(3) 0.8579(2) 0.0289(8) Uani d . 1 1 . . C C33 0.1322(3) 0.0594(3) 0.8878(2) 0.0275(8) Uani d . 1 1 . . C C34 0.1354(3) -0.0447(3) 0.9358(2) 0.0280(8) Uani d . 1 1 . . C C35 0.2140(4) -0.1071(3) 0.9918(2) 0.0327(9) Uani d . 1 1 . . H H35A 0.2811 -0.0839 1.0055 0.039 Uiso calc R 1 1 . . C C36 0.1912(4) -0.2044(3) 1.0272(2) 0.0371(10) Uani d . 1 1 . . H H36A 0.2453 -0.2494 1.0643 0.045 Uiso calc R 1 1 . . C C37 0.0907(4) -0.2375(3) 1.0094(2) 0.0362(10) Uani d . 1 1 . . H H37A 0.0783 -0.3049 1.0344 0.043 Uiso calc R 1 1 . . C C38 0.0081(4) -0.1743(3) 0.9558(2) 0.0336(9) Uani d . 1 1 . . H H38A -0.0622 -0.1958 0.9457 0.040 Uiso calc R 1 1 . . C C39 0.0324(3) -0.0785(3) 0.9177(2) 0.0278(8) Uani d . 1 1 . . C C40 -0.0330(3) 0.0060(3) 0.8596(2) 0.0261(8) Uani d . 1 1 . . C C41 -0.1936(3) 0.1278(3) 0.8021(2) 0.0283(8) Uani d . 1 1 . . C C42 -0.3180(3) 0.1873(3) 0.7987(2) 0.0304(9) Uani d . 1 1 . . C C43 -0.4266(4) 0.1563(3) 0.8165(2) 0.0371(9) Uani d . 1 1 . . H H43A -0.4289 0.0836 0.8290 0.045 Uiso calc R 1 1 . . C C44 -0.5307(4) 0.2330(4) 0.8155(3) 0.0449(11) Uani d . 1 1 . . H H44A -0.6060 0.2128 0.8266 0.054 Uiso calc R 1 1 . . C C45 -0.5282(4) 0.3408(4) 0.7982(2) 0.0429(10) Uani d . 1 1 . . H H45A -0.6017 0.3921 0.7982 0.052 Uiso calc R 1 1 . . C C46 -0.4210(4) 0.3733(3) 0.7813(2) 0.0370(9) Uani d . 1 1 . . H H46A -0.4194 0.4461 0.7705 0.044 Uiso calc R 1 1 . . C C47 -0.3148(3) 0.2958(3) 0.7807(2) 0.0306(9) Uani d . 1 1 . . C C48 -0.1881(3) 0.3018(3) 0.7726(2) 0.0280(8) Uani d . 1 1 . . B B1 0.0978(4) 0.2079(3) 0.6339(2) 0.0249(9) Uani d . 1 1 . . B B2 0.0129(4) 0.1702(3) 0.7743(2) 0.0279(9) Uani d . 1 1 . . Cl Cl1 0.56413(18) -0.11952(13) 0.96265(11) 0.0654(5) Uani d PD 0.853(3) 1 A 1 Cl Cl2 0.48293(16) -0.33714(14) 0.98225(11) 0.0751(6) Uani d PD 0.853(3) 1 A 1 C C1S 0.6196(3) -0.2070(2) 0.9018(2) 0.0474(14) Uani d PGD 0.853(3) 1 A 1 C C2S 0.5819(3) -0.3012(3) 0.9095(2) 0.0512(14) Uani d PGD 0.853(3) 1 A 1 C C3S 0.6268(3) -0.3692(2) 0.8585(2) 0.0517(15) Uani d PGD 0.853(3) 1 A 1 H H3S 0.6010 -0.4336 0.8637 0.062 Uiso calc PR 0.853(3) 1 A 1 C C4S 0.7094(3) -0.3431(3) 0.7999(2) 0.0545(15) Uani d PGD 0.853(3) 1 A 1 H H4S 0.7401 -0.3896 0.7651 0.065 Uiso calc PR 0.853(3) 1 A 1 C C5S 0.7472(3) -0.2489(3) 0.79230(19) 0.0587(16) Uani d PGD 0.853(3) 1 A 1 H H5S 0.8036 -0.2311 0.7523 0.070 Uiso calc PR 0.853(3) 1 A 1 C C6S 0.7023(3) -0.1809(2) 0.8433(2) 0.0521(15) Uani d PGD 0.853(3) 1 A 1 H H6S 0.7280 -0.1165 0.8380 0.063 Uiso calc PR 0.853(3) 1 A 1 Cl Cl1B 0.8119(17) -0.2195(15) 0.7949(11) 0.150 Uiso d PD 0.147(3) 1 A 2 Cl Cl2B 0.6724(19) -0.4007(14) 0.8314(13) 0.150 Uiso d PD 0.147(3) 1 A 2 C C1B 0.691(4) -0.213(3) 0.860(3) 0.150 Uiso d PD 0.147(3) 1 A 2 C C2B 0.633(4) -0.297(3) 0.879(3) 0.150 Uiso d PD 0.147(3) 1 A 2 C C3B 0.537(4) -0.293(3) 0.932(3) 0.150 Uiso d PD 0.147(3) 1 A 2 H H3B 0.4897 -0.3447 0.9400 0.180 Uiso calc PR 0.147(3) 1 A 2 C C4B 0.511(4) -0.212(3) 0.975(2) 0.150 Uiso d PD 0.147(3) 1 A 2 H H4B 0.4566 -0.2158 1.0183 0.180 Uiso calc PR 0.147(3) 1 A 2 C C5B 0.564(5) -0.126(3) 0.952(3) 0.150 Uiso d PD 0.147(3) 1 A 2 H H5B 0.5325 -0.0626 0.9717 0.180 Uiso calc PR 0.147(3) 1 A 2 C C6B 0.664(4) -0.132(3) 0.902(3) 0.150 Uiso d PD 0.147(3) 1 A 2 H H6B 0.7137 -0.0823 0.8962 0.180 Uiso calc PR 0.147(3) 1 A 2 Cl Cl3 0.54357(17) 0.87526(14) 0.63271(11) 0.0643(6) Uani d PD 0.756(3) 1 B 1 Cl Cl4 0.3882(3) 0.9583(2) 0.77344(15) 0.1175(12) Uani d PD 0.756(3) 1 B 1 C C7S 0.4474(4) 0.8065(4) 0.6886(3) 0.0567(15) Uani d PGDU 0.756(3) 1 B 1 C C8S 0.3815(5) 0.8417(4) 0.7513(3) 0.086(2) Uani d PGDU 0.756(3) 1 B 1 C C9S 0.3048(5) 0.7829(5) 0.7950(3) 0.127(4) Uani d PGDU 0.756(3) 1 B 1 H H9S 0.2597 0.8070 0.8379 0.152 Uiso calc PR 0.756(3) 1 B 1 C C10S 0.2941(6) 0.6888(5) 0.7759(4) 0.165(5) Uani d PGDU 0.756(3) 1 B 1 H H10S 0.2418 0.6486 0.8057 0.198 Uiso calc PR 0.756(3) 1 B 1 C C11S 0.3601(5) 0.6535(4) 0.7131(4) 0.105(3) Uani d PGDU 0.756(3) 1 B 1 H H11S 0.3528 0.5892 0.7001 0.126 Uiso calc PR 0.756(3) 1 B 1 C C12S 0.4368(5) 0.7124(4) 0.6695(3) 0.0711(18) Uani d PGDU 0.756(3) 1 B 1 H H12S 0.4819 0.6883 0.6266 0.085 Uiso calc PR 0.756(3) 1 B 1 Cl Cl3A 0.4619(7) 0.6519(6) 0.6474(5) 0.100 Uiso d PD 0.244(3) 1 B 2 Cl Cl4A 0.2807(9) 0.6672(7) 0.7869(6) 0.100 Uiso d PD 0.244(3) 1 B 2 C C7A 0.428(3) 0.7624(16) 0.6879(16) 0.100 Uiso d PD 0.244(3) 1 B 2 C C8A 0.351(2) 0.7671(14) 0.7529(13) 0.100 Uiso d PD 0.244(3) 1 B 2 C C9A 0.329(3) 0.8547(14) 0.7878(14) 0.100 Uiso d PD 0.244(3) 1 B 2 H H9A 0.2809 0.8563 0.8340 0.120 Uiso calc PR 0.244(3) 1 B 2 C C10A 0.379(3) 0.9402(13) 0.7545(17) 0.100 Uiso d PD 0.244(3) 1 B 2 H H10A 0.3496 1.0071 0.7685 0.120 Uiso calc PR 0.244(3) 1 B 2 C C11A 0.474(2) 0.9261(13) 0.7002(13) 0.100 Uiso d PD 0.244(3) 1 B 2 H H11B 0.5235 0.9764 0.6871 0.120 Uiso calc PR 0.244(3) 1 B 2 C C12A 0.496(2) 0.8382(16) 0.6651(15) 0.100 Uiso d PD 0.244(3) 1 B 2 H H12B 0.5578 0.8302 0.6259 0.120 Uiso calc PR 0.244(3) 1 B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0287(14) 0.0285(13) 0.0252(14) -0.0085(11) 0.0055(11) -0.0060(11) N1 0.0220(16) 0.0341(17) 0.0281(17) -0.0083(14) 0.0026(13) -0.0042(14) N2 0.0230(17) 0.0257(16) 0.0283(17) -0.0076(13) 0.0040(13) -0.0076(13) N3 0.0318(19) 0.0330(17) 0.0280(17) -0.0114(14) 0.0047(14) -0.0083(14) N4 0.0249(16) 0.0264(16) 0.0266(17) -0.0070(13) -0.0003(13) -0.0052(13) N5 0.0277(18) 0.0272(16) 0.0290(17) -0.0053(13) 0.0045(13) -0.0053(13) N6 0.0208(16) 0.0269(16) 0.0248(16) -0.0070(12) 0.0013(13) -0.0070(12) N7 0.0309(18) 0.0265(16) 0.0289(17) -0.0070(14) 0.0030(14) -0.0035(13) N8 0.0258(17) 0.0317(17) 0.0275(17) -0.0095(13) 0.0031(13) -0.0077(13) N9 0.0247(17) 0.0334(18) 0.0314(18) -0.0077(14) 0.0025(14) -0.0090(14) N10 0.0235(16) 0.0251(16) 0.0283(17) -0.0066(13) 0.0002(13) -0.0056(13) N11 0.0295(18) 0.0260(16) 0.0284(17) -0.0065(13) 0.0033(14) -0.0088(13) N12 0.0247(17) 0.0297(16) 0.0258(16) -0.0069(13) 0.0013(13) -0.0076(13) C1 0.0201(19) 0.031(2) 0.027(2) -0.0043(15) 0.0059(15) -0.0074(16) C2 0.031(2) 0.028(2) 0.026(2) -0.0045(16) 0.0097(16) -0.0016(15) C3 0.034(2) 0.036(2) 0.032(2) -0.0038(18) 0.0043(18) 0.0005(17) C4 0.043(3) 0.033(2) 0.039(2) 0.0019(19) 0.009(2) 0.0008(18) C5 0.050(3) 0.023(2) 0.044(3) -0.0062(19) 0.018(2) -0.0049(18) C6 0.046(3) 0.031(2) 0.039(2) -0.0144(19) 0.012(2) -0.0061(18) C7 0.034(2) 0.0260(19) 0.027(2) -0.0080(16) 0.0099(17) -0.0054(15) C8 0.031(2) 0.0277(19) 0.0232(19) -0.0097(16) 0.0040(16) -0.0067(15) C9 0.025(2) 0.031(2) 0.028(2) -0.0088(16) 0.0015(16) -0.0070(16) C10 0.027(2) 0.034(2) 0.030(2) -0.0088(17) -0.0029(16) -0.0038(16) C11 0.034(2) 0.043(2) 0.041(2) -0.0170(19) -0.0051(19) -0.0058(19) C12 0.031(2) 0.047(3) 0.059(3) -0.017(2) -0.006(2) -0.001(2) C13 0.022(2) 0.047(3) 0.054(3) -0.0054(19) 0.0044(19) -0.006(2) C14 0.029(2) 0.041(2) 0.039(2) -0.0042(18) 0.0006(18) -0.0051(18) C15 0.023(2) 0.035(2) 0.035(2) -0.0081(16) 0.0000(16) -0.0037(17) C16 0.0216(19) 0.0274(19) 0.030(2) -0.0035(15) 0.0018(16) -0.0054(16) C17 0.029(2) 0.0200(17) 0.028(2) -0.0078(15) 0.0063(16) -0.0059(14) C18 0.034(2) 0.0275(19) 0.029(2) -0.0134(17) 0.0021(17) -0.0049(16) C19 0.041(2) 0.031(2) 0.035(2) -0.0103(18) 0.0033(19) -0.0108(17) C20 0.055(3) 0.044(2) 0.032(2) -0.016(2) 0.002(2) -0.0161(19) C21 0.052(3) 0.051(3) 0.035(2) -0.019(2) -0.007(2) -0.016(2) C22 0.039(2) 0.037(2) 0.036(2) -0.0131(19) -0.0072(19) -0.0041(18) C23 0.030(2) 0.029(2) 0.028(2) -0.0143(16) 0.0005(16) -0.0053(16) C24 0.025(2) 0.029(2) 0.027(2) -0.0096(16) 0.0026(16) -0.0028(15) C25 0.029(2) 0.0253(19) 0.028(2) -0.0064(16) 0.0059(16) -0.0038(15) C26 0.033(2) 0.031(2) 0.031(2) -0.0106(17) 0.0075(17) -0.0079(16) C27 0.042(2) 0.033(2) 0.044(3) -0.0098(19) 0.001(2) -0.0110(19) C28 0.054(3) 0.036(2) 0.060(3) -0.016(2) 0.003(2) -0.020(2) C29 0.053(3) 0.045(3) 0.052(3) -0.017(2) -0.002(2) -0.023(2) C30 0.033(2) 0.043(2) 0.041(2) -0.0116(19) -0.0017(19) -0.0098(19) C31 0.032(2) 0.034(2) 0.032(2) -0.0123(17) 0.0047(17) -0.0086(17) C32 0.023(2) 0.035(2) 0.030(2) -0.0087(16) 0.0067(16) -0.0082(16) C33 0.023(2) 0.030(2) 0.029(2) -0.0039(16) 0.0034(16) -0.0091(16) C34 0.029(2) 0.0277(19) 0.026(2) -0.0024(16) 0.0037(16) -0.0081(15) C35 0.034(2) 0.035(2) 0.030(2) -0.0038(17) 0.0000(17) -0.0120(17) C36 0.041(2) 0.039(2) 0.027(2) 0.0008(19) -0.0018(18) -0.0067(17) C37 0.051(3) 0.028(2) 0.027(2) -0.0072(19) 0.0083(19) -0.0040(16) C38 0.039(2) 0.031(2) 0.031(2) -0.0089(18) 0.0053(18) -0.0078(17) C39 0.030(2) 0.0272(19) 0.027(2) -0.0054(16) 0.0044(16) -0.0096(16) C40 0.025(2) 0.0277(19) 0.028(2) -0.0072(15) 0.0032(16) -0.0102(15) C41 0.029(2) 0.034(2) 0.0237(19) -0.0085(17) 0.0022(16) -0.0103(16) C42 0.029(2) 0.038(2) 0.027(2) -0.0073(17) -0.0003(16) -0.0110(16) C43 0.030(2) 0.047(2) 0.036(2) -0.0124(19) 0.0014(18) -0.0078(19) C44 0.029(2) 0.059(3) 0.048(3) -0.012(2) -0.001(2) -0.009(2) C45 0.030(2) 0.055(3) 0.039(3) -0.001(2) 0.0025(19) -0.010(2) C46 0.032(2) 0.042(2) 0.034(2) -0.0022(18) -0.0049(18) -0.0080(18) C47 0.027(2) 0.038(2) 0.027(2) -0.0052(17) 0.0012(16) -0.0104(17) C48 0.030(2) 0.030(2) 0.0238(19) -0.0068(16) 0.0026(16) -0.0062(15) B1 0.020(2) 0.026(2) 0.032(2) -0.0069(17) 0.0040(17) -0.0105(18) B2 0.031(2) 0.025(2) 0.030(2) -0.0101(18) 0.0004(19) -0.0040(18) Cl1 0.0745(11) 0.0570(9) 0.0660(11) -0.0034(8) -0.0059(8) -0.0257(8) Cl2 0.0632(11) 0.0838(12) 0.0820(13) -0.0262(9) 0.0176(9) -0.0200(9) C1S 0.045(3) 0.046(3) 0.046(3) 0.008(2) -0.011(3) -0.014(2) C2S 0.046(4) 0.052(3) 0.053(4) 0.000(3) -0.020(3) -0.008(3) C3S 0.047(4) 0.055(4) 0.057(4) -0.003(3) -0.007(3) -0.029(3) C4S 0.056(4) 0.060(4) 0.045(3) -0.004(3) -0.007(3) -0.013(3) C5S 0.043(4) 0.069(4) 0.055(4) -0.002(3) -0.001(3) -0.002(3) C6S 0.046(3) 0.057(4) 0.046(3) -0.006(3) -0.013(3) 0.004(3) Cl3 0.0588(11) 0.0620(11) 0.0677(12) -0.0099(8) 0.0028(9) -0.0078(9) Cl4 0.107(2) 0.141(2) 0.0879(18) 0.0560(17) -0.0365(15) -0.0658(16) C7S 0.035(4) 0.079(4) 0.043(3) 0.012(3) -0.006(2) -0.008(3) C8S 0.052(5) 0.130(6) 0.039(4) 0.043(4) -0.007(3) -0.003(3) C9S 0.066(6) 0.189(9) 0.061(6) 0.044(6) 0.016(4) 0.037(5) C10S 0.128(11) 0.189(13) 0.128(11) -0.030(10) 0.046(7) 0.061(8) C11S 0.060(5) 0.090(5) 0.127(7) -0.007(4) -0.006(4) 0.057(4) C12S 0.062(5) 0.077(5) 0.067(5) -0.018(4) -0.006(3) 0.009(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 B1 O1 B2 132.8(3) C24 N1 C1 116.7(3) C1 N2 C8 113.1(3) C1 N2 B1 122.9(3) C8 N2 B1 123.5(3) C8 N3 C9 117.2(3) C16 N4 C9 112.5(3) C16 N4 B1 123.2(3) C9 N4 B1 122.9(3) C17 N5 C16 116.4(3) C17 N6 C24 113.2(3) C17 N6 B1 123.8(3) C24 N6 B1 122.2(3) C25 N7 C48 117.1(3) C32 N8 C25 112.7(3) C32 N8 B2 122.2(3) C25 N8 B2 123.5(3) C33 N9 C32 116.6(3) C40 N10 C33 113.6(3) C40 N10 B2 123.4(3) C33 N10 B2 122.8(3) C40 N11 C41 117.2(3) C48 N12 C41 112.0(3) C48 N12 B2 123.8(3) C41 N12 B2 122.6(3) N1 C1 N2 122.1(3) N1 C1 C2 130.6(3) N2 C1 C2 106.1(3) C3 C2 C7 120.9(3) C3 C2 C1 132.5(4) C7 C2 C1 106.7(3) C4 C3 C2 117.9(4) C4 C3 H3A 121.1 C2 C3 H3A 121.1 C3 C4 C5 121.5(4) C3 C4 H4A 119.3 C5 C4 H4A 119.3 C6 C5 C4 121.3(4) C6 C5 H5A 119.3 C4 C5 H5A 119.3 C5 C6 C7 118.2(4) C5 C6 H6A 120.9 C7 C6 H6A 120.9 C6 C7 C2 120.1(4) C6 C7 C8 132.6(4) C2 C7 C8 107.3(3) N3 C8 N2 122.0(3) N3 C8 C7 131.7(3) N2 C8 C7 105.1(3) N3 C9 N4 122.8(3) N3 C9 C10 129.5(3) N4 C9 C10 106.0(3) C11 C10 C15 120.7(4) C11 C10 C9 131.7(4) C15 C10 C9 107.3(3) C12 C11 C10 117.7(4) C12 C11 H11A 121.2 C10 C11 H11A 121.2 C11 C12 C13 121.7(4) C11 C12 H12A 119.1 C13 C12 H12A 119.1 C14 C13 C12 121.5(4) C14 C13 H13A 119.3 C12 C13 H13A 119.3 C13 C14 C15 118.0(4) C13 C14 H14A 121.0 C15 C14 H14A 121.0 C14 C15 C10 120.4(3) C14 C15 C16 132.4(4) C10 C15 C16 106.9(3) N5 C16 N4 122.5(3) N5 C16 C15 129.0(3) N4 C16 C15 106.2(3) N5 C17 N6 122.8(3) N5 C17 C18 129.5(3) N6 C17 C18 105.8(3) C19 C18 C23 120.9(3) C19 C18 C17 131.3(4) C23 C18 C17 107.5(3) C20 C19 C18 117.3(4) C20 C19 H19A 121.3 C18 C19 H19A 121.3 C19 C20 C21 121.6(4) C19 C20 H20A 119.2 C21 C20 H20A 119.2 C22 C21 C20 122.2(4) C22 C21 H21A 118.9 C20 C21 H21A 118.9 C21 C22 C23 117.0(4) C21 C22 H22A 121.5 C23 C22 H22A 121.5 C22 C23 C18 120.9(4) C22 C23 C24 131.8(4) C18 C23 C24 106.9(3) N1 C24 N6 123.2(3) N1 C24 C23 129.6(3) N6 C24 C23 105.5(3) N7 C25 N8 122.9(3) N7 C25 C26 129.5(3) N8 C25 C26 105.6(3) C27 C26 C31 120.9(4) C27 C26 C25 131.7(4) C31 C26 C25 107.1(3) C28 C27 C26 117.6(4) C28 C27 H27A 121.2 C26 C27 H27A 121.2 C27 C28 C29 121.8(4) C27 C28 H28A 119.1 C29 C28 H28A 119.1 C30 C29 C28 121.3(4) C30 C29 H29A 119.3 C28 C29 H29A 119.3 C29 C30 C31 118.0(4) C29 C30 H30A 121.0 C31 C30 H30A 121.0 C30 C31 C26 120.5(4) C30 C31 C32 131.7(4) C26 C31 C32 107.6(3) N9 C32 N8 123.0(3) N9 C32 C31 129.4(3) N8 C32 C31 105.7(3) N9 C33 N10 122.3(3) N9 C33 C34 131.1(3) N10 C33 C34 105.5(3) C35 C34 C39 120.7(3) C35 C34 C33 132.3(3) C39 C34 C33 107.0(3) C36 C35 C34 117.7(4) C36 C35 H35A 121.1 C34 C35 H35A 121.1 C35 C36 C37 121.5(4) C35 C36 H36A 119.2 C37 C36 H36A 119.2 C38 C37 C36 121.6(4) C38 C37 H37A 119.2 C36 C37 H37A 119.2 C39 C38 C37 117.5(4) C39 C38 H38A 121.2 C37 C38 H38A 121.2 C38 C39 C34 120.8(3) C38 C39 C40 132.2(3) C34 C39 C40 106.9(3) N11 C40 N10 122.0(3) N11 C40 C39 131.3(3) N10 C40 C39 105.6(3) N11 C41 N12 122.4(3) N11 C41 C42 129.9(3) N12 C41 C42 106.1(3) C43 C42 C47 120.6(4) C43 C42 C41 131.9(4) C47 C42 C41 107.2(3) C44 C43 C42 118.4(4) C44 C43 H43A 120.8 C42 C43 H43A 120.8 C43 C44 C45 121.3(4) C43 C44 H44A 119.4 C45 C44 H44A 119.4 C46 C45 C44 121.2(4) C46 C45 H45A 119.4 C44 C45 H45A 119.4 C45 C46 C47 117.9(4) C45 C46 H46A 121.1 C47 C46 H46A 121.1 C46 C47 C42 120.6(4) C46 C47 C48 131.9(4) C42 C47 C48 107.1(3) N7 C48 N12 122.4(3) N7 C48 C47 129.1(3) N12 C48 C47 106.3(3) O1 B1 N6 114.0(3) O1 B1 N2 117.0(3) N6 B1 N2 102.9(3) O1 B1 N4 116.0(3) N6 B1 N4 102.4(3) N2 B1 N4 102.6(3) O1 B2 N10 111.0(3) O1 B2 N8 118.4(3) N10 B2 N8 102.8(3) O1 B2 N12 117.3(3) N10 B2 N12 102.4(3) N8 B2 N12 102.9(3) C2S C1S C6S 120.0 C2S C1S Cl1 121.4(2) C6S C1S Cl1 118.6(2) C1S C2S C3S 120.0 C1S C2S Cl2 121.2(2) C3S C2S Cl2 118.8(2) C4S C3S C2S 120.0 C4S C3S H3S 120.0 C2S C3S H3S 120.0 C5S C4S C3S 120.0 C5S C4S H4S 120.0 C3S C4S H4S 120.0 C4S C5S C6S 120.0 C4S C5S H5S 120.0 C6S C5S H5S 120.0 C5S C6S C1S 120.0 C5S C6S H6S 120.0 C1S C6S H6S 120.0 C6B C1B C2B 119.8(8) C6B C1B Cl1B 119.5(8) C2B C1B Cl1B 120.0(7) C3B C2B C1B 120.1(7) C3B C2B Cl2B 119.6(7) C1B C2B Cl2B 120.1(7) C2B C3B C4B 119.4(8) C2B C3B H3B 120.3 C4B C3B H3B 120.3 C3B C4B C5B 119.5(8) C3B C4B H4B 120.2 C5B C4B H4B 120.2 C6B C5B C4B 119.5(9) C6B C5B H5B 120.2 C4B C5B H5B 120.2 C1B C6B C5B 119.2(8) C1B C6B H6B 120.4 C5B C6B H6B 120.4 C8S C7S C12S 120.0 C8S C7S Cl3 122.2(3) C12S C7S Cl3 117.8(3) C9S C8S C7S 120.0 C9S C8S Cl4 119.0(3) C7S C8S Cl4 120.9(3) C8S C9S C10S 120.0 C8S C9S H9S 120.0 C10S C9S H9S 120.0 C11S C10S C9S 120.0 C11S C10S H10S 120.0 C9S C10S H10S 120.0 C10S C11S C12S 120.0 C10S C11S H11S 120.0 C12S C11S H11S 120.0 C11S C12S C7S 120.0 C11S C12S H12S 120.0 C7S C12S H12S 120.0 C12A C7A C8A 119.5(7) C12A C7A Cl3A 118.6(7) C8A C7A Cl3A 120.7(7) C9A C8A C7A 120.1(5) C9A C8A Cl4A 120.5(6) C7A C8A Cl4A 119.4(6) C8A C9A C10A 119.4(7) C8A C9A H9A 120.3 C10A C9A H9A 120.3 C9A C10A C11A 119.0(7) C9A C10A H10A 120.5 C11A C10A H10A 120.5 C10A C11A C12A 119.8(7) C10A C11A H11B 120.1 C12A C11A H11B 120.1 C7A C12A C11A 119.5(6) C7A C12A H12B 120.3 C11A C12A H12B 120.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 B1 1.411(5) O1 B2 1.411(5) N1 C24 1.343(5) N1 C1 1.355(4) N2 C1 1.357(5) N2 C8 1.365(4) N2 B1 1.510(5) N3 C8 1.341(5) N3 C9 1.347(5) N4 C16 1.364(4) N4 C9 1.370(4) N4 B1 1.513(5) N5 C17 1.350(5) N5 C16 1.352(4) N6 C17 1.350(4) N6 C24 1.365(4) N6 B1 1.501(5) N7 C25 1.336(5) N7 C48 1.346(5) N8 C32 1.366(5) N8 C25 1.374(5) N8 B2 1.504(5) N9 C33 1.341(5) N9 C32 1.349(5) N10 C40 1.360(4) N10 C33 1.361(5) N10 B2 1.504(5) N11 C40 1.337(5) N11 C41 1.347(5) N12 C48 1.368(5) N12 C41 1.376(5) N12 B2 1.508(5) C1 C2 1.449(5) C2 C3 1.388(5) C2 C7 1.424(5) C3 C4 1.377(6) C3 H3A 0.9500 C4 C5 1.394(6) C4 H4A 0.9500 C5 C6 1.382(6) C5 H5A 0.9500 C6 C7 1.388(5) C6 H6A 0.9500 C7 C8 1.453(5) C9 C10 1.451(5) C10 C11 1.395(5) C10 C15 1.420(5) C11 C12 1.382(6) C11 H11A 0.9500 C12 C13 1.388(6) C12 H12A 0.9500 C13 C14 1.383(6) C13 H13A 0.9500 C14 C15 1.393(5) C14 H14A 0.9500 C15 C16 1.453(5) C17 C18 1.454(5) C18 C19 1.403(5) C18 C23 1.406(5) C19 C20 1.378(6) C19 H19A 0.9500 C20 C21 1.390(6) C20 H20A 0.9500 C21 C22 1.381(6) C21 H21A 0.9500 C22 C23 1.404(5) C22 H22A 0.9500 C23 C24 1.457(5) C25 C26 1.458(5) C26 C27 1.392(5) C26 C31 1.412(5) C27 C28 1.384(6) C27 H27A 0.9500 C28 C29 1.391(6) C28 H28A 0.9500 C29 C30 1.380(6) C29 H29A 0.9500 C30 C31 1.400(5) C30 H30A 0.9500 C31 C32 1.457(5) C33 C34 1.462(5) C34 C35 1.389(5) C34 C39 1.426(5) C35 C36 1.388(6) C35 H35A 0.9500 C36 C37 1.394(6) C36 H36A 0.9500 C37 C38 1.391(6) C37 H37A 0.9500 C38 C39 1.389(5) C38 H38A 0.9500 C39 C40 1.461(5) C41 C42 1.454(5) C42 C43 1.385(5) C42 C47 1.418(5) C43 C44 1.373(6) C43 H43A 0.9500 C44 C45 1.407(6) C44 H44A 0.9500 C45 C46 1.378(6) C45 H45A 0.9500 C46 C47 1.397(5) C46 H46A 0.9500 C47 C48 1.458(5) Cl1 C1S 1.721(3) Cl2 C2S 1.711(3) C1S C2S 1.3900 C1S C6S 1.3900 C2S C3S 1.3900 C3S C4S 1.3900 C3S H3S 0.9500 C4S C5S 1.3900 C4S H4S 0.9500 C5S C6S 1.3900 C5S H5S 0.9500 C6S H6S 0.9500 Cl1B C1B 1.720(6) Cl2B C2B 1.710(6) C1B C6B 1.390(5) C1B C2B 1.392(5) C2B C3B 1.389(5) C3B C4B 1.392(5) C3B H3B 0.9500 C4B C5B 1.393(5) C4B H4B 0.9500 C5B C6B 1.391(5) C5B H5B 0.9500 C6B H6B 0.9500 Cl3 C7S 1.713(4) Cl4 C8S 1.689(5) C7S C8S 1.3900 C7S C12S 1.3900 C8S C9S 1.3900 C9S C10S 1.3900 C9S H9S 0.9500 C10S C11S 1.3900 C10S H10S 0.9500 C11S C12S 1.3900 C11S H11S 0.9500 C12S H12S 0.9500 Cl3A C7A 1.712(6) Cl4A C8A 1.685(6) C7A C12A 1.389(5) C7A C8A 1.395(5) C8A C9A 1.387(5) C9A C10A 1.391(5) C9A H9A 0.9500 C10A C11A 1.392(5) C10A H10A 0.9500 C11A C12A 1.393(5) C11A H11B 0.9500 C12A H12B 0.9500