# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_I _chemical_name_common 'CrOTi Falzone' _chemical_name_systematic ? _chemical_formula_iupac ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H77 B2 Cl4 Cr F48 N6 O4 Ti' _chemical_formula_weight 2782.14 _chemical_melting_point ? 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' 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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4112(3) _cell_length_b 18.3529(5) _cell_length_c 46.9774(11) _cell_angle_alpha 90 _cell_angle_beta 90.4300(10) _cell_angle_gamma 90 _cell_volume 11562.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9785 _cell_measurement_temperature 110.(2) _cell_measurement_theta_max 26.1805 _cell_measurement_theta_min 2.2194 _exptl_absorpt_coefficient_mu 0.389 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_crystal_colour pink-orange _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description rod _exptl_crystal_F_000 5588 _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.100 _exptl_special_details ; ; _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 53 _diffrn_reflns_limit_l_min -59 _diffrn_reflns_number 139961 _diffrn_reflns_theta_full 26.56 _diffrn_reflns_theta_max 26.56 _diffrn_reflns_theta_min 1.19 _diffrn_ambient_temperature 110.(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _diffrn_measurement_device_type 'Bruker-Nonius X8 Kappa APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type ? _reflns_number_gt 19058 _reflns_number_total 23703 _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.27B (Bruker AXS Inc., 2012)' _computing_data_collection 'Bruker Instrument Service v2012.12.0.3' _computing_data_reduction 'SAINT V8.27B (Bruker AXS Inc., 2012)' _computing_molecular_graphics ? _computing_publication_material ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.692 _refine_diff_density_min -1.725 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1684 _refine_ls_number_reflns 23703 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0858 _refine_ls_R_factor_gt 0.0691 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0904P)^2^+36.2499P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1800 _refine_ls_wR_factor_ref 0.1920 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr1 0.22346(4) 0.31074(3) 0.38300(2) 0.01401(12) Uani d . . . 1.0 . . Ti Ti1 0.40716(4) 0.26836(3) 0.43692(2) 0.01602(13) Uani d . . . 1.0 . . O O1 0.32823(17) 0.28950(12) 0.40745(5) 0.0180(5) Uani d . . . 1.0 . . O O2 0.33145(18) 0.19793(13) 0.45452(5) 0.0205(5) Uani d . . . 1.0 . . O O3 0.51584(18) 0.23175(13) 0.41757(5) 0.0211(5) Uani d . . . 1.0 . . O O4 0.40731(19) 0.36093(13) 0.45330(5) 0.0250(5) Uani d . . . 1.0 . . N N1 0.1043(2) 0.33539(15) 0.35620(6) 0.0169(5) Uani d . . . 1.0 . . N N2 0.3066(2) 0.29461(15) 0.34658(6) 0.0182(6) Uani d . . . 1.0 . . N N3 0.2744(2) 0.41599(15) 0.37780(6) 0.0178(6) Uani d . . . 1.0 . . N N4 0.1249(2) 0.32834(15) 0.41645(6) 0.0190(6) Uani d . . . 1.0 . . N N5 0.1685(2) 0.20500(15) 0.38668(6) 0.0181(6) Uani d . . . 1.0 . . N N6 0.5101(2) 0.25391(16) 0.47735(6) 0.0203(6) Uani d . . . 1.0 . . C C1 0.1173(2) 0.37998(18) 0.33360(7) 0.0178(6) Uani d . . . 1.0 . . C C2 0.0373(3) 0.40191(19) 0.31693(8) 0.0227(7) Uani d . . . 1.0 . . H H2 0.0473 0.4338 0.3013 0.027 Uiso calc U . R 1.0 . . C C3 -0.0569(3) 0.37720(19) 0.32317(8) 0.0232(7) Uani d . . . 1.0 . . H H3 -0.1124 0.392 0.3119 0.028 Uiso calc U . R 1.0 . . C C4 -0.0701(3) 0.33091(19) 0.34584(8) 0.0225(7) Uani d . . . 1.0 . . H H4 -0.1346 0.313 0.3502 0.027 Uiso calc U . R 1.0 . . C C5 0.0117(2) 0.31056(18) 0.36229(7) 0.0185(7) Uani d . . . 1.0 . . C C6 0.2242(3) 0.40516(19) 0.32721(7) 0.0207(7) Uani d . . . 1.0 . . C C7 0.2245(3) 0.4512(2) 0.29989(8) 0.0301(8) Uani d . . . 1.0 . . H H7A 0.1832 0.4947 0.3026 0.045 Uiso calc U . R 1.0 . . H H7B 0.1975 0.4224 0.2841 0.045 Uiso calc U . R 1.0 . . H H7C 0.293 0.4659 0.2956 0.045 Uiso calc U . R 1.0 . . C C8 0.2929(2) 0.33810(19) 0.32359(7) 0.0197(7) Uani d . . . 1.0 . . C C9 0.3426(3) 0.3234(2) 0.29823(8) 0.0267(8) Uani d . . . 1.0 . . H H9 0.3329 0.354 0.2821 0.032 Uiso calc U . R 1.0 . . C C10 0.4059(3) 0.2641(2) 0.29668(8) 0.0306(9) Uani d . . . 1.0 . . H H10 0.4373 0.2522 0.2792 0.037 Uiso calc U . R 1.0 . . C C11 0.4229(3) 0.2224(2) 0.32058(8) 0.0299(8) Uani d . . . 1.0 . . H H11 0.4682 0.1826 0.3202 0.036 Uiso calc U . R 1.0 . . C C12 0.3725(3) 0.2400(2) 0.34513(8) 0.0242(7) Uani d . . . 1.0 . . H H12 0.3852 0.2121 0.3618 0.029 Uiso calc U . R 1.0 . . C C13 0.2654(2) 0.45021(19) 0.35228(8) 0.0207(7) Uani d . . . 1.0 . . C C14 0.2982(3) 0.5216(2) 0.34913(9) 0.0288(8) Uani d . . . 1.0 . . H H14 0.2903 0.5458 0.3314 0.035 Uiso calc U . R 1.0 . . C C15 0.3424(3) 0.5572(2) 0.37187(9) 0.0313(9) Uani d . . . 1.0 . . H H15 0.363 0.6065 0.37 0.038 Uiso calc U . R 1.0 . . C C16 0.3563(3) 0.5208(2) 0.39715(9) 0.0262(8) Uani d . . . 1.0 . . H H16 0.3891 0.5437 0.4127 0.031 Uiso calc U . R 1.0 . . C C17 0.3217(3) 0.45015(18) 0.39943(8) 0.0211(7) Uani d . . . 1.0 . . H H17 0.3316 0.4248 0.4168 0.025 Uiso calc U . R 1.0 . . C C18 0.0001(2) 0.26000(19) 0.38809(7) 0.0208(7) Uani d . . . 1.0 . . C C19 -0.1090(3) 0.2348(2) 0.39023(9) 0.0315(9) Uani d . . . 1.0 . . H H19A -0.1519 0.277 0.3937 0.047 Uiso calc U . R 1.0 . . H H19B -0.1154 0.2001 0.406 0.047 Uiso calc U . R 1.0 . . H H19C -0.1291 0.2112 0.3724 0.047 Uiso calc U . R 1.0 . . C C20 0.0311(3) 0.30169(19) 0.41524(7) 0.0228(7) Uani d . . . 1.0 . . C C21 -0.0326(3) 0.3086(2) 0.43832(9) 0.0346(9) Uani d . . . 1.0 . . H H21 -0.0981 0.289 0.4374 0.042 Uiso calc U . R 1.0 . . C C22 0.0004(3) 0.3443(3) 0.46264(9) 0.0415(11) Uani d . . . 1.0 . . H H22 -0.0428 0.3499 0.4784 0.05 Uiso calc U . R 1.0 . . C C23 0.0954(3) 0.3713(2) 0.46382(8) 0.0340(9) Uani d . . . 1.0 . . H H23 0.119 0.3963 0.4803 0.041 Uiso calc U . R 1.0 . . C C24 0.1561(3) 0.36159(19) 0.44056(7) 0.0241(7) Uani d . . . 1.0 . . H H24 0.2227 0.379 0.4415 0.029 Uiso calc U . R 1.0 . . C C25 0.0689(3) 0.19272(19) 0.38593(7) 0.0204(7) Uani d . . . 1.0 . . C C26 0.0325(3) 0.1217(2) 0.38598(8) 0.0279(8) Uani d . . . 1.0 . . H H26 -0.0372 0.1132 0.3844 0.033 Uiso calc U . R 1.0 . . C C27 0.0974(3) 0.0638(2) 0.38825(8) 0.0308(9) Uani d . . . 1.0 . . H H27 0.0729 0.0153 0.3879 0.037 Uiso calc U . R 1.0 . . C C28 0.1975(3) 0.0768(2) 0.39103(8) 0.0293(8) Uani d . . . 1.0 . . H H28 0.2432 0.0378 0.3936 0.035 Uiso calc U . R 1.0 . . C C29 0.2304(3) 0.14808(19) 0.39000(7) 0.0233(7) Uani d . . . 1.0 . . H H29 0.2999 0.1572 0.3917 0.028 Uiso calc U . R 1.0 . . C C30 0.3144(3) 0.17425(17) 0.48140(7) 0.0186(7) Uani d . . . 1.0 . . C C31 0.3929(3) 0.16787(18) 0.50098(7) 0.0203(7) Uani d . . . 1.0 . . C C32 0.3720(3) 0.1469(2) 0.52871(8) 0.0256(8) Uani d . . . 1.0 . . H H32 0.4251 0.1437 0.5422 0.031 Uiso calc U . R 1.0 . . C C33 0.2754(3) 0.1305(2) 0.53733(7) 0.0252(8) Uani d . . . 1.0 . . C C34 0.1995(3) 0.13545(19) 0.51721(7) 0.0234(7) Uani d . . . 1.0 . . H H34 0.1334 0.1235 0.5227 0.028 Uiso calc U . R 1.0 . . C C35 0.2168(3) 0.15731(18) 0.48920(7) 0.0201(7) Uani d . . . 1.0 . . C C36 0.4984(3) 0.18242(19) 0.49175(8) 0.0230(7) Uani d . . . 1.0 . . H H36A 0.5429 0.1809 0.5087 0.028 Uiso calc U . R 1.0 . . H H36B 0.5196 0.1433 0.4786 0.028 Uiso calc U . R 1.0 . . C C37 0.2545(3) 0.1089(3) 0.56765(8) 0.0377(10) Uani d . . . 1.0 . . H H37A 0.1822 0.1058 0.5704 0.057 Uiso calc U . R 1.0 . . H H37B 0.2826 0.1454 0.5806 0.057 Uiso calc U . R 1.0 . . H H37C 0.2848 0.0614 0.5716 0.057 Uiso calc U . R 1.0 . . C C38 0.1338(3) 0.1625(2) 0.46756(8) 0.0261(8) Uani d . . . 1.0 . . H H38A 0.1374 0.2096 0.4578 0.039 Uiso calc U . R 1.0 . . H H38B 0.0694 0.1582 0.4772 0.039 Uiso calc U . R 1.0 . . H H38C 0.1404 0.1231 0.4536 0.039 Uiso calc U . R 1.0 . . C C39 0.5989(2) 0.19265(19) 0.42367(7) 0.0199(7) Uani d . . . 1.0 . . C C40 0.6522(3) 0.20518(19) 0.44894(8) 0.0221(7) Uani d . . . 1.0 . . C C41 0.7371(3) 0.1641(2) 0.45466(8) 0.0245(7) Uani d . . . 1.0 . . H H41 0.7737 0.1727 0.4717 0.029 Uiso calc U . R 1.0 . . C C42 0.7694(3) 0.1107(2) 0.43592(8) 0.0249(8) Uani d . . . 1.0 . . C C43 0.7153(3) 0.09893(19) 0.41100(7) 0.0214(7) Uani d . . . 1.0 . . H H43 0.7371 0.0625 0.3981 0.026 Uiso calc U . R 1.0 . . C C44 0.6296(3) 0.13912(19) 0.40438(7) 0.0204(7) Uani d . . . 1.0 . . C C45 0.6165(3) 0.2635(2) 0.46897(8) 0.0256(8) Uani d . . . 1.0 . . H H45A 0.6588 0.2631 0.4863 0.031 Uiso calc U . R 1.0 . . H H45B 0.6243 0.3117 0.4597 0.031 Uiso calc U . R 1.0 . . C C46 0.8617(3) 0.0656(2) 0.44228(9) 0.0318(9) Uani d . . . 1.0 . . H H46A 0.8469 0.0303 0.4573 0.048 Uiso calc U . R 1.0 . . H H46B 0.9159 0.0977 0.4486 0.048 Uiso calc U . R 1.0 . . H H46C 0.8819 0.0396 0.425 0.048 Uiso calc U . R 1.0 . . C C47 0.5698(3) 0.1253(2) 0.37775(7) 0.0246(7) Uani d . . . 1.0 . . H H47A 0.5702 0.1691 0.3658 0.037 Uiso calc U . R 1.0 . . H H47B 0.501 0.1133 0.3828 0.037 Uiso calc U . R 1.0 . . H H47C 0.5992 0.0845 0.3673 0.037 Uiso calc U . R 1.0 . . C C48 0.4600(3) 0.3816(2) 0.47843(8) 0.0274(8) Uani d . . . 1.0 . . H H48A 0.4205 0.4175 0.4893 0.033 Uiso calc U . R 1.0 . . H H48B 0.5243 0.4044 0.4733 0.033 Uiso calc U . R 1.0 . . C C49 0.4784(3) 0.3145(2) 0.49632(8) 0.0263(8) Uani d . . . 1.0 . . H H49A 0.531 0.3245 0.5107 0.032 Uiso calc U . R 1.0 . . H H49B 0.4166 0.3008 0.5064 0.032 Uiso calc U . R 1.0 . . 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 Cr1 0.0148(3) 0.0122(2) 0.0151(2) -0.00194(19) -0.00188(19) 0.00047(18) Ti1 0.0171(3) 0.0138(3) 0.0172(3) -0.0014(2) -0.0032(2) -0.0013(2) O1 0.0184(12) 0.0158(11) 0.0199(11) -0.0014(9) -0.0025(9) 0.0001(9) O2 0.0226(12) 0.0223(12) 0.0166(11) -0.0050(10) -0.0031(9) 0.0009(9) O3 0.0191(12) 0.0212(12) 0.0229(12) 0.0023(9) -0.0014(10) 0.0021(9) O4 0.0311(14) 0.0175(12) 0.0262(13) 0.0005(10) -0.0093(11) -0.0061(10) N1 0.0180(14) 0.0141(13) 0.0186(13) -0.0022(10) -0.0011(11) 0.0009(10) N2 0.0169(14) 0.0195(14) 0.0183(13) -0.0041(11) -0.0007(11) 0.0005(11) N3 0.0165(14) 0.0145(13) 0.0226(14) -0.0021(11) -0.0017(11) 0.0008(11) N4 0.0222(15) 0.0148(13) 0.0199(13) 0.0002(11) -0.0006(11) 0.0023(11) N5 0.0224(15) 0.0155(13) 0.0164(13) -0.0029(11) -0.0023(11) 0.0006(10) N6 0.0205(15) 0.0195(14) 0.0208(14) -0.0030(11) -0.0045(11) -0.0036(11) C1 0.0189(17) 0.0161(16) 0.0184(15) -0.0011(13) -0.0015(13) -0.0004(12) C2 0.0249(18) 0.0177(17) 0.0256(17) -0.0012(14) -0.0041(14) 0.0035(13) C3 0.0203(18) 0.0224(17) 0.0269(18) 0.0040(14) -0.0083(14) -0.0014(14) C4 0.0151(16) 0.0233(18) 0.0290(18) -0.0003(13) -0.0012(14) -0.0014(14) C5 0.0166(16) 0.0176(16) 0.0212(16) -0.0018(12) -0.0007(13) -0.0015(13) C6 0.0207(17) 0.0199(17) 0.0216(16) -0.0055(13) -0.0023(13) 0.0065(13) C7 0.030(2) 0.031(2) 0.0293(19) -0.0081(16) -0.0050(16) 0.0141(16) C8 0.0133(16) 0.0252(17) 0.0205(16) -0.0079(13) -0.0022(13) 0.0015(13) C9 0.0202(18) 0.040(2) 0.0194(16) -0.0095(16) -0.0017(14) 0.0020(15) C10 0.0234(19) 0.048(2) 0.0202(17) -0.0050(17) 0.0035(15) -0.0076(16) C11 0.0252(19) 0.036(2) 0.0283(19) 0.0032(16) 0.0007(15) -0.0086(16) C12 0.0227(18) 0.0280(19) 0.0219(17) 0.0011(14) -0.0021(14) -0.0023(14) C13 0.0153(16) 0.0184(17) 0.0283(18) -0.0035(13) -0.0025(14) 0.0054(13) C14 0.0246(19) 0.0214(18) 0.040(2) -0.0040(15) -0.0045(16) 0.0108(16) C15 0.029(2) 0.0154(17) 0.050(2) -0.0048(15) -0.0022(18) 0.0000(16) C16 0.0211(18) 0.0181(17) 0.039(2) -0.0028(14) -0.0052(15) -0.0065(15) C17 0.0199(17) 0.0175(16) 0.0259(17) -0.0008(13) -0.0037(14) -0.0024(13) C18 0.0160(17) 0.0228(17) 0.0236(17) -0.0037(13) 0.0008(13) 0.0041(13) C19 0.0210(19) 0.037(2) 0.036(2) -0.0082(16) 0.0003(16) 0.0073(17) C20 0.0238(18) 0.0215(17) 0.0230(17) 0.0019(14) 0.0010(14) 0.0033(14) C21 0.028(2) 0.043(2) 0.032(2) -0.0014(17) 0.0092(17) -0.0003(18) C22 0.042(3) 0.051(3) 0.031(2) 0.006(2) 0.0152(19) -0.0062(19) C23 0.045(2) 0.034(2) 0.0239(18) 0.0024(18) 0.0046(17) -0.0078(16) C24 0.0294(19) 0.0212(17) 0.0216(17) 0.0007(14) -0.0011(14) -0.0013(13) C25 0.0217(17) 0.0206(17) 0.0188(15) -0.0053(13) -0.0016(13) 0.0030(13) C26 0.028(2) 0.0276(19) 0.0277(18) -0.0129(16) -0.0049(15) 0.0035(15) C27 0.046(2) 0.0175(18) 0.0293(19) -0.0100(16) -0.0040(17) 0.0017(14) C28 0.042(2) 0.0170(17) 0.0284(18) 0.0010(16) -0.0029(16) -0.0007(14) C29 0.0289(19) 0.0186(17) 0.0222(16) -0.0006(14) -0.0018(14) 0.0005(13) C30 0.0247(18) 0.0133(15) 0.0177(15) -0.0017(13) -0.0012(13) 0.0000(12) C31 0.0229(18) 0.0168(16) 0.0210(16) 0.0026(13) -0.0020(13) 0.0001(13) C32 0.033(2) 0.0230(18) 0.0204(17) 0.0016(15) -0.0057(15) 0.0022(14) C33 0.033(2) 0.0237(18) 0.0189(16) -0.0009(15) -0.0020(15) 0.0017(14) C34 0.0259(19) 0.0199(17) 0.0245(17) -0.0011(14) 0.0048(14) 0.0008(14) C35 0.0238(18) 0.0156(16) 0.0209(16) -0.0002(13) -0.0021(14) -0.0005(13) C36 0.0243(18) 0.0213(17) 0.0233(17) 0.0013(14) -0.0057(14) -0.0005(14) C37 0.042(2) 0.048(3) 0.0226(19) -0.006(2) -0.0007(17) 0.0076(18) C38 0.0231(19) 0.0291(19) 0.0262(18) -0.0076(15) -0.0030(15) 0.0068(15) C39 0.0159(16) 0.0195(16) 0.0243(17) -0.0021(13) 0.0010(13) 0.0056(13) C40 0.0159(16) 0.0239(18) 0.0265(17) -0.0058(13) 0.0010(14) 0.0025(14) C41 0.0156(17) 0.0302(19) 0.0277(18) -0.0054(14) -0.0038(14) 0.0044(15) C42 0.0172(17) 0.0284(19) 0.0293(18) -0.0008(14) 0.0030(14) 0.0093(15) C43 0.0172(17) 0.0199(17) 0.0271(17) -0.0022(13) 0.0061(14) 0.0051(14) C44 0.0188(17) 0.0209(17) 0.0215(16) -0.0017(13) 0.0026(13) 0.0062(13) C45 0.0209(18) 0.0256(19) 0.0303(19) -0.0060(14) -0.0071(15) -0.0025(15) C46 0.0202(19) 0.039(2) 0.036(2) 0.0047(16) -0.0018(16) 0.0059(17) C47 0.0259(19) 0.0269(19) 0.0210(17) 0.0070(15) 0.0005(14) 0.0027(14) C48 0.034(2) 0.0199(18) 0.0278(18) -0.0025(15) -0.0083(16) -0.0085(14) C49 0.029(2) 0.0265(19) 0.0235(17) -0.0026(15) -0.0069(15) -0.0083(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cr1 O1 . 1.850(2) ? Cr1 N1 . 2.076(3) ? Cr1 N2 . 2.070(3) ? Cr1 N3 . 2.064(3) ? Cr1 N4 . 2.086(3) ? Cr1 N5 . 2.084(3) ? Ti1 O1 . 1.779(2) ? Ti1 O2 . 1.843(2) ? Ti1 O3 . 1.850(2) ? Ti1 O4 . 1.865(2) ? Ti1 N6 . 2.355(3) ? O2 C30 . 1.356(4) ? O3 C39 . 1.354(4) ? O4 C48 . 1.423(4) ? N1 C1 . 1.353(4) ? N1 C5 . 1.356(4) ? N2 C8 . 1.354(4) ? N2 C12 . 1.339(5) ? N3 C13 . 1.358(4) ? N3 C17 . 1.349(4) ? N4 C20 . 1.351(5) ? N4 C24 . 1.350(5) ? N5 C25 . 1.355(5) ? N5 C29 . 1.343(5) ? N6 C36 . 1.485(4) ? N6 C45 . 1.493(5) ? N6 C49 . 1.490(4) ? C1 C2 . 1.383(5) ? C1 C6 . 1.538(5) ? C2 H2 . 0.95 ? C2 C3 . 1.376(5) ? C3 H3 . 0.95 ? C3 C4 . 1.375(5) ? C4 H4 . 0.95 ? C4 C5 . 1.388(5) ? C5 C18 . 1.535(5) ? C6 C7 . 1.536(5) ? C6 C8 . 1.548(5) ? C6 C13 . 1.538(5) ? C7 H7A . 0.98 ? C7 H7B . 0.98 ? C7 H7C . 0.98 ? C8 C9 . 1.396(5) ? C9 H9 . 0.95 ? C9 C10 . 1.382(6) ? C10 H10 . 0.95 ? C10 C11 . 1.377(6) ? C11 H11 . 0.95 ? C11 C12 . 1.380(5) ? C12 H12 . 0.95 ? C13 C14 . 1.389(5) ? C14 H14 . 0.95 ? C14 C15 . 1.382(6) ? C15 H15 . 0.95 ? C15 C16 . 1.374(6) ? C16 H16 . 0.95 ? C16 C17 . 1.381(5) ? C17 H17 . 0.95 ? C18 C19 . 1.538(5) ? C18 C20 . 1.542(5) ? C18 C25 . 1.546(5) ? C19 H19A . 0.98 ? C19 H19B . 0.98 ? C19 H19C . 0.98 ? C20 C21 . 1.391(5) ? C21 H21 . 0.95 ? C21 C22 . 1.386(6) ? C22 H22 . 0.95 ? C22 C23 . 1.368(7) ? C23 H23 . 0.95 ? C23 C24 . 1.379(5) ? C24 H24 . 0.95 ? C25 C26 . 1.391(5) ? C26 H26 . 0.95 ? C26 C27 . 1.378(6) ? C27 H27 . 0.95 ? C27 C28 . 1.369(6) ? C28 H28 . 0.95 ? C28 C29 . 1.381(5) ? C29 H29 . 0.95 ? C30 C31 . 1.398(5) ? C30 C35 . 1.397(5) ? C31 C32 . 1.389(5) ? C31 C36 . 1.507(5) ? C32 H32 . 0.95 ? C32 C33 . 1.393(5) ? C33 C34 . 1.387(5) ? C33 C37 . 1.507(5) ? C34 H34 . 0.95 ? C34 C35 . 1.397(5) ? C35 C38 . 1.505(5) ? C36 H36A . 0.99 ? C36 H36B . 0.99 ? C37 H37A . 0.98 ? C37 H37B . 0.98 ? C37 H37C . 0.98 ? C38 H38A . 0.98 ? C38 H38B . 0.98 ? C38 H38C . 0.98 ? C39 C40 . 1.400(5) ? C39 C44 . 1.401(5) ? C40 C41 . 1.390(5) ? C40 C45 . 1.506(5) ? C41 H41 . 0.95 ? C41 C42 . 1.388(5) ? C42 C43 . 1.390(5) ? C42 C46 . 1.518(5) ? C43 H43 . 0.95 ? C43 C44 . 1.398(5) ? C44 C47 . 1.503(5) ? C45 H45A . 0.99 ? C45 H45B . 0.99 ? C46 H46A . 0.98 ? C46 H46B . 0.98 ? C46 H46C . 0.98 ? C47 H47A . 0.98 ? C47 H47B . 0.98 ? C47 H47C . 0.98 ? C48 H48A . 0.99 ? C48 H48B . 0.99 ? C48 C49 . 1.509(5) ? C49 H49A . 0.99 ? C49 H49B . 0.99 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cr1 N1 . . 178.90(11) ? O1 Cr1 N2 . . 94.13(11) ? O1 Cr1 N3 . . 91.17(11) ? O1 Cr1 N4 . . 92.71(11) ? O1 Cr1 N5 . . 91.13(11) ? N1 Cr1 N4 . . 86.23(11) ? N1 Cr1 N5 . . 88.98(11) ? N2 Cr1 N1 . . 86.94(11) ? N2 Cr1 N4 . . 173.12(11) ? N2 Cr1 N5 . . 97.38(11) ? N3 Cr1 N1 . . 88.74(11) ? N3 Cr1 N2 . . 81.69(11) ? N3 Cr1 N4 . . 98.98(11) ? N3 Cr1 N5 . . 177.57(11) ? N5 Cr1 N4 . . 81.67(11) ? O1 Ti1 O2 . . 100.11(11) ? O1 Ti1 O3 . . 99.40(11) ? O1 Ti1 O4 . . 96.96(11) ? O1 Ti1 N6 . . 173.72(11) ? O2 Ti1 O3 . . 113.86(11) ? O2 Ti1 O4 . . 116.91(11) ? O2 Ti1 N6 . . 83.16(10) ? O3 Ti1 O4 . . 122.35(12) ? O3 Ti1 N6 . . 84.02(10) ? O4 Ti1 N6 . . 76.77(11) ? Ti1 O1 Cr1 . . 166.88(14) ? C30 O2 Ti1 . . 137.7(2) ? C39 O3 Ti1 . . 137.6(2) ? C48 O4 Ti1 . . 125.7(2) ? C1 N1 Cr1 . . 120.3(2) ? C1 N1 C5 . . 119.5(3) ? C5 N1 Cr1 . . 120.1(2) ? C8 N2 Cr1 . . 120.3(2) ? C12 N2 Cr1 . . 120.6(2) ? C12 N2 C8 . . 119.1(3) ? C13 N3 Cr1 . . 120.7(2) ? C17 N3 Cr1 . . 120.0(2) ? C17 N3 C13 . . 119.2(3) ? C20 N4 Cr1 . . 120.5(2) ? C24 N4 Cr1 . . 120.5(2) ? C24 N4 C20 . . 118.8(3) ? C25 N5 Cr1 . . 120.1(2) ? C29 N5 Cr1 . . 121.0(2) ? C29 N5 C25 . . 118.8(3) ? C36 N6 Ti1 . . 113.8(2) ? C36 N6 C45 . . 109.2(3) ? C36 N6 C49 . . 110.8(3) ? C45 N6 Ti1 . . 109.3(2) ? C49 N6 Ti1 . . 103.3(2) ? C49 N6 C45 . . 110.3(3) ? N1 C1 C2 . . 121.1(3) ? N1 C1 C6 . . 117.4(3) ? C2 C1 C6 . . 121.5(3) ? C1 C2 H2 . . 120.2 ? C3 C2 C1 . . 119.5(3) ? C3 C2 H2 . . 120.2 ? C2 C3 H3 . . 120.3 ? C4 C3 C2 . . 119.5(3) ? C4 C3 H3 . . 120.3 ? C3 C4 H4 . . 120.2 ? C3 C4 C5 . . 119.5(3) ? C5 C4 H4 . . 120.2 ? N1 C5 C4 . . 120.9(3) ? N1 C5 C18 . . 117.9(3) ? C4 C5 C18 . . 121.2(3) ? C1 C6 C8 . . 109.8(3) ? C1 C6 C13 . . 110.0(3) ? C7 C6 C1 . . 109.7(3) ? C7 C6 C8 . . 109.9(3) ? C7 C6 C13 . . 109.9(3) ? C13 C6 C8 . . 107.5(3) ? C6 C7 H7A . . 109.5 ? C6 C7 H7B . . 109.5 ? C6 C7 H7C . . 109.5 ? H7A C7 H7B . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? N2 C8 C6 . . 117.3(3) ? N2 C8 C9 . . 120.3(3) ? C9 C8 C6 . . 122.4(3) ? C8 C9 H9 . . 120.2 ? C10 C9 C8 . . 119.6(3) ? C10 C9 H9 . . 120.2 ? C9 C10 H10 . . 120.2 ? C11 C10 C9 . . 119.6(3) ? C11 C10 H10 . . 120.2 ? C10 C11 H11 . . 120.9 ? C10 C11 C12 . . 118.2(4) ? C12 C11 H11 . . 120.9 ? N2 C12 C11 . . 123.1(3) ? N2 C12 H12 . . 118.5 ? C11 C12 H12 . . 118.5 ? N3 C13 C6 . . 117.1(3) ? N3 C13 C14 . . 120.3(3) ? C14 C13 C6 . . 122.5(3) ? C13 C14 H14 . . 120.1 ? C15 C14 C13 . . 119.9(4) ? C15 C14 H14 . . 120.1 ? C14 C15 H15 . . 120.3 ? C16 C15 C14 . . 119.5(3) ? C16 C15 H15 . . 120.3 ? C15 C16 H16 . . 120.7 ? C15 C16 C17 . . 118.7(3) ? C17 C16 H16 . . 120.7 ? N3 C17 C16 . . 122.3(3) ? N3 C17 H17 . . 118.9 ? C16 C17 H17 . . 118.9 ? C5 C18 C19 . . 109.6(3) ? C5 C18 C20 . . 108.9(3) ? C5 C18 C25 . . 111.5(3) ? C19 C18 C20 . . 110.2(3) ? C19 C18 C25 . . 109.4(3) ? C20 C18 C25 . . 107.0(3) ? C18 C19 H19A . . 109.5 ? C18 C19 H19B . . 109.5 ? C18 C19 H19C . . 109.5 ? H19A C19 H19B . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? N4 C20 C18 . . 117.4(3) ? N4 C20 C21 . . 120.8(3) ? C21 C20 C18 . . 121.8(3) ? C20 C21 H21 . . 120.3 ? C22 C21 C20 . . 119.4(4) ? C22 C21 H21 . . 120.3 ? C21 C22 H22 . . 120.1 ? C23 C22 C21 . . 119.7(4) ? C23 C22 H22 . . 120.1 ? C22 C23 H23 . . 120.8 ? C22 C23 C24 . . 118.4(4) ? C24 C23 H23 . . 120.8 ? N4 C24 C23 . . 122.9(4) ? N4 C24 H24 . . 118.6 ? C23 C24 H24 . . 118.6 ? N5 C25 C18 . . 117.0(3) ? N5 C25 C26 . . 120.1(3) ? C26 C25 C18 . . 122.6(3) ? C25 C26 H26 . . 120.0 ? C27 C26 C25 . . 120.1(4) ? C27 C26 H26 . . 120.0 ? C26 C27 H27 . . 120.3 ? C28 C27 C26 . . 119.4(3) ? C28 C27 H27 . . 120.3 ? C27 C28 H28 . . 120.8 ? C27 C28 C29 . . 118.4(4) ? C29 C28 H28 . . 120.8 ? N5 C29 C28 . . 122.9(4) ? N5 C29 H29 . . 118.5 ? C28 C29 H29 . . 118.5 ? O2 C30 C31 . . 120.5(3) ? O2 C30 C35 . . 118.7(3) ? C35 C30 C31 . . 120.8(3) ? C30 C31 C36 . . 120.0(3) ? C32 C31 C30 . . 119.0(3) ? C32 C31 C36 . . 121.0(3) ? C31 C32 H32 . . 119.1 ? C31 C32 C33 . . 121.8(3) ? C33 C32 H32 . . 119.1 ? C32 C33 C37 . . 120.8(3) ? C34 C33 C32 . . 117.8(3) ? C34 C33 C37 . . 121.3(4) ? C33 C34 H34 . . 118.8 ? C33 C34 C35 . . 122.3(3) ? C35 C34 H34 . . 118.8 ? C30 C35 C38 . . 119.9(3) ? C34 C35 C30 . . 118.3(3) ? C34 C35 C38 . . 121.8(3) ? N6 C36 C31 . . 113.0(3) ? N6 C36 H36A . . 109.0 ? N6 C36 H36B . . 109.0 ? C31 C36 H36A . . 109.0 ? C31 C36 H36B . . 109.0 ? H36A C36 H36B . . 107.8 ? C33 C37 H37A . . 109.5 ? C33 C37 H37B . . 109.5 ? C33 C37 H37C . . 109.5 ? H37A C37 H37B . . 109.5 ? H37A C37 H37C . . 109.5 ? H37B C37 H37C . . 109.5 ? C35 C38 H38A . . 109.5 ? C35 C38 H38B . . 109.5 ? C35 C38 H38C . . 109.5 ? H38A C38 H38B . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? O3 C39 C40 . . 120.4(3) ? O3 C39 C44 . . 118.7(3) ? C40 C39 C44 . . 120.9(3) ? C39 C40 C45 . . 118.9(3) ? C41 C40 C39 . . 119.2(3) ? C41 C40 C45 . . 121.9(3) ? C40 C41 H41 . . 119.4 ? C42 C41 C40 . . 121.2(3) ? C42 C41 H41 . . 119.4 ? C41 C42 C43 . . 118.7(3) ? C41 C42 C46 . . 121.2(3) ? C43 C42 C46 . . 120.0(3) ? C42 C43 H43 . . 119.1 ? C42 C43 C44 . . 121.9(3) ? C44 C43 H43 . . 119.1 ? C39 C44 C47 . . 119.9(3) ? C43 C44 C39 . . 118.1(3) ? C43 C44 C47 . . 121.9(3) ? N6 C45 C40 . . 112.9(3) ? N6 C45 H45A . . 109.0 ? N6 C45 H45B . . 109.0 ? C40 C45 H45A . . 109.0 ? C40 C45 H45B . . 109.0 ? H45A C45 H45B . . 107.8 ? C42 C46 H46A . . 109.5 ? C42 C46 H46B . . 109.5 ? C42 C46 H46C . . 109.5 ? H46A C46 H46B . . 109.5 ? H46A C46 H46C . . 109.5 ? H46B C46 H46C . . 109.5 ? C44 C47 H47A . . 109.5 ? C44 C47 H47B . . 109.5 ? C44 C47 H47C . . 109.5 ? H47A C47 H47B . . 109.5 ? H47A C47 H47C . . 109.5 ? H47B C47 H47C . . 109.5 ? O4 C48 H48A . . 109.9 ? O4 C48 H48B . . 109.9 ? O4 C48 C49 . . 108.8(3) ? H48A C48 H48B . . 108.3 ? C49 C48 H48A . . 109.9 ? C49 C48 H48B . . 109.9 ? N6 C49 C48 . . 108.8(3) ? N6 C49 H49A . . 109.9 ? N6 C49 H49B . . 109.9 ? C48 C49 H49A . . 109.9 ? C48 C49 H49B . . 109.9 ? H49A C49 H49B . . 108.3 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Cr1 N1 C1 C2 . . . . -174.5(2) ? Cr1 N1 C1 C6 . . . . 5.6(4) ? Cr1 N1 C5 C4 . . . . 175.2(2) ? Cr1 N1 C5 C18 . . . . -4.2(4) ? Cr1 N2 C8 C6 . . . . 7.9(4) ? Cr1 N2 C8 C9 . . . . -174.4(2) ? Cr1 N2 C12 C11 . . . . 173.6(3) ? Cr1 N3 C13 C6 . . . . -4.9(4) ? Cr1 N3 C13 C14 . . . . 178.8(3) ? Cr1 N3 C17 C16 . . . . -179.3(3) ? Cr1 N4 C20 C18 . . . . -1.5(4) ? Cr1 N4 C20 C21 . . . . 175.3(3) ? Cr1 N4 C24 C23 . . . . -176.7(3) ? Cr1 N5 C25 C18 . . . . -11.4(4) ? Cr1 N5 C25 C26 . . . . 174.6(3) ? Cr1 N5 C29 C28 . . . . -176.5(3) ? Ti1 O2 C30 C31 . . . . -41.1(5) ? Ti1 O2 C30 C35 . . . . 138.0(3) ? Ti1 O3 C39 C40 . . . . -39.1(5) ? Ti1 O3 C39 C44 . . . . 140.3(3) ? Ti1 O4 C48 C49 . . . . -24.0(4) ? Ti1 N6 C36 C31 . . . . -57.6(3) ? Ti1 N6 C45 C40 . . . . -65.2(3) ? Ti1 N6 C49 C48 . . . . -39.9(3) ? O1 Ti1 O2 C30 . . . . -147.9(3) ? O1 Ti1 O3 C39 . . . . -165.3(3) ? O1 Ti1 O4 C48 . . . . -179.2(3) ? O2 Ti1 O1 Cr1 . . . . 43.2(6) ? O2 Ti1 O3 C39 . . . . -59.8(3) ? O2 Ti1 O4 C48 . . . . 75.8(3) ? O2 C30 C31 C32 . . . . 176.8(3) ? O2 C30 C31 C36 . . . . -4.2(5) ? O2 C30 C35 C34 . . . . -177.8(3) ? O2 C30 C35 C38 . . . . 2.6(5) ? O3 Ti1 O1 Cr1 . . . . 159.7(6) ? O3 Ti1 O2 C30 . . . . 107.1(3) ? O3 Ti1 O4 C48 . . . . -73.4(3) ? O3 C39 C40 C41 . . . . 179.9(3) ? O3 C39 C40 C45 . . . . -0.9(5) ? O3 C39 C44 C43 . . . . -179.7(3) ? O3 C39 C44 C47 . . . . -0.9(5) ? O4 Ti1 O1 Cr1 . . . . -75.8(6) ? O4 Ti1 O2 C30 . . . . -44.7(4) ? O4 Ti1 O3 C39 . . . . 90.2(3) ? O4 C48 C49 N6 . . . . 42.9(4) ? N1 C1 C2 C3 . . . . -0.9(5) ? N1 C1 C6 C7 . . . . 176.5(3) ? N1 C1 C6 C8 . . . . 55.7(4) ? N1 C1 C6 C13 . . . . -62.5(4) ? N1 C5 C18 C19 . . . . -176.8(3) ? N1 C5 C18 C20 . . . . 62.5(4) ? N1 C5 C18 C25 . . . . -55.5(4) ? N2 Cr1 O1 Ti1 . . . . -167.4(6) ? N2 C8 C9 C10 . . . . 0.0(5) ? N3 Cr1 O1 Ti1 . . . . 110.9(6) ? N3 C13 C14 C15 . . . . 1.7(6) ? N4 Cr1 O1 Ti1 . . . . 11.8(6) ? N4 C20 C21 C22 . . . . 1.0(6) ? N5 Cr1 O1 Ti1 . . . . -69.9(6) ? N5 C25 C26 C27 . . . . 3.3(5) ? N6 Ti1 O2 C30 . . . . 26.7(3) ? N6 Ti1 O3 C39 . . . . 20.0(3) ? N6 Ti1 O4 C48 . . . . 0.6(3) ? C1 N1 C5 C4 . . . . -0.7(5) ? C1 N1 C5 C18 . . . . 179.9(3) ? C1 C2 C3 C4 . . . . -0.2(5) ? C1 C6 C8 N2 . . . . -63.9(4) ? C1 C6 C8 C9 . . . . 118.4(3) ? C1 C6 C13 N3 . . . . 62.1(4) ? C1 C6 C13 C14 . . . . -121.7(4) ? C2 C1 C6 C7 . . . . -3.4(5) ? C2 C1 C6 C8 . . . . -124.3(3) ? C2 C1 C6 C13 . . . . 117.6(3) ? C2 C3 C4 C5 . . . . 0.8(5) ? C3 C4 C5 N1 . . . . -0.4(5) ? C3 C4 C5 C18 . . . . 179.0(3) ? C4 C5 C18 C19 . . . . 3.8(5) ? C4 C5 C18 C20 . . . . -116.9(3) ? C4 C5 C18 C25 . . . . 125.1(3) ? C5 N1 C1 C2 . . . . 1.3(5) ? C5 N1 C1 C6 . . . . -178.6(3) ? C5 C18 C20 N4 . . . . -58.8(4) ? C5 C18 C20 C21 . . . . 124.5(4) ? C5 C18 C25 N5 . . . . 64.8(4) ? C5 C18 C25 C26 . . . . -121.3(4) ? C6 C1 C2 C3 . . . . 179.1(3) ? C6 C8 C9 C10 . . . . 177.6(3) ? C6 C13 C14 C15 . . . . -174.4(3) ? C7 C6 C8 N2 . . . . 175.4(3) ? C7 C6 C8 C9 . . . . -2.3(4) ? C7 C6 C13 N3 . . . . -177.0(3) ? C7 C6 C13 C14 . . . . -0.8(5) ? C8 N2 C12 C11 . . . . -4.6(5) ? C8 C6 C13 N3 . . . . -57.5(4) ? C8 C6 C13 C14 . . . . 118.8(4) ? C8 C9 C10 C11 . . . . -3.2(6) ? C9 C10 C11 C12 . . . . 2.5(6) ? C10 C11 C12 N2 . . . . 1.4(6) ? C12 N2 C8 C6 . . . . -173.9(3) ? C12 N2 C8 C9 . . . . 3.8(5) ? C13 N3 C17 C16 . . . . 4.1(5) ? C13 C6 C8 N2 . . . . 55.8(4) ? C13 C6 C8 C9 . . . . -121.9(3) ? C13 C14 C15 C16 . . . . 2.0(6) ? C14 C15 C16 C17 . . . . -2.7(6) ? C15 C16 C17 N3 . . . . -0.4(5) ? C17 N3 C13 C6 . . . . 171.6(3) ? C17 N3 C13 C14 . . . . -4.7(5) ? C18 C20 C21 C22 . . . . 177.6(4) ? C18 C25 C26 C27 . . . . -170.4(3) ? C19 C18 C20 N4 . . . . -179.1(3) ? C19 C18 C20 C21 . . . . 4.2(5) ? C19 C18 C25 N5 . . . . -173.7(3) ? C19 C18 C25 C26 . . . . 0.1(5) ? C20 N4 C24 C23 . . . . -1.8(5) ? C20 C18 C25 N5 . . . . -54.3(4) ? C20 C18 C25 C26 . . . . 119.6(4) ? C20 C21 C22 C23 . . . . -0.9(7) ? C21 C22 C23 C24 . . . . -0.5(7) ? C22 C23 C24 N4 . . . . 1.9(6) ? C24 N4 C20 C18 . . . . -176.4(3) ? C24 N4 C20 C21 . . . . 0.3(5) ? C25 N5 C29 C28 . . . . 3.9(5) ? C25 C18 C20 N4 . . . . 61.9(4) ? C25 C18 C20 C21 . . . . -114.8(4) ? C25 C26 C27 C28 . . . . 1.3(6) ? C26 C27 C28 C29 . . . . -3.2(6) ? C27 C28 C29 N5 . . . . 0.6(6) ? C29 N5 C25 C18 . . . . 168.2(3) ? C29 N5 C25 C26 . . . . -5.8(5) ? C30 C31 C32 C33 . . . . 1.5(5) ? C30 C31 C36 N6 . . . . 52.3(4) ? C31 C30 C35 C34 . . . . 1.4(5) ? C31 C30 C35 C38 . . . . -178.3(3) ? C31 C32 C33 C34 . . . . 0.2(5) ? C31 C32 C33 C37 . . . . -179.2(4) ? C32 C31 C36 N6 . . . . -128.7(3) ? C32 C33 C34 C35 . . . . -1.2(5) ? C33 C34 C35 C30 . . . . 0.4(5) ? C33 C34 C35 C38 . . . . -179.9(3) ? C35 C30 C31 C32 . . . . -2.3(5) ? C35 C30 C31 C36 . . . . 176.7(3) ? C36 N6 C45 C40 . . . . 59.9(4) ? C36 N6 C49 C48 . . . . -162.1(3) ? C36 C31 C32 C33 . . . . -177.5(3) ? C37 C33 C34 C35 . . . . 178.2(4) ? C39 C40 C41 C42 . . . . -0.5(5) ? C39 C40 C45 N6 . . . . 54.6(4) ? C40 C39 C44 C43 . . . . -0.4(5) ? C40 C39 C44 C47 . . . . 178.4(3) ? C40 C41 C42 C43 . . . . 0.2(5) ? C40 C41 C42 C46 . . . . -179.6(3) ? C41 C40 C45 N6 . . . . -126.2(3) ? C41 C42 C43 C44 . . . . 0.0(5) ? C42 C43 C44 C39 . . . . 0.1(5) ? C42 C43 C44 C47 . . . . -178.7(3) ? C44 C39 C40 C41 . . . . 0.5(5) ? C44 C39 C40 C45 . . . . 179.8(3) ? C45 N6 C36 C31 . . . . -179.9(3) ? C45 N6 C49 C48 . . . . 76.8(4) ? C45 C40 C41 C42 . . . . -179.7(3) ? C46 C42 C43 C44 . . . . 179.8(3) ? C49 N6 C36 C31 . . . . 58.3(4) ? C49 N6 C45 C40 . . . . -178.1(3) ? _shelx_res_file ; TITL rds031_0m in P2(1)/n CELL 0.71073 13.4112 18.3529 46.9774 90 90.43 90 ZERR 4 0.0003 0.0005 0.0011 0 0.001 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Ti Cr F B Cl UNIT 460 308 24 16 4 4 192 8 16 DFIX 1.34 0.01 F46A C113 F47A C113 F48A C113 DFIX 1.74 0.005 Cl4T C2S Cl4S C2S DFIX 1.74 0.005 Cl2S C1S Cl1S C1S DFIX 1.74 0.008 Cl2S C1T Cl1S C1T SADI 0.01 F17 C73 F18 C73 F16 C73 DANG 2.145 0.005 F46A F47A F47A F48A F48A F46A DELU F47A DELU 0.005 0.005 C1S C1T SIMU 0.005 0.02 1.9 C1S C1T ISOR 0.005 0.008 F46A F48A ISOR 0.005 0.004 F47A L.S. 12 PLAN -10 0 0 TEMP -163 HTAB BOND $H CONF acta 50 fmap 2 OMIT 0 0 2 REM C:/frames/rsommer/rds031/work/rds031_0m.hkl WGHT 0.090400 36.249901 FVAR 0.05108 0.84500 0.41470 0.74272 CR1 6 0.223463 0.310740 0.382998 11.00000 0.01476 0.01218 = 0.01507 0.00047 -0.00188 -0.00194 TI1 5 0.407159 0.268360 0.436922 11.00000 0.01708 0.01377 = 0.01715 -0.00126 -0.00320 -0.00142 O1 4 0.328231 0.289499 0.407455 11.00000 0.01836 0.01584 = 0.01992 0.00010 -0.00249 -0.00137 O2 4 0.331455 0.197934 0.454524 11.00000 0.02258 0.02226 = 0.01656 0.00094 -0.00305 -0.00502 O3 4 0.515844 0.231749 0.417571 11.00000 0.01906 0.02119 = 0.02292 0.00215 -0.00139 0.00226 O4 4 0.407311 0.360931 0.453297 11.00000 0.03113 0.01753 = 0.02624 -0.00611 -0.00928 0.00045 N1 3 0.104342 0.335386 0.356198 11.00000 0.01801 0.01406 = 0.01859 0.00091 -0.00113 -0.00219 N2 3 0.306571 0.294613 0.346585 11.00000 0.01691 0.01952 = 0.01826 0.00049 -0.00070 -0.00414 N3 3 0.274353 0.415991 0.377800 11.00000 0.01646 0.01448 = 0.02256 0.00083 -0.00171 -0.00207 N4 3 0.124924 0.328342 0.416452 11.00000 0.02219 0.01485 = 0.01991 0.00228 -0.00058 0.00017 N5 3 0.168487 0.204998 0.386680 11.00000 0.02242 0.01546 = 0.01643 0.00063 -0.00230 -0.00285 N6 3 0.510145 0.253908 0.477345 11.00000 0.02045 0.01949 = 0.02083 -0.00357 -0.00452 -0.00304 C1 1 0.117264 0.379983 0.333596 11.00000 0.01890 0.01607 = 0.01844 -0.00041 -0.00151 -0.00110 C2 1 0.037293 0.401910 0.316929 11.00000 0.02486 0.01768 = 0.02557 0.00354 -0.00413 -0.00123 AFIX 43 H2 2 0.047330 0.433801 0.301281 11.00000 -1.20000 AFIX 0 C3 1 -0.056923 0.377204 0.323172 11.00000 0.02027 0.02240 = 0.02691 -0.00139 -0.00834 0.00401 AFIX 43 H3 2 -0.112440 0.392023 0.311906 11.00000 -1.20000 AFIX 0 C4 1 -0.070065 0.330913 0.345838 11.00000 0.01505 0.02330 = 0.02904 -0.00137 -0.00121 -0.00027 AFIX 43 H4 2 -0.134617 0.312984 0.350205 11.00000 -1.20000 AFIX 0 C5 1 0.011664 0.310563 0.362293 11.00000 0.01664 0.01756 = 0.02120 -0.00146 -0.00074 -0.00183 C6 1 0.224199 0.405160 0.327209 11.00000 0.02066 0.01987 = 0.02163 0.00652 -0.00231 -0.00553 C7 1 0.224498 0.451198 0.299894 11.00000 0.03019 0.03068 = 0.02927 0.01408 -0.00498 -0.00810 AFIX 137 H7A 2 0.183240 0.494675 0.302627 11.00000 -1.50000 H7B 2 0.197480 0.422353 0.284066 11.00000 -1.50000 H7C 2 0.292965 0.465933 0.295566 11.00000 -1.50000 AFIX 0 C8 1 0.292946 0.338097 0.323592 11.00000 0.01334 0.02523 = 0.02050 0.00155 -0.00224 -0.00785 C9 1 0.342583 0.323390 0.298225 11.00000 0.02020 0.04045 = 0.01944 0.00196 -0.00165 -0.00946 AFIX 43 H9 2 0.332943 0.353957 0.282118 11.00000 -1.20000 AFIX 0 C10 1 0.405853 0.264086 0.296676 11.00000 0.02344 0.04823 = 0.02017 -0.00765 0.00346 -0.00497 AFIX 43 H10 2 0.437344 0.252192 0.279235 11.00000 -1.20000 AFIX 0 C11 1 0.422925 0.222373 0.320580 11.00000 0.02523 0.03617 = 0.02830 -0.00860 0.00067 0.00316 AFIX 43 H11 2 0.468155 0.182556 0.320176 11.00000 -1.20000 AFIX 0 C12 1 0.372546 0.239984 0.345134 11.00000 0.02274 0.02797 = 0.02187 -0.00233 -0.00209 0.00107 AFIX 43 H12 2 0.385249 0.212050 0.361796 11.00000 -1.20000 AFIX 0 C13 1 0.265432 0.450208 0.352281 11.00000 0.01527 0.01841 = 0.02833 0.00544 -0.00249 -0.00348 C14 1 0.298214 0.521553 0.349133 11.00000 0.02459 0.02144 = 0.04035 0.01076 -0.00453 -0.00402 AFIX 43 H14 2 0.290266 0.545791 0.331392 11.00000 -1.20000 AFIX 0 C15 1 0.342423 0.557185 0.371875 11.00000 0.02886 0.01545 = 0.04969 -0.00003 -0.00224 -0.00479 AFIX 43 H15 2 0.363041 0.606473 0.370042 11.00000 -1.20000 AFIX 0 C16 1 0.356312 0.520766 0.397149 11.00000 0.02110 0.01806 = 0.03937 -0.00653 -0.00517 -0.00283 AFIX 43 H16 2 0.389071 0.543714 0.412747 11.00000 -1.20000 AFIX 0 C17 1 0.321722 0.450154 0.399433 11.00000 0.01988 0.01746 = 0.02588 -0.00244 -0.00367 -0.00076 AFIX 43 H17 2 0.331629 0.424750 0.416845 11.00000 -1.20000 AFIX 0 C18 1 0.000054 0.259999 0.388091 11.00000 0.01603 0.02283 = 0.02364 0.00406 0.00085 -0.00370 C19 1 -0.108982 0.234809 0.390229 11.00000 0.02095 0.03718 = 0.03627 0.00730 0.00031 -0.00819 AFIX 137 H19A 2 -0.151919 0.277044 0.393697 11.00000 -1.50000 H19B 2 -0.115384 0.200128 0.405972 11.00000 -1.50000 H19C 2 -0.129134 0.211201 0.372381 11.00000 -1.50000 AFIX 0 C20 1 0.031084 0.301693 0.415244 11.00000 0.02375 0.02153 = 0.02303 0.00325 0.00098 0.00185 C21 1 -0.032595 0.308601 0.438317 11.00000 0.02817 0.04332 = 0.03246 -0.00030 0.00924 -0.00143 AFIX 43 H21 2 -0.098125 0.289035 0.437420 11.00000 -1.20000 AFIX 0 C22 1 0.000369 0.344283 0.462636 11.00000 0.04232 0.05148 = 0.03083 -0.00616 0.01523 0.00561 AFIX 43 H22 2 -0.042832 0.349922 0.478418 11.00000 -1.20000 AFIX 0 C23 1 0.095379 0.371346 0.463817 11.00000 0.04463 0.03360 = 0.02386 -0.00780 0.00459 0.00238 AFIX 43 H23 2 0.118965 0.396262 0.480264 11.00000 -1.20000 AFIX 0 C24 1 0.156082 0.361586 0.440558 11.00000 0.02938 0.02117 = 0.02158 -0.00125 -0.00115 0.00072 AFIX 43 H24 2 0.222718 0.379017 0.441545 11.00000 -1.20000 AFIX 0 C25 1 0.068899 0.192718 0.385929 11.00000 0.02169 0.02058 = 0.01878 0.00298 -0.00160 -0.00530 C26 1 0.032508 0.121749 0.385977 11.00000 0.02818 0.02763 = 0.02770 0.00350 -0.00489 -0.01291 AFIX 43 H26 2 -0.037192 0.113218 0.384440 11.00000 -1.20000 AFIX 0 C27 1 0.097387 0.063815 0.388252 11.00000 0.04573 0.01745 = 0.02929 0.00171 -0.00397 -0.01000 AFIX 43 H27 2 0.072875 0.015256 0.387896 11.00000 -1.20000 AFIX 0 C28 1 0.197499 0.076837 0.391029 11.00000 0.04248 0.01698 = 0.02837 -0.00067 -0.00294 0.00096 AFIX 43 H28 2 0.243227 0.037813 0.393598 11.00000 -1.20000 AFIX 0 C29 1 0.230389 0.148083 0.390005 11.00000 0.02892 0.01862 = 0.02220 0.00050 -0.00176 -0.00063 AFIX 43 H29 2 0.299893 0.157232 0.391729 11.00000 -1.20000 AFIX 0 C30 1 0.314431 0.174246 0.481402 11.00000 0.02474 0.01334 = 0.01767 -0.00002 -0.00118 -0.00169 C31 1 0.392928 0.167867 0.500982 11.00000 0.02290 0.01684 = 0.02102 0.00012 -0.00202 0.00264 C32 1 0.372036 0.146933 0.528713 11.00000 0.03322 0.02296 = 0.02043 0.00224 -0.00569 0.00158 AFIX 43 H32 2 0.425072 0.143715 0.542173 11.00000 -1.20000 AFIX 0 C33 1 0.275432 0.130523 0.537335 11.00000 0.03290 0.02366 = 0.01887 0.00171 -0.00199 -0.00091 C34 1 0.199521 0.135453 0.517210 11.00000 0.02592 0.01989 = 0.02451 0.00082 0.00484 -0.00107 AFIX 43 H34 2 0.133435 0.123546 0.522671 11.00000 -1.20000 AFIX 0 C35 1 0.216816 0.157307 0.489198 11.00000 0.02380 0.01557 = 0.02091 -0.00055 -0.00208 -0.00019 C36 1 0.498425 0.182416 0.491747 11.00000 0.02432 0.02133 = 0.02328 -0.00046 -0.00565 0.00125 AFIX 23 H36A 2 0.542896 0.180885 0.508653 11.00000 -1.20000 H36B 2 0.519612 0.143273 0.478614 11.00000 -1.20000 AFIX 0 C37 1 0.254454 0.108892 0.567649 11.00000 0.04226 0.04827 = 0.02264 0.00764 -0.00066 -0.00623 AFIX 137 H37A 2 0.182234 0.105817 0.570441 11.00000 -1.50000 H37B 2 0.282649 0.145431 0.580618 11.00000 -1.50000 H37C 2 0.284838 0.061360 0.571604 11.00000 -1.50000 AFIX 0 C38 1 0.133766 0.162513 0.467556 11.00000 0.02309 0.02909 = 0.02618 0.00681 -0.00304 -0.00762 AFIX 137 H38A 2 0.137385 0.209604 0.457784 11.00000 -1.50000 H38B 2 0.069425 0.158235 0.477166 11.00000 -1.50000 H38C 2 0.140423 0.123088 0.453630 11.00000 -1.50000 AFIX 0 C39 1 0.598887 0.192651 0.423668 11.00000 0.01591 0.01951 = 0.02432 0.00560 0.00098 -0.00213 C40 1 0.652185 0.205182 0.448936 11.00000 0.01592 0.02393 = 0.02652 0.00254 0.00096 -0.00581 C41 1 0.737118 0.164113 0.454661 11.00000 0.01563 0.03019 = 0.02772 0.00441 -0.00383 -0.00538 AFIX 43 H41 2 0.773744 0.172729 0.471719 11.00000 -1.20000 AFIX 0 C42 1 0.769409 0.110748 0.435919 11.00000 0.01715 0.02836 = 0.02935 0.00932 0.00296 -0.00084 C43 1 0.715285 0.098925 0.411000 11.00000 0.01718 0.01989 = 0.02708 0.00512 0.00608 -0.00221 AFIX 43 H43 2 0.737101 0.062497 0.398100 11.00000 -1.20000 AFIX 0 C44 1 0.629640 0.139118 0.404377 11.00000 0.01882 0.02086 = 0.02154 0.00617 0.00260 -0.00173 C45 1 0.616481 0.263513 0.468969 11.00000 0.02091 0.02560 = 0.03030 -0.00247 -0.00708 -0.00604 AFIX 23 H45A 2 0.658843 0.263078 0.486318 11.00000 -1.20000 H45B 2 0.624315 0.311652 0.459744 11.00000 -1.20000 AFIX 0 C46 1 0.861708 0.065585 0.442275 11.00000 0.02019 0.03881 = 0.03650 0.00592 -0.00178 0.00470 AFIX 137 H46A 2 0.846879 0.030277 0.457310 11.00000 -1.50000 H46B 2 0.915911 0.097687 0.448594 11.00000 -1.50000 H46C 2 0.881940 0.039625 0.425028 11.00000 -1.50000 AFIX 0 C47 1 0.569809 0.125296 0.377746 11.00000 0.02589 0.02686 = 0.02104 0.00268 0.00055 0.00701 AFIX 137 H47A 2 0.570241 0.169053 0.365792 11.00000 -1.50000 H47B 2 0.500997 0.113287 0.382822 11.00000 -1.50000 H47C 2 0.599173 0.084533 0.367259 11.00000 -1.50000 AFIX 0 C48 1 0.460014 0.381590 0.478434 11.00000 0.03419 0.01993 = 0.02781 -0.00848 -0.00831 -0.00250 AFIX 23 H48A 2 0.420462 0.417468 0.489311 11.00000 -1.20000 H48B 2 0.524345 0.404420 0.473348 11.00000 -1.20000 AFIX 0 C49 1 0.478356 0.314534 0.496318 11.00000 0.02872 0.02646 = 0.02351 -0.00829 -0.00687 -0.00262 AFIX 23 H49A 2 0.530952 0.324534 0.510692 11.00000 -1.20000 H49B 2 0.416616 0.300812 0.506419 11.00000 -1.20000 AFIX 0 CL1S 9 0.807298 0.426753 0.425363 11.00000 0.09387 0.08476 = 0.22096 0.02591 -0.03321 0.02868 CL2S 9 0.594412 0.445445 0.419920 11.00000 0.07222 0.10126 = 0.06587 0.00669 0.01113 0.00442 PART 1 C1S 1 0.711666 0.483612 0.414174 41.00000 0.04561 0.04017 = 0.04325 -0.00012 -0.00496 0.00410 AFIX 23 H1SA 2 0.719376 0.493904 0.393621 41.00000 -1.20000 H1SB 2 0.716498 0.530460 0.424540 41.00000 -1.20000 AFIX 0 PART 0 PART 2 C1T 1 0.694621 0.385018 0.418181 -41.00000 0.05011 0.04236 = 0.03761 0.00892 0.00727 0.00544 AFIX 23 H1TA 2 0.684239 0.345116 0.432026 -41.00000 -1.20000 H1TB 2 0.696737 0.363202 0.398921 -41.00000 -1.20000 AFIX 0 PART 0 CL3S 9 0.030542 0.276864 0.542398 11.00000 0.03576 0.09385 = 0.09835 -0.02763 -0.00538 0.01532 PART 1 CL4S 9 0.159715 0.392101 0.542602 31.00000 0.08860 0.05591 = 0.06587 -0.00129 -0.02171 -0.03628 PART 0 PART 2 CL4T 9 0.214880 0.368296 0.533292 -31.00000 0.07724 0.18691 = 0.08891 0.03275 -0.04568 -0.03194 PART 0 C2S 1 0.151103 0.301973 0.553103 11.00000 0.05335 0.05307 = 0.08523 -0.01581 -0.02163 0.00512 PART 1 AFIX 23 H2SA 2 0.159531 0.297209 0.573974 31.00000 -1.20000 H2SB 2 0.201939 0.271700 0.543535 31.00000 -1.20000 AFIX 23 PART 0 PART 2 H2SC 2 0.192573 0.257348 0.553315 -31.00000 -1.20000 H2SD 2 0.147290 0.319557 0.572988 -31.00000 -1.20000 AFIX 0 PART 0 F1 7 -0.126911 -0.081197 0.373991 11.00000 0.02899 0.11766 = 0.05663 -0.00525 0.01156 0.01895 F2 7 -0.133683 -0.115262 0.331506 11.00000 0.02570 0.08331 = 0.05621 0.00186 -0.01747 -0.00074 F3 7 -0.124472 -0.194318 0.364622 11.00000 0.01778 0.07171 = 0.25463 0.09294 -0.01792 -0.01044 F4 7 0.237663 -0.046474 0.293367 11.00000 0.12149 0.06427 = 0.05059 0.01547 0.04334 -0.01008 F5 7 0.167838 0.040385 0.314877 11.00000 0.04496 0.03851 = 0.08630 0.03936 -0.00207 0.00233 F6 7 0.308610 0.002362 0.329788 11.00000 0.03019 0.06511 = 0.08589 0.04800 -0.00241 -0.01302 F7 7 0.027495 -0.049364 0.456821 11.00000 0.02600 0.05937 = 0.03972 -0.00502 0.00138 0.01797 F8 7 0.078598 -0.118188 0.490772 11.00000 0.03235 0.02707 = 0.03608 -0.00106 0.01653 -0.00568 F9 7 0.115278 -0.004052 0.490859 11.00000 0.04119 0.02623 = 0.03918 -0.01523 0.01932 -0.00499 F10 7 0.424018 0.065045 0.431976 11.00000 0.03155 0.01585 = 0.07186 0.00471 0.00924 -0.00491 F11 7 0.488359 0.006953 0.467302 11.00000 0.03484 0.04634 = 0.04189 -0.01572 -0.00642 -0.01524 F12 7 0.522856 -0.025398 0.424624 11.00000 0.02175 0.02636 = 0.05060 -0.00987 0.00985 -0.00662 F13 7 0.408257 -0.233760 0.292198 11.00000 0.09430 0.09750 = 0.02318 -0.00068 0.00474 0.04552 F14 7 0.520234 -0.313992 0.294655 11.00000 0.03789 0.06924 = 0.03866 -0.01410 0.02019 0.00697 F15 7 0.366700 -0.343909 0.298531 11.00000 0.07969 0.14027 = 0.03652 -0.04692 0.02523 -0.07214 PART 1 F16 7 0.633207 -0.270710 0.419366 11.00000 0.05272 0.08733 = 0.08505 -0.03800 -0.04592 0.02599 F17 7 0.580009 -0.375850 0.417472 11.00000 0.06111 0.09114 = 0.17122 0.07935 -0.05862 -0.01670 F18 7 0.684557 -0.338320 0.387116 11.00000 0.03981 0.17968 = 0.07432 -0.03914 -0.01693 0.06544 PART 0 F19 7 0.035151 -0.518269 0.391680 11.00000 0.07097 0.02293 = 0.04953 0.00444 -0.02352 -0.02331 F20 7 -0.060138 -0.425299 0.386385 11.00000 0.02364 0.06683 = 0.07657 -0.02742 -0.01439 -0.00452 F21 7 0.056968 -0.445927 0.356793 11.00000 0.04959 0.03137 = 0.03021 -0.00493 -0.01530 -0.00980 PART 1 F22 7 0.314948 -0.426583 0.476643 11.00000 0.07960 0.18410 = 0.05035 0.04540 -0.00435 0.06527 F23 7 0.213032 -0.355867 0.494789 11.00000 0.10394 0.05453 = 0.02582 0.00143 -0.01588 -0.02662 F24 7 0.165185 -0.460315 0.485316 11.00000 0.15487 0.07520 = 0.03697 0.03173 -0.03694 -0.08230 PART 0 C50 1 0.180693 -0.170180 0.373667 11.00000 0.01815 0.01323 = 0.01810 -0.00287 0.00178 0.00165 C51 1 0.076865 -0.172894 0.373092 11.00000 0.01899 0.01702 = 0.02440 -0.00003 0.00182 -0.00197 AFIX 43 H51 2 0.043384 -0.206097 0.385240 11.00000 -1.20000 AFIX 0 C52 1 0.020878 -0.127996 0.355093 11.00000 0.01945 0.02199 = 0.03193 -0.00099 -0.00162 0.00172 C53 1 0.066144 -0.078284 0.337266 11.00000 0.02543 0.02442 = 0.03152 0.00707 -0.00432 0.00486 AFIX 43 H53 2 0.027705 -0.048382 0.324852 11.00000 -1.20000 AFIX 0 C54 1 0.169176 -0.073328 0.338025 11.00000 0.02458 0.02163 = 0.02669 0.00469 0.00159 0.00230 C55 1 0.225014 -0.117993 0.355853 11.00000 0.01708 0.01797 = 0.02386 0.00010 0.00230 0.00114 AFIX 43 H55 2 0.295544 -0.113168 0.356036 11.00000 -1.20000 AFIX 0 C56 1 -0.090678 -0.131192 0.356064 11.00000 0.01992 0.03922 = 0.05075 0.01496 -0.00329 0.00308 C57 1 0.220723 -0.020093 0.319042 11.00000 0.03185 0.03775 = 0.04095 0.01828 0.00300 0.00226 C58 1 0.271607 -0.156365 0.420981 11.00000 0.01914 0.01198 = 0.01671 0.00035 0.00098 0.00122 C59 1 0.193956 -0.138503 0.439196 11.00000 0.01838 0.01687 = 0.01865 0.00132 0.00186 -0.00297 AFIX 43 H59 2 0.135951 -0.168217 0.439126 11.00000 -1.20000 AFIX 0 C60 1 0.197728 -0.079059 0.457467 11.00000 0.02231 0.01643 = 0.01555 0.00199 0.00331 0.00245 C61 1 0.281214 -0.034803 0.458852 11.00000 0.02317 0.01342 = 0.01882 -0.00275 -0.00018 0.00058 AFIX 43 H61 2 0.284246 0.005738 0.471403 11.00000 -1.20000 AFIX 0 C62 1 0.360963 -0.052115 0.441044 11.00000 0.01867 0.01482 = 0.01948 0.00113 -0.00009 -0.00098 C63 1 0.356283 -0.111232 0.422535 11.00000 0.01569 0.01479 = 0.01924 0.00090 0.00271 0.00013 AFIX 43 H63 2 0.411604 -0.121365 0.410658 11.00000 -1.20000 AFIX 0 C64 1 0.106001 -0.062199 0.474091 11.00000 0.02338 0.02021 = 0.02498 -0.00461 0.00455 0.00238 C65 1 0.449141 -0.002114 0.441164 11.00000 0.02200 0.01919 = 0.03280 -0.00432 0.00135 -0.00308 C66 1 0.352134 -0.244788 0.380222 11.00000 0.01774 0.01075 = 0.01914 -0.00043 0.00076 -0.00322 C67 1 0.355642 -0.255641 0.350771 11.00000 0.01598 0.01585 = 0.02032 -0.00319 0.00105 -0.00218 AFIX 43 H67 2 0.299247 -0.242847 0.339479 11.00000 -1.20000 AFIX 0 C68 1 0.439289 -0.284635 0.337483 11.00000 0.01893 0.02006 = 0.02617 -0.00666 0.00526 -0.00376 C69 1 0.522827 -0.305212 0.353159 11.00000 0.01618 0.02276 = 0.03946 -0.01245 0.00523 -0.00049 AFIX 43 H69 2 0.580112 -0.324691 0.344138 11.00000 -1.20000 AFIX 0 C70 1 0.519648 -0.296270 0.382602 11.00000 0.01748 0.01731 = 0.03812 -0.00689 -0.00576 0.00034 C71 1 0.436799 -0.266320 0.395617 11.00000 0.02022 0.01508 = 0.02022 -0.00217 -0.00193 -0.00172 AFIX 43 H71 2 0.437542 -0.260201 0.415699 11.00000 -1.20000 AFIX 0 C72 1 0.434448 -0.294873 0.305990 11.00000 0.02635 0.04341 = 0.02979 -0.01305 0.00950 -0.00616 C73 1 0.604791 -0.320326 0.400894 11.00000 0.02566 0.02891 = 0.05656 -0.00504 -0.01138 0.00402 C74 1 0.199960 -0.290755 0.408517 11.00000 0.01596 0.01394 = 0.01869 -0.00127 0.00272 -0.00026 C75 1 0.139101 -0.336540 0.391976 11.00000 0.01911 0.01738 = 0.01814 -0.00111 -0.00160 0.00101 AFIX 43 H75 2 0.122062 -0.322282 0.373118 11.00000 -1.20000 AFIX 0 C76 1 0.102994 -0.402308 0.402449 11.00000 0.01915 0.01714 = 0.02554 -0.00251 -0.00210 -0.00166 C77 1 0.127798 -0.426584 0.429523 11.00000 0.02210 0.01700 = 0.02555 0.00211 -0.00001 -0.00326 AFIX 43 H77 2 0.103360 -0.471713 0.436501 11.00000 -1.20000 AFIX 0 C78 1 0.189285 -0.382998 0.446065 11.00000 0.02166 0.02094 = 0.02046 0.00145 -0.00132 -0.00112 C79 1 0.224297 -0.316702 0.435839 11.00000 0.01845 0.01593 = 0.01829 -0.00170 -0.00221 -0.00296 AFIX 43 H79 2 0.266162 -0.287939 0.447755 11.00000 -1.20000 AFIX 0 C80 1 0.033763 -0.447675 0.384572 11.00000 0.02940 0.02017 = 0.03550 -0.00060 -0.00879 -0.00611 C81 1 0.220132 -0.408786 0.474959 11.00000 0.04046 0.03382 = 0.02695 0.00774 -0.00439 -0.00892 B1 8 0.251010 -0.216224 0.395857 11.00000 0.01508 0.01544 = 0.01534 -0.00121 0.00018 -0.00070 F25 7 0.914205 0.580572 0.239571 11.00000 0.08450 0.03997 = 0.10453 -0.03417 -0.03998 0.01594 F26 7 1.047301 0.556997 0.220134 11.00000 0.11176 0.07958 = 0.06192 -0.03039 0.03693 -0.07613 F27 7 1.012111 0.513715 0.261397 11.00000 0.12190 0.03768 = 0.05685 0.01697 -0.05801 -0.03886 F28 7 0.842174 0.331504 0.137913 11.00000 0.03388 0.02849 = 0.01932 -0.00403 0.00084 -0.00235 F29 7 0.984491 0.385740 0.138380 11.00000 0.02567 0.05233 = 0.02664 -0.00326 0.01215 -0.00271 F30 7 0.849400 0.448321 0.135803 11.00000 0.05069 0.02732 = 0.02169 0.00899 -0.00356 0.00726 F31 7 0.797718 0.025393 0.302477 11.00000 0.08924 0.03109 = 0.06051 -0.00234 0.02392 -0.02873 F32 7 0.708561 0.099899 0.322928 11.00000 0.07587 0.05910 = 0.12237 0.05546 0.06978 0.02544 F33 7 0.851113 0.071252 0.340482 11.00000 0.13370 0.09859 = 0.05727 0.05970 -0.06028 -0.08630 F34 7 1.150625 0.164791 0.268924 11.00000 0.02426 0.03664 = 0.04472 -0.01352 -0.00187 0.00799 F35 7 1.146729 0.210843 0.310919 11.00000 0.02893 0.03836 = 0.03116 0.00072 -0.01606 -0.00128 F36 7 1.138015 0.280661 0.274164 11.00000 0.02095 0.02999 = 0.04485 0.00851 -0.00667 -0.00490 F37 7 0.497508 0.497365 0.227154 11.00000 0.06233 0.03902 = 0.06063 -0.00935 -0.03026 0.02240 F38 7 0.562053 0.571064 0.256532 11.00000 0.08804 0.02332 = 0.04244 0.00747 -0.00228 -0.00687 F39 7 0.424075 0.521237 0.266616 11.00000 0.06288 0.09426 = 0.15226 0.08390 0.07399 0.06008 F40 7 0.522085 0.392289 0.354202 11.00000 0.04256 0.12961 = 0.03770 -0.00914 0.01934 0.01448 F41 7 0.681162 0.409243 0.356475 11.00000 0.06314 0.12017 = 0.03800 -0.01257 -0.00297 -0.04847 F42 7 0.623023 0.304771 0.351462 11.00000 0.11903 0.06767 = 0.03078 0.00841 0.02262 0.00543 F43 7 0.718732 0.011105 0.202417 11.00000 0.04835 0.02405 = 0.08280 0.01383 0.02049 0.00758 F44 7 0.819144 0.076911 0.179341 11.00000 0.03756 0.02474 = 0.06244 -0.00874 0.01874 -0.00133 F45 7 0.679369 0.046248 0.160870 11.00000 0.08248 0.08099 = 0.08407 -0.06016 -0.05908 0.05174 PART 1 F46 7 0.373205 0.184421 0.228980 21.00000 0.02069 0.13097 = 0.04640 0.03596 0.00763 -0.00051 PART 0 PART 2 F46A 7 0.371675 0.145023 0.209632 -21.00000 0.01995 0.03457 = 0.06446 0.01463 -0.00471 -0.01216 PART 0 PART 1 F47 7 0.374865 0.180896 0.184238 21.00000 0.01930 0.18576 = 0.06009 -0.06709 -0.01661 0.00939 PART 0 PART 2 F47A 7 0.389549 0.235488 0.181343 -21.00000 0.02637 0.03392 = 0.02567 0.00379 -0.01172 0.00268 PART 0 PART 1 F48 7 0.387534 0.280076 0.206228 21.00000 0.01903 0.04829 = 0.21884 0.03130 -0.01160 0.00695 PART 0 PART 2 F48A 7 0.377826 0.253830 0.226173 -21.00000 0.03087 0.05329 = 0.04106 -0.01627 -0.00219 0.00209 PART 0 C82 1 0.824632 0.353171 0.226031 11.00000 0.01254 0.01357 = 0.01959 0.00264 0.00050 0.00291 C83 1 0.874976 0.412869 0.238039 11.00000 0.01990 0.01698 = 0.01570 0.00197 -0.00030 0.00073 AFIX 43 H83 2 0.870400 0.420724 0.257975 11.00000 -1.20000 AFIX 0 C84 1 0.931488 0.461144 0.221852 11.00000 0.01850 0.01777 = 0.02247 0.00081 0.00042 -0.00012 C85 1 0.938689 0.452343 0.192617 11.00000 0.01713 0.01577 = 0.02181 0.00504 0.00368 0.00218 AFIX 43 H85 2 0.977245 0.484930 0.181487 11.00000 -1.20000 AFIX 0 C86 1 0.888088 0.394704 0.180096 11.00000 0.01522 0.01800 = 0.01638 0.00206 0.00089 0.00501 C87 1 0.833176 0.345916 0.196366 11.00000 0.01380 0.01441 = 0.01954 0.00118 -0.00030 0.00332 AFIX 43 H87 2 0.800434 0.306463 0.187130 11.00000 -1.20000 AFIX 0 C88 1 0.980060 0.525625 0.235635 11.00000 0.03681 0.02260 = 0.02207 0.00161 0.00426 -0.00881 C89 1 0.890598 0.389500 0.148249 11.00000 0.02154 0.02309 = 0.02008 0.00187 0.00236 0.00077 C90 1 0.833557 0.246834 0.265936 11.00000 0.01972 0.01372 = 0.01417 -0.00331 0.00072 -0.00020 C91 1 0.792780 0.190718 0.282577 11.00000 0.01927 0.01639 = 0.01898 -0.00083 -0.00007 -0.00269 AFIX 43 H91 2 0.722934 0.182276 0.281719 11.00000 -1.20000 AFIX 0 C92 1 0.851278 0.147168 0.300248 11.00000 0.03124 0.01342 = 0.01564 0.00037 0.00072 -0.00080 C93 1 0.953428 0.156327 0.301567 11.00000 0.02857 0.01518 = 0.01509 -0.00046 -0.00489 0.00377 AFIX 43 H93 2 0.993453 0.126749 0.313689 11.00000 -1.20000 AFIX 0 C94 1 0.995907 0.209682 0.284780 11.00000 0.02042 0.01488 = 0.01792 -0.00503 -0.00464 0.00011 C95 1 0.936910 0.254319 0.267424 11.00000 0.01985 0.01222 = 0.01737 -0.00071 -0.00048 -0.00058 AFIX 43 H95 2 0.968176 0.290881 0.256299 11.00000 -1.20000 AFIX 0 C96 1 0.803116 0.087229 0.316949 11.00000 0.03503 0.01961 = 0.02480 0.00626 0.00211 -0.00083 C97 1 1.106932 0.216120 0.284458 11.00000 0.02560 0.02004 = 0.02539 -0.00208 -0.00575 0.00218 C98 1 0.689055 0.349223 0.266614 11.00000 0.01471 0.01442 = 0.02385 0.00005 0.00200 -0.00471 C99 1 0.632561 0.405319 0.254104 11.00000 0.01880 0.01658 = 0.03055 0.00117 0.00510 -0.00307 AFIX 43 H99 2 0.639289 0.414349 0.234299 11.00000 -1.20000 AFIX 0 C100 1 0.567238 0.448015 0.269680 11.00000 0.01889 0.01554 = 0.04247 -0.00065 0.00659 -0.00237 C101 1 0.556711 0.437999 0.298728 11.00000 0.02005 0.02271 = 0.04059 -0.01063 0.01084 -0.00445 AFIX 43 H101 2 0.512380 0.467446 0.309424 11.00000 -1.20000 AFIX 0 C102 1 0.612650 0.383842 0.311726 11.00000 0.01927 0.02711 = 0.03016 -0.00702 0.00799 -0.00897 C103 1 0.677523 0.340125 0.295900 11.00000 0.01757 0.01984 = 0.02381 -0.00224 0.00274 -0.00686 AFIX 43 H103 2 0.714731 0.303227 0.305378 11.00000 -1.20000 AFIX 0 C104 1 0.510886 0.508393 0.254930 11.00000 0.03606 0.02441 = 0.05214 0.00539 0.02021 0.01113 C105 1 0.608333 0.374300 0.343218 11.00000 0.02700 0.04661 = 0.03092 -0.00926 0.00896 -0.00885 C106 1 0.688344 0.243317 0.227214 11.00000 0.01834 0.01550 = 0.01686 0.00578 -0.00083 -0.00294 C107 1 0.730492 0.182990 0.213498 11.00000 0.01578 0.01839 = 0.02150 0.00398 -0.00095 -0.00042 AFIX 43 H107 2 0.800126 0.174666 0.215440 11.00000 -1.20000 AFIX 0 C108 1 0.674228 0.135116 0.197223 11.00000 0.02366 0.01766 = 0.02165 0.00276 -0.00392 -0.00167 C109 1 0.571804 0.144253 0.194245 11.00000 0.02194 0.02374 = 0.01982 0.00227 -0.00624 -0.00610 AFIX 43 H109 2 0.533004 0.111264 0.183201 11.00000 -1.20000 AFIX 0 C110 1 0.528247 0.202554 0.207783 11.00000 0.01667 0.02803 = 0.02035 0.00694 -0.00292 -0.00308 C111 1 0.585268 0.251359 0.223845 11.00000 0.01639 0.02037 = 0.01759 0.00324 0.00150 0.00119 AFIX 43 H111 2 0.553031 0.291292 0.232769 11.00000 -1.20000 AFIX 0 C112 1 0.721662 0.068683 0.184657 11.00000 0.02540 0.02186 = 0.03275 -0.00550 -0.00837 -0.00108 C113 1 0.417274 0.210874 0.206711 11.00000 0.02203 0.03551 = 0.02686 0.00399 -0.00446 -0.00153 B2 8 0.759791 0.298491 0.246291 11.00000 0.01549 0.01453 = 0.01716 0.00199 0.00044 -0.00022 HKLF 4 REM rds031_0m in P2(1)/n REM R1 = 0.0691 for 19058 Fo > 4sig(Fo) and 0.0858 for all 23703 data REM 1684 parameters refined using 39 restraints END WGHT 0.0904 36.2581 REM Instructions for potential hydrogen bonds EQIV $1 x-1, y, z HTAB C2 F27_$1 HTAB C17 O4 HTAB C23 Cl4S HTAB C23 Cl4T HTAB C24 O4 HTAB C36 F11 EQIV $2 -x+1, -y, -z+1 HTAB C45 F23_$2 HTAB C48 Cl2S HTAB C1S F41 EQIV $3 -x+1, -y+1, -z+1 HTAB C1S Cl4S_$3 EQIV $4 x, y+1, z HTAB C1S F17_$4 HTAB C1T F41 REM Highest difference peak 1.692, deepest hole -1.725, 1-sigma level 0.096 Q1 1 0.9187 0.0299 0.0494 11.00000 0.05 1.69 Q2 1 0.7249 0.4253 0.4337 11.00000 0.05 1.51 Q3 1 0.8313 0.4998 0.4413 11.00000 0.05 1.46 Q4 1 0.0926 0.5033 0.2391 11.00000 0.05 1.36 Q5 1 0.2687 -0.4801 0.4702 11.00000 0.05 1.29 Q6 1 0.9802 0.5809 0.2273 11.00000 0.05 1.13 Q7 1 0.6217 -0.3915 0.3936 11.00000 0.05 1.12 Q8 1 0.7617 0.1234 0.3392 11.00000 0.05 0.97 Q9 1 0.2789 -0.3715 0.4874 11.00000 0.05 0.89 Q10 1 0.4553 0.4827 0.2444 11.00000 0.05 0.83 ; _shelx_res_checksum 80683 _shelx_hkl_file ; 1 0 0 0.00 0.03 1 0 0 0.02 0.02 -1 0 0 0.00 0.03 1 0 0 -0.01 0.02 -1 0 0 -0.04 0.03 -1 0 0 0.02 0.03 2 0 0 6.48 0.20 -2 0 0 5.87 0.20 2 0 0 5.91 0.21 2 0 0 5.91 0.21 -2 0 0 6.53 0.22 -2 0 0 5.44 0.21 3 0 0 -0.04 0.11 3 0 0 -0.03 0.10 -3 0 0 -0.05 0.12 -3 0 0 -0.14 0.09 -3 0 0 -0.08 0.11 4 0 0 181.65 4.79 -4 0 0 186.45 4.79 4 0 0 181.30 4.65 -4 0 0 190.51 4.66 -4 0 0 177.99 4.79 5 0 0 0.31 0.11 -5 0 0 -0.03 0.14 -5 0 0 0.03 0.14 5 0 0 -0.10 0.13 6 0 0 33.35 0.95 -6 0 0 32.26 0.95 6 0 0 31.97 0.90 7 0 0 0.20 0.13 7 0 0 0.13 0.15 -7 0 0 0.27 0.17 8 0 0 5.55 0.27 8 0 0 4.61 0.31 -8 0 0 4.81 0.32 9 0 0 -0.32 0.17 -9 0 0 -0.21 0.19 -10 0 0 30.69 1.00 10 0 0 30.46 0.98 -11 0 0 0.38 0.25 11 0 0 0.54 0.22 -12 0 0 4.63 0.41 12 0 0 5.00 0.39 -13 0 0 0.11 0.30 -14 0 0 5.61 0.48 -15 0 0 0.09 0.34 -16 0 0 1.90 0.41 0 -1 0 -0.25 0.02 0 -1 0 -0.25 0.02 0 -1 0 -0.28 0.02 0 1 0 -0.27 0.02 0 1 0 -0.24 0.02 0 1 0 -0.29 0.02 1 -1 0 0.65 0.06 -1 -1 0 0.85 0.06 -1 -1 0 0.91 0.07 -1 -1 0 0.87 0.08 1 1 0 0.72 0.06 -1 1 0 0.74 0.06 -1 1 0 0.88 0.07 2 -1 0 0.85 0.10 -2 -1 0 0.75 0.09 2 -1 0 1.20 0.11 -2 -1 0 1.06 0.10 2 1 0 0.80 0.09 2 1 0 1.04 0.10 -2 1 0 0.96 0.11 -2 1 0 1.32 0.12 2 1 0 1.08 0.10 -2 1 0 0.93 0.10 -3 -1 0 104.18 2.67 3 -1 0 99.16 2.68 -3 -1 0 95.66 2.67 -3 -1 0 105.58 2.60 -3 1 0 103.40 2.68 3 1 0 102.10 2.59 3 1 0 97.25 2.67 -3 1 0 100.53 2.68 -3 1 0 109.07 2.61 4 -1 0 4.38 0.24 -4 -1 0 4.22 0.20 -4 -1 0 4.36 0.23 -4 -1 0 4.29 0.23 4 1 0 4.24 0.19 -4 1 0 4.19 0.24 4 1 0 4.04 0.23 -4 1 0 4.65 0.24 -5 -1 0 23.33 0.73 -5 -1 0 25.66 0.74 5 -1 0 24.25 0.73 5 1 0 23.68 0.69 5 1 0 24.34 0.73 -5 1 0 24.62 0.74 -5 1 0 25.56 0.74 -6 -1 0 4.79 0.28 -6 -1 0 3.93 0.27 6 -1 0 4.44 0.27 6 1 0 4.40 0.27 6 1 0 4.20 0.21 -6 1 0 4.21 0.29 7 -1 0 2.64 0.23 -7 -1 0 2.91 0.24 7 1 0 3.08 0.24 -7 1 0 2.85 0.25 7 1 0 2.91 0.22 8 -1 0 6.76 0.36 -8 -1 0 6.68 0.36 8 1 0 6.07 0.29 -8 1 0 6.50 0.37 8 1 0 6.86 0.20 8 1 0 6.52 0.34 8 1 0 6.58 0.20 9 -1 0 1.06 0.21 -9 -1 0 1.53 0.25 -9 1 0 1.16 0.23 9 1 0 1.50 0.21 9 1 0 1.39 0.17 10 -1 0 43.76 1.31 -10 -1 0 43.79 1.33 10 1 0 43.05 1.29 -10 1 0 42.84 1.32 10 1 0 42.81 1.21 -11 -1 0 17.54 0.72 11 -1 0 18.20 0.69 11 1 0 17.48 0.68 -11 1 0 17.50 0.71 12 -1 0 42.27 1.31 -12 -1 0 41.64 1.31 -12 1 0 38.83 1.31 12 1 0 39.57 1.27 -13 -1 0 1.52 0.34 13 -1 0 1.67 0.32 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2 0 247.79 6.54 5 2 0 247.48 6.34 5 2 0 248.39 6.52 -6 -2 0 0.27 0.15 6 -2 0 0.01 0.16 -6 -2 0 0.03 0.14 -6 2 0 0.07 0.17 6 2 0 -0.33 0.13 6 2 0 0.32 0.12 7 -2 0 1.43 0.20 -7 -2 0 1.66 0.20 7 2 0 1.30 0.16 -7 2 0 1.44 0.21 7 2 0 1.54 0.19 -8 -2 0 68.39 1.89 8 -2 0 68.07 1.90 8 2 0 67.46 1.80 8 2 0 67.08 1.89 -8 2 0 68.21 1.91 -9 -2 0 6.58 0.39 9 -2 0 6.79 0.39 9 2 0 7.14 0.32 -9 2 0 6.18 0.41 9 2 0 7.18 0.37 9 2 0 7.09 0.24 10 -2 0 0.68 0.24 -10 -2 0 1.31 0.25 10 2 0 1.08 0.09 10 2 0 0.98 0.22 10 2 0 0.80 0.17 -10 2 0 0.98 0.26 10 2 0 1.20 0.09 11 -2 0 0.43 0.23 -11 -2 0 0.02 0.23 -11 2 0 0.25 0.26 11 2 0 0.83 0.18 11 2 0 0.72 0.23 -12 -2 0 3.12 0.36 12 -2 0 4.11 0.36 -12 2 0 2.95 0.38 12 2 0 4.01 0.35 -13 -2 0 2.16 0.36 13 -2 0 2.66 0.35 -13 2 0 2.03 0.36 -14 -2 0 -0.17 0.31 -14 2 0 0.15 0.33 -15 -2 0 13.68 0.77 -15 2 0 13.03 0.75 -16 -2 0 1.53 0.41 -16 2 0 1.47 0.44 0 -3 0 0.03 0.10 0 -3 0 0.08 0.09 0 3 0 0.03 0.10 0 3 0 0.03 0.10 0 3 0 0.04 0.05 0 3 0 0.07 0.09 -1 -3 0 16.36 0.50 -1 -3 0 16.69 0.52 1 -3 0 16.04 0.50 -1 -3 0 16.24 0.49 1 -3 0 16.84 0.51 -1 -3 0 17.10 0.49 -1 3 0 16.63 0.50 1 3 0 17.30 0.50 1 3 0 16.49 0.50 1 3 0 17.48 0.52 1 3 0 16.79 0.49 -1 3 0 17.09 0.51 -2 -3 0 0.20 0.12 -2 -3 0 0.05 0.12 -2 -3 0 0.35 0.12 2 -3 0 0.41 0.15 2 3 0 0.07 0.12 2 3 0 0.09 0.12 -2 3 0 0.39 0.14 2 3 0 0.15 0.12 -2 3 0 0.65 0.15 3 -3 0 45.37 1.27 -3 -3 0 47.47 1.26 -3 -3 0 44.48 1.25 3 3 0 46.34 1.23 -3 3 0 46.56 1.27 3 3 0 46.12 1.26 -4 -3 0 11.45 0.41 -4 -3 0 12.30 0.41 4 -3 0 12.00 0.43 -4 3 0 12.17 0.44 4 3 0 12.15 0.40 4 3 0 12.30 0.41 5 -3 0 0.07 0.14 -5 -3 0 0.33 0.14 -5 -3 0 0.19 0.14 -5 3 0 0.27 0.07 -5 3 0 0.47 0.16 5 3 0 0.49 0.14 5 3 0 0.16 0.12 -6 -3 0 43.38 1.27 6 -3 0 46.03 1.30 6 3 0 45.28 1.28 -6 3 0 46.65 1.18 6 3 0 45.59 1.23 -6 3 0 43.95 1.30 7 -3 0 0.59 0.18 -7 -3 0 0.25 0.16 -7 3 0 -0.10 0.17 7 3 0 0.55 0.16 7 3 0 0.65 0.14 -8 -3 0 28.07 0.90 8 -3 0 29.70 0.92 8 3 0 29.83 0.84 8 3 0 28.56 0.89 -8 3 0 28.38 0.93 9 -3 0 33.16 1.02 -9 -3 0 32.23 1.02 9 3 0 31.79 1.00 -9 3 0 32.22 1.04 9 3 0 32.22 0.93 -10 -3 0 5.77 0.40 10 -3 0 5.73 0.39 10 3 0 5.84 0.37 10 3 0 5.55 0.31 -10 3 0 6.37 0.42 -11 -3 0 10.47 0.56 11 -3 0 10.61 0.53 11 3 0 10.84 0.44 11 3 0 10.52 0.52 11 3 0 10.56 0.35 -11 3 0 10.72 0.56 -12 -3 0 2.23 0.34 12 -3 0 2.57 0.33 12 3 0 2.42 0.31 12 3 0 2.78 0.25 -12 3 0 2.92 0.37 -13 -3 0 8.55 0.54 13 -3 0 8.23 0.54 -13 3 0 7.58 0.55 -14 -3 0 0.84 0.34 -14 3 0 -0.08 0.32 -15 -3 0 3.95 0.47 -15 3 0 3.32 0.46 -16 -3 0 0.51 0.39 -16 3 0 -0.22 0.38 0 -4 0 18.68 0.57 0 -4 0 18.50 0.58 0 4 0 17.99 0.56 0 4 0 17.98 0.58 0 4 0 20.69 0.61 -1 -4 0 0.34 0.14 -1 -4 0 0.28 0.13 -1 -4 0 0.12 0.10 1 -4 0 0.30 0.14 1 4 0 0.33 0.14 1 4 0 -0.03 0.14 -1 4 0 0.08 0.14 -2 -4 0 364.32 10.40 -2 -4 0 354.87 9.53 2 -4 0 358.87 9.51 -2 -4 0 366.79 9.48 -2 4 0 354.78 9.56 2 4 0 348.90 9.16 2 4 0 374.60 10.47 2 4 0 366.10 9.61 -3 -4 0 88.02 2.27 -3 -4 0 82.82 2.26 3 -4 0 84.33 2.28 -3 -4 0 85.32 2.48 -3 4 0 84.23 2.28 3 4 0 84.69 2.26 3 4 0 85.09 2.20 4 -4 0 23.15 0.70 -4 -4 0 23.26 0.69 -4 -4 0 22.82 0.68 4 4 0 21.36 0.66 -4 4 0 21.94 0.70 4 4 0 22.54 0.68 -5 -4 0 43.30 1.22 5 -4 0 43.29 1.23 -5 -4 0 43.87 1.21 5 4 0 41.44 1.21 5 4 0 41.20 1.17 -5 4 0 42.41 1.24 5 4 0 44.98 1.19 -6 -4 0 12.11 0.46 6 -4 0 11.97 0.47 -6 4 0 11.32 0.48 6 4 0 11.96 0.42 6 4 0 11.82 0.45 -6 4 0 12.43 0.37 6 4 0 11.73 0.41 -7 -4 0 0.35 0.17 7 -4 0 0.43 0.18 7 4 0 0.56 0.16 -7 4 0 0.37 0.20 -7 4 0 0.48 0.07 7 4 0 0.54 0.16 8 -4 0 4.29 0.32 -8 -4 0 4.22 0.30 8 4 0 4.04 0.29 -8 4 0 4.56 0.34 8 4 0 4.04 0.26 9 -4 0 0.18 0.20 -9 -4 0 0.34 0.21 9 4 0 -0.11 0.17 -9 4 0 0.14 0.21 9 4 0 0.15 0.15 10 -4 0 0.93 0.24 -10 -4 0 1.20 0.26 10 4 0 1.43 0.20 10 4 0 1.67 0.25 -10 4 0 1.32 0.27 -11 -4 0 14.83 0.64 11 -4 0 14.59 0.64 11 4 0 14.54 0.54 11 4 0 15.38 0.62 -11 4 0 14.33 0.67 -12 -4 0 5.74 0.45 12 -4 0 6.78 0.47 12 4 0 5.91 0.44 12 4 0 5.98 0.35 -12 4 0 6.07 0.47 -13 -4 0 9.98 0.61 13 -4 0 10.72 0.62 -13 4 0 10.07 0.63 -14 -4 0 0.40 0.34 -14 4 0 0.30 0.36 -15 -4 0 3.48 0.46 -15 4 0 3.02 0.46 15 4 0 2.71 0.40 -16 -4 0 0.53 0.39 -16 4 0 0.86 0.41 0 -5 0 0.04 0.14 0 5 0 0.00 0.14 0 5 0 0.33 0.14 -1 -5 0 2.23 0.16 1 -5 0 1.85 0.18 -1 -5 0 2.61 0.19 1 5 0 2.36 0.19 -1 5 0 1.90 0.18 1 5 0 2.42 0.19 -2 -5 0 11.93 0.39 -2 -5 0 10.94 0.40 2 -5 0 10.60 0.40 -2 5 0 10.47 0.40 2 5 0 10.34 0.39 2 5 0 10.58 0.40 -3 -5 0 18.38 0.60 3 -5 0 18.01 0.59 -3 -5 0 17.93 0.57 3 5 0 18.40 0.57 -3 5 0 17.42 0.58 3 5 0 18.35 0.57 -4 -5 0 1.74 0.18 4 -5 0 1.62 0.20 -4 -5 0 1.42 0.17 4 5 0 1.67 0.18 4 5 0 1.96 0.18 -4 5 0 1.75 0.20 5 -5 0 71.46 1.98 -5 -5 0 71.29 1.96 5 5 0 73.84 1.91 -5 5 0 70.08 1.99 5 5 0 72.04 1.96 -6 -5 0 8.73 0.39 6 -5 0 8.60 0.40 6 5 0 9.22 0.37 6 5 0 9.12 0.39 6 5 0 9.10 0.39 -6 5 0 9.01 0.41 -7 -5 0 0.14 0.17 7 -5 0 0.17 0.18 7 5 0 -0.02 0.17 -7 5 0 0.09 0.19 -7 5 0 0.22 0.10 7 5 0 0.38 0.15 7 5 0 -0.08 0.15 8 -5 0 13.91 0.57 -8 -5 0 13.45 0.54 8 5 0 13.79 0.49 8 5 0 13.05 0.54 -8 5 0 13.80 0.59 8 5 0 13.65 0.53 -8 5 0 15.17 0.41 9 -5 0 0.03 0.21 -9 -5 0 0.08 0.20 -9 5 0 0.20 0.24 9 5 0 0.16 0.16 9 5 0 -0.06 0.19 9 5 0 0.41 0.19 10 -5 0 3.53 0.34 -10 -5 0 3.20 0.31 10 5 0 3.76 0.32 10 5 0 3.14 0.26 -10 5 0 3.59 0.36 10 5 0 3.55 0.31 -11 -5 0 10.62 0.54 11 -5 0 10.70 0.55 11 5 0 10.92 0.45 11 5 0 10.75 0.52 11 5 0 9.79 0.51 -11 5 0 11.87 0.60 -12 -5 0 0.21 0.28 12 -5 0 0.24 0.27 -12 5 0 0.53 0.30 12 5 0 -0.23 0.22 12 5 0 0.30 0.20 12 5 0 -0.01 0.25 13 -5 0 2.97 0.39 -13 -5 0 2.44 0.37 13 5 0 2.57 0.38 -13 5 0 2.99 0.41 -14 -5 0 0.01 0.32 -14 5 0 -0.44 0.32 14 5 0 0.20 0.29 -15 -5 0 3.97 0.48 -15 5 0 3.80 0.51 15 5 0 4.12 0.47 -16 -5 0 2.86 0.48 -16 5 0 2.35 0.46 0 -6 0 0.33 0.15 0 6 0 0.12 0.14 0 6 0 0.21 0.15 1 -6 0 12.55 0.45 -1 -6 0 12.81 0.45 -1 -6 0 12.61 0.43 1 6 0 13.06 0.45 1 6 0 12.93 0.45 -1 6 0 11.95 0.45 -2 -6 0 26.55 0.81 2 -6 0 27.41 0.82 -2 -6 0 27.60 0.84 -2 6 0 27.03 0.82 2 6 0 26.42 0.80 -3 -6 0 132.34 3.76 -3 -6 0 127.23 3.43 3 -6 0 130.76 3.45 -3 6 0 129.28 3.46 3 6 0 128.24 3.43 3 6 0 129.11 3.33 -4 -6 0 96.96 2.63 4 -6 0 99.69 2.64 -4 -6 0 95.65 2.86 4 6 0 98.01 2.62 -4 6 0 96.73 2.64 4 6 0 97.14 2.54 5 -6 0 2.96 0.26 -5 -6 0 3.00 0.24 5 6 0 2.66 0.23 5 6 0 3.19 0.25 -5 6 0 3.28 0.27 6 -6 0 53.18 1.55 -6 -6 0 53.52 1.53 6 6 0 55.59 1.53 6 6 0 53.48 1.51 -6 6 0 54.62 1.57 7 -6 0 1.36 0.23 -7 -6 0 1.80 0.23 7 6 0 1.60 0.22 7 6 0 1.52 0.20 -7 6 0 1.65 0.24 7 6 0 1.47 0.23 -8 -6 0 11.16 0.50 8 -6 0 11.32 0.51 8 6 0 11.79 0.48 8 6 0 11.78 0.44 8 6 0 11.71 0.48 -8 6 0 11.66 0.54 -9 -6 0 25.72 0.87 9 -6 0 25.72 0.89 -9 6 0 27.59 0.72 9 6 0 26.31 0.82 -9 6 0 23.97 0.90 9 6 0 25.72 0.86 9 6 0 26.96 0.87 10 -6 0 0.14 0.24 -10 -6 0 -0.19 0.23 10 6 0 0.16 0.18 10 6 0 0.34 0.23 10 6 0 0.08 0.21 -10 6 0 -0.04 0.27 -11 -6 0 67.99 1.96 11 -6 0 64.37 1.98 11 6 0 66.87 1.90 11 6 0 67.93 1.94 -11 6 0 65.48 1.99 11 6 0 65.41 1.83 12 -6 0 0.26 0.29 -12 -6 0 0.60 0.29 -12 6 0 -0.12 0.29 12 6 0 0.43 0.27 12 6 0 0.37 0.20 -13 -6 0 12.67 0.66 13 -6 0 12.75 0.68 -13 6 0 11.92 0.70 13 6 0 12.46 0.62 -14 -6 0 1.25 0.37 14 6 0 0.64 0.35 -14 6 0 0.75 0.38 -15 -6 0 1.61 0.42 -15 6 0 1.05 0.43 15 6 0 2.31 0.41 -16 6 0 0.33 0.41 0 -7 0 0.12 0.16 0 7 0 0.07 0.16 0 7 0 0.29 0.17 -1 -7 0 24.54 0.77 1 -7 0 25.16 0.79 1 -7 0 24.44 0.77 -1 -7 0 23.91 0.76 1 7 0 23.64 0.74 1 7 0 24.47 0.76 -1 7 0 24.22 0.77 -2 -7 0 13.28 0.47 -2 -7 0 13.54 0.50 2 -7 0 14.12 0.50 2 7 0 12.94 0.49 -2 7 0 12.83 0.50 2 7 0 13.62 0.48 -3 -7 0 32.07 0.99 3 -7 0 32.52 0.96 -3 -7 0 31.69 0.95 3 7 0 30.75 0.94 -3 7 0 31.23 0.96 3 7 0 30.73 0.92 -4 -7 0 0.90 0.19 -4 -7 0 0.68 0.17 4 -7 0 0.83 0.21 4 7 0 0.60 0.16 -4 7 0 0.65 0.21 4 7 0 0.54 0.17 5 -7 0 2.05 0.24 -5 -7 0 1.72 0.22 5 7 0 2.18 0.22 5 7 0 2.36 0.24 -5 7 0 1.87 0.24 6 -7 0 9.20 0.45 -6 -7 0 9.12 0.42 6 7 0 8.03 0.39 6 7 0 7.94 0.40 -6 7 0 8.60 0.45 7 -7 0 6.10 0.40 -7 -7 0 6.59 0.39 -7 7 0 7.09 0.43 7 7 0 6.66 0.38 7 7 0 6.15 0.35 8 -7 0 79.75 2.27 -8 -7 0 78.49 2.24 8 7 0 80.84 2.19 -8 7 0 77.49 2.27 8 7 0 78.85 2.23 8 7 0 83.48 2.18 9 -7 0 0.87 0.28 -9 -7 0 1.34 0.26 -9 7 0 1.50 0.31 9 7 0 1.38 0.25 9 7 0 1.19 0.21 9 7 0 1.04 0.26 10 -7 0 -0.03 0.25 -10 -7 0 -0.27 0.24 10 7 0 0.14 0.19 10 7 0 -0.18 0.23 -10 7 0 -0.15 0.27 10 7 0 -0.21 0.21 -11 -7 0 13.36 0.62 11 -7 0 12.36 0.63 11 7 0 12.67 0.52 11 7 0 12.44 0.60 -11 7 0 12.51 0.67 11 7 0 13.33 0.58 -12 -7 0 8.59 0.58 12 -7 0 10.23 0.59 -12 7 0 8.44 0.59 12 7 0 8.59 0.43 12 7 0 10.14 0.57 -13 -7 0 0.14 0.30 13 -7 0 0.24 0.31 13 7 0 0.31 0.29 -13 7 0 0.06 0.35 -14 -7 0 3.00 0.45 14 7 0 4.05 0.44 -14 7 0 3.22 0.46 -15 -7 0 -0.43 0.35 -15 7 0 -0.26 0.37 -16 -7 0 6.91 0.62 -16 7 0 6.21 0.62 0 -8 0 82.22 2.26 0 8 0 83.71 2.26 0 8 0 80.82 2.19 1 -8 0 37.72 1.13 -1 -8 0 38.99 1.18 1 -8 0 39.49 1.21 -1 -8 0 37.24 1.13 1 8 0 39.01 1.22 1 8 0 36.38 1.10 1 8 0 37.71 1.13 -1 8 0 39.44 1.14 -2 -8 0 70.97 2.08 2 -8 0 68.74 1.96 -2 -8 0 68.20 1.94 -2 8 0 71.04 1.97 2 8 0 69.27 1.94 2 8 0 72.46 1.90 3 -8 0 13.51 0.52 -3 -8 0 11.46 0.47 -3 -8 0 13.67 0.52 3 8 0 13.48 0.51 -3 8 0 12.97 0.52 3 8 0 12.94 0.49 -4 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0.71 2 1 -58 7.64 0.80 1 -1 -58 6.99 0.72 1 -1 -58 7.17 0.60 1 -1 -58 7.74 0.72 1 1 -58 5.96 0.57 1 1 -58 6.69 0.74 1 1 -58 6.51 0.66 1 1 -58 7.52 0.71 0 -1 -58 18.06 1.11 0 -1 -58 16.74 0.98 0 1 -58 18.24 0.99 0 1 -58 17.07 0.82 0 1 -58 17.57 1.00 0 1 -58 16.29 0.96 -1 -1 -58 0.71 0.47 -1 -1 -58 0.38 0.31 -1 -1 -58 0.42 0.51 -1 -1 -58 -0.01 0.44 -1 1 -58 0.55 0.45 -1 1 -58 0.15 0.43 -2 -1 -58 -0.32 0.49 -2 -1 -58 0.84 0.52 -2 -1 -58 0.05 0.42 -2 1 -58 0.32 0.45 -2 1 -58 0.24 0.49 2 -2 -58 0.02 0.51 2 -2 -58 1.56 0.47 2 -2 -58 0.96 0.56 2 -2 -58 1.81 0.53 2 -2 -58 0.66 0.38 2 2 -58 1.20 0.47 2 2 -58 0.91 0.41 2 2 -58 0.83 0.47 1 -2 -58 1.75 0.40 1 -2 -58 1.27 0.48 1 -2 -58 1.64 0.50 1 -2 -58 1.08 0.52 1 2 -58 1.44 0.46 1 2 -58 1.51 0.54 1 2 -58 1.15 0.48 1 2 -58 1.27 0.48 0 -2 -58 0.56 0.46 0 -2 -58 0.74 0.49 0 2 -58 0.72 0.44 0 2 -58 -0.01 0.33 0 2 -58 -0.04 0.44 -1 -2 -58 2.41 0.55 -1 2 -58 2.49 0.54 -1 2 -58 2.44 0.53 -1 2 -58 4.04 0.45 -1 2 -58 3.21 0.57 -2 -2 -58 0.11 0.48 -2 -2 -58 0.21 0.54 -2 2 -58 -0.27 0.44 -2 2 -58 0.67 0.45 -2 2 -58 -0.19 0.38 2 -3 -58 3.26 0.61 2 -3 -58 3.90 0.59 2 -3 -58 3.56 0.50 2 3 -58 3.77 0.57 2 3 -58 3.94 0.59 2 3 -58 4.74 0.54 2 3 -58 4.12 0.60 1 -3 -58 3.74 0.62 1 -3 -58 2.65 0.45 1 3 -58 3.48 0.60 1 3 -58 3.02 0.54 1 3 -58 2.86 0.55 0 -3 -58 1.62 0.39 0 -3 -58 1.55 0.47 0 -3 -58 1.75 0.55 0 3 -58 1.62 0.51 0 3 -58 1.79 0.54 0 3 -58 2.01 0.49 0 3 -58 1.83 0.41 -1 -3 -58 0.29 0.46 -1 -3 -58 0.43 0.46 -1 -3 -58 1.06 0.53 -1 3 -58 1.09 0.38 -1 3 -58 0.36 0.47 -1 3 -58 0.53 0.46 -2 -3 -58 1.19 0.30 -2 -3 -58 1.56 0.55 -2 -3 -58 1.27 0.48 -2 -3 -58 1.69 0.47 -2 3 -58 1.53 0.50 -2 3 -58 2.11 0.52 1 -4 -58 0.35 0.49 1 -4 -58 -0.44 0.35 1 -4 -58 -0.25 0.43 1 4 -58 0.02 0.45 1 4 -58 -0.35 0.50 1 4 -58 0.09 0.44 0 -4 -58 1.07 0.47 0 4 -58 0.88 0.47 0 4 -58 1.13 0.49 0 4 -58 0.85 0.39 -1 -4 -58 0.48 0.47 -1 -4 -58 0.40 0.51 -1 4 -58 0.59 0.46 -1 4 -58 0.93 0.49 -1 4 -58 0.38 0.40 1 0 -59 1.22 0.50 0 0 -59 0.44 0.43 0 0 -59 0.46 0.44 0 0 -59 1.30 0.50 0 -1 -59 2.06 0.58 0 -1 -59 3.68 0.58 0 1 -59 2.96 0.55 0 1 -59 2.80 0.54 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 27938 _database_code_depnum_ccdc_archive 'CCDC 973877' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x12031 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H50 B2 Cr F48 N5 O' _chemical_formula_weight 2239.00 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.817(5) _cell_length_b 16.704(4) _cell_length_c 28.732(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.620(11) _cell_angle_gamma 90.00 _cell_volume 9510(4) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9700 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 32.53 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4468 _exptl_absorpt_coefficient_mu 0.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9135 _exptl_absorpt_correction_T_max 0.9440 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa Axis X8 Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 205349 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 35.10 _reflns_number_total 21029 _reflns_number_gt 15693 _reflns_threshold_expression >2sigma(I) _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SIR92 _computing_structure_refinement XL _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+9.6993P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21029 _refine_ls_number_parameters 736 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1822 _refine_ls_wR_factor_gt 0.1706 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.0000 0.080376(17) 0.2500 0.01615(7) Uani 1 2 d S . . O1 O 0.0000 0.19254(9) 0.2500 0.0227(3) Uani 1 2 d S . . H1H H -0.0391 0.2093 0.2441 0.034 Uiso 0.50 1 calc PR . . N1 N 0.08062(6) 0.07113(7) 0.20480(4) 0.0180(2) Uani 1 1 d . . . N2 N 0.07651(6) 0.07830(7) 0.29948(4) 0.0210(2) Uani 1 1 d . . . N3 N 0.0000 -0.04482(10) 0.2500 0.0212(3) Uani 1 2 d S . . C1 C 0.08520(7) 0.11963(9) 0.16756(5) 0.0208(2) Uani 1 1 d . . . H1 H 0.0533 0.1618 0.1641 0.025 Uiso 1 1 calc R . . C2 C 0.13428(8) 0.11072(9) 0.13424(5) 0.0235(3) Uani 1 1 d . . . H2 H 0.1356 0.1452 0.1080 0.028 Uiso 1 1 calc R . . C3 C 0.18142(8) 0.05067(10) 0.13997(5) 0.0256(3) Uani 1 1 d . . . H3 H 0.2150 0.0420 0.1171 0.031 Uiso 1 1 calc R . . C4 C 0.17921(8) 0.00318(10) 0.17940(5) 0.0247(3) Uani 1 1 d . . . H4 H 0.2125 -0.0369 0.1844 0.030 Uiso 1 1 calc R . . C5 C 0.12821(7) 0.01432(8) 0.21163(5) 0.0203(2) Uani 1 1 d . . . C6 C 0.12416(8) -0.03601(9) 0.25640(6) 0.0257(3) Uani 1 1 d . . . C7 C 0.18541(10) -0.09171(12) 0.25971(7) 0.0383(4) Uani 1 1 d . . . H7A H 0.1853 -0.1282 0.2330 0.057 Uiso 1 1 calc R . . H7B H 0.1833 -0.1228 0.2886 0.057 Uiso 1 1 calc R . . H7C H 0.2269 -0.0598 0.2597 0.057 Uiso 1 1 calc R . . C8 C 0.12454(8) 0.02090(10) 0.29841(5) 0.0257(3) Uani 1 1 d . . . C9 C 0.17445(11) 0.01820(14) 0.33266(6) 0.0395(4) Uani 1 1 d . . . H9 H 0.2069 -0.0237 0.3326 0.047 Uiso 1 1 calc R . . C10 C 0.17709(11) 0.07643(16) 0.36692(7) 0.0440(5) Uani 1 1 d . . . H10 H 0.2110 0.0745 0.3905 0.053 Uiso 1 1 calc R . . C11 C 0.13026(9) 0.13684(14) 0.36650(6) 0.0363(4) Uani 1 1 d . . . H11 H 0.1316 0.1781 0.3892 0.044 Uiso 1 1 calc R . . C12 C 0.08114(8) 0.13602(11) 0.33218(6) 0.0281(3) Uani 1 1 d . . . H12 H 0.0490 0.1782 0.3315 0.034 Uiso 1 1 calc R . . C13 C 0.05876(9) -0.08548(9) 0.25403(6) 0.0268(3) Uani 1 1 d . . . C14 C 0.05997(11) -0.16877(10) 0.25475(8) 0.0396(5) Uani 1 1 d . . . H14 H 0.1015 -0.1967 0.2585 0.048 Uiso 1 1 calc R . . C15 C 0.0000 -0.21027(14) 0.2500 0.0478(8) Uani 1 2 d S . . H15 H 0.0000 -0.2671 0.2500 0.057 Uiso 1 2 calc SR . . B1 B 0.37474(7) 0.15494(9) 0.09784(5) 0.0173(2) Uani 1 1 d . . . C16 C 0.31693(7) 0.19946(8) 0.12950(5) 0.0168(2) Uani 1 1 d . . . C17 C 0.30484(7) 0.18044(8) 0.17622(5) 0.0172(2) Uani 1 1 d . . . H17 H 0.3327 0.1419 0.1913 0.021 Uiso 1 1 calc R . . C18 C 0.25279(7) 0.21659(8) 0.20123(5) 0.0176(2) Uani 1 1 d . . . C19 C 0.21083(7) 0.27332(8) 0.18080(5) 0.0186(2) Uani 1 1 d . . . H19 H 0.1751 0.2972 0.1977 0.022 Uiso 1 1 calc R . . C20 C 0.22273(7) 0.29413(8) 0.13471(5) 0.0179(2) Uani 1 1 d . . . C21 C 0.27496(7) 0.25887(8) 0.10992(5) 0.0186(2) Uani 1 1 d . . . H21 H 0.2825 0.2755 0.0788 0.022 Uiso 1 1 calc R . . C22 C 0.24185(8) 0.19257(9) 0.25088(5) 0.0217(3) Uani 1 1 d . . . F1 F 0.25360(6) 0.11455(6) 0.25808(3) 0.0322(2) Uani 1 1 d . . . F2 F 0.28279(6) 0.23124(7) 0.28068(3) 0.0348(2) Uani 1 1 d . . . F3 F 0.17892(6) 0.20730(8) 0.26462(4) 0.0404(3) Uani 1 1 d . . . C23 C 0.17841(8) 0.35557(9) 0.11162(5) 0.0226(3) Uani 1 1 d . . . F4 F 0.16862(5) 0.34083(6) 0.06635(3) 0.0295(2) Uani 1 1 d . . . F5 F 0.11731(5) 0.36008(7) 0.13109(4) 0.0359(2) Uani 1 1 d . . . F6 F 0.20488(6) 0.42968(6) 0.11436(4) 0.0360(2) Uani 1 1 d . . . C24 C 0.42220(7) 0.22372(8) 0.07380(5) 0.0172(2) Uani 1 1 d . . . C25 C 0.44037(7) 0.22313(9) 0.02678(5) 0.0197(2) Uani 1 1 d . . . H25 H 0.4234 0.1819 0.0071 0.024 Uiso 1 1 calc R . . C26 C 0.48256(8) 0.28121(10) 0.00807(5) 0.0236(3) Uani 1 1 d . . . C27 C 0.50877(8) 0.34249(9) 0.03527(5) 0.0243(3) Uani 1 1 d . A . H27 H 0.5380 0.3816 0.0225 0.029 Uiso 1 1 calc R . . C28 C 0.49086(8) 0.34471(9) 0.08167(6) 0.0251(3) Uani 1 1 d . . . C29 C 0.44841(8) 0.28660(9) 0.10048(5) 0.0227(3) Uani 1 1 d . A . H29 H 0.4370 0.2899 0.1325 0.027 Uiso 1 1 calc R . . C30 C 0.50229(11) 0.27835(14) -0.04206(6) 0.0390(4) Uani 1 1 d . . . F7 F 0.46381(16) 0.2337(2) -0.06730(5) 0.1763(19) Uani 1 1 d . . . F8 F 0.56519(10) 0.25439(11) -0.04802(5) 0.0735(6) Uani 1 1 d . . . F9 F 0.50160(9) 0.35151(11) -0.06182(5) 0.0660(5) Uani 1 1 d . . . C31 C 0.51841(13) 0.40909(13) 0.11233(8) 0.0464(6) Uani 0.712(13) 1 d P A 1 F10 F 0.5508(4) 0.4647(3) 0.09020(17) 0.093(2) Uani 0.712(13) 1 d P A 1 F11 F 0.5622(2) 0.3778(3) 0.14439(18) 0.0834(15) Uani 0.712(13) 1 d P A 1 F12 F 0.4731(3) 0.4419(3) 0.1387(2) 0.0780(18) Uani 0.712(13) 1 d P A 1 C31' C 0.51841(13) 0.40909(13) 0.11233(8) 0.0464(6) Uani 0.288(13) 1 d P A 2 F10' F 0.4732(10) 0.4735(11) 0.1121(10) 0.148(8) Uani 0.288(13) 1 d P A 2 F11' F 0.524(2) 0.3976(12) 0.1524(3) 0.181(14) Uani 0.288(13) 1 d P A 2 F12' F 0.5701(9) 0.4436(13) 0.0971(6) 0.138(8) Uani 0.288(13) 1 d P A 2 C32 C 0.34001(7) 0.09847(8) 0.05727(5) 0.0173(2) Uani 1 1 d . . . C33 C 0.27286(7) 0.10112(8) 0.04229(5) 0.0185(2) Uani 1 1 d . B . H33 H 0.2436 0.1398 0.0555 0.022 Uiso 1 1 calc R . . C34 C 0.24703(7) 0.04877(9) 0.00842(5) 0.0207(2) Uani 1 1 d . . . C35 C 0.28853(8) -0.00701(9) -0.01267(5) 0.0228(3) Uani 1 1 d . B . H35 H 0.2711 -0.0431 -0.0353 0.027 Uiso 1 1 calc R . . C36 C 0.35598(7) -0.00873(8) 0.00013(5) 0.0212(2) Uani 1 1 d . . . C37 C 0.38104(7) 0.04179(8) 0.03471(5) 0.0198(2) Uani 1 1 d . B . H37 H 0.4273 0.0380 0.0434 0.024 Uiso 1 1 calc R . . C38 C 0.17434(8) 0.05280(12) -0.00570(6) 0.0290(3) Uani 0.652(7) 1 d P B 3 F13 F 0.16486(14) 0.0892(2) -0.04568(12) 0.0557(11) Uani 0.652(7) 1 d P B 3 F14 F 0.13464(10) 0.0827(3) 0.02487(9) 0.0606(14) Uani 0.652(7) 1 d P B 3 F15 F 0.14838(11) -0.02255(13) -0.01475(13) 0.0550(10) Uani 0.652(7) 1 d P B 3 C38' C 0.17434(8) 0.05280(12) -0.00570(6) 0.0290(3) Uani 0.348(7) 1 d P B 4 F13' F 0.1362(2) 0.0194(6) 0.0223(3) 0.100(5) Uani 0.348(7) 1 d P B 4 F14' F 0.1609(3) 0.0350(8) -0.0456(2) 0.104(5) Uani 0.348(7) 1 d P B 4 F15' F 0.1528(3) 0.1333(3) -0.0023(4) 0.089(3) Uani 0.348(7) 1 d P B 4 C39 C 0.40377(9) -0.06266(11) -0.02505(6) 0.0312(3) Uani 1 1 d . B . F16 F 0.43538(7) -0.02355(9) -0.05925(5) 0.0535(4) Uani 1 1 d . . . F17 F 0.45418(8) -0.08909(9) 0.00225(5) 0.0553(4) Uani 1 1 d . . . F18 F 0.37426(8) -0.12483(10) -0.04464(7) 0.0738(6) Uani 1 1 d . . . C40 C 0.42021(7) 0.09474(8) 0.13104(5) 0.0178(2) Uani 1 1 d . . . C41 C 0.48623(7) 0.10960(9) 0.14644(5) 0.0199(2) Uani 1 1 d . . . H41 H 0.5073 0.1585 0.1380 0.024 Uiso 1 1 calc R . . C42 C 0.52226(7) 0.05469(9) 0.17382(5) 0.0224(3) Uani 1 1 d . . . C43 C 0.49382(8) -0.01746(9) 0.18718(5) 0.0243(3) Uani 1 1 d . . . H43 H 0.5186 -0.0549 0.2055 0.029 Uiso 1 1 calc R . . C44 C 0.42781(8) -0.03314(9) 0.17291(5) 0.0226(3) Uani 1 1 d . . . C45 C 0.39237(7) 0.02149(8) 0.14563(5) 0.0209(2) Uani 1 1 d . . . H45 H 0.3474 0.0089 0.1364 0.025 Uiso 1 1 calc R . . C46 C 0.59205(8) 0.07498(11) 0.19040(6) 0.0288(3) Uani 1 1 d . . . F19 F 0.59074(6) 0.12516(9) 0.22684(5) 0.0492(3) Uani 1 1 d . . . F20 F 0.62672(6) 0.01158(8) 0.20575(6) 0.0525(4) Uani 1 1 d . . . F21 F 0.62930(7) 0.10823(12) 0.15807(5) 0.0630(5) Uani 1 1 d . . . C47 C 0.39570(9) -0.11089(10) 0.18603(7) 0.0318(3) Uani 1 1 d . . . F22 F 0.40493(13) -0.16721(10) 0.15511(7) 0.0881(7) Uani 1 1 d . . . F23 F 0.42019(10) -0.14155(10) 0.22538(7) 0.0771(6) Uani 1 1 d . . . F24 F 0.33028(7) -0.10546(9) 0.19223(9) 0.0871(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.01709(13) 0.01213(11) 0.01934(14) 0.000 0.00485(10) 0.000 O1 0.0211(7) 0.0191(6) 0.0280(7) 0.000 -0.0019(6) 0.000 N1 0.0174(5) 0.0181(5) 0.0187(5) 0.0024(4) 0.0033(4) -0.0006(4) N2 0.0191(5) 0.0220(5) 0.0222(5) 0.0028(4) 0.0051(4) 0.0003(4) N3 0.0264(8) 0.0141(6) 0.0231(8) 0.000 0.0099(6) 0.000 C1 0.0191(6) 0.0228(6) 0.0206(6) 0.0044(5) 0.0012(5) -0.0038(5) C2 0.0232(6) 0.0288(7) 0.0187(6) 0.0017(5) 0.0026(5) -0.0094(5) C3 0.0212(6) 0.0333(7) 0.0225(6) -0.0033(5) 0.0071(5) -0.0065(5) C4 0.0199(6) 0.0284(7) 0.0260(7) -0.0013(5) 0.0070(5) 0.0014(5) C5 0.0187(6) 0.0204(6) 0.0220(6) 0.0011(5) 0.0052(5) 0.0014(4) C6 0.0278(7) 0.0227(6) 0.0268(7) 0.0070(5) 0.0084(6) 0.0095(5) C7 0.0370(9) 0.0362(9) 0.0418(10) 0.0119(7) 0.0096(8) 0.0201(7) C8 0.0266(7) 0.0299(7) 0.0207(6) 0.0091(5) 0.0060(5) 0.0070(6) C9 0.0379(10) 0.0550(12) 0.0256(8) 0.0131(8) -0.0009(7) 0.0170(8) C10 0.0393(10) 0.0730(15) 0.0198(7) 0.0077(8) -0.0031(7) 0.0073(10) C11 0.0277(8) 0.0590(12) 0.0225(7) -0.0056(7) 0.0047(6) -0.0064(8) C12 0.0199(6) 0.0347(8) 0.0297(7) -0.0070(6) 0.0050(5) -0.0040(6) C13 0.0339(8) 0.0170(6) 0.0297(7) 0.0048(5) 0.0150(6) 0.0056(5) C14 0.0492(11) 0.0166(6) 0.0537(11) 0.0076(7) 0.0268(9) 0.0098(6) C15 0.0661(19) 0.0122(8) 0.0660(19) 0.000 0.0400(16) 0.000 B1 0.0166(6) 0.0182(6) 0.0170(6) -0.0010(5) 0.0037(5) -0.0013(5) C16 0.0167(5) 0.0171(5) 0.0165(5) -0.0010(4) 0.0030(4) -0.0025(4) C17 0.0177(5) 0.0172(5) 0.0167(5) -0.0007(4) 0.0024(4) -0.0020(4) C18 0.0191(5) 0.0184(5) 0.0155(5) -0.0011(4) 0.0039(4) -0.0040(4) C19 0.0170(5) 0.0201(5) 0.0189(6) -0.0035(4) 0.0040(4) -0.0014(4) C20 0.0173(5) 0.0184(5) 0.0181(5) -0.0022(4) 0.0021(4) -0.0005(4) C21 0.0188(6) 0.0199(5) 0.0172(5) -0.0004(4) 0.0034(4) -0.0007(4) C22 0.0241(6) 0.0224(6) 0.0187(6) -0.0010(5) 0.0054(5) -0.0031(5) F1 0.0517(7) 0.0210(4) 0.0242(5) 0.0034(3) 0.0093(4) -0.0034(4) F2 0.0524(7) 0.0326(5) 0.0191(4) -0.0001(4) -0.0053(4) -0.0120(5) F3 0.0322(5) 0.0606(7) 0.0288(5) 0.0119(5) 0.0175(4) 0.0088(5) C23 0.0221(6) 0.0238(6) 0.0219(6) -0.0023(5) -0.0006(5) 0.0027(5) F4 0.0322(5) 0.0346(5) 0.0215(4) -0.0026(4) -0.0055(4) 0.0056(4) F5 0.0239(5) 0.0492(6) 0.0346(5) 0.0009(5) 0.0037(4) 0.0142(4) F6 0.0428(6) 0.0200(4) 0.0448(6) 0.0015(4) -0.0154(5) 0.0007(4) C24 0.0162(5) 0.0183(5) 0.0172(5) -0.0012(4) 0.0034(4) -0.0005(4) C25 0.0183(6) 0.0236(6) 0.0173(6) -0.0005(4) 0.0020(4) -0.0031(5) C26 0.0225(6) 0.0316(7) 0.0168(6) 0.0016(5) 0.0031(5) -0.0057(5) C27 0.0230(6) 0.0250(6) 0.0249(7) 0.0016(5) 0.0063(5) -0.0058(5) C28 0.0273(7) 0.0223(6) 0.0258(7) -0.0058(5) 0.0085(5) -0.0075(5) C29 0.0250(6) 0.0222(6) 0.0211(6) -0.0048(5) 0.0087(5) -0.0046(5) C30 0.0427(10) 0.0553(11) 0.0191(7) 0.0020(7) 0.0052(7) -0.0227(9) F7 0.218(3) 0.290(4) 0.0220(7) -0.0408(13) 0.0324(11) -0.220(3) F8 0.0962(13) 0.0858(12) 0.0393(7) 0.0193(7) 0.0418(8) 0.0465(10) F9 0.0750(10) 0.0834(11) 0.0401(7) 0.0357(7) 0.0241(7) 0.0293(9) C31 0.0582(13) 0.0396(10) 0.0419(11) -0.0197(8) 0.0237(10) -0.0278(9) F10 0.174(6) 0.0552(17) 0.0507(16) -0.0151(14) 0.037(2) -0.082(3) F11 0.091(3) 0.084(2) 0.075(3) -0.032(2) -0.035(2) -0.030(2) F12 0.089(3) 0.060(2) 0.086(3) -0.055(2) 0.046(2) -0.0238(18) C31' 0.0582(13) 0.0396(10) 0.0419(11) -0.0197(8) 0.0237(10) -0.0278(9) F10' 0.175(13) 0.076(9) 0.191(18) -0.093(11) -0.044(13) 0.048(8) F11' 0.40(4) 0.119(13) 0.025(3) 0.001(6) -0.025(11) -0.182(18) F12' 0.102(8) 0.193(14) 0.119(10) -0.129(10) 0.078(7) -0.127(9) C32 0.0168(5) 0.0180(5) 0.0173(5) -0.0003(4) 0.0032(4) -0.0002(4) C33 0.0169(5) 0.0219(6) 0.0166(5) 0.0010(4) 0.0032(4) -0.0003(4) C34 0.0172(6) 0.0282(6) 0.0167(6) 0.0001(5) 0.0016(4) -0.0013(5) C35 0.0239(6) 0.0256(6) 0.0189(6) -0.0042(5) 0.0019(5) -0.0030(5) C36 0.0215(6) 0.0204(6) 0.0219(6) -0.0040(5) 0.0043(5) -0.0008(5) C37 0.0161(5) 0.0209(6) 0.0223(6) -0.0035(5) 0.0028(4) 0.0000(4) C38 0.0203(6) 0.0444(9) 0.0223(7) -0.0022(6) -0.0010(5) -0.0018(6) F13 0.0289(10) 0.088(2) 0.0499(18) 0.0394(17) -0.0129(10) -0.0060(13) F14 0.0178(8) 0.125(4) 0.0393(14) -0.0408(19) -0.0031(8) 0.0129(14) F15 0.0290(10) 0.0415(11) 0.094(3) -0.0055(12) -0.0164(12) -0.0124(8) C38' 0.0203(6) 0.0444(9) 0.0223(7) -0.0022(6) -0.0010(5) -0.0018(6) F13' 0.020(2) 0.168(10) 0.111(7) 0.081(7) -0.002(3) -0.018(4) F14' 0.034(3) 0.236(14) 0.042(4) -0.072(7) -0.017(2) 0.024(5) F15' 0.041(3) 0.056(3) 0.170(8) -0.013(4) -0.053(4) 0.017(2) C39 0.0298(8) 0.0300(7) 0.0340(8) -0.0140(6) 0.0032(6) 0.0028(6) F16 0.0510(8) 0.0637(9) 0.0465(7) -0.0079(6) 0.0263(6) 0.0094(6) F17 0.0539(8) 0.0558(8) 0.0562(8) -0.0146(6) -0.0027(6) 0.0334(7) F18 0.0448(8) 0.0601(9) 0.1167(14) -0.0647(10) 0.0170(8) -0.0094(7) C40 0.0164(5) 0.0195(5) 0.0177(5) -0.0022(4) 0.0031(4) 0.0004(4) C41 0.0174(5) 0.0234(6) 0.0187(6) -0.0027(5) 0.0010(4) -0.0020(4) C42 0.0176(6) 0.0291(7) 0.0205(6) -0.0036(5) -0.0006(5) 0.0009(5) C43 0.0228(6) 0.0262(6) 0.0237(7) -0.0005(5) -0.0012(5) 0.0048(5) C44 0.0227(6) 0.0192(6) 0.0260(7) -0.0001(5) 0.0009(5) 0.0023(5) C45 0.0177(6) 0.0199(6) 0.0251(6) -0.0007(5) 0.0011(5) 0.0000(4) C46 0.0220(7) 0.0376(8) 0.0267(7) -0.0038(6) -0.0034(5) 0.0007(6) F19 0.0314(6) 0.0607(8) 0.0552(8) -0.0320(6) -0.0106(5) 0.0016(5) F20 0.0314(6) 0.0463(7) 0.0792(10) -0.0049(7) -0.0228(6) 0.0085(5) F21 0.0270(6) 0.1196(14) 0.0423(7) 0.0197(8) -0.0053(5) -0.0271(7) C47 0.0310(8) 0.0219(7) 0.0423(9) 0.0065(6) -0.0040(7) 0.0010(6) F22 0.1382(18) 0.0358(7) 0.0912(13) -0.0242(8) 0.0413(12) -0.0337(10) F23 0.0927(13) 0.0540(9) 0.0836(12) 0.0423(9) -0.0383(10) -0.0328(9) F24 0.0322(7) 0.0463(8) 0.183(2) 0.0581(11) 0.0195(10) 0.0011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cr1 O1 1.8735(16) . ? Cr1 N2 2.0675(14) 2 ? Cr1 N2 2.0675(14) . ? Cr1 N1 2.0755(12) . ? Cr1 N1 2.0755(12) 2 ? Cr1 N3 2.0912(17) . ? O1 H1H 0.8400 . ? N1 C1 1.3459(17) . ? N1 C5 1.3508(18) . ? N2 C12 1.349(2) . ? N2 C8 1.3515(19) . ? N3 C13 1.3518(18) 2 ? N3 C13 1.3518(18) . ? C1 C2 1.380(2) . ? C1 H1 0.9500 . ? C2 C3 1.379(2) . ? C2 H2 0.9500 . ? C3 C4 1.384(2) . ? C3 H3 0.9500 . ? C4 C5 1.3904(19) . ? C4 H4 0.9500 . ? C5 C6 1.539(2) . ? C6 C7 1.532(2) . ? C6 C8 1.536(2) . ? C6 C13 1.538(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.388(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.371(3) . ? C10 H10 0.9500 . ? C11 C12 1.378(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.392(2) . ? C14 C15 1.381(3) . ? C14 H14 0.9500 . ? C15 C14 1.381(3) 2 ? C15 H15 0.9500 . ? B1 C24 1.6420(19) . ? B1 C32 1.645(2) . ? B1 C40 1.648(2) . ? B1 C16 1.6479(19) . ? C16 C17 1.4026(18) . ? C16 C21 1.4080(19) . ? C17 C18 1.4003(18) . ? C17 H17 0.9500 . ? C18 C19 1.387(2) . ? C18 C22 1.5000(19) . ? C19 C20 1.3915(19) . ? C19 H19 0.9500 . ? C20 C21 1.3934(18) . ? C20 C23 1.501(2) . ? C21 H21 0.9500 . ? C22 F3 1.3350(18) . ? C22 F2 1.3393(18) . ? C22 F1 1.3396(18) . ? C23 F4 1.3359(18) . ? C23 F5 1.3414(18) . ? C23 F6 1.3464(18) . ? C24 C29 1.397(2) . ? C24 C25 1.4018(19) . ? C25 C26 1.3925(19) . ? C25 H25 0.9500 . ? C26 C27 1.385(2) . ? C26 C30 1.497(2) . ? C27 C28 1.384(2) . ? C27 H27 0.9500 . ? C28 C29 1.397(2) . ? C28 C31 1.490(2) . ? C29 H29 0.9500 . ? C30 F7 1.285(2) . ? C30 F8 1.322(3) . ? C30 F9 1.347(3) . ? C31 F10 1.299(4) . ? C31 F12 1.302(4) . ? C31 F11 1.363(5) . ? C32 C33 1.395(2) . ? C32 C37 1.4102(18) . ? C33 C34 1.401(2) . ? C33 H33 0.9500 . ? C34 C35 1.387(2) . ? C34 C38 1.494(2) . ? C35 C36 1.383(2) . ? C35 H35 0.9500 . ? C36 C37 1.391(2) . ? C36 C39 1.499(2) . ? C37 H37 0.9500 . ? C38 F14 1.286(3) . ? C38 F13 1.311(3) . ? C38 F15 1.383(3) . ? C39 F18 1.315(2) . ? C39 F17 1.338(2) . ? C39 F16 1.341(2) . ? C40 C41 1.399(2) . ? C40 C45 1.4079(19) . ? C41 C42 1.399(2) . ? C41 H41 0.9500 . ? C42 C43 1.386(2) . ? C42 C46 1.497(2) . ? C43 C44 1.391(2) . ? C43 H43 0.9500 . ? C44 C45 1.389(2) . ? C44 C47 1.496(2) . ? C45 H45 0.9500 . ? C46 F21 1.316(2) . ? C46 F20 1.335(2) . ? C46 F19 1.341(2) . ? C47 F22 1.308(2) . ? C47 F24 1.314(2) . ? C47 F23 1.328(2) . ? 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 O1 Cr1 N2 90.96(4) . 2 ? O1 Cr1 N2 90.96(4) . . ? N2 Cr1 N2 178.08(7) 2 . ? O1 Cr1 N1 94.27(3) . . ? N2 Cr1 N1 97.60(5) 2 . ? N2 Cr1 N1 82.26(5) . . ? O1 Cr1 N1 94.27(3) . 2 ? N2 Cr1 N1 82.26(5) 2 2 ? N2 Cr1 N1 97.60(5) . 2 ? N1 Cr1 N1 171.46(6) . 2 ? O1 Cr1 N3 180.0 . . ? N2 Cr1 N3 89.04(4) 2 . ? N2 Cr1 N3 89.04(4) . . ? N1 Cr1 N3 85.73(3) . . ? N1 Cr1 N3 85.73(3) 2 . ? Cr1 O1 H1H 109.5 . . ? C1 N1 C5 119.03(12) . . ? C1 N1 Cr1 120.78(9) . . ? C5 N1 Cr1 120.16(9) . . ? C12 N2 C8 118.71(14) . . ? C12 N2 Cr1 120.71(11) . . ? C8 N2 Cr1 120.51(11) . . ? C13 N3 C13 119.68(18) 2 . ? C13 N3 Cr1 120.16(9) 2 . ? C13 N3 Cr1 120.16(9) . . ? N1 C1 C2 122.73(14) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 118.50(14) . . ? C3 C2 H2 120.7 . . ? C1 C2 H2 120.7 . . ? C2 C3 C4 119.15(13) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C3 C4 C5 119.86(14) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? N1 C5 C4 120.58(13) . . ? N1 C5 C6 117.53(12) . . ? C4 C5 C6 121.88(13) . . ? C7 C6 C8 109.27(15) . . ? C7 C6 C13 110.07(14) . . ? C8 C6 C13 111.36(12) . . ? C7 C6 C5 109.58(12) . . ? C8 C6 C5 108.59(12) . . ? C13 C6 C5 107.94(13) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 120.22(16) . . ? N2 C8 C6 117.34(14) . . ? C9 C8 C6 122.29(15) . . ? C10 C9 C8 120.15(18) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 119.38(18) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 118.16(19) . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? N2 C12 C11 123.20(17) . . ? N2 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? N3 C13 C14 121.22(17) . . ? N3 C13 C6 117.29(13) . . ? C14 C13 C6 121.47(15) . . ? C15 C14 C13 119.04(18) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C14 C15 C14 119.8(2) . 2 ? C14 C15 H15 120.1 . . ? C14 C15 H15 120.1 2 . ? C24 B1 C32 109.90(11) . . ? C24 B1 C40 111.00(11) . . ? C32 B1 C40 106.40(11) . . ? C24 B1 C16 108.74(11) . . ? C32 B1 C16 111.22(11) . . ? C40 B1 C16 109.58(11) . . ? C17 C16 C21 115.83(12) . . ? C17 C16 B1 123.57(12) . . ? C21 C16 B1 120.58(11) . . ? C18 C17 C16 121.86(13) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 121.26(12) . . ? C19 C18 C22 119.54(12) . . ? C17 C18 C22 119.19(13) . . ? C18 C19 C20 117.80(12) . . ? C18 C19 H19 121.1 . . ? C20 C19 H19 121.1 . . ? C19 C20 C21 121.02(13) . . ? C19 C20 C23 119.15(12) . . ? C21 C20 C23 119.83(12) . . ? C20 C21 C16 122.17(12) . . ? C20 C21 H21 118.9 . . ? C16 C21 H21 118.9 . . ? F3 C22 F2 106.46(13) . . ? F3 C22 F1 107.16(12) . . ? F2 C22 F1 105.51(13) . . ? F3 C22 C18 112.16(13) . . ? F2 C22 C18 112.72(12) . . ? F1 C22 C18 112.35(12) . . ? F4 C23 F5 107.11(13) . . ? F4 C23 F6 106.18(13) . . ? F5 C23 F6 106.07(12) . . ? F4 C23 C20 112.49(12) . . ? F5 C23 C20 112.37(12) . . ? F6 C23 C20 112.16(12) . . ? C29 C24 C25 115.87(12) . . ? C29 C24 B1 120.42(11) . . ? C25 C24 B1 123.69(12) . . ? C26 C25 C24 121.91(13) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C27 C26 C25 121.33(13) . . ? C27 C26 C30 117.78(14) . . ? C25 C26 C30 120.88(14) . . ? C28 C27 C26 117.69(13) . . ? C28 C27 H27 121.2 . . ? C26 C27 H27 121.2 . . ? C27 C28 C29 121.07(14) . . ? C27 C28 C31 119.52(14) . . ? C29 C28 C31 119.40(14) . . ? C28 C29 C24 122.12(13) . . ? C28 C29 H29 118.9 . . ? C24 C29 H29 118.9 . . ? F7 C30 F8 107.8(3) . . ? F7 C30 F9 106.6(2) . . ? F8 C30 F9 103.02(16) . . ? F7 C30 C26 113.70(15) . . ? F8 C30 C26 112.99(17) . . ? F9 C30 C26 112.00(18) . . ? F10 C31 F12 109.3(4) . . ? F10 C31 F11 106.9(4) . . ? F12 C31 F11 102.0(4) . . ? F10 C31 C28 114.0(3) . . ? F12 C31 C28 113.4(2) . . ? F11 C31 C28 110.4(3) . . ? C33 C32 C37 115.62(12) . . ? C33 C32 B1 126.23(12) . . ? C37 C32 B1 118.16(12) . . ? C32 C33 C34 122.32(13) . . ? C32 C33 H33 118.8 . . ? C34 C33 H33 118.8 . . ? C35 C34 C33 120.60(13) . . ? C35 C34 C38 119.10(14) . . ? C33 C34 C38 120.30(13) . . ? C36 C35 C34 118.28(13) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? C35 C36 C37 120.93(13) . . ? C35 C36 C39 119.86(14) . . ? C37 C36 C39 119.14(14) . . ? C36 C37 C32 122.16(13) . . ? C36 C37 H37 118.9 . . ? C32 C37 H37 118.9 . . ? F14 C38 F13 109.6(3) . . ? F14 C38 F15 104.6(2) . . ? F13 C38 F15 102.0(2) . . ? F14 C38 C34 115.29(16) . . ? F13 C38 C34 112.80(17) . . ? F15 C38 C34 111.45(17) . . ? F18 C39 F17 108.41(17) . . ? F18 C39 F16 106.28(17) . . ? F17 C39 F16 103.80(16) . . ? F18 C39 C36 113.62(15) . . ? F17 C39 C36 112.75(14) . . ? F16 C39 C36 111.32(15) . . ? C41 C40 C45 115.36(13) . . ? C41 C40 B1 125.36(12) . . ? C45 C40 B1 119.28(12) . . ? C40 C41 C42 122.10(13) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C43 C42 C41 121.27(14) . . ? C43 C42 C46 119.06(14) . . ? C41 C42 C46 119.65(14) . . ? C42 C43 C44 117.75(14) . . ? C42 C43 H43 121.1 . . ? C44 C43 H43 121.1 . . ? C45 C44 C43 120.71(14) . . ? C45 C44 C47 119.91(14) . . ? C43 C44 C47 119.35(14) . . ? C44 C45 C40 122.80(14) . . ? C44 C45 H45 118.6 . . ? C40 C45 H45 118.6 . . ? F21 C46 F20 106.11(16) . . ? F21 C46 F19 107.64(17) . . ? F20 C46 F19 104.60(15) . . ? F21 C46 C42 113.22(14) . . ? F20 C46 C42 113.34(15) . . ? F19 C46 C42 111.36(13) . . ? F22 C47 F24 106.7(2) . . ? F22 C47 F23 104.38(19) . . ? F24 C47 F23 105.26(19) . . ? F22 C47 C44 112.96(16) . . ? F24 C47 C44 113.40(14) . . ? F23 C47 C44 113.36(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cr1 N1 C1 -41.66(11) . . . . ? N2 Cr1 N1 C1 49.88(12) 2 . . . ? N2 Cr1 N1 C1 -132.06(12) . . . . ? N1 Cr1 N1 C1 138.36(11) 2 . . . ? N3 Cr1 N1 C1 138.34(11) . . . . ? O1 Cr1 N1 C5 140.48(11) . . . . ? N2 Cr1 N1 C5 -127.98(11) 2 . . . ? N2 Cr1 N1 C5 50.09(11) . . . . ? N1 Cr1 N1 C5 -39.50(11) 2 . . . ? N3 Cr1 N1 C5 -39.52(11) . . . . ? O1 Cr1 N2 C12 32.68(11) . . . . ? N2 Cr1 N2 C12 -147.29(11) 2 . . . ? N1 Cr1 N2 C12 126.86(12) . . . . ? N1 Cr1 N2 C12 -61.75(12) 2 . . . ? N3 Cr1 N2 C12 -147.32(11) . . . . ? O1 Cr1 N2 C8 -144.45(11) . . . . ? N2 Cr1 N2 C8 35.58(11) 2 . . . ? N1 Cr1 N2 C8 -50.27(11) . . . . ? N1 Cr1 N2 C8 121.12(11) 2 . . . ? N3 Cr1 N2 C8 35.55(11) . . . . ? O1 Cr1 N3 C13 6(73) . . . 2 ? N2 Cr1 N3 C13 -37.76(9) 2 . . 2 ? N2 Cr1 N3 C13 142.24(9) . . . 2 ? N1 Cr1 N3 C13 -135.45(9) . . . 2 ? N1 Cr1 N3 C13 44.55(9) 2 . . 2 ? O1 Cr1 N3 C13 -174(69) . . . . ? N2 Cr1 N3 C13 142.24(9) 2 . . . ? N2 Cr1 N3 C13 -37.76(9) . . . . ? N1 Cr1 N3 C13 44.55(9) . . . . ? N1 Cr1 N3 C13 -135.45(9) 2 . . . ? C5 N1 C1 C2 4.2(2) . . . . ? Cr1 N1 C1 C2 -173.71(11) . . . . ? N1 C1 C2 C3 -1.5(2) . . . . ? C1 C2 C3 C4 -1.9(2) . . . . ? C2 C3 C4 C5 2.6(2) . . . . ? C1 N1 C5 C4 -3.4(2) . . . . ? Cr1 N1 C5 C4 174.49(11) . . . . ? C1 N1 C5 C6 175.72(13) . . . . ? Cr1 N1 C5 C6 -6.39(18) . . . . ? C3 C4 C5 N1 0.1(2) . . . . ? C3 C4 C5 C6 -179.02(15) . . . . ? N1 C5 C6 C7 -175.25(15) . . . . ? C4 C5 C6 C7 3.9(2) . . . . ? N1 C5 C6 C8 -55.96(18) . . . . ? C4 C5 C6 C8 123.15(16) . . . . ? N1 C5 C6 C13 64.88(17) . . . . ? C4 C5 C6 C13 -116.00(16) . . . . ? C12 N2 C8 C9 5.0(2) . . . . ? Cr1 N2 C8 C9 -177.76(13) . . . . ? C12 N2 C8 C6 -170.66(13) . . . . ? Cr1 N2 C8 C6 6.53(18) . . . . ? C7 C6 C8 N2 175.42(14) . . . . ? C13 C6 C8 N2 -62.77(17) . . . . ? C5 C6 C8 N2 55.94(17) . . . . ? C7 C6 C8 C9 -0.2(2) . . . . ? C13 C6 C8 C9 121.62(18) . . . . ? C5 C6 C8 C9 -119.67(17) . . . . ? N2 C8 C9 C10 -2.9(3) . . . . ? C6 C8 C9 C10 172.55(17) . . . . ? C8 C9 C10 C11 -0.4(3) . . . . ? C9 C10 C11 C12 1.4(3) . . . . ? C8 N2 C12 C11 -4.1(2) . . . . ? Cr1 N2 C12 C11 178.74(13) . . . . ? C10 C11 C12 N2 0.8(3) . . . . ? C13 N3 C13 C14 -0.87(13) 2 . . . ? Cr1 N3 C13 C14 179.12(13) . . . . ? C13 N3 C13 C6 177.46(16) 2 . . . ? Cr1 N3 C13 C6 -2.54(16) . . . . ? C7 C6 C13 N3 -178.64(13) . . . . ? C8 C6 C13 N3 60.02(17) . . . . ? C5 C6 C13 N3 -59.08(16) . . . . ? C7 C6 C13 C14 -0.3(2) . . . . ? C8 C6 C13 C14 -121.65(17) . . . . ? C5 C6 C13 C14 119.25(17) . . . . ? N3 C13 C14 C15 1.7(3) . . . . ? C6 C13 C14 C15 -176.53(14) . . . . ? C13 C14 C15 C14 -0.84(12) . . . 2 ? C24 B1 C16 C17 -128.21(13) . . . . ? C32 B1 C16 C17 110.64(14) . . . . ? C40 B1 C16 C17 -6.72(17) . . . . ? C24 B1 C16 C21 53.40(16) . . . . ? C32 B1 C16 C21 -67.75(15) . . . . ? C40 B1 C16 C21 174.89(12) . . . . ? C21 C16 C17 C18 1.99(19) . . . . ? B1 C16 C17 C18 -176.47(12) . . . . ? C16 C17 C18 C19 -0.2(2) . . . . ? C16 C17 C18 C22 179.01(12) . . . . ? C17 C18 C19 C20 -0.9(2) . . . . ? C22 C18 C19 C20 179.85(12) . . . . ? C18 C19 C20 C21 0.2(2) . . . . ? C18 C19 C20 C23 -179.76(12) . . . . ? C19 C20 C21 C16 1.7(2) . . . . ? C23 C20 C21 C16 -178.34(13) . . . . ? C17 C16 C21 C20 -2.7(2) . . . . ? B1 C16 C21 C20 175.79(12) . . . . ? C19 C18 C22 F3 22.49(19) . . . . ? C17 C18 C22 F3 -156.74(13) . . . . ? C19 C18 C22 F2 -97.66(16) . . . . ? C17 C18 C22 F2 83.10(16) . . . . ? C19 C18 C22 F1 143.28(13) . . . . ? C17 C18 C22 F1 -35.95(18) . . . . ? C19 C20 C23 F4 -146.10(13) . . . . ? C21 C20 C23 F4 33.93(19) . . . . ? C19 C20 C23 F5 -25.13(19) . . . . ? C21 C20 C23 F5 154.90(13) . . . . ? C19 C20 C23 F6 94.27(16) . . . . ? C21 C20 C23 F6 -85.70(16) . . . . ? C32 B1 C24 C29 169.78(13) . . . . ? C40 B1 C24 C29 -72.79(16) . . . . ? C16 B1 C24 C29 47.82(17) . . . . ? C32 B1 C24 C25 -11.72(18) . . . . ? C40 B1 C24 C25 105.70(15) . . . . ? C16 B1 C24 C25 -133.69(14) . . . . ? C29 C24 C25 C26 0.7(2) . . . . ? B1 C24 C25 C26 -177.87(14) . . . . ? C24 C25 C26 C27 0.2(2) . . . . ? C24 C25 C26 C30 178.81(16) . . . . ? C25 C26 C27 C28 -0.8(2) . . . . ? C30 C26 C27 C28 -179.55(17) . . . . ? C26 C27 C28 C29 0.7(2) . . . . ? C26 C27 C28 C31 179.40(19) . . . . ? C27 C28 C29 C24 0.2(3) . . . . ? C31 C28 C29 C24 -178.54(18) . . . . ? C25 C24 C29 C28 -0.8(2) . . . . ? B1 C24 C29 C28 177.76(14) . . . . ? C27 C26 C30 F7 -163.4(3) . . . . ? C25 C26 C30 F7 17.9(4) . . . . ? C27 C26 C30 F8 73.3(2) . . . . ? C25 C26 C30 F8 -105.4(2) . . . . ? C27 C26 C30 F9 -42.5(2) . . . . ? C25 C26 C30 F9 138.82(17) . . . . ? C27 C28 C31 F10 8.7(5) . . . . ? C29 C28 C31 F10 -172.6(4) . . . . ? C27 C28 C31 F12 134.6(4) . . . . ? C29 C28 C31 F12 -46.6(5) . . . . ? C27 C28 C31 F11 -111.6(3) . . . . ? C29 C28 C31 F11 67.1(3) . . . . ? C24 B1 C32 C33 -104.96(15) . . . . ? C40 B1 C32 C33 134.79(13) . . . . ? C16 B1 C32 C33 15.51(18) . . . . ? C24 B1 C32 C37 74.62(15) . . . . ? C40 B1 C32 C37 -45.64(15) . . . . ? C16 B1 C32 C37 -164.91(12) . . . . ? C37 C32 C33 C34 2.5(2) . . . . ? B1 C32 C33 C34 -177.89(13) . . . . ? C32 C33 C34 C35 -1.8(2) . . . . ? C32 C33 C34 C38 178.64(14) . . . . ? C33 C34 C35 C36 -0.9(2) . . . . ? C38 C34 C35 C36 178.65(14) . . . . ? C34 C35 C36 C37 2.7(2) . . . . ? C34 C35 C36 C39 -174.17(15) . . . . ? C35 C36 C37 C32 -2.0(2) . . . . ? C39 C36 C37 C32 174.93(14) . . . . ? C33 C32 C37 C36 -0.6(2) . . . . ? B1 C32 C37 C36 179.73(13) . . . . ? C35 C34 C38 F14 155.9(3) . . . . ? C33 C34 C38 F14 -24.5(3) . . . . ? C35 C34 C38 F13 -77.1(3) . . . . ? C33 C34 C38 F13 102.5(3) . . . . ? C35 C34 C38 F15 36.9(3) . . . . ? C33 C34 C38 F15 -143.5(2) . . . . ? C35 C36 C39 F18 -24.8(3) . . . . ? C37 C36 C39 F18 158.20(18) . . . . ? C35 C36 C39 F17 -148.71(16) . . . . ? C37 C36 C39 F17 34.3(2) . . . . ? C35 C36 C39 F16 95.10(19) . . . . ? C37 C36 C39 F16 -81.9(2) . . . . ? C24 B1 C40 C41 14.66(18) . . . . ? C32 B1 C40 C41 134.19(13) . . . . ? C16 B1 C40 C41 -105.46(14) . . . . ? C24 B1 C40 C45 -164.92(12) . . . . ? C32 B1 C40 C45 -45.38(15) . . . . ? C16 B1 C40 C45 74.97(15) . . . . ? C45 C40 C41 C42 1.0(2) . . . . ? B1 C40 C41 C42 -178.60(13) . . . . ? C40 C41 C42 C43 -0.2(2) . . . . ? C40 C41 C42 C46 -178.23(13) . . . . ? C41 C42 C43 C44 -0.8(2) . . . . ? C46 C42 C43 C44 177.26(14) . . . . ? C42 C43 C44 C45 0.9(2) . . . . ? C42 C43 C44 C47 179.09(15) . . . . ? C43 C44 C45 C40 -0.1(2) . . . . ? C47 C44 C45 C40 -178.29(14) . . . . ? C41 C40 C45 C44 -0.8(2) . . . . ? B1 C40 C45 C44 178.79(13) . . . . ? C43 C42 C46 F21 138.73(17) . . . . ? C41 C42 C46 F21 -43.2(2) . . . . ? C43 C42 C46 F20 17.8(2) . . . . ? C41 C42 C46 F20 -164.15(15) . . . . ? C43 C42 C46 F19 -99.82(18) . . . . ? C41 C42 C46 F19 78.24(19) . . . . ? C45 C44 C47 F22 87.7(2) . . . . ? C43 C44 C47 F22 -90.5(2) . . . . ? C45 C44 C47 F24 -33.8(3) . . . . ? C43 C44 C47 F24 147.98(19) . . . . ? C45 C44 C47 F23 -153.79(18) . . . . ? C43 C44 C47 F23 28.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 35.10 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.937 _refine_diff_density_min -0.934 _refine_diff_density_rms 0.080 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.250 0.500 230 30 ' ' 2 0.750 0.250 1.000 230 30 ' ' 3 0.750 0.750 0.500 230 30 ' ' 4 0.250 0.750 1.000 230 30 ' ' _platon_squeeze_details ; Acta Cryst. (1990), A46, 194 as the 'BYPASS procedure' P. v.d. Sluis & A.L. Spek ; _database_code_depnum_ccdc_archive 'CCDC 973878' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_x13001 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H65 B2 Cl Cr F48 N5 O2' _chemical_formula_weight 2401.65 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall -C loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.011(6) _cell_length_b 16.672(6) _cell_length_c 28.937(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.074(16) _cell_angle_gamma 90.00 _cell_volume 9654(6) _cell_formula_units_Z 4 _cell_measurement_temperature 110 _cell_measurement_reflns_used 9905 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 24.21 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.652 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4820 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9608 _exptl_absorpt_correction_T_max 0.9851 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 110 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Kappa Axis X8 Apex2' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_reflns_number 65421 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 24.90 _reflns_number_total 8272 _reflns_number_gt 4858 _reflns_threshold_expression >2sigma(I) _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _computing_data_collection Apex2 _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution XS _computing_structure_refinement XL _computing_molecular_graphics NRCVAX _computing_publication_material cif2tables.py _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0964P)^2^+1.9113P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8272 _refine_ls_number_parameters 836 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1195 _refine_ls_R_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1551 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Cr1 Cr 0.0000 0.56897(5) 0.2500 0.0259(3) Uani 1 2 d S . . Cl1 Cl 0.0000 0.70431(9) 0.2500 0.0340(4) Uani 1 2 d S . . N1 N 0.07703(15) 0.5662(2) 0.20185(11) 0.0273(8) Uani 1 1 d . . . N2 N 0.07856(15) 0.56097(19) 0.29686(11) 0.0261(8) Uani 1 1 d . . . N3 N 0.0000 0.4443(3) 0.2500 0.0260(11) Uani 1 2 d S . . C1 C 0.12431(19) 0.5080(3) 0.20428(14) 0.0303(10) Uani 1 1 d . . . C2 C 0.1729(2) 0.5003(3) 0.17092(16) 0.0418(12) Uani 1 1 d . . . H2 H 0.2045 0.4579 0.1724 0.050 Uiso 1 1 calc R . . C3 C 0.1749(2) 0.5549(3) 0.13564(16) 0.0431(12) Uani 1 1 d . . . H3 H 0.2075 0.5499 0.1120 0.052 Uiso 1 1 calc R . . C4 C 0.1297(2) 0.6173(3) 0.13444(15) 0.0385(11) Uani 1 1 d . . . H4 H 0.1319 0.6568 0.1108 0.046 Uiso 1 1 calc R . . C5 C 0.0818(2) 0.6209(3) 0.16798(14) 0.0310(10) Uani 1 1 d . . . H5 H 0.0506 0.6639 0.1673 0.037 Uiso 1 1 calc R . . C6 C 0.12292(19) 0.4525(3) 0.24725(14) 0.0309(10) Uani 1 1 d . . . C7 C 0.1837(2) 0.3959(3) 0.24626(17) 0.0399(11) Uani 1 1 d . . . H7A H 0.2248 0.4277 0.2458 0.060 Uiso 1 1 calc R . . H7B H 0.1816 0.3623 0.2185 0.060 Uiso 1 1 calc R . . H7C H 0.1832 0.3618 0.2738 0.060 Uiso 1 1 calc R . . C8 C 0.12651(19) 0.5041(2) 0.29118(14) 0.0277(10) Uani 1 1 d . . . C9 C 0.17705(19) 0.4960(3) 0.32348(15) 0.0318(10) Uani 1 1 d . . . H9 H 0.2106 0.4565 0.3192 0.038 Uiso 1 1 calc R . . C10 C 0.1790(2) 0.5449(3) 0.36166(14) 0.0327(10) Uani 1 1 d . . . H10 H 0.2126 0.5379 0.3845 0.039 Uiso 1 1 calc R . . C11 C 0.1316(2) 0.6038(3) 0.36628(14) 0.0319(10) Uani 1 1 d . . . H11 H 0.1326 0.6393 0.3920 0.038 Uiso 1 1 calc R . . C12 C 0.08296(19) 0.6106(3) 0.33325(15) 0.0312(10) Uani 1 1 d . . . H12 H 0.0509 0.6523 0.3362 0.037 Uiso 1 1 calc R . . C13 C 0.0585(2) 0.4032(3) 0.24817(15) 0.0317(10) Uani 1 1 d . . . C14 C 0.0593(2) 0.3201(3) 0.24813(16) 0.0396(11) Uani 1 1 d . . . H14 H 0.1006 0.2920 0.2468 0.048 Uiso 1 1 calc R . . C15 C 0.0000 0.2788(4) 0.2500 0.0487(19) Uani 1 2 d S . . H15 H 0.0000 0.2218 0.2500 0.058 Uiso 1 2 calc SR . . B1 B 0.1284(2) 0.1510(3) 0.09498(17) 0.0289(11) Uani 1 1 d . . . C16 C 0.18585(19) 0.1945(2) 0.12713(14) 0.0277(10) Uani 1 1 d . . . C17 C 0.22783(19) 0.2539(2) 0.10865(15) 0.0283(10) Uani 1 1 d . . . H17 H 0.2205 0.2711 0.0778 0.034 Uiso 1 1 calc R . . C18 C 0.27991(19) 0.2887(2) 0.13385(14) 0.0287(10) Uani 1 1 d . . . C19 C 0.29086(19) 0.2665(3) 0.17962(15) 0.0319(10) Uani 1 1 d . . . H19 H 0.3260 0.2899 0.1971 0.038 Uiso 1 1 calc R . . C20 C 0.24914(19) 0.2094(2) 0.19887(14) 0.0287(10) Uani 1 1 d . . . C21 C 0.19788(18) 0.1748(2) 0.17305(14) 0.0268(9) Uani 1 1 d . . . H21 H 0.1699 0.1362 0.1875 0.032 Uiso 1 1 calc R . . C22 C 0.3229(2) 0.3508(3) 0.11219(15) 0.0340(11) Uani 1 1 d . . . F1 F 0.33355(12) 0.33750(16) 0.06748(9) 0.0458(7) Uani 1 1 d . . . F2 F 0.29609(12) 0.42495(15) 0.11474(10) 0.0479(7) Uani 1 1 d . . . F3 F 0.38334(12) 0.35623(16) 0.13207(9) 0.0495(7) Uani 1 1 d . . . C23 C 0.2587(2) 0.1838(3) 0.24744(15) 0.0353(11) Uani 1 1 d . . . F4 F 0.25155(16) 0.10432(16) 0.25380(9) 0.0612(8) Uani 1 1 d . . . F5 F 0.31828(13) 0.2031(2) 0.26477(10) 0.0693(9) Uani 1 1 d . . . F6 F 0.21333(13) 0.21526(16) 0.27639(9) 0.0499(7) Uani 1 1 d . . . C24 C 0.08115(18) 0.2204(2) 0.07102(14) 0.0282(10) Uani 1 1 d . . . C25 C 0.06105(19) 0.2191(2) 0.02464(15) 0.0305(10) Uani 1 1 d . . . H25 H 0.0767 0.1772 0.0052 0.037 Uiso 1 1 calc R . . C26 C 0.01887(19) 0.2772(3) 0.00608(14) 0.0315(10) Uani 1 1 d . . . C27 C -0.00511(19) 0.3395(3) 0.03306(15) 0.0320(10) Uani 1 1 d . A . H27 H -0.0343 0.3788 0.0205 0.038 Uiso 1 1 calc R . . C28 C 0.0146(2) 0.3428(3) 0.07835(15) 0.0334(10) Uani 1 1 d . . . C29 C 0.0572(2) 0.2850(3) 0.09697(15) 0.0353(11) Uani 1 1 d . A . H29 H 0.0705 0.2897 0.1284 0.042 Uiso 1 1 calc R . . C30 C -0.0035(2) 0.2717(4) -0.04284(17) 0.0496(14) Uani 1 1 d . . . F7 F 0.0099(2) 0.3385(3) -0.06613(13) 0.133(2) Uani 1 1 d . . . F8 F 0.0219(3) 0.2151(4) -0.06565(13) 0.203(4) Uani 1 1 d . . . F9 F -0.06808(14) 0.2664(2) -0.04779(10) 0.0710(9) Uani 1 1 d . . . C31 C -0.0091(2) 0.4101(3) 0.10795(16) 0.0501(14) Uani 0.63(3) 1 d PD A 1 F10 F 0.0308(5) 0.4735(6) 0.1056(7) 0.110(5) Uani 0.63(3) 1 d PD A 1 F11 F -0.0673(4) 0.4380(7) 0.0938(4) 0.066(3) Uani 0.63(3) 1 d PD A 1 F12 F -0.0168(10) 0.3943(9) 0.1520(3) 0.132(6) Uani 0.63(3) 1 d PD A 1 C31' C -0.0091(2) 0.4101(3) 0.10795(16) 0.0501(14) Uani 0.37(3) 1 d PD A 2 F10' F -0.0456(13) 0.3791(10) 0.1418(7) 0.095(7) Uani 0.37(3) 1 d PD A 2 F11' F 0.0401(7) 0.4471(17) 0.1296(10) 0.127(10) Uani 0.37(3) 1 d PD A 2 F12' F -0.0461(15) 0.4663(14) 0.0891(6) 0.101(8) Uani 0.37(3) 1 d PD A 2 C32 C 0.16222(19) 0.0937(2) 0.05472(14) 0.0293(10) Uani 1 1 d . . . C33 C 0.12158(19) 0.0376(2) 0.03212(14) 0.0302(10) Uani 1 1 d . B . H33 H 0.0757 0.0348 0.0403 0.036 Uiso 1 1 calc R . . C34 C 0.14539(19) -0.0139(2) -0.00154(15) 0.0306(10) Uani 1 1 d . . . C35 C 0.2122(2) -0.0127(3) -0.01384(15) 0.0334(10) Uani 1 1 d . B . H35 H 0.2292 -0.0493 -0.0360 0.040 Uiso 1 1 calc R . . C36 C 0.25350(18) 0.0432(3) 0.00701(14) 0.0287(10) Uani 1 1 d . . . C37 C 0.22837(19) 0.0960(2) 0.03995(14) 0.0288(10) Uani 1 1 d . B . H37 H 0.2575 0.1351 0.0528 0.035 Uiso 1 1 calc R . . C38 C 0.0984(2) -0.0685(2) -0.02603(15) 0.0437(12) Uani 0.570(19) 1 d PD B 3 F13 F 0.1245(5) -0.1306(6) -0.0466(4) 0.077(4) Uani 0.570(19) 1 d PD B 3 F14 F 0.0622(4) -0.0296(4) -0.0570(3) 0.063(3) Uani 0.570(19) 1 d PD B 3 F15 F 0.0529(4) -0.0964(6) 0.0034(3) 0.059(3) Uani 0.570(19) 1 d PD B 3 C38' C 0.0984(2) -0.0685(2) -0.02603(15) 0.0437(12) Uani 0.430(19) 1 d PD B 4 F13' F 0.0359(4) -0.0695(10) -0.0129(7) 0.107(8) Uani 0.430(19) 1 d PD B 4 F14' F 0.1188(6) -0.1443(4) -0.0231(6) 0.067(4) Uani 0.430(19) 1 d PD B 4 F15' F 0.0978(11) -0.0553(11) -0.0715(3) 0.141(10) Uani 0.430(19) 1 d PD B 4 C39 C 0.3249(2) 0.0478(2) -0.00730(14) 0.0385(11) Uani 0.728(15) 1 d PD B 5 F16 F 0.3500(3) -0.0240(2) -0.0177(2) 0.056(2) Uani 0.728(15) 1 d PD B 5 F17 F 0.3343(4) 0.0906(4) -0.04510(17) 0.056(2) Uani 0.728(15) 1 d PD B 5 F18 F 0.3662(3) 0.0776(5) 0.0237(2) 0.066(3) Uani 0.728(15) 1 d PD B 5 C39' C 0.3249(2) 0.0478(2) -0.00730(14) 0.0385(11) Uani 0.272(15) 1 d PD B 6 F16' F 0.3393(10) 0.1195(11) -0.0243(14) 0.21(2) Uani 0.272(15) 1 d PD B 6 F17' F 0.3613(9) 0.041(2) 0.0305(4) 0.106(11) Uani 0.272(15) 1 d PD B 6 F18' F 0.3475(9) -0.0059(17) -0.0364(10) 0.19(2) Uani 0.272(15) 1 d PD B 6 C40 C 0.08317(19) 0.0911(2) 0.12764(14) 0.0290(10) Uani 1 1 d . . . C41 C 0.0186(2) 0.1075(3) 0.14373(14) 0.0342(11) Uani 1 1 d . C . H41 H -0.0020 0.1566 0.1352 0.041 Uiso 1 1 calc R . . C42 C -0.0163(2) 0.0544(3) 0.17181(15) 0.0369(11) Uani 1 1 d . . . C43 C 0.0116(2) -0.0178(3) 0.18534(16) 0.0417(12) Uani 1 1 d . C . H43 H -0.0124 -0.0543 0.2043 0.050 Uiso 1 1 calc R . . C44 C 0.0756(2) -0.0352(3) 0.17032(15) 0.0345(11) Uani 1 1 d . . . C45 C 0.1097(2) 0.0176(3) 0.14247(15) 0.0323(10) Uani 1 1 d . C . H45 H 0.1535 0.0035 0.1327 0.039 Uiso 1 1 calc R . . C46 C -0.0844(2) 0.0767(3) 0.18884(14) 0.0510(14) Uani 0.718(13) 1 d PD C 7 F19 F -0.1308(4) 0.0237(6) 0.1859(5) 0.163(6) Uani 0.718(13) 1 d PD C 7 F20 F -0.0816(3) 0.1000(4) 0.23231(16) 0.058(2) Uani 0.718(13) 1 d PD C 7 F21 F -0.1079(4) 0.1449(7) 0.1694(3) 0.139(5) Uani 0.718(13) 1 d PD C 7 C46' C -0.0844(2) 0.0767(3) 0.18884(14) 0.0510(14) Uani 0.282(13) 1 d PD C 8 F19' F -0.0918(8) 0.1324(9) 0.2197(6) 0.110(11) Uani 0.282(13) 1 d PD C 8 F20' F -0.1264(6) 0.0902(10) 0.1544(4) 0.066(5) Uani 0.282(13) 1 d PD C 8 F21' F -0.1112(5) 0.0098(6) 0.2078(5) 0.049(5) Uani 0.282(13) 1 d PD C 8 C47 C 0.1066(2) -0.1133(3) 0.18455(19) 0.0474(13) Uani 1 1 d . C . F22 F 0.17326(14) -0.11390(18) 0.18037(14) 0.0847(12) Uani 1 1 d . . . F23 F 0.08596(16) -0.17543(18) 0.16058(12) 0.0738(9) Uani 1 1 d . . . F24 F 0.09438(18) -0.13249(18) 0.22825(11) 0.0778(10) Uani 1 1 d . . . O1S O 0.23446(18) 0.7148(2) 0.06889(13) 0.0670(11) Uani 1 1 d . . . C1S C 0.2244(3) 0.7953(4) 0.0540(2) 0.0814(19) Uani 1 1 d . . . H1S1 H 0.1875 0.8206 0.0715 0.098 Uiso 1 1 calc R . . H1S2 H 0.2135 0.7970 0.0207 0.098 Uiso 1 1 calc R . . C2S C 0.2892(4) 0.8376(4) 0.0635(3) 0.102(2) Uani 1 1 d . . . H2S1 H 0.2814 0.8940 0.0726 0.122 Uiso 1 1 calc R . . H2S2 H 0.3185 0.8367 0.0359 0.122 Uiso 1 1 calc R . . C3S C 0.3203(3) 0.7899(4) 0.1032(2) 0.0771(18) Uani 1 1 d . . . H3S1 H 0.3652 0.7697 0.0948 0.093 Uiso 1 1 calc R . . H3S2 H 0.3241 0.8232 0.1314 0.093 Uiso 1 1 calc R . . C4S C 0.2728(3) 0.7226(4) 0.1103(2) 0.0731(17) Uani 1 1 d . . . H4S1 H 0.2975 0.6723 0.1166 0.088 Uiso 1 1 calc R . . H4S2 H 0.2431 0.7340 0.1368 0.088 Uiso 1 1 calc R . . 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 Cr1 0.0244(5) 0.0246(5) 0.0287(6) 0.000 -0.0019(4) 0.000 Cl1 0.0385(8) 0.0259(8) 0.0375(10) 0.000 0.0017(6) 0.000 N1 0.0249(18) 0.030(2) 0.027(2) -0.0036(16) -0.0062(14) -0.0023(16) N2 0.0266(18) 0.0268(19) 0.025(2) -0.0026(16) 0.0011(14) -0.0021(16) N3 0.033(3) 0.024(3) 0.020(3) 0.000 -0.008(2) 0.000 C1 0.029(2) 0.033(2) 0.029(3) -0.002(2) -0.0020(18) 0.002(2) C2 0.039(3) 0.053(3) 0.033(3) -0.006(2) 0.001(2) 0.010(2) C3 0.035(3) 0.067(4) 0.027(3) -0.002(3) 0.0031(19) 0.005(2) C4 0.038(3) 0.055(3) 0.023(3) 0.003(2) -0.0049(19) -0.002(2) C5 0.033(2) 0.035(3) 0.025(3) 0.004(2) -0.0034(18) 0.000(2) C6 0.030(2) 0.032(2) 0.031(3) -0.001(2) -0.0083(18) 0.0073(19) C7 0.034(2) 0.040(3) 0.046(3) -0.005(2) -0.008(2) 0.011(2) C8 0.027(2) 0.029(2) 0.027(3) 0.0024(19) 0.0000(17) 0.0005(19) C9 0.026(2) 0.033(3) 0.036(3) 0.002(2) -0.0028(18) 0.0033(19) C10 0.033(2) 0.039(3) 0.026(3) 0.000(2) -0.0040(18) -0.009(2) C11 0.034(2) 0.036(3) 0.026(3) 0.000(2) -0.0005(19) -0.011(2) C12 0.026(2) 0.031(2) 0.036(3) -0.003(2) -0.0014(18) -0.0012(19) C13 0.034(2) 0.030(2) 0.031(3) -0.003(2) -0.0097(18) 0.004(2) C14 0.043(3) 0.027(3) 0.048(3) -0.006(2) -0.014(2) 0.006(2) C15 0.059(5) 0.024(4) 0.063(5) 0.000 -0.024(4) 0.000 B1 0.027(2) 0.029(3) 0.031(3) 0.000(2) -0.002(2) 0.003(2) C16 0.030(2) 0.025(2) 0.028(3) -0.0007(19) -0.0010(17) 0.0045(19) C17 0.029(2) 0.028(2) 0.028(3) 0.0017(19) -0.0014(18) 0.0057(19) C18 0.029(2) 0.026(2) 0.032(3) -0.0022(19) 0.0007(18) 0.0045(19) C19 0.030(2) 0.035(3) 0.031(3) -0.011(2) -0.0033(19) 0.007(2) C20 0.030(2) 0.030(2) 0.025(2) 0.0002(19) -0.0029(18) 0.007(2) C21 0.024(2) 0.027(2) 0.029(3) -0.0021(19) 0.0018(17) 0.0065(18) C22 0.032(2) 0.039(3) 0.031(3) -0.007(2) -0.0007(19) 0.000(2) F1 0.0478(15) 0.0543(17) 0.0353(17) -0.0045(13) 0.0087(12) -0.0098(13) F2 0.0486(16) 0.0314(15) 0.0636(19) 0.0028(13) 0.0129(13) 0.0000(12) F3 0.0363(15) 0.0600(18) 0.0522(18) 0.0026(14) -0.0061(12) -0.0130(13) C23 0.039(3) 0.037(3) 0.030(3) -0.001(2) -0.003(2) 0.007(2) F4 0.109(2) 0.0354(16) 0.0390(18) 0.0021(13) -0.0154(15) 0.0175(16) F5 0.0428(16) 0.123(3) 0.0423(19) 0.0202(18) -0.0181(13) -0.0187(17) F6 0.0606(17) 0.0574(18) 0.0316(16) 0.0068(13) 0.0096(13) 0.0217(14) C24 0.023(2) 0.035(3) 0.026(2) -0.002(2) -0.0019(17) -0.0053(19) C25 0.029(2) 0.030(2) 0.032(3) -0.003(2) 0.0007(18) -0.0017(19) C26 0.025(2) 0.044(3) 0.025(3) 0.003(2) -0.0001(18) 0.002(2) C27 0.027(2) 0.034(3) 0.036(3) 0.001(2) -0.0043(18) 0.0012(19) C28 0.034(2) 0.030(2) 0.036(3) -0.002(2) -0.0035(19) 0.000(2) C29 0.035(2) 0.042(3) 0.029(3) -0.002(2) -0.0107(19) 0.003(2) C30 0.039(3) 0.079(4) 0.031(3) 0.010(3) 0.005(2) 0.025(3) F7 0.137(4) 0.207(5) 0.055(2) 0.069(3) -0.042(2) -0.110(4) F8 0.238(6) 0.326(8) 0.044(2) -0.079(4) -0.065(3) 0.235(6) F9 0.058(2) 0.108(3) 0.047(2) 0.0063(18) -0.0221(14) -0.0161(18) C31 0.057(3) 0.043(3) 0.050(4) -0.016(3) -0.016(3) 0.017(3) F10 0.076(6) 0.071(5) 0.183(13) -0.075(7) 0.022(6) -0.021(5) F11 0.049(4) 0.049(5) 0.099(6) -0.041(4) -0.019(3) 0.025(4) F12 0.264(15) 0.101(9) 0.031(4) -0.025(5) -0.029(7) 0.132(10) C31' 0.057(3) 0.043(3) 0.050(4) -0.016(3) -0.016(3) 0.017(3) F10' 0.137(14) 0.098(10) 0.050(11) -0.032(9) 0.035(9) 0.011(9) F11' 0.112(12) 0.111(16) 0.16(2) -0.095(14) -0.078(13) 0.018(11) F12' 0.18(2) 0.051(10) 0.070(9) -0.019(7) -0.059(12) 0.059(11) C32 0.029(2) 0.031(2) 0.027(3) 0.0061(19) -0.0029(18) 0.0018(19) C33 0.024(2) 0.032(2) 0.035(3) 0.001(2) -0.0057(18) 0.0005(19) C34 0.029(2) 0.029(2) 0.033(3) 0.001(2) -0.0042(18) 0.0017(19) C35 0.035(2) 0.036(3) 0.029(3) 0.002(2) 0.0000(18) 0.005(2) C36 0.024(2) 0.034(2) 0.028(3) 0.002(2) -0.0017(17) 0.0025(19) C37 0.030(2) 0.033(2) 0.024(2) 0.003(2) -0.0031(18) -0.0019(19) C38 0.040(3) 0.044(3) 0.047(4) -0.008(3) -0.004(2) -0.008(3) F13 0.051(4) 0.101(7) 0.078(8) -0.071(6) -0.020(5) 0.025(4) F14 0.043(4) 0.078(5) 0.067(6) -0.013(4) -0.024(3) 0.002(4) F15 0.050(5) 0.064(5) 0.063(4) -0.014(4) -0.004(4) -0.030(4) C38' 0.040(3) 0.044(3) 0.047(4) -0.008(3) -0.004(2) -0.008(3) F13' 0.015(4) 0.118(13) 0.188(19) -0.114(12) -0.023(7) 0.014(6) F14' 0.067(6) 0.039(5) 0.094(11) -0.041(5) -0.037(7) 0.002(4) F15' 0.182(18) 0.179(18) 0.063(8) 0.039(9) -0.070(9) -0.139(15) C39 0.037(3) 0.047(3) 0.032(3) 0.001(3) 0.005(2) -0.001(2) F16 0.045(3) 0.037(3) 0.084(5) 0.008(3) 0.026(3) 0.016(2) F17 0.040(3) 0.076(4) 0.054(3) 0.027(3) 0.007(2) 0.002(3) F18 0.034(3) 0.125(6) 0.040(3) -0.039(4) 0.010(3) -0.023(3) C39' 0.037(3) 0.047(3) 0.032(3) 0.001(3) 0.005(2) -0.001(2) F16' 0.059(14) 0.114(18) 0.45(5) 0.20(3) 0.12(2) 0.038(12) F17' 0.013(7) 0.23(3) 0.071(12) 0.070(15) -0.008(6) -0.009(11) F18' 0.055(12) 0.39(5) 0.13(2) -0.19(3) 0.065(13) -0.10(2) C40 0.029(2) 0.031(2) 0.027(3) -0.0002(19) -0.0049(17) -0.0031(19) C41 0.032(2) 0.041(3) 0.029(3) -0.003(2) -0.0013(19) 0.005(2) C42 0.027(2) 0.054(3) 0.029(3) -0.008(2) -0.0020(19) -0.004(2) C43 0.037(3) 0.050(3) 0.038(3) 0.000(2) 0.001(2) -0.011(2) C44 0.037(3) 0.034(3) 0.032(3) 0.001(2) -0.003(2) -0.006(2) C45 0.031(2) 0.036(3) 0.031(3) 0.002(2) 0.0010(18) 0.000(2) C46 0.037(3) 0.084(4) 0.032(3) 0.012(3) 0.006(2) 0.012(3) F19 0.026(4) 0.179(10) 0.284(14) -0.184(9) 0.037(6) -0.043(5) F20 0.050(3) 0.076(4) 0.049(3) -0.020(3) 0.007(2) 0.029(3) F21 0.065(5) 0.254(12) 0.097(6) 0.094(7) 0.043(4) 0.086(7) C46' 0.037(3) 0.084(4) 0.032(3) 0.012(3) 0.006(2) 0.012(3) F19' 0.017(7) 0.053(11) 0.26(3) -0.108(15) -0.022(11) 0.012(8) F20' 0.022(6) 0.103(13) 0.074(10) -0.004(9) -0.017(5) -0.021(7) F21' 0.006(6) 0.078(10) 0.064(9) 0.038(8) 0.012(5) -0.003(5) C47 0.050(3) 0.039(3) 0.054(4) 0.014(3) -0.002(2) -0.008(2) F22 0.0440(18) 0.059(2) 0.151(4) 0.052(2) -0.0059(19) 0.0026(16) F23 0.093(2) 0.0441(18) 0.084(3) -0.0094(17) -0.0205(18) 0.0024(17) F24 0.124(3) 0.058(2) 0.052(2) 0.0223(17) 0.0085(19) 0.0180(19) O1S 0.066(2) 0.077(3) 0.057(3) 0.007(2) -0.0076(19) -0.007(2) C1S 0.083(5) 0.084(5) 0.077(5) 0.018(4) -0.008(3) 0.001(4) C2S 0.105(6) 0.087(5) 0.113(6) 0.032(5) -0.028(5) -0.023(4) C3S 0.081(4) 0.066(4) 0.084(5) 0.001(4) -0.016(3) -0.016(4) C4S 0.076(4) 0.082(5) 0.061(4) 0.002(3) -0.019(3) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cr1 N3 2.078(5) . ? Cr1 N2 2.079(3) 2 ? Cr1 N2 2.079(3) . ? Cr1 N1 2.080(3) . ? Cr1 N1 2.080(3) 2 ? Cr1 Cl1 2.2562(19) . ? N1 C5 1.343(5) . ? N1 C1 1.357(5) . ? N2 C12 1.342(5) . ? N2 C8 1.359(5) . ? N3 C13 1.357(5) . ? N3 C13 1.357(5) 2 ? C1 C2 1.377(6) . ? C1 C6 1.551(6) . ? C2 C3 1.368(6) . ? C2 H2 0.9500 . ? C3 C4 1.378(6) . ? C3 H3 0.9500 . ? C4 C5 1.367(6) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C13 1.529(6) . ? C6 C8 1.537(6) . ? C6 C7 1.538(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.383(5) . ? C9 C10 1.373(6) . ? C9 H9 0.9500 . ? C10 C11 1.372(6) . ? C10 H10 0.9500 . ? C11 C12 1.368(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.385(6) . ? C14 C15 1.374(5) . ? C14 H14 0.9500 . ? C15 C14 1.374(5) 2 ? C15 H15 0.9500 . ? B1 C16 1.646(6) . ? B1 C40 1.647(6) . ? B1 C24 1.647(6) . ? B1 C32 1.652(6) . ? C16 C21 1.389(5) . ? C16 C17 1.404(6) . ? C17 C18 1.397(6) . ? C17 H17 0.9500 . ? C18 C19 1.392(6) . ? C18 C22 1.485(6) . ? C19 C20 1.384(6) . ? C19 H19 0.9500 . ? C20 C21 1.393(5) . ? C20 C23 1.481(6) . ? C21 H21 0.9500 . ? C22 F1 1.330(5) . ? C22 F3 1.342(5) . ? C22 F2 1.349(5) . ? C23 F5 1.332(5) . ? C23 F6 1.343(5) . ? C23 F4 1.346(5) . ? C24 C29 1.398(6) . ? C24 C25 1.401(6) . ? C25 C26 1.391(6) . ? C25 H25 0.9500 . ? C26 C27 1.386(6) . ? C26 C30 1.487(6) . ? C27 C28 1.369(6) . ? C27 H27 0.9500 . ? C28 C29 1.395(6) . ? C28 C31 1.489(6) . ? C29 H29 0.9500 . ? C30 F8 1.259(6) . ? C30 F9 1.303(5) . ? C30 F7 1.330(6) . ? C31 F12 1.310(6) . ? C31 F11 1.319(6) . ? C31 F10 1.327(6) . ? C32 C37 1.392(5) . ? C32 C33 1.401(6) . ? C33 C34 1.384(6) . ? C33 H33 0.9500 . ? C34 C35 1.384(5) . ? C34 C38 1.488(6) . ? C35 C36 1.384(6) . ? C35 H35 0.9500 . ? C36 C37 1.392(6) . ? C36 C39 1.490(5) . ? C37 H37 0.9500 . ? C38 F13 1.303(6) . ? C38 F14 1.322(6) . ? C38 F15 1.330(6) . ? C39 F18 1.315(5) . ? C39 F17 1.319(5) . ? C39 F16 1.333(5) . ? C40 C41 1.400(5) . ? C40 C45 1.403(6) . ? C41 C42 1.391(6) . ? C41 H41 0.9500 . ? C42 C43 1.384(6) . ? C42 C46 1.495(6) . ? C43 C44 1.384(6) . ? C43 H43 0.9500 . ? C44 C45 1.375(6) . ? C44 C47 1.500(6) . ? C45 H45 0.9500 . ? C46 F19 1.285(5) . ? C46 F20 1.318(5) . ? C46 F21 1.353(6) . ? C47 F23 1.313(5) . ? C47 F24 1.327(6) . ? C47 F22 1.340(5) . ? O1S C1S 1.424(7) . ? O1S C4S 1.428(6) . ? C1S C2S 1.501(8) . ? C1S H1S1 0.9900 . ? C1S H1S2 0.9900 . ? C2S C3S 1.530(9) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.485(8) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? 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 N3 Cr1 N2 86.32(9) . 2 ? N3 Cr1 N2 86.32(9) . . ? N2 Cr1 N2 172.64(18) 2 . ? N3 Cr1 N1 88.72(9) . . ? N2 Cr1 N1 97.01(12) 2 . ? N2 Cr1 N1 82.82(12) . . ? N3 Cr1 N1 88.72(9) . 2 ? N2 Cr1 N1 82.82(12) 2 2 ? N2 Cr1 N1 97.01(12) . 2 ? N1 Cr1 N1 177.44(18) . 2 ? N3 Cr1 Cl1 180.0 . . ? N2 Cr1 Cl1 93.68(9) 2 . ? N2 Cr1 Cl1 93.68(9) . . ? N1 Cr1 Cl1 91.28(9) . . ? N1 Cr1 Cl1 91.28(9) 2 . ? C5 N1 C1 118.3(3) . . ? C5 N1 Cr1 121.8(3) . . ? C1 N1 Cr1 119.9(3) . . ? C12 N2 C8 118.6(3) . . ? C12 N2 Cr1 121.4(3) . . ? C8 N2 Cr1 120.0(3) . . ? C13 N3 C13 119.3(5) . 2 ? C13 N3 Cr1 120.3(2) . . ? C13 N3 Cr1 120.3(2) 2 . ? N1 C1 C2 121.5(4) . . ? N1 C1 C6 117.1(3) . . ? C2 C1 C6 121.4(4) . . ? C3 C2 C1 118.9(4) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C2 C3 C4 120.0(4) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? N1 C5 C4 122.6(4) . . ? N1 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C13 C6 C8 109.0(3) . . ? C13 C6 C7 109.7(3) . . ? C8 C6 C7 108.8(3) . . ? C13 C6 C1 110.5(3) . . ? C8 C6 C1 109.1(3) . . ? C7 C6 C1 109.6(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 120.1(4) . . ? N2 C8 C6 117.3(3) . . ? C9 C8 C6 122.5(4) . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.0(4) . . ? C11 C10 H10 120.5 . . ? C9 C10 H10 120.5 . . ? C12 C11 C10 118.8(4) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N2 C12 C11 122.9(4) . . ? N2 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? N3 C13 C14 121.1(4) . . ? N3 C13 C6 117.2(4) . . ? C14 C13 C6 121.7(4) . . ? C15 C14 C13 119.4(4) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C14 119.8(6) . 2 ? C14 C15 H15 120.1 . . ? C14 C15 H15 120.1 2 . ? C16 B1 C40 109.1(3) . . ? C16 B1 C24 109.2(3) . . ? C40 B1 C24 110.6(3) . . ? C16 B1 C32 111.5(3) . . ? C40 B1 C32 106.3(3) . . ? C24 B1 C32 110.2(3) . . ? C21 C16 C17 115.3(4) . . ? C21 C16 B1 123.8(4) . . ? C17 C16 B1 120.9(4) . . ? C18 C17 C16 122.7(4) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C19 C18 C17 120.2(4) . . ? C19 C18 C22 119.7(4) . . ? C17 C18 C22 120.1(4) . . ? C20 C19 C18 118.1(4) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C21 120.8(4) . . ? C19 C20 C23 120.2(4) . . ? C21 C20 C23 119.0(4) . . ? C16 C21 C20 122.8(4) . . ? C16 C21 H21 118.6 . . ? C20 C21 H21 118.6 . . ? F1 C22 F3 106.4(3) . . ? F1 C22 F2 105.7(4) . . ? F3 C22 F2 105.8(3) . . ? F1 C22 C18 112.8(4) . . ? F3 C22 C18 112.8(4) . . ? F2 C22 C18 112.7(3) . . ? F5 C23 F6 106.1(4) . . ? F5 C23 F4 106.3(4) . . ? F6 C23 F4 103.1(3) . . ? F5 C23 C20 113.7(4) . . ? F6 C23 C20 113.1(3) . . ? F4 C23 C20 113.6(4) . . ? C29 C24 C25 115.4(4) . . ? C29 C24 B1 120.8(4) . . ? C25 C24 B1 123.9(4) . . ? C26 C25 C24 122.2(4) . . ? C26 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? C27 C26 C25 121.0(4) . . ? C27 C26 C30 118.6(4) . . ? C25 C26 C30 120.4(4) . . ? C28 C27 C26 118.0(4) . . ? C28 C27 H27 121.0 . . ? C26 C27 H27 121.0 . . ? C27 C28 C29 121.2(4) . . ? C27 C28 C31 119.2(4) . . ? C29 C28 C31 119.6(4) . . ? C28 C29 C24 122.3(4) . . ? C28 C29 H29 118.8 . . ? C24 C29 H29 118.8 . . ? F8 C30 F9 106.9(5) . . ? F8 C30 F7 106.3(5) . . ? F9 C30 F7 101.7(4) . . ? F8 C30 C26 115.1(4) . . ? F9 C30 C26 114.0(4) . . ? F7 C30 C26 111.7(5) . . ? F12 C31 F11 105.5(6) . . ? F12 C31 F10 106.3(6) . . ? F11 C31 F10 103.5(6) . . ? F12 C31 C28 116.5(6) . . ? F11 C31 C28 111.7(5) . . ? F10 C31 C28 112.3(6) . . ? C37 C32 C33 115.3(4) . . ? C37 C32 B1 126.2(4) . . ? C33 C32 B1 118.5(3) . . ? C34 C33 C32 122.9(4) . . ? C34 C33 H33 118.6 . . ? C32 C33 H33 118.6 . . ? C35 C34 C33 120.3(4) . . ? C35 C34 C38 119.8(4) . . ? C33 C34 C38 119.8(4) . . ? C34 C35 C36 118.4(4) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C35 C36 C37 120.5(4) . . ? C35 C36 C39 119.1(4) . . ? C37 C36 C39 120.3(4) . . ? C32 C37 C36 122.5(4) . . ? C32 C37 H37 118.8 . . ? C36 C37 H37 118.8 . . ? F13 C38 F14 107.5(6) . . ? F13 C38 F15 106.8(6) . . ? F14 C38 F15 103.3(5) . . ? F13 C38 C34 116.8(6) . . ? F14 C38 C34 111.5(5) . . ? F15 C38 C34 109.9(5) . . ? F18 C39 F17 105.8(5) . . ? F18 C39 F16 104.9(5) . . ? F17 C39 F16 104.1(5) . . ? F18 C39 C36 115.6(5) . . ? F17 C39 C36 113.3(4) . . ? F16 C39 C36 112.3(4) . . ? C41 C40 C45 114.6(4) . . ? C41 C40 B1 125.5(4) . . ? C45 C40 B1 119.8(3) . . ? C42 C41 C40 122.3(4) . . ? C42 C41 H41 118.8 . . ? C40 C41 H41 118.8 . . ? C43 C42 C41 121.1(4) . . ? C43 C42 C46 119.4(4) . . ? C41 C42 C46 119.5(4) . . ? C42 C43 C44 117.8(4) . . ? C42 C43 H43 121.1 . . ? C44 C43 H43 121.1 . . ? C45 C44 C43 120.6(4) . . ? C45 C44 C47 120.8(4) . . ? C43 C44 C47 118.6(4) . . ? C44 C45 C40 123.5(4) . . ? C44 C45 H45 118.3 . . ? C40 C45 H45 118.3 . . ? F19 C46 F20 107.2(6) . . ? F19 C46 F21 107.4(5) . . ? F20 C46 F21 99.5(5) . . ? F19 C46 C42 117.7(5) . . ? F20 C46 C42 110.5(4) . . ? F21 C46 C42 112.9(4) . . ? F23 C47 F24 104.8(4) . . ? F23 C47 F22 105.0(4) . . ? F24 C47 F22 105.6(4) . . ? F23 C47 C44 114.2(4) . . ? F24 C47 C44 113.2(4) . . ? F22 C47 C44 113.1(4) . . ? C1S O1S C4S 104.0(5) . . ? O1S C1S C2S 105.5(5) . . ? O1S C1S H1S1 110.6 . . ? C2S C1S H1S1 110.6 . . ? O1S C1S H1S2 110.6 . . ? C2S C1S H1S2 110.6 . . ? H1S1 C1S H1S2 108.8 . . ? C1S C2S C3S 104.1(5) . . ? C1S C2S H2S1 110.9 . . ? C3S C2S H2S1 110.9 . . ? C1S C2S H2S2 110.9 . . ? C3S C2S H2S2 110.9 . . ? H2S1 C2S H2S2 109.0 . . ? C4S C3S C2S 103.6(5) . . ? C4S C3S H3S1 111.0 . . ? C2S C3S H3S1 111.0 . . ? C4S C3S H3S2 111.0 . . ? C2S C3S H3S2 111.0 . . ? H3S1 C3S H3S2 109.0 . . ? O1S C4S C3S 107.3(5) . . ? O1S C4S H4S1 110.3 . . ? C3S C4S H4S1 110.3 . . ? O1S C4S H4S2 110.3 . . ? C3S C4S H4S2 110.3 . . ? H4S1 C4S H4S2 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cr1 N1 C5 144.5(3) . . . . ? N2 Cr1 N1 C5 58.3(3) 2 . . . ? N2 Cr1 N1 C5 -129.1(3) . . . . ? N1 Cr1 N1 C5 144.5(3) 2 . . . ? Cl1 Cr1 N1 C5 -35.5(3) . . . . ? N3 Cr1 N1 C1 -35.7(3) . . . . ? N2 Cr1 N1 C1 -121.8(3) 2 . . . ? N2 Cr1 N1 C1 50.8(3) . . . . ? N1 Cr1 N1 C1 -35.7(3) 2 . . . ? Cl1 Cr1 N1 C1 144.3(3) . . . . ? N3 Cr1 N2 C12 -139.7(3) . . . . ? N2 Cr1 N2 C12 -139.7(3) 2 . . . ? N1 Cr1 N2 C12 131.1(3) . . . . ? N1 Cr1 N2 C12 -51.5(3) 2 . . . ? Cl1 Cr1 N2 C12 40.3(3) . . . . ? N3 Cr1 N2 C8 39.7(3) . . . . ? N2 Cr1 N2 C8 39.7(3) 2 . . . ? N1 Cr1 N2 C8 -49.5(3) . . . . ? N1 Cr1 N2 C8 127.9(3) 2 . . . ? Cl1 Cr1 N2 C8 -140.3(3) . . . . ? N2 Cr1 N3 C13 136.6(2) 2 . . . ? N2 Cr1 N3 C13 -43.4(2) . . . . ? N1 Cr1 N3 C13 39.5(2) . . . . ? N1 Cr1 N3 C13 -140.5(2) 2 . . . ? Cl1 Cr1 N3 C13 -3(100) . . . . ? N2 Cr1 N3 C13 -43.4(2) 2 . . 2 ? N2 Cr1 N3 C13 136.6(2) . . . 2 ? N1 Cr1 N3 C13 -140.5(2) . . . 2 ? N1 Cr1 N3 C13 39.5(2) 2 . . 2 ? Cl1 Cr1 N3 C13 177(100) . . . 2 ? C5 N1 C1 C2 -5.5(6) . . . . ? Cr1 N1 C1 C2 174.7(3) . . . . ? C5 N1 C1 C6 172.2(3) . . . . ? Cr1 N1 C1 C6 -7.6(5) . . . . ? N1 C1 C2 C3 2.8(7) . . . . ? C6 C1 C2 C3 -174.8(4) . . . . ? C1 C2 C3 C4 1.3(7) . . . . ? C2 C3 C4 C5 -2.6(7) . . . . ? C1 N1 C5 C4 4.1(6) . . . . ? Cr1 N1 C5 C4 -176.0(3) . . . . ? C3 C4 C5 N1 -0.1(6) . . . . ? N1 C1 C6 C13 64.2(5) . . . . ? C2 C1 C6 C13 -118.1(4) . . . . ? N1 C1 C6 C8 -55.6(4) . . . . ? C2 C1 C6 C8 122.1(4) . . . . ? N1 C1 C6 C7 -174.7(3) . . . . ? C2 C1 C6 C7 3.0(5) . . . . ? C12 N2 C8 C9 2.6(6) . . . . ? Cr1 N2 C8 C9 -176.8(3) . . . . ? C12 N2 C8 C6 -175.5(3) . . . . ? Cr1 N2 C8 C6 5.0(4) . . . . ? C13 C6 C8 N2 -63.7(4) . . . . ? C7 C6 C8 N2 176.7(3) . . . . ? C1 C6 C8 N2 57.1(4) . . . . ? C13 C6 C8 C9 118.2(4) . . . . ? C7 C6 C8 C9 -1.4(5) . . . . ? C1 C6 C8 C9 -121.0(4) . . . . ? N2 C8 C9 C10 0.4(6) . . . . ? C6 C8 C9 C10 178.5(4) . . . . ? C8 C9 C10 C11 -2.6(6) . . . . ? C9 C10 C11 C12 1.7(6) . . . . ? C8 N2 C12 C11 -3.6(6) . . . . ? Cr1 N2 C12 C11 175.8(3) . . . . ? C10 C11 C12 N2 1.4(6) . . . . ? C13 N3 C13 C14 0.0(3) 2 . . . ? Cr1 N3 C13 C14 -180.0(3) . . . . ? C13 N3 C13 C6 -178.7(4) 2 . . . ? Cr1 N3 C13 C6 1.3(4) . . . . ? C8 C6 C13 N3 59.7(4) . . . . ? C7 C6 C13 N3 178.8(3) . . . . ? C1 C6 C13 N3 -60.2(4) . . . . ? C8 C6 C13 C14 -119.0(4) . . . . ? C7 C6 C13 C14 0.1(6) . . . . ? C1 C6 C13 C14 121.1(4) . . . . ? N3 C13 C14 C15 0.0(6) . . . . ? C6 C13 C14 C15 178.6(3) . . . . ? C13 C14 C15 C14 0.0(3) . . . 2 ? C40 B1 C16 C21 7.2(5) . . . . ? C24 B1 C16 C21 128.1(4) . . . . ? C32 B1 C16 C21 -109.9(4) . . . . ? C40 B1 C16 C17 -174.6(3) . . . . ? C24 B1 C16 C17 -53.7(5) . . . . ? C32 B1 C16 C17 68.3(5) . . . . ? C21 C16 C17 C18 2.5(5) . . . . ? B1 C16 C17 C18 -175.8(4) . . . . ? C16 C17 C18 C19 -1.8(6) . . . . ? C16 C17 C18 C22 179.6(4) . . . . ? C17 C18 C19 C20 0.3(6) . . . . ? C22 C18 C19 C20 178.9(4) . . . . ? C18 C19 C20 C21 0.3(6) . . . . ? C18 C19 C20 C23 -180.0(4) . . . . ? C17 C16 C21 C20 -1.9(6) . . . . ? B1 C16 C21 C20 176.4(4) . . . . ? C19 C20 C21 C16 0.5(6) . . . . ? C23 C20 C21 C16 -179.2(4) . . . . ? C19 C18 C22 F1 146.0(4) . . . . ? C17 C18 C22 F1 -35.4(5) . . . . ? C19 C18 C22 F3 25.4(5) . . . . ? C17 C18 C22 F3 -156.0(4) . . . . ? C19 C18 C22 F2 -94.4(4) . . . . ? C17 C18 C22 F2 84.2(5) . . . . ? C19 C20 C23 F5 -17.0(6) . . . . ? C21 C20 C23 F5 162.7(4) . . . . ? C19 C20 C23 F6 104.1(4) . . . . ? C21 C20 C23 F6 -76.2(5) . . . . ? C19 C20 C23 F4 -138.8(4) . . . . ? C21 C20 C23 F4 40.9(5) . . . . ? C16 B1 C24 C29 -45.2(5) . . . . ? C40 B1 C24 C29 74.8(5) . . . . ? C32 B1 C24 C29 -168.0(3) . . . . ? C16 B1 C24 C25 136.0(4) . . . . ? C40 B1 C24 C25 -104.0(4) . . . . ? C32 B1 C24 C25 13.2(5) . . . . ? C29 C24 C25 C26 -1.5(6) . . . . ? B1 C24 C25 C26 177.4(4) . . . . ? C24 C25 C26 C27 0.2(6) . . . . ? C24 C25 C26 C30 -177.5(4) . . . . ? C25 C26 C27 C28 0.8(6) . . . . ? C30 C26 C27 C28 178.5(4) . . . . ? C26 C27 C28 C29 -0.4(6) . . . . ? C26 C27 C28 C31 178.7(4) . . . . ? C27 C28 C29 C24 -1.0(7) . . . . ? C31 C28 C29 C24 179.9(4) . . . . ? C25 C24 C29 C28 1.9(6) . . . . ? B1 C24 C29 C28 -177.0(4) . . . . ? C27 C26 C30 F8 177.9(6) . . . . ? C25 C26 C30 F8 -4.4(8) . . . . ? C27 C26 C30 F9 -58.0(6) . . . . ? C25 C26 C30 F9 119.7(5) . . . . ? C27 C26 C30 F7 56.5(6) . . . . ? C25 C26 C30 F7 -125.8(5) . . . . ? C27 C28 C31 F12 149.2(11) . . . . ? C29 C28 C31 F12 -31.7(12) . . . . ? C27 C28 C31 F11 27.9(9) . . . . ? C29 C28 C31 F11 -153.1(8) . . . . ? C27 C28 C31 F10 -87.9(11) . . . . ? C29 C28 C31 F10 91.1(11) . . . . ? C16 B1 C32 C37 -16.6(6) . . . . ? C40 B1 C32 C37 -135.4(4) . . . . ? C24 B1 C32 C37 104.8(4) . . . . ? C16 B1 C32 C33 164.4(4) . . . . ? C40 B1 C32 C33 45.6(5) . . . . ? C24 B1 C32 C33 -74.2(5) . . . . ? C37 C32 C33 C34 1.9(6) . . . . ? B1 C32 C33 C34 -179.0(4) . . . . ? C32 C33 C34 C35 1.1(6) . . . . ? C32 C33 C34 C38 -176.3(4) . . . . ? C33 C34 C35 C36 -2.5(6) . . . . ? C38 C34 C35 C36 174.9(4) . . . . ? C34 C35 C36 C37 0.8(6) . . . . ? C34 C35 C36 C39 -177.4(4) . . . . ? C33 C32 C37 C36 -3.6(6) . . . . ? B1 C32 C37 C36 177.3(4) . . . . ? C35 C36 C37 C32 2.4(6) . . . . ? C39 C36 C37 C32 -179.5(4) . . . . ? C35 C34 C38 F13 22.4(9) . . . . ? C33 C34 C38 F13 -160.2(8) . . . . ? C35 C34 C38 F14 -101.7(6) . . . . ? C33 C34 C38 F14 75.7(6) . . . . ? C35 C34 C38 F15 144.2(7) . . . . ? C33 C34 C38 F15 -38.3(7) . . . . ? C35 C36 C39 F18 -155.2(6) . . . . ? C37 C36 C39 F18 26.6(7) . . . . ? C35 C36 C39 F17 82.5(6) . . . . ? C37 C36 C39 F17 -95.7(6) . . . . ? C35 C36 C39 F16 -35.0(6) . . . . ? C37 C36 C39 F16 146.8(5) . . . . ? C16 B1 C40 C41 103.6(4) . . . . ? C24 B1 C40 C41 -16.5(6) . . . . ? C32 B1 C40 C41 -136.1(4) . . . . ? C16 B1 C40 C45 -74.9(5) . . . . ? C24 B1 C40 C45 165.0(4) . . . . ? C32 B1 C40 C45 45.5(5) . . . . ? C45 C40 C41 C42 -0.6(6) . . . . ? B1 C40 C41 C42 -179.1(4) . . . . ? C40 C41 C42 C43 0.2(7) . . . . ? C40 C41 C42 C46 178.3(4) . . . . ? C41 C42 C43 C44 0.5(6) . . . . ? C46 C42 C43 C44 -177.6(4) . . . . ? C42 C43 C44 C45 -0.7(6) . . . . ? C42 C43 C44 C47 -179.8(4) . . . . ? C43 C44 C45 C40 0.2(7) . . . . ? C47 C44 C45 C40 179.4(4) . . . . ? C41 C40 C45 C44 0.4(6) . . . . ? B1 C40 C45 C44 179.0(4) . . . . ? C43 C42 C46 F19 -48.0(10) . . . . ? C41 C42 C46 F19 133.9(9) . . . . ? C43 C42 C46 F20 75.6(6) . . . . ? C41 C42 C46 F20 -102.5(6) . . . . ? C43 C42 C46 F21 -174.0(7) . . . . ? C41 C42 C46 F21 7.9(8) . . . . ? C45 C44 C47 F23 -100.4(5) . . . . ? C43 C44 C47 F23 78.8(6) . . . . ? C45 C44 C47 F24 139.8(4) . . . . ? C43 C44 C47 F24 -41.0(6) . . . . ? C45 C44 C47 F22 19.7(7) . . . . ? C43 C44 C47 F22 -161.1(4) . . . . ? C4S O1S C1S C2S 39.3(6) . . . . ? O1S C1S C2S C3S -26.2(7) . . . . ? C1S C2S C3S C4S 3.7(8) . . . . ? C1S O1S C4S C3S -37.4(6) . . . . ? C2S C3S C4S O1S 20.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 24.90 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.594 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 973879'