# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Babil Menjon' _publ_contact_author_address ; Facultad de Ciencias (Edificio D) C/Pedro Cerbuna 12 Zaragoza E-50010 ; _publ_contact_author_email menjon@unizar.es _publ_author_name 'Babil Menjon' # Attachment '- Cr paper.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 777393' #TrackingRef '- Cr paper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H56 Cl2 Cr F20 N3' _chemical_formula_weight 1213.89 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 14.0188(19) _cell_length_b 19.074(3) _cell_length_c 20.581(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.079(3) _cell_angle_gamma 90.00 _cell_volume 5499.8(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 872 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 23.7 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2484 _exptl_absorpt_coefficient_mu 0.411 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8867 _exptl_absorpt_correction_T_max 0.9798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14925 _diffrn_reflns_av_R_equivalents 0.0457 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.08 _reflns_number_total 8005 _reflns_number_gt 6950 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0500P)^2^+3.3117P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 8005 _refine_ls_number_parameters 721 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1189 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _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 Cr Cr 0.10454(5) -0.12348(4) -0.06758(4) 0.01622(18) Uani 1 1 d . . . F2 F 0.0945(2) 0.04625(16) -0.03141(15) 0.0293(8) Uani 1 1 d . . . F3 F -0.0025(3) 0.12004(17) 0.05325(18) 0.0389(9) Uani 1 1 d . . . F4 F -0.1355(3) 0.0585(2) 0.12639(17) 0.0428(10) Uani 1 1 d . . . F5 F -0.1736(2) -0.0817(2) 0.11062(18) 0.0404(9) Uani 1 1 d . . . F6 F -0.0783(2) -0.15742(17) 0.02757(15) 0.0291(8) Uani 1 1 d . . . F8 F 0.0283(2) -0.28867(16) -0.08477(15) 0.0275(7) Uani 1 1 d . . . F9 F -0.1235(2) -0.34599(16) -0.14466(17) 0.0347(8) Uani 1 1 d . . . F10 F -0.2584(2) -0.26490(19) -0.20641(16) 0.0366(9) Uani 1 1 d . . . F11 F -0.2380(2) -0.12354(18) -0.20697(15) 0.0317(8) Uani 1 1 d . . . F12 F -0.0920(2) -0.06257(15) -0.14308(16) 0.0256(7) Uani 1 1 d . . . F14 F 0.3012(2) -0.21913(16) -0.04046(14) 0.0267(7) Uani 1 1 d . . . F15 F 0.4055(2) -0.30126(17) -0.11374(16) 0.0315(8) Uani 1 1 d . . . F16 F 0.3530(3) -0.32434(19) -0.24087(17) 0.0402(9) Uani 1 1 d . . . F17 F 0.1956(2) -0.26030(18) -0.29331(16) 0.0347(8) Uani 1 1 d . . . F18 F 0.0939(2) -0.17316(17) -0.22330(14) 0.0270(7) Uani 1 1 d . . . F20 F 0.2950(2) -0.04346(17) -0.12579(14) 0.0249(7) Uani 1 1 d . . . F21 F 0.4446(2) 0.02174(16) -0.07210(17) 0.0306(8) Uani 1 1 d . . . F22 F 0.4726(2) 0.02546(19) 0.05935(18) 0.0396(9) Uani 1 1 d . . . F23 F 0.3398(3) -0.03280(19) 0.13640(15) 0.0391(9) Uani 1 1 d . . . F24 F 0.1859(2) -0.09401(17) 0.08502(15) 0.0302(8) Uani 1 1 d . . . N1 N 0.1156(3) -0.2373(2) 0.0469(2) 0.0218(10) Uani 1 1 d . A . N2 N 0.1034(3) -0.0158(3) -0.1868(2) 0.0245(11) Uani 1 1 d . . . C1 C 0.0162(4) -0.0609(3) -0.0062(2) 0.0197(12) Uani 1 1 d . . . C2 C 0.0294(4) 0.0108(3) 0.0029(3) 0.0223(12) Uani 1 1 d . . . C3 C -0.0199(4) 0.0506(3) 0.0466(3) 0.0261(13) Uani 1 1 d . . . C4 C -0.0872(4) 0.0197(3) 0.0836(3) 0.0299(14) Uani 1 1 d . . . C5 C -0.1044(4) -0.0498(3) 0.0750(3) 0.0252(13) Uani 1 1 d . . . C6 C -0.0545(4) -0.0880(3) 0.0314(3) 0.0224(12) Uani 1 1 d . . . C7 C -0.0212(4) -0.1718(3) -0.1100(3) 0.0195(12) Uani 1 1 d . . . C8 C -0.0359(4) -0.2436(3) -0.1133(3) 0.0230(12) Uani 1 1 d . . . C9 C -0.1142(4) -0.2759(3) -0.1447(3) 0.0249(13) Uani 1 1 d . . . C10 C -0.1821(4) -0.2352(3) -0.1757(3) 0.0236(13) Uani 1 1 d . . . C11 C -0.1711(4) -0.1633(3) -0.1750(3) 0.0237(12) Uani 1 1 d . . . C12 C -0.0934(4) -0.1349(3) -0.1418(3) 0.0203(12) Uani 1 1 d . . . C13 C 0.1901(4) -0.1901(3) -0.1268(3) 0.0172(11) Uani 1 1 d . . . C14 C 0.2710(4) -0.2252(3) -0.1036(3) 0.0211(12) Uani 1 1 d . . . C15 C 0.3260(4) -0.2694(3) -0.1406(3) 0.0205(12) Uani 1 1 d . . . C16 C 0.3006(4) -0.2811(3) -0.2050(3) 0.0238(13) Uani 1 1 d . . . C17 C 0.2215(4) -0.2487(3) -0.2301(3) 0.0269(13) Uani 1 1 d . . . C18 C 0.1698(4) -0.2037(3) -0.1924(3) 0.0216(12) Uani 1 1 d . . . C19 C 0.2291(4) -0.0731(3) -0.0240(2) 0.0180(11) Uani 1 1 d . . . C20 C 0.3000(4) -0.0428(3) -0.0600(2) 0.0189(12) Uani 1 1 d . . . C21 C 0.3800(4) -0.0093(3) -0.0340(3) 0.0223(12) Uani 1 1 d . . . C22 C 0.3942(4) -0.0055(3) 0.0327(3) 0.0272(13) Uani 1 1 d . . . C23 C 0.3266(4) -0.0348(3) 0.0715(3) 0.0251(13) Uani 1 1 d . . . C24 C 0.2482(4) -0.0670(3) 0.0427(3) 0.0202(12) Uani 1 1 d . . . C25 C 0.1120(4) -0.1977(3) 0.0051(3) 0.0194(12) Uani 1 1 d . . . C26 C 0.1134(4) -0.2851(3) 0.1012(3) 0.0254(13) Uani 1 1 d D . . C27 C 0.1547(16) -0.2511(11) 0.1615(7) 0.079(8) Uani 0.50 1 d PD A 1 H27A H 0.2200 -0.2356 0.1539 0.118 Uiso 0.50 1 calc PR A 1 H27B H 0.1556 -0.2850 0.1974 0.118 Uiso 0.50 1 calc PR A 1 H27C H 0.1156 -0.2106 0.1727 0.118 Uiso 0.50 1 calc PR A 1 C28 C 0.0134(9) -0.3109(12) 0.1072(14) 0.043(6) Uani 0.50 1 d PD A 1 H28A H -0.0075 -0.3344 0.0668 0.065 Uiso 0.50 1 calc PR A 1 H28B H -0.0288 -0.2712 0.1153 0.065 Uiso 0.50 1 calc PR A 1 H28C H 0.0111 -0.3441 0.1434 0.065 Uiso 0.50 1 calc PR A 1 C29 C 0.1775(15) -0.3421(8) 0.0777(9) 0.074(7) Uani 0.50 1 d PD A 1 H29A H 0.1485 -0.3636 0.0385 0.111 Uiso 0.50 1 calc PR A 1 H29B H 0.1862 -0.3778 0.1116 0.111 Uiso 0.50 1 calc PR A 1 H29C H 0.2396 -0.3221 0.0676 0.111 Uiso 0.50 1 calc PR A 1 C27' C 0.0881(18) -0.2389(9) 0.1575(7) 0.079(8) Uani 0.50 1 d PD A 2 H27D H 0.1393 -0.2048 0.1660 0.119 Uiso 0.50 1 calc PR A 2 H27E H 0.0800 -0.2679 0.1963 0.119 Uiso 0.50 1 calc PR A 2 H27F H 0.0284 -0.2140 0.1468 0.119 Uiso 0.50 1 calc PR A 2 C28' C 0.0316(13) -0.3347(12) 0.0921(15) 0.054(8) Uani 0.50 1 d PD A 2 H28D H -0.0270 -0.3083 0.0820 0.082 Uiso 0.50 1 calc PR A 2 H28E H 0.0240 -0.3617 0.1321 0.082 Uiso 0.50 1 calc PR A 2 H28F H 0.0441 -0.3668 0.0562 0.082 Uiso 0.50 1 calc PR A 2 C29' C 0.2078(10) -0.3199(12) 0.1156(10) 0.078(7) Uani 0.50 1 d PD A 2 H29D H 0.2572 -0.2841 0.1223 0.116 Uiso 0.50 1 calc PR A 2 H29E H 0.2239 -0.3498 0.0788 0.116 Uiso 0.50 1 calc PR A 2 H29F H 0.2038 -0.3486 0.1549 0.116 Uiso 0.50 1 calc PR A 2 C30 C 0.1023(4) -0.0513(3) -0.1426(3) 0.0186(11) Uani 1 1 d . . . C31 C 0.1103(4) 0.0239(3) -0.2471(3) 0.0453(19) Uani 1 1 d D . . C32 C 0.1259(7) -0.0287(4) -0.3019(4) 0.069(3) Uani 1 1 d D . . H32A H 0.0692 -0.0584 -0.3078 0.104 Uiso 1 1 calc R . . H32B H 0.1815 -0.0580 -0.2908 0.104 Uiso 1 1 calc R . . H32C H 0.1368 -0.0033 -0.3424 0.104 Uiso 1 1 calc R . . C33 C 0.0175(6) 0.0578(5) -0.2610(5) 0.088(3) Uani 1 1 d D . . H33A H 0.0051 0.0923 -0.2270 0.132 Uiso 1 1 calc R . . H33B H -0.0331 0.0223 -0.2621 0.132 Uiso 1 1 calc R . . H33C H 0.0186 0.0815 -0.3033 0.132 Uiso 1 1 calc R . . C34 C 0.1977(5) 0.0687(4) -0.2406(3) 0.0468(19) Uani 1 1 d D . . H34A H 0.1888 0.1042 -0.2069 0.070 Uiso 1 1 calc R . . H34B H 0.2085 0.0920 -0.2822 0.070 Uiso 1 1 calc R . . H34C H 0.2529 0.0394 -0.2285 0.070 Uiso 1 1 calc R . . N3 N 0.6074(3) -0.1703(2) -0.0320(2) 0.0167(10) Uani 1 1 d . . . C35 C 0.5853(4) -0.1794(3) -0.1046(2) 0.0194(12) Uani 1 1 d . . . H35A H 0.6447 -0.1708 -0.1279 0.023 Uiso 1 1 calc R . . H35B H 0.5668 -0.2288 -0.1125 0.023 Uiso 1 1 calc R . . C36 C 0.5079(4) -0.1329(3) -0.1342(3) 0.0228(12) Uani 1 1 d . . . H36A H 0.5243 -0.0831 -0.1262 0.027 Uiso 1 1 calc R . . H36B H 0.4466 -0.1429 -0.1136 0.027 Uiso 1 1 calc R . . C37 C 0.4972(4) -0.1458(3) -0.2067(3) 0.0254(13) Uani 1 1 d . . . H37A H 0.4864 -0.1965 -0.2144 0.030 Uiso 1 1 calc R . . H37B H 0.5574 -0.1328 -0.2273 0.030 Uiso 1 1 calc R . . C38 C 0.4154(4) -0.1048(3) -0.2389(3) 0.0332(15) Uani 1 1 d . . . H38A H 0.4118 -0.1152 -0.2855 0.050 Uiso 1 1 calc R . . H38B H 0.4264 -0.0544 -0.2325 0.050 Uiso 1 1 calc R . . H38C H 0.3553 -0.1181 -0.2194 0.050 Uiso 1 1 calc R . . C39 C 0.6284(4) -0.0945(3) -0.0151(3) 0.0224(12) Uani 1 1 d . . . H39A H 0.5678 -0.0680 -0.0195 0.027 Uiso 1 1 calc R . . H39B H 0.6496 -0.0924 0.0313 0.027 Uiso 1 1 calc R . . C40 C 0.7018(4) -0.0570(3) -0.0541(3) 0.0227(12) Uani 1 1 d . . . H40A H 0.6836 -0.0593 -0.1010 0.027 Uiso 1 1 calc R . . H40B H 0.7649 -0.0796 -0.0474 0.027 Uiso 1 1 calc R . . C41 C 0.7068(4) 0.0202(3) -0.0316(3) 0.0307(14) Uani 1 1 d . . . H41A H 0.6438 0.0425 -0.0399 0.037 Uiso 1 1 calc R . . H41B H 0.7212 0.0216 0.0158 0.037 Uiso 1 1 calc R . . C42 C 0.7816(5) 0.0612(3) -0.0659(3) 0.0384(16) Uani 1 1 d . . . H42A H 0.7822 0.1097 -0.0501 0.058 Uiso 1 1 calc R . . H42B H 0.7669 0.0608 -0.1128 0.058 Uiso 1 1 calc R . . H42C H 0.8444 0.0399 -0.0571 0.058 Uiso 1 1 calc R . . C43 C 0.5205(4) -0.1936(3) 0.0045(2) 0.0208(12) Uani 1 1 d . . . H43A H 0.5023 -0.2411 -0.0108 0.025 Uiso 1 1 calc R . . H43B H 0.4669 -0.1617 -0.0074 0.025 Uiso 1 1 calc R . . C44 C 0.5316(4) -0.1955(3) 0.0784(3) 0.0284(13) Uani 1 1 d . . . H44A H 0.5795 -0.2313 0.0918 0.034 Uiso 1 1 calc R . . H44B H 0.5541 -0.1494 0.0948 0.034 Uiso 1 1 calc R . . C45 C 0.4361(4) -0.2131(3) 0.1071(3) 0.0263(13) Uani 1 1 d . . . H45A H 0.3882 -0.1780 0.0919 0.032 Uiso 1 1 calc R . . H45B H 0.4148 -0.2596 0.0909 0.032 Uiso 1 1 calc R . . C46 C 0.4404(5) -0.2141(5) 0.1805(3) 0.057(2) Uani 1 1 d . . . H46A H 0.3773 -0.2257 0.1964 0.086 Uiso 1 1 calc R . . H46B H 0.4599 -0.1678 0.1969 0.086 Uiso 1 1 calc R . . H46C H 0.4868 -0.2493 0.1958 0.086 Uiso 1 1 calc R . . C47 C 0.6948(4) -0.2134(3) -0.0129(3) 0.0205(12) Uani 1 1 d . . . H47A H 0.7078 -0.2081 0.0344 0.025 Uiso 1 1 calc R . . H47B H 0.7503 -0.1939 -0.0353 0.025 Uiso 1 1 calc R . . C48 C 0.6869(4) -0.2924(3) -0.0289(3) 0.0214(12) Uani 1 1 d . . . H48A H 0.6254 -0.3108 -0.0139 0.026 Uiso 1 1 calc R . . H48B H 0.6883 -0.2993 -0.0766 0.026 Uiso 1 1 calc R . . C49 C 0.7698(4) -0.3327(3) 0.0045(3) 0.0270(13) Uani 1 1 d . . . H49A H 0.7739 -0.3797 -0.0156 0.032 Uiso 1 1 calc R . . H49B H 0.8301 -0.3077 -0.0036 0.032 Uiso 1 1 calc R . . C50 C 0.7614(4) -0.3415(3) 0.0766(3) 0.0348(15) Uani 1 1 d . . . H50A H 0.8169 -0.3673 0.0943 0.052 Uiso 1 1 calc R . . H50B H 0.7030 -0.3676 0.0853 0.052 Uiso 1 1 calc R . . H50C H 0.7588 -0.2952 0.0972 0.052 Uiso 1 1 calc R . . Cl2 Cl 0.11184(14) 0.51178(9) 0.67104(9) 0.0523(5) Uani 1 1 d . . . Cl1 Cl 0.09444(15) 0.57374(12) 0.79878(9) 0.0621(6) Uani 1 1 d . . . C51 C 0.1727(6) 0.5490(4) 0.7379(4) 0.054(2) Uani 1 1 d . . . H51A H 0.2082 0.5908 0.7236 0.064 Uiso 1 1 calc R . . H51B H 0.2196 0.5149 0.7561 0.064 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 Cr 0.0180(4) 0.0156(4) 0.0150(4) 0.0000(4) -0.0006(3) -0.0014(4) F2 0.0347(19) 0.0226(17) 0.0306(19) -0.0015(14) 0.0033(15) -0.0043(15) F3 0.041(2) 0.0235(18) 0.052(2) -0.0133(17) 0.0031(17) 0.0042(16) F4 0.037(2) 0.051(2) 0.041(2) -0.0165(19) 0.0063(17) 0.0161(19) F5 0.030(2) 0.052(2) 0.040(2) 0.0027(18) 0.0158(16) 0.0037(18) F6 0.0280(18) 0.0321(19) 0.0277(19) 0.0013(15) 0.0053(14) -0.0058(15) F8 0.0353(19) 0.0156(16) 0.0309(19) 0.0014(13) -0.0083(15) -0.0014(15) F9 0.040(2) 0.0226(18) 0.041(2) -0.0086(16) 0.0004(16) -0.0105(16) F10 0.0290(19) 0.046(2) 0.034(2) -0.0088(17) -0.0066(15) -0.0114(17) F11 0.0221(17) 0.044(2) 0.0288(19) -0.0001(16) -0.0037(14) -0.0029(16) F12 0.0227(17) 0.0212(16) 0.0327(18) 0.0025(14) -0.0035(14) -0.0022(13) F14 0.0267(17) 0.0308(18) 0.0221(17) 0.0016(14) -0.0034(13) 0.0003(14) F15 0.0242(18) 0.0262(18) 0.044(2) -0.0036(15) -0.0017(15) 0.0025(14) F16 0.039(2) 0.040(2) 0.042(2) -0.0170(17) 0.0064(17) 0.0077(17) F17 0.037(2) 0.044(2) 0.0227(18) -0.0136(16) -0.0010(15) 0.0036(17) F18 0.0293(17) 0.0325(19) 0.0190(17) -0.0028(13) -0.0037(13) 0.0064(15) F20 0.0201(16) 0.0308(18) 0.0236(17) -0.0002(14) -0.0006(13) -0.0047(14) F21 0.0198(17) 0.0222(17) 0.050(2) 0.0037(16) -0.0016(15) -0.0010(14) F22 0.0244(19) 0.042(2) 0.052(2) -0.0168(18) -0.0148(16) -0.0031(17) F23 0.044(2) 0.053(2) 0.0192(18) -0.0112(16) -0.0093(15) 0.0009(19) F24 0.0336(19) 0.0348(19) 0.0223(18) -0.0033(15) 0.0011(15) -0.0033(16) N1 0.026(3) 0.018(2) 0.021(3) -0.002(2) 0.000(2) 0.000(2) N2 0.017(2) 0.028(3) 0.028(3) 0.010(2) 0.001(2) -0.003(2) C1 0.017(3) 0.027(3) 0.015(3) -0.006(2) -0.002(2) 0.003(2) C2 0.014(3) 0.023(3) 0.029(3) 0.001(2) -0.001(2) 0.004(2) C3 0.026(3) 0.022(3) 0.030(3) -0.005(3) -0.009(2) 0.007(2) C4 0.028(3) 0.041(4) 0.021(3) -0.005(3) -0.003(3) 0.012(3) C5 0.024(3) 0.029(3) 0.023(3) 0.007(3) 0.010(2) 0.000(3) C6 0.024(3) 0.026(3) 0.017(3) -0.001(2) -0.002(2) 0.001(2) C7 0.021(3) 0.023(3) 0.015(3) -0.004(2) 0.001(2) -0.008(2) C8 0.028(3) 0.028(3) 0.014(3) -0.003(2) 0.007(2) -0.002(3) C9 0.036(3) 0.026(3) 0.014(3) -0.006(2) 0.009(2) -0.012(3) C10 0.016(3) 0.040(3) 0.015(3) -0.009(3) 0.002(2) -0.010(3) C11 0.023(3) 0.032(3) 0.017(3) 0.002(2) 0.000(2) 0.003(3) C12 0.018(3) 0.023(3) 0.020(3) 0.001(2) 0.003(2) -0.003(2) C13 0.021(3) 0.011(3) 0.021(3) 0.003(2) 0.005(2) -0.007(2) C14 0.026(3) 0.016(3) 0.020(3) -0.001(2) -0.007(2) -0.009(2) C15 0.015(3) 0.011(3) 0.035(3) 0.001(2) 0.001(2) 0.000(2) C16 0.024(3) 0.014(3) 0.034(3) -0.014(2) 0.010(3) -0.001(2) C17 0.031(3) 0.024(3) 0.026(3) -0.005(3) 0.006(3) 0.001(3) C18 0.020(3) 0.027(3) 0.018(3) 0.005(2) -0.005(2) 0.002(2) C19 0.020(3) 0.016(3) 0.018(3) -0.003(2) -0.001(2) 0.005(2) C20 0.025(3) 0.016(3) 0.016(3) -0.007(2) -0.006(2) 0.005(2) C21 0.023(3) 0.013(3) 0.031(3) -0.003(2) 0.002(2) 0.007(2) C22 0.019(3) 0.016(3) 0.046(4) 0.000(3) -0.015(3) 0.001(2) C23 0.029(3) 0.024(3) 0.022(3) -0.008(2) -0.010(2) 0.007(3) C24 0.026(3) 0.010(3) 0.024(3) -0.004(2) -0.002(2) 0.003(2) C25 0.017(3) 0.015(3) 0.025(3) -0.001(2) -0.001(2) -0.001(2) C26 0.035(3) 0.021(3) 0.020(3) 0.010(2) -0.001(2) -0.003(3) C27 0.107(18) 0.095(17) 0.031(10) 0.031(10) -0.045(11) -0.059(15) C28 0.038(9) 0.037(13) 0.053(19) 0.030(11) -0.017(8) -0.020(9) C29 0.121(19) 0.043(11) 0.059(13) 0.040(10) 0.013(12) 0.025(12) C27' 0.17(3) 0.050(11) 0.020(9) 0.012(8) -0.016(12) -0.018(15) C28' 0.086(16) 0.050(17) 0.027(11) -0.001(10) -0.003(10) -0.019(13) C29' 0.046(11) 0.113(19) 0.073(14) 0.064(14) 0.001(10) 0.040(12) C30 0.015(3) 0.019(3) 0.021(3) -0.002(2) 0.001(2) 0.000(2) C31 0.032(4) 0.051(5) 0.053(5) 0.028(4) 0.001(3) 0.004(3) C32 0.102(7) 0.058(5) 0.047(5) 0.002(4) -0.002(5) -0.027(5) C33 0.068(6) 0.088(7) 0.107(8) 0.069(6) -0.007(6) 0.001(5) C34 0.061(5) 0.047(4) 0.032(4) 0.008(3) -0.005(3) -0.020(4) N3 0.016(2) 0.013(2) 0.020(2) -0.0032(18) 0.0014(18) -0.0008(18) C35 0.019(3) 0.021(3) 0.019(3) -0.002(2) 0.000(2) 0.000(2) C36 0.017(3) 0.030(3) 0.022(3) 0.001(2) 0.004(2) -0.004(2) C37 0.022(3) 0.035(3) 0.020(3) -0.002(2) 0.004(2) 0.002(3) C38 0.026(3) 0.053(4) 0.020(3) -0.001(3) 0.000(2) 0.004(3) C39 0.025(3) 0.021(3) 0.020(3) 0.000(2) -0.003(2) 0.001(2) C40 0.022(3) 0.022(3) 0.024(3) 0.004(2) -0.005(2) -0.008(2) C41 0.024(3) 0.020(3) 0.048(4) 0.009(3) -0.006(3) -0.003(3) C42 0.043(4) 0.027(4) 0.045(4) 0.013(3) -0.011(3) -0.009(3) C43 0.024(3) 0.018(3) 0.020(3) 0.001(2) -0.001(2) 0.000(2) C44 0.022(3) 0.037(4) 0.026(3) 0.004(3) -0.001(2) -0.004(3) C45 0.024(3) 0.032(3) 0.023(3) 0.002(3) 0.005(2) 0.007(3) C46 0.042(4) 0.111(7) 0.020(4) 0.019(4) 0.002(3) -0.006(4) C47 0.014(3) 0.027(3) 0.021(3) -0.001(2) 0.003(2) 0.000(2) C48 0.024(3) 0.020(3) 0.021(3) -0.006(2) 0.005(2) -0.001(2) C49 0.029(3) 0.024(3) 0.028(3) 0.004(2) 0.005(3) 0.004(3) C50 0.030(3) 0.033(3) 0.042(4) 0.014(3) 0.003(3) 0.009(3) Cl2 0.0638(12) 0.0474(11) 0.0455(11) -0.0099(9) 0.0003(9) -0.0175(10) Cl1 0.0661(13) 0.0809(15) 0.0384(11) -0.0053(10) -0.0112(9) 0.0089(11) C51 0.048(4) 0.055(5) 0.058(5) 0.000(4) -0.007(4) -0.016(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 Cr C25 2.059(6) . ? Cr C30 2.068(6) . ? Cr C7 2.146(5) . ? Cr C13 2.156(5) . ? Cr C19 2.160(5) . ? Cr C1 2.161(5) . ? F2 C2 1.355(6) . ? F3 C3 1.353(6) . ? F4 C4 1.351(6) . ? F5 C5 1.378(6) . ? F6 C6 1.368(6) . ? F8 C8 1.363(6) . ? F9 C9 1.343(6) . ? F10 C10 1.347(6) . ? F11 C11 1.358(6) . ? F12 C12 1.381(6) . ? F14 C14 1.357(6) . ? F15 C15 1.367(6) . ? F16 C16 1.343(6) . ? F17 C17 1.357(7) . ? F18 C18 1.351(6) . ? F20 C20 1.354(6) . ? F21 C21 1.357(6) . ? F22 C22 1.348(6) . ? F23 C23 1.343(6) . ? F24 C24 1.357(6) . ? N1 C25 1.145(7) . ? N1 C26 1.445(7) . ? N2 C30 1.135(7) . ? N2 C31 1.459(8) . ? C1 C6 1.380(7) . ? C1 C2 1.391(8) . ? C2 C3 1.381(7) . ? C3 C4 1.367(8) . ? C4 C5 1.357(8) . ? C5 C6 1.368(7) . ? C7 C12 1.379(8) . ? C7 C8 1.385(7) . ? C8 C9 1.397(8) . ? C9 C10 1.369(8) . ? C10 C11 1.380(8) . ? C11 C12 1.376(7) . ? C13 C14 1.386(7) . ? C13 C18 1.394(7) . ? C14 C15 1.389(7) . ? C15 C16 1.378(8) . ? C16 C17 1.355(8) . ? C17 C18 1.380(8) . ? C19 C20 1.387(7) . ? C19 C24 1.393(7) . ? C20 C21 1.381(7) . ? C21 C22 1.380(8) . ? C22 C23 1.379(8) . ? C23 C24 1.376(8) . ? C26 C28' 1.493(9) . ? C26 C28 1.494(8) . ? C26 C27 1.498(8) . ? C26 C29' 1.500(8) . ? C26 C29 1.502(9) . ? C26 C27' 1.508(9) . ? C31 C33 1.472(7) . ? C31 C34 1.496(7) . ? C31 C32 1.531(7) . ? N3 C39 1.514(7) . ? N3 C47 1.515(7) . ? N3 C43 1.521(6) . ? N3 C35 1.525(6) . ? C35 C36 1.512(7) . ? C36 C37 1.513(7) . ? C37 C38 1.521(8) . ? C39 C40 1.509(7) . ? C40 C41 1.544(8) . ? C41 C42 1.506(8) . ? C43 C44 1.524(8) . ? C44 C45 1.520(7) . ? C45 C46 1.510(8) . ? C47 C48 1.546(7) . ? C48 C49 1.535(8) . ? C49 C50 1.501(8) . ? Cl2 C51 1.744(7) . ? Cl1 C51 1.758(8) . ? 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 C25 Cr C30 177.3(2) . . ? C25 Cr C7 91.1(2) . . ? C30 Cr C7 89.6(2) . . ? C25 Cr C13 89.5(2) . . ? C30 Cr C13 87.9(2) . . ? C7 Cr C13 89.0(2) . . ? C25 Cr C19 89.1(2) . . ? C30 Cr C19 90.2(2) . . ? C7 Cr C19 178.8(2) . . ? C13 Cr C19 92.22(19) . . ? C25 Cr C1 88.3(2) . . ? C30 Cr C1 94.3(2) . . ? C7 Cr C1 89.8(2) . . ? C13 Cr C1 177.4(2) . . ? C19 Cr C1 89.04(19) . . ? C25 N1 C26 175.7(5) . . ? C30 N2 C31 173.9(6) . . ? C6 C1 C2 112.8(5) . . ? C6 C1 Cr 124.0(4) . . ? C2 C1 Cr 123.1(4) . . ? F2 C2 C3 115.3(5) . . ? F2 C2 C1 120.6(5) . . ? C3 C2 C1 124.1(5) . . ? F3 C3 C4 119.4(5) . . ? F3 C3 C2 120.8(5) . . ? C4 C3 C2 119.8(5) . . ? F4 C4 C5 121.9(5) . . ? F4 C4 C3 120.0(6) . . ? C5 C4 C3 118.1(5) . . ? C4 C5 C6 120.8(5) . . ? C4 C5 F5 119.2(5) . . ? C6 C5 F5 120.0(5) . . ? C5 C6 F6 115.1(5) . . ? C5 C6 C1 124.3(5) . . ? F6 C6 C1 120.6(5) . . ? C12 C7 C8 112.1(5) . . ? C12 C7 Cr 123.5(4) . . ? C8 C7 Cr 124.3(4) . . ? F8 C8 C7 120.5(5) . . ? F8 C8 C9 114.6(5) . . ? C7 C8 C9 124.9(5) . . ? F9 C9 C10 119.9(5) . . ? F9 C9 C8 121.0(5) . . ? C10 C9 C8 119.1(5) . . ? F10 C10 C9 120.5(5) . . ? F10 C10 C11 120.6(5) . . ? C9 C10 C11 118.9(5) . . ? F11 C11 C12 122.8(5) . . ? F11 C11 C10 118.3(5) . . ? C12 C11 C10 118.9(5) . . ? C11 C12 C7 126.1(5) . . ? C11 C12 F12 113.3(5) . . ? C7 C12 F12 120.6(5) . . ? C14 C13 C18 112.3(5) . . ? C14 C13 Cr 123.7(4) . . ? C18 C13 Cr 124.0(4) . . ? F14 C14 C13 120.8(5) . . ? F14 C14 C15 114.6(5) . . ? C13 C14 C15 124.6(5) . . ? F15 C15 C16 119.7(5) . . ? F15 C15 C14 120.6(5) . . ? C16 C15 C14 119.7(5) . . ? F16 C16 C17 121.8(5) . . ? F16 C16 C15 120.0(5) . . ? C17 C16 C15 118.2(5) . . ? C16 C17 F17 118.6(5) . . ? C16 C17 C18 120.6(5) . . ? F17 C17 C18 120.8(5) . . ? F18 C18 C17 115.1(5) . . ? F18 C18 C13 120.3(5) . . ? C17 C18 C13 124.5(5) . . ? C20 C19 C24 112.1(5) . . ? C20 C19 Cr 123.2(4) . . ? C24 C19 Cr 124.7(4) . . ? F20 C20 C21 113.9(5) . . ? F20 C20 C19 121.2(4) . . ? C21 C20 C19 124.9(5) . . ? F21 C21 C22 118.5(5) . . ? F21 C21 C20 121.8(5) . . ? C22 C21 C20 119.7(5) . . ? F22 C22 C23 120.6(5) . . ? F22 C22 C21 120.9(5) . . ? C23 C22 C21 118.5(5) . . ? F23 C23 C24 121.4(5) . . ? F23 C23 C22 119.5(5) . . ? C24 C23 C22 119.1(5) . . ? F24 C24 C23 114.5(5) . . ? F24 C24 C19 119.8(5) . . ? C23 C24 C19 125.7(5) . . ? N1 C25 Cr 177.8(5) . . ? N1 C26 C28' 109.9(14) . . ? N1 C26 C28 108.6(12) . . ? C28' C26 C28 23.6(13) . . ? N1 C26 C27 110.5(9) . . ? C28' C26 C27 130.6(15) . . ? C28 C26 C27 114.2(14) . . ? N1 C26 C29' 112.8(8) . . ? C28' C26 C29' 114.3(15) . . ? C28 C26 C29' 131.4(14) . . ? C27 C26 C29' 73.5(13) . . ? N1 C26 C29 100.2(7) . . ? C28' C26 C29 88.1(13) . . ? C28 C26 C29 111.2(13) . . ? C27 C26 C29 111.2(13) . . ? C29' C26 C29 37.7(11) . . ? N1 C26 C27' 103.8(8) . . ? C28' C26 C27' 105.5(13) . . ? C28 C26 C27' 83.2(13) . . ? C27 C26 C27' 37.4(11) . . ? C29' C26 C27' 109.8(13) . . ? C29 C26 C27' 146.2(12) . . ? N2 C30 Cr 174.7(5) . . ? N2 C31 C33 108.0(5) . . ? N2 C31 C34 107.5(5) . . ? C33 C31 C34 118.7(6) . . ? N2 C31 C32 107.7(5) . . ? C33 C31 C32 107.0(7) . . ? C34 C31 C32 107.6(6) . . ? C39 N3 C47 108.1(4) . . ? C39 N3 C43 108.5(4) . . ? C47 N3 C43 111.6(4) . . ? C39 N3 C35 111.4(4) . . ? C47 N3 C35 109.0(4) . . ? C43 N3 C35 108.3(4) . . ? C36 C35 N3 116.5(4) . . ? C35 C36 C37 110.2(4) . . ? C36 C37 C38 113.1(4) . . ? C40 C39 N3 117.4(5) . . ? C39 C40 C41 108.4(5) . . ? C42 C41 C40 112.3(5) . . ? N3 C43 C44 116.5(4) . . ? C45 C44 C43 109.4(5) . . ? C46 C45 C44 112.8(5) . . ? N3 C47 C48 115.0(4) . . ? C49 C48 C47 110.2(4) . . ? C50 C49 C48 114.5(4) . . ? Cl2 C51 Cl1 111.8(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.685 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.066 #=== END data_3 _database_code_depnum_ccdc_archive 'CCDC 777394' #TrackingRef '- Cr paper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59.75 H57.50 Cl3.50 Cr F20 N3' _chemical_formula_weight 1373.66 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9690(2) _cell_length_b 14.2368(2) _cell_length_c 18.3719(3) _cell_angle_alpha 88.5890(10) _cell_angle_beta 87.8770(10) _cell_angle_gamma 88.9560(10) _cell_volume 3127.01(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 18627 _cell_measurement_theta_min 3.7782 _cell_measurement_theta_max 28.8442 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1401 _exptl_absorpt_coefficient_mu 0.433 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8812 _exptl_absorpt_correction_T_max 0.9340 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean 16.0655 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48256 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 26.25 _diffrn_orient_matrix_UB_11 -0.0268468990 _diffrn_orient_matrix_UB_12 0.0366533586 _diffrn_orient_matrix_UB_13 0.0196603868 _diffrn_orient_matrix_UB_21 -0.0028119342 _diffrn_orient_matrix_UB_22 0.0275556992 _diffrn_orient_matrix_UB_23 -0.0325143681 _diffrn_orient_matrix_UB_31 -0.0526814664 _diffrn_orient_matrix_UB_32 -0.0192855770 _diffrn_orient_matrix_UB_33 -0.0066974698 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -53.00 52.60 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -19.8053 77.0000 0.0000 0.0000 0.0000 176 #__ type_ start__ end____ width___ exp.time_ 2 omega -53.00 52.60 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -19.8053 77.0000 240.0000 0.0000 0.0000 176 #__ type_ start__ end____ width___ exp.time_ 3 omega -11.00 43.60 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 22.2271 77.0000 0.0000 0.0000 0.0000 91 #__ type_ start__ end____ width___ exp.time_ 4 omega -11.00 94.60 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 22.2271 77.0000 210.0000 0.0000 0.0000 176 #__ type_ start__ end____ width___ exp.time_ 5 omega 40.00 94.60 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 22.2271 77.0000 330.0000 0.0000 0.0000 91 #__ type_ start__ end____ width___ exp.time_ 6 omega -11.00 94.60 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - 22.2271 77.0000 120.0000 0.0000 0.0000 176 #__ type_ start__ end____ width___ exp.time_ 7 omega -95.00 55.00 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -19.8053 0.0000 30.0000 0.0000 0.0000 250 #__ type_ start__ end____ width___ exp.time_ 8 omega -95.00 55.00 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -19.8053 0.0000 210.0000 0.0000 0.0000 250 #__ type_ start__ end____ width___ exp.time_ 9 omega -95.00 -58.40 0.6000 9.0000 omega____ theta____ kappa____ phi______ omega'___ theta'___ frames - -19.8053 0.0000 60.0000 0.0000 0.0000 61 ; _reflns_number_total 12586 _reflns_number_gt 8852 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.2600P)^2^+0.0000P] 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 12586 _refine_ls_number_parameters 827 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_gt 0.0954 _refine_ls_wR_factor_ref 0.3389 _refine_ls_wR_factor_gt 0.3208 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.000 _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 Cr Cr 0.21667(5) 0.66871(5) 0.27835(4) 0.0165(2) Uani 1 1 d . . . F2 F 0.1091(2) 0.7950(2) 0.14289(17) 0.0353(7) Uani 1 1 d . . . F3 F 0.1135(4) 0.7787(3) -0.0004(2) 0.0650(12) Uani 1 1 d . . . F4 F 0.2427(5) 0.6431(4) -0.0661(2) 0.0936(18) Uani 1 1 d . . . F5 F 0.3594(4) 0.5170(3) 0.0174(2) 0.0695(12) Uani 1 1 d . . . F6 F 0.3430(2) 0.5224(2) 0.16104(15) 0.0333(7) Uani 1 1 d . . . F8 F 0.1004(2) 0.86665(19) 0.34465(16) 0.0324(7) Uani 1 1 d . . . F9 F 0.1534(3) 1.0449(2) 0.3364(2) 0.0558(10) Uani 1 1 d . . . F10 F 0.3422(3) 1.1005(2) 0.2598(3) 0.0617(11) Uani 1 1 d . . . F11 F 0.4711(2) 0.9707(2) 0.18770(18) 0.0409(8) Uani 1 1 d . . . F12 F 0.4149(2) 0.7913(2) 0.19078(15) 0.0287(6) Uani 1 1 d . . . F14 F 0.0354(2) 0.59326(19) 0.40601(15) 0.0277(6) Uani 1 1 d . . . F15 F 0.0268(3) 0.5968(2) 0.55018(16) 0.0439(9) Uani 1 1 d . . . F16 F 0.1929(4) 0.6784(2) 0.62264(16) 0.0528(10) Uani 1 1 d . . . F17 F 0.3652(3) 0.7603(2) 0.54687(18) 0.0492(9) Uani 1 1 d . . . F18 F 0.3730(2) 0.7650(2) 0.40209(16) 0.0324(7) Uani 1 1 d . . . F20 F 0.3063(2) 0.48770(18) 0.38206(15) 0.0265(6) Uani 1 1 d . . . F21 F 0.2469(3) 0.3101(2) 0.39810(19) 0.0429(8) Uani 1 1 d . . . F22 F 0.0847(3) 0.2400(2) 0.3151(2) 0.0571(11) Uani 1 1 d . . . F23 F -0.0185(3) 0.3541(2) 0.2167(2) 0.0512(9) Uani 1 1 d . . . F24 F 0.0373(2) 0.5334(2) 0.20003(16) 0.0307(7) Uani 1 1 d . . . N1 N -0.0448(3) 0.7300(3) 0.2790(2) 0.0230(8) Uani 1 1 d . . . N2 N 0.4785(3) 0.6108(3) 0.2927(2) 0.0228(8) Uani 1 1 d . . . C1 C 0.2258(4) 0.6597(3) 0.1615(2) 0.0232(10) Uani 1 1 d . . . C2 C 0.1712(4) 0.7222(4) 0.1155(3) 0.0290(11) Uani 1 1 d . . . C3 C 0.1745(5) 0.7164(5) 0.0407(3) 0.0429(15) Uani 1 1 d . . . C4 C 0.2370(7) 0.6499(5) 0.0076(3) 0.0550(18) Uani 1 1 d . . . C5 C 0.2960(6) 0.5840(5) 0.0500(3) 0.0442(15) Uani 1 1 d . . . C6 C 0.2863(4) 0.5906(4) 0.1239(3) 0.0288(11) Uani 1 1 d . . . C7 C 0.2539(4) 0.8161(3) 0.2691(2) 0.0211(9) Uani 1 1 d . . . C8 C 0.1936(4) 0.8874(3) 0.3036(3) 0.0283(11) Uani 1 1 d . . . C9 C 0.2200(5) 0.9803(4) 0.3014(3) 0.0378(13) Uani 1 1 d . . . C10 C 0.3124(5) 1.0101(4) 0.2633(4) 0.0409(14) Uani 1 1 d . . . C11 C 0.3781(4) 0.9433(4) 0.2257(3) 0.0305(11) Uani 1 1 d . . . C12 C 0.3471(4) 0.8509(3) 0.2292(3) 0.0258(10) Uani 1 1 d . . . C13 C 0.2052(4) 0.6771(3) 0.3950(2) 0.0212(9) Uani 1 1 d . . . C14 C 0.1214(4) 0.6365(3) 0.4377(2) 0.0227(10) Uani 1 1 d . . . C15 C 0.1144(5) 0.6367(3) 0.5130(3) 0.0310(12) Uani 1 1 d . . . C16 C 0.1976(6) 0.6772(4) 0.5491(3) 0.0385(14) Uani 1 1 d . . . C17 C 0.2833(5) 0.7187(4) 0.5114(3) 0.0335(12) Uani 1 1 d . . . C18 C 0.2844(4) 0.7193(3) 0.4352(3) 0.0263(10) Uani 1 1 d . . . C19 C 0.1769(4) 0.5217(3) 0.2884(2) 0.0205(9) Uani 1 1 d . . . C20 C 0.2262(4) 0.4596(3) 0.3382(3) 0.0229(10) Uani 1 1 d . . . C21 C 0.1966(4) 0.3656(3) 0.3472(3) 0.0330(12) Uani 1 1 d . . . C22 C 0.1158(5) 0.3303(4) 0.3066(4) 0.0377(13) Uani 1 1 d . . . C23 C 0.0643(4) 0.3885(4) 0.2568(3) 0.0344(12) Uani 1 1 d . . . C24 C 0.0956(4) 0.4814(3) 0.2496(3) 0.0251(10) Uani 1 1 d . . . C25 C 0.0485(4) 0.7042(3) 0.2767(2) 0.0220(10) Uani 1 1 d . . . C26 C -0.1544(4) 0.7640(3) 0.2853(3) 0.0254(10) Uani 1 1 d . . . C27 C -0.2149(4) 0.7761(3) 0.2208(3) 0.0278(11) Uani 1 1 d . . . C28 C -0.3241(4) 0.8090(3) 0.2285(3) 0.0309(11) Uani 1 1 d . . . H28A H -0.3669 0.8182 0.1863 0.037 Uiso 1 1 calc R . . C29 C -0.3710(4) 0.8283(4) 0.2942(3) 0.0345(12) Uani 1 1 d . . . H29A H -0.4466 0.8496 0.2978 0.041 Uiso 1 1 calc R . . C30 C -0.3091(4) 0.8172(4) 0.3580(3) 0.0321(12) Uani 1 1 d . . . H30A H -0.3428 0.8328 0.4039 0.038 Uiso 1 1 calc R . . C31 C -0.2000(4) 0.7839(3) 0.3543(3) 0.0272(11) Uani 1 1 d . . . C32 C -0.1620(4) 0.7523(4) 0.1483(3) 0.0353(12) Uani 1 1 d . . . H32A H -0.2184 0.7570 0.1110 0.053 Uiso 1 1 calc R . . H32B H -0.1313 0.6880 0.1505 0.053 Uiso 1 1 calc R . . H32C H -0.1017 0.7962 0.1360 0.053 Uiso 1 1 calc R . . C33 C -0.1355(4) 0.7684(4) 0.4216(3) 0.0323(11) Uani 1 1 d . . . H33A H -0.1769 0.7959 0.4631 0.048 Uiso 1 1 calc R . . H33B H -0.0625 0.7982 0.4152 0.048 Uiso 1 1 calc R . . H33C H -0.1247 0.7008 0.4307 0.048 Uiso 1 1 calc R . . C34 C 0.3857(4) 0.6330(3) 0.2859(2) 0.0192(9) Uani 1 1 d . . . C35 C 0.5898(4) 0.5807(3) 0.3017(3) 0.0275(11) Uani 1 1 d . . . C36 C 0.6549(4) 0.5611(3) 0.2399(3) 0.0329(12) Uani 1 1 d . . . C37 C 0.7656(4) 0.5311(4) 0.2508(4) 0.0435(15) Uani 1 1 d . . . H37A H 0.8128 0.5154 0.2100 0.052 Uiso 1 1 calc R . . C38 C 0.8070(4) 0.5240(4) 0.3206(4) 0.0431(15) Uani 1 1 d . . . H38A H 0.8827 0.5053 0.3270 0.052 Uiso 1 1 calc R . . C39 C 0.7397(4) 0.5439(4) 0.3799(4) 0.0414(15) Uani 1 1 d . . . H39A H 0.7690 0.5379 0.4272 0.050 Uiso 1 1 calc R . . C40 C 0.6279(4) 0.5731(3) 0.3724(3) 0.0346(12) Uani 1 1 d . . . C41 C 0.6085(5) 0.5690(5) 0.1660(3) 0.0430(14) Uani 1 1 d . . . H41A H 0.5755 0.6318 0.1587 0.064 Uiso 1 1 calc R . . H41B H 0.5509 0.5216 0.1615 0.064 Uiso 1 1 calc R . . H41C H 0.6686 0.5586 0.1292 0.064 Uiso 1 1 calc R . . C42 C 0.5547(5) 0.5981(4) 0.4373(3) 0.0393(13) Uani 1 1 d . . . H42A H 0.5888 0.5737 0.4818 0.059 Uiso 1 1 calc R . . H42B H 0.4810 0.5704 0.4330 0.059 Uiso 1 1 calc R . . H42C H 0.5466 0.6666 0.4396 0.059 Uiso 1 1 calc R . . N3 N 0.2006(3) 0.8951(3) 0.7825(2) 0.0243(9) Uani 1 1 d . . . C43 C 0.2693(4) 0.9528(4) 0.8319(3) 0.0307(11) Uani 1 1 d . . . H43A H 0.3450 0.9596 0.8090 0.037 Uiso 1 1 calc R . . H43B H 0.2349 1.0164 0.8347 0.037 Uiso 1 1 calc R . . C44 C 0.2817(5) 0.9142(5) 0.9086(3) 0.0453(15) Uani 1 1 d . . . H44A H 0.3249 0.8543 0.9075 0.054 Uiso 1 1 calc R . . H44B H 0.2070 0.9017 0.9313 0.054 Uiso 1 1 calc R . . C45 C 0.3419(6) 0.9856(7) 0.9530(4) 0.071(3) Uani 1 1 d . . . H45A H 0.4178 0.9958 0.9314 0.085 Uiso 1 1 calc R . . H45B H 0.3005 1.0464 0.9519 0.085 Uiso 1 1 calc R . . C46 C 0.3502(7) 0.9504(9) 1.0303(4) 0.088(3) Uani 1 1 d . . . H46A H 0.3890 0.9967 1.0584 0.133 Uiso 1 1 calc R . . H46B H 0.3921 0.8907 1.0313 0.133 Uiso 1 1 calc R . . H46C H 0.2749 0.9411 1.0518 0.133 Uiso 1 1 calc R . . C47 C 0.0818(4) 0.8831(4) 0.8147(3) 0.0294(11) Uani 1 1 d . . . H47A H 0.0403 0.8439 0.7815 0.035 Uiso 1 1 calc R . . H47B H 0.0866 0.8478 0.8617 0.035 Uiso 1 1 calc R . . C48 C 0.0145(4) 0.9722(4) 0.8279(3) 0.0383(13) Uani 1 1 d . . . H48A H 0.0070 1.0082 0.7815 0.046 Uiso 1 1 calc R . . H48B H 0.0533 1.0119 0.8622 0.046 Uiso 1 1 calc R . . C49 C -0.1012(5) 0.9475(5) 0.8598(4) 0.0500(16) Uani 1 1 d . . . H49A H -0.1482 1.0055 0.8610 0.060 Uiso 1 1 calc R . . H49B H -0.1362 0.9035 0.8268 0.060 Uiso 1 1 calc R . . C50 C -0.1017(8) 0.9041(8) 0.9347(5) 0.090(3) Uani 1 1 d U . . H50A H -0.1786 0.8895 0.9506 0.135 Uiso 1 1 calc R . . H50B H -0.0707 0.9482 0.9684 0.135 Uiso 1 1 calc R . . H50C H -0.0562 0.8462 0.9342 0.135 Uiso 1 1 calc R . . C51 C 0.1993(4) 0.9468(3) 0.7097(3) 0.0286(11) Uani 1 1 d . . . H51A H 0.1700 1.0114 0.7177 0.034 Uiso 1 1 calc R . . H51B H 0.2773 0.9521 0.6905 0.034 Uiso 1 1 calc R . . C52 C 0.1315(7) 0.9032(4) 0.6525(3) 0.0528(18) Uani 1 1 d . B . H52A H 0.0524 0.8999 0.6700 0.063 Uiso 1 1 calc R . . H52B H 0.1593 0.8383 0.6441 0.063 Uiso 1 1 calc R . . C53 C 0.1389(6) 0.9599(7) 0.5813(4) 0.071(2) Uani 1 1 d . . . H53A H 0.2166 0.9621 0.5611 0.085 Uiso 1 1 calc R A 1 H53B H 0.1095 1.0248 0.5875 0.085 Uiso 1 1 calc R A 1 C54 C 0.0565(13) 0.8972(10) 0.5287(7) 0.041(3) Uani 0.50 1 d P B 1 H54A H 0.0545 0.9266 0.4800 0.061 Uiso 0.50 1 calc PR B 1 H54B H -0.0194 0.8957 0.5506 0.061 Uiso 0.50 1 calc PR B 1 H54C H 0.0865 0.8329 0.5251 0.061 Uiso 0.50 1 calc PR B 1 C54' C 0.1113(14) 0.9274(11) 0.5141(8) 0.048(4) Uani 0.50 1 d P B 2 H54D H 0.1639 0.9521 0.4765 0.071 Uiso 0.50 1 calc PR B 2 H54E H 0.0352 0.9484 0.5032 0.071 Uiso 0.50 1 calc PR B 2 H54F H 0.1153 0.8585 0.5149 0.071 Uiso 0.50 1 calc PR B 2 C55 C 0.2493(4) 0.7966(3) 0.7752(3) 0.0288(11) Uani 1 1 d . . . H55A H 0.1987 0.7602 0.7457 0.035 Uiso 1 1 calc R . . H55B H 0.2497 0.7665 0.8244 0.035 Uiso 1 1 calc R . . C56 C 0.3669(4) 0.7884(4) 0.7411(3) 0.0307(11) Uani 1 1 d . . . H56A H 0.4183 0.8281 0.7675 0.037 Uiso 1 1 calc R . . H56B H 0.3668 0.8107 0.6896 0.037 Uiso 1 1 calc R . . C57 C 0.4064(5) 0.6862(4) 0.7453(4) 0.0405(14) Uani 1 1 d . . . H57A H 0.4094 0.6659 0.7971 0.049 Uiso 1 1 calc R . . H57B H 0.3512 0.6468 0.7220 0.049 Uiso 1 1 calc R . . C58 C 0.5202(5) 0.6700(5) 0.7086(4) 0.0517(16) Uani 1 1 d . . . H58A H 0.5414 0.6034 0.7133 0.077 Uiso 1 1 calc R . . H58B H 0.5756 0.7081 0.7318 0.077 Uiso 1 1 calc R . . H58C H 0.5173 0.6881 0.6568 0.077 Uiso 1 1 calc R . . Cl1 Cl 0.5187(3) 1.0218(2) 0.3852(2) 0.0860(9) Uani 0.70 1 d PD C 1 Cl2 Cl 0.3087(3) 1.0579(3) 0.4599(2) 0.1032(12) Uani 0.70 1 d PD C 1 C59 C 0.4391(5) 1.0993(5) 0.4354(5) 0.053(2) Uani 0.70 1 d PDU C 1 H59A H 0.4305 1.1587 0.4067 0.064 Uiso 0.70 1 calc PR C 1 H59B H 0.4788 1.1137 0.4800 0.064 Uiso 0.70 1 calc PR C 1 Cl1' Cl 0.4354(6) 0.9437(5) 0.4328(5) 0.0860(9) Uani 0.30 1 d PD D 2 Cl2' Cl 0.3687(7) 1.1334(6) 0.4383(5) 0.1032(12) Uani 0.30 1 d PD D 2 C59' C 0.4841(8) 1.0570(6) 0.4321(13) 0.053(2) Uani 0.30 1 d PDU D 2 H59C H 0.5283 1.0702 0.3865 0.064 Uiso 0.30 1 calc PR D 2 H59D H 0.5327 1.0654 0.4738 0.064 Uiso 0.30 1 calc PR D 2 Cl3 Cl -0.4556(4) 0.7332(3) 0.0225(2) 0.0898(11) Uani 0.50 1 d PD E 1 Cl4 Cl -0.4002(4) 0.7892(3) -0.1211(3) 0.0898(11) Uani 0.50 1 d PD E 1 C60 C -0.4201(17) 0.6920(5) -0.0635(4) 0.085(5) Uani 0.50 1 d PDU E 1 H60A H -0.4808 0.6529 -0.0811 0.103 Uiso 0.50 1 calc PR E 1 H60B H -0.3508 0.6531 -0.0621 0.103 Uiso 0.50 1 calc PR E 1 Cl5 Cl -0.0769(5) 0.5774(4) 0.0053(5) 0.142(3) Uani 0.50 1 d PDU . 2 C61 C -0.0126(16) 0.4858(11) 0.0521(5) 0.048(6) Uani 0.25 1 d PDU . 2 H61A H -0.0702 0.4436 0.0738 0.058 Uiso 0.25 1 calc PR . 2 H61B H 0.0301 0.5112 0.0921 0.058 Uiso 0.25 1 calc PR . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0132(4) 0.0156(4) 0.0206(4) 0.0018(3) -0.0021(3) 0.0001(3) F2 0.0276(16) 0.0344(17) 0.0438(17) 0.0162(13) -0.0087(13) 0.0000(13) F3 0.082(3) 0.071(3) 0.043(2) 0.0340(19) -0.0262(19) -0.015(2) F4 0.165(5) 0.099(4) 0.0160(17) 0.004(2) -0.002(2) -0.011(4) F5 0.100(3) 0.068(3) 0.040(2) -0.0179(19) 0.018(2) 0.012(2) F6 0.0325(16) 0.0356(17) 0.0319(15) -0.0072(12) 0.0001(12) 0.0060(13) F8 0.0285(16) 0.0222(15) 0.0462(17) -0.0058(12) 0.0030(13) 0.0015(12) F9 0.050(2) 0.0219(17) 0.095(3) -0.0065(17) 0.002(2) 0.0046(15) F10 0.055(2) 0.0179(17) 0.112(3) 0.0122(18) -0.011(2) -0.0104(16) F11 0.0269(16) 0.0398(18) 0.056(2) 0.0219(15) -0.0056(14) -0.0151(14) F12 0.0165(13) 0.0357(16) 0.0336(15) 0.0055(12) 0.0017(11) -0.0055(12) F14 0.0246(14) 0.0247(15) 0.0330(15) 0.0049(11) 0.0046(11) -0.0019(11) F15 0.072(2) 0.0262(16) 0.0314(16) 0.0050(12) 0.0229(16) 0.0005(15) F16 0.110(3) 0.0296(17) 0.0189(15) -0.0043(12) -0.0059(16) 0.0045(18) F17 0.073(3) 0.041(2) 0.0353(17) -0.0116(14) -0.0268(17) 0.0021(18) F18 0.0261(15) 0.0334(17) 0.0385(16) -0.0054(13) -0.0081(12) -0.0023(12) F20 0.0275(15) 0.0192(14) 0.0329(15) 0.0026(11) -0.0067(12) 0.0012(11) F21 0.0430(19) 0.0233(16) 0.061(2) 0.0181(14) 0.0018(15) 0.0045(14) F22 0.049(2) 0.0174(16) 0.105(3) 0.0090(17) -0.011(2) -0.0128(15) F23 0.0391(19) 0.0312(18) 0.085(3) -0.0074(17) -0.0184(18) -0.0139(15) F24 0.0261(15) 0.0290(16) 0.0378(16) -0.0017(12) -0.0100(12) -0.0038(12) N1 0.017(2) 0.0172(19) 0.035(2) 0.0042(16) -0.0070(16) -0.0017(15) N2 0.017(2) 0.0168(19) 0.035(2) 0.0010(15) -0.0031(16) 0.0002(15) C1 0.016(2) 0.030(3) 0.024(2) 0.0024(18) -0.0048(18) -0.0079(19) C2 0.027(3) 0.029(3) 0.032(3) 0.008(2) -0.005(2) -0.012(2) C3 0.049(4) 0.053(4) 0.028(3) 0.019(3) -0.014(2) -0.016(3) C4 0.084(5) 0.064(4) 0.018(3) 0.003(3) -0.003(3) -0.011(4) C5 0.057(4) 0.047(4) 0.028(3) -0.009(2) 0.009(3) -0.010(3) C6 0.025(3) 0.034(3) 0.028(2) -0.002(2) -0.003(2) -0.006(2) C7 0.016(2) 0.023(2) 0.024(2) 0.0037(17) -0.0065(17) -0.0009(18) C8 0.021(2) 0.021(2) 0.042(3) 0.003(2) -0.004(2) -0.0011(19) C9 0.030(3) 0.018(3) 0.066(4) -0.001(2) -0.008(3) 0.005(2) C10 0.035(3) 0.019(3) 0.070(4) 0.009(2) -0.018(3) -0.006(2) C11 0.016(2) 0.030(3) 0.045(3) 0.015(2) -0.010(2) -0.009(2) C12 0.019(2) 0.025(2) 0.034(3) 0.0089(19) -0.0109(19) -0.0025(19) C13 0.026(2) 0.014(2) 0.023(2) -0.0007(16) -0.0041(18) 0.0091(18) C14 0.030(3) 0.012(2) 0.025(2) 0.0007(17) -0.0002(19) 0.0053(18) C15 0.047(3) 0.018(2) 0.027(2) 0.0037(19) 0.009(2) 0.006(2) C16 0.072(4) 0.020(3) 0.023(2) -0.0010(19) 0.000(3) 0.013(3) C17 0.048(3) 0.020(2) 0.033(3) -0.008(2) -0.016(2) 0.007(2) C18 0.029(3) 0.020(2) 0.030(2) -0.0007(18) -0.005(2) 0.0029(19) C19 0.017(2) 0.016(2) 0.028(2) -0.0011(17) 0.0046(18) 0.0000(17) C20 0.019(2) 0.019(2) 0.030(2) -0.0004(18) 0.0061(19) 0.0027(18) C21 0.029(3) 0.020(2) 0.049(3) 0.011(2) 0.006(2) 0.003(2) C22 0.030(3) 0.016(2) 0.067(4) -0.001(2) 0.003(3) -0.003(2) C23 0.023(3) 0.029(3) 0.052(3) -0.008(2) 0.002(2) -0.009(2) C24 0.018(2) 0.022(2) 0.035(3) -0.0039(19) -0.0006(19) 0.0027(18) C25 0.024(3) 0.017(2) 0.025(2) 0.0033(17) -0.0041(18) -0.0038(18) C26 0.015(2) 0.016(2) 0.045(3) 0.0018(19) -0.008(2) 0.0000(18) C27 0.022(2) 0.018(2) 0.044(3) 0.005(2) -0.011(2) -0.0029(19) C28 0.022(2) 0.021(2) 0.051(3) 0.003(2) -0.017(2) -0.0032(19) C29 0.017(2) 0.021(3) 0.065(4) 0.003(2) -0.007(2) 0.0032(19) C30 0.019(2) 0.023(3) 0.054(3) -0.003(2) 0.000(2) 0.0031(19) C31 0.022(2) 0.015(2) 0.045(3) 0.0029(19) -0.007(2) -0.0019(18) C32 0.026(3) 0.040(3) 0.041(3) 0.006(2) -0.012(2) 0.000(2) C33 0.028(3) 0.028(3) 0.040(3) -0.004(2) -0.003(2) 0.005(2) C34 0.019(2) 0.015(2) 0.023(2) -0.0001(16) -0.0003(17) -0.0033(17) C35 0.013(2) 0.017(2) 0.053(3) 0.005(2) -0.008(2) 0.0004(18) C36 0.017(2) 0.018(2) 0.063(4) -0.003(2) 0.005(2) -0.0004(19) C37 0.020(3) 0.023(3) 0.088(5) -0.003(3) 0.003(3) -0.003(2) C38 0.019(3) 0.017(3) 0.093(5) 0.008(3) -0.003(3) -0.001(2) C39 0.026(3) 0.020(3) 0.079(4) 0.018(3) -0.019(3) -0.005(2) C40 0.025(3) 0.019(3) 0.060(4) 0.015(2) -0.013(2) -0.005(2) C41 0.027(3) 0.046(3) 0.056(4) -0.012(3) 0.011(3) -0.003(2) C42 0.033(3) 0.042(3) 0.043(3) 0.016(2) -0.012(2) -0.002(2) N3 0.020(2) 0.023(2) 0.030(2) -0.0027(16) -0.0027(16) -0.0039(16) C43 0.024(3) 0.032(3) 0.037(3) -0.011(2) -0.002(2) -0.006(2) C44 0.043(3) 0.054(4) 0.041(3) -0.011(3) -0.016(3) -0.001(3) C45 0.041(4) 0.134(8) 0.039(4) -0.026(4) 0.001(3) -0.032(4) C46 0.057(5) 0.172(10) 0.038(4) -0.028(5) -0.008(3) 0.006(6) C47 0.021(2) 0.030(3) 0.038(3) -0.002(2) -0.002(2) -0.008(2) C48 0.025(3) 0.039(3) 0.051(3) -0.011(3) 0.002(2) -0.004(2) C49 0.027(3) 0.070(5) 0.051(4) 0.009(3) 0.006(3) 0.015(3) C50 0.078(4) 0.107(5) 0.083(4) 0.020(4) 0.008(4) 0.016(4) C51 0.031(3) 0.024(3) 0.031(3) -0.0017(19) 0.000(2) 0.002(2) C52 0.089(5) 0.025(3) 0.047(3) -0.009(2) -0.036(3) 0.019(3) C53 0.051(4) 0.126(8) 0.035(3) 0.000(4) -0.001(3) 0.024(4) C54 0.056(9) 0.035(8) 0.032(7) -0.007(5) -0.020(6) 0.017(6) C54' 0.060(10) 0.041(9) 0.043(8) -0.002(6) -0.011(7) 0.012(7) C55 0.026(3) 0.019(2) 0.042(3) 0.002(2) -0.007(2) -0.0013(19) C56 0.024(3) 0.025(3) 0.044(3) -0.004(2) -0.005(2) 0.002(2) C57 0.032(3) 0.023(3) 0.067(4) -0.004(2) -0.007(3) 0.001(2) C58 0.038(3) 0.038(3) 0.078(5) -0.010(3) 0.004(3) 0.009(3) Cl1 0.0617(17) 0.0686(19) 0.127(3) 0.0045(17) 0.0044(17) 0.0022(14) Cl2 0.0629(19) 0.161(4) 0.086(2) -0.030(2) 0.0140(16) -0.0150(19) C59 0.045(3) 0.065(4) 0.049(3) -0.014(3) 0.016(3) 0.011(3) Cl1' 0.0617(17) 0.0686(19) 0.127(3) 0.0045(17) 0.0044(17) 0.0022(14) Cl2' 0.0629(19) 0.161(4) 0.086(2) -0.030(2) 0.0140(16) -0.0150(19) C59' 0.045(3) 0.065(4) 0.049(3) -0.014(3) 0.016(3) 0.011(3) Cl3 0.106(3) 0.081(2) 0.083(2) 0.0307(17) -0.0230(18) -0.0227(19) Cl4 0.106(3) 0.081(2) 0.083(2) 0.0307(17) -0.0230(18) -0.0227(19) C60 0.098(7) 0.081(7) 0.079(6) 0.006(5) -0.012(5) -0.012(5) Cl5 0.128(4) 0.127(4) 0.176(5) -0.051(4) -0.033(4) -0.036(3) C61 0.053(7) 0.054(7) 0.039(7) -0.014(5) -0.015(5) -0.014(5) _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 Cr C25 2.068(5) . ? Cr C34 2.086(5) . ? Cr C13 2.149(4) . ? Cr C1 2.153(5) . ? Cr C7 2.155(5) . ? Cr C19 2.157(4) . ? F2 C2 1.359(6) . ? F3 C3 1.368(7) . ? F4 C4 1.359(7) . ? F5 C5 1.345(7) . ? F6 C6 1.360(6) . ? F8 C8 1.355(6) . ? F9 C9 1.364(6) . ? F10 C10 1.342(6) . ? F11 C11 1.350(6) . ? F12 C12 1.356(6) . ? F14 C14 1.365(6) . ? F15 C15 1.356(6) . ? F16 C16 1.350(6) . ? F17 C17 1.351(6) . ? F18 C18 1.369(6) . ? F20 C20 1.348(6) . ? F21 C21 1.359(6) . ? F22 C22 1.348(6) . ? F23 C23 1.361(6) . ? F24 C24 1.364(6) . ? N1 C25 1.168(6) . ? N1 C26 1.393(6) . ? N2 C34 1.159(6) . ? N2 C35 1.406(6) . ? C1 C2 1.384(7) . ? C1 C6 1.393(7) . ? C2 C3 1.378(8) . ? C3 C4 1.339(10) . ? C4 C5 1.402(10) . ? C5 C6 1.363(7) . ? C7 C8 1.388(7) . ? C7 C12 1.402(6) . ? C8 C9 1.365(7) . ? C9 C10 1.356(8) . ? C10 C11 1.401(8) . ? C11 C12 1.373(7) . ? C13 C14 1.376(7) . ? C13 C18 1.379(7) . ? C14 C15 1.384(7) . ? C15 C16 1.361(8) . ? C16 C17 1.353(8) . ? C17 C18 1.399(7) . ? C19 C24 1.370(7) . ? C19 C20 1.396(6) . ? C20 C21 1.395(7) . ? C21 C22 1.355(8) . ? C22 C23 1.375(8) . ? C23 C24 1.382(7) . ? C26 C31 1.394(7) . ? C26 C27 1.416(7) . ? C27 C28 1.384(7) . ? C27 C32 1.498(8) . ? C28 C29 1.345(8) . ? C29 C30 1.413(8) . ? C30 C31 1.380(7) . ? C31 C33 1.492(7) . ? C35 C36 1.384(8) . ? C35 C40 1.395(8) . ? C36 C37 1.404(7) . ? C36 C41 1.486(9) . ? C37 C38 1.393(10) . ? C38 C39 1.363(9) . ? C39 C40 1.404(7) . ? C40 C42 1.499(8) . ? N3 C51 1.512(6) . ? N3 C43 1.514(6) . ? N3 C55 1.516(6) . ? N3 C47 1.530(6) . ? C43 C44 1.510(8) . ? C44 C45 1.526(9) . ? C45 C46 1.501(11) . ? C47 C48 1.511(7) . ? C48 C49 1.527(8) . ? C49 C50 1.494(11) . ? C51 C52 1.504(8) . ? C52 C53 1.521(10) . ? C53 C54' 1.383(17) . ? C53 C54 1.687(16) . ? C55 C56 1.522(7) . ? C56 C57 1.523(7) . ? C57 C58 1.514(8) . ? Cl1 C59 1.710(5) . ? Cl2 C59 1.720(5) . ? Cl1' C59' 1.724(5) . ? Cl2' C59' 1.744(5) . ? Cl3 C60 1.735(5) . ? Cl4 C60 1.736(5) . ? Cl5 C61 1.728(5) . ? Cl5 C61 1.731(5) 2_565 ? C61 Cl5 1.731(5) 2_565 ? 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 C25 Cr C34 177.00(17) . . ? C25 Cr C13 88.26(17) . . ? C34 Cr C13 88.74(17) . . ? C25 Cr C1 91.04(18) . . ? C34 Cr C1 91.96(17) . . ? C13 Cr C1 179.18(17) . . ? C25 Cr C7 88.66(17) . . ? C34 Cr C7 91.47(17) . . ? C13 Cr C7 90.43(17) . . ? C1 Cr C7 89.99(17) . . ? C25 Cr C19 90.56(17) . . ? C34 Cr C19 89.28(17) . . ? C13 Cr C19 89.17(17) . . ? C1 Cr C19 90.40(17) . . ? C7 Cr C19 179.14(17) . . ? C25 N1 C26 176.5(5) . . ? C34 N2 C35 178.1(5) . . ? C2 C1 C6 112.6(4) . . ? C2 C1 Cr 123.3(4) . . ? C6 C1 Cr 124.1(3) . . ? F2 C2 C3 115.4(5) . . ? F2 C2 C1 120.6(4) . . ? C3 C2 C1 124.0(5) . . ? C4 C3 F3 119.5(5) . . ? C4 C3 C2 120.4(5) . . ? F3 C3 C2 120.0(6) . . ? C3 C4 F4 121.7(6) . . ? C3 C4 C5 119.4(5) . . ? F4 C4 C5 118.9(6) . . ? F5 C5 C6 122.3(6) . . ? F5 C5 C4 119.9(5) . . ? C6 C5 C4 117.8(6) . . ? F6 C6 C5 114.2(5) . . ? F6 C6 C1 120.1(4) . . ? C5 C6 C1 125.6(5) . . ? C8 C7 C12 111.7(4) . . ? C8 C7 Cr 125.2(3) . . ? C12 C7 Cr 123.1(3) . . ? F8 C8 C9 114.5(4) . . ? F8 C8 C7 119.8(4) . . ? C9 C8 C7 125.7(5) . . ? C10 C9 F9 118.8(5) . . ? C10 C9 C8 120.3(5) . . ? F9 C9 C8 120.8(5) . . ? F10 C10 C9 122.6(6) . . ? F10 C10 C11 119.2(5) . . ? C9 C10 C11 118.2(5) . . ? F11 C11 C12 121.4(5) . . ? F11 C11 C10 119.6(5) . . ? C12 C11 C10 119.1(5) . . ? F12 C12 C11 115.0(4) . . ? F12 C12 C7 119.9(4) . . ? C11 C12 C7 125.0(5) . . ? C14 C13 C18 112.9(4) . . ? C14 C13 Cr 123.6(3) . . ? C18 C13 Cr 123.4(3) . . ? F14 C14 C13 120.1(4) . . ? F14 C14 C15 114.8(4) . . ? C13 C14 C15 125.1(5) . . ? F15 C15 C16 120.7(4) . . ? F15 C15 C14 120.6(5) . . ? C16 C15 C14 118.7(5) . . ? F16 C16 C17 120.0(5) . . ? F16 C16 C15 119.9(5) . . ? C17 C16 C15 120.1(5) . . ? F17 C17 C16 120.3(5) . . ? F17 C17 C18 120.7(5) . . ? C16 C17 C18 119.0(5) . . ? F18 C18 C13 121.3(4) . . ? F18 C18 C17 114.5(4) . . ? C13 C18 C17 124.2(5) . . ? C24 C19 C20 113.3(4) . . ? C24 C19 Cr 123.1(3) . . ? C20 C19 Cr 123.5(3) . . ? F20 C20 C21 115.1(4) . . ? F20 C20 C19 121.4(4) . . ? C21 C20 C19 123.5(5) . . ? C22 C21 F21 120.0(5) . . ? C22 C21 C20 120.0(5) . . ? F21 C21 C20 119.9(5) . . ? F22 C22 C21 121.0(5) . . ? F22 C22 C23 120.1(5) . . ? C21 C22 C23 118.9(5) . . ? F23 C23 C22 119.2(5) . . ? F23 C23 C24 121.3(5) . . ? C22 C23 C24 119.5(5) . . ? F24 C24 C19 120.5(4) . . ? F24 C24 C23 114.6(4) . . ? C19 C24 C23 124.9(5) . . ? N1 C25 Cr 174.9(4) . . ? N1 C26 C31 119.0(4) . . ? N1 C26 C27 117.9(4) . . ? C31 C26 C27 123.0(4) . . ? C28 C27 C26 117.0(5) . . ? C28 C27 C32 122.3(5) . . ? C26 C27 C32 120.7(4) . . ? C29 C28 C27 121.6(5) . . ? C28 C29 C30 120.8(5) . . ? C31 C30 C29 120.6(5) . . ? C30 C31 C26 117.1(5) . . ? C30 C31 C33 121.0(5) . . ? C26 C31 C33 122.0(4) . . ? N2 C34 Cr 177.1(4) . . ? C36 C35 C40 124.0(5) . . ? C36 C35 N2 118.2(5) . . ? C40 C35 N2 117.8(5) . . ? C35 C36 C37 116.7(6) . . ? C35 C36 C41 121.4(5) . . ? C37 C36 C41 121.9(5) . . ? C38 C37 C36 120.9(6) . . ? C39 C38 C37 120.4(5) . . ? C38 C39 C40 121.2(6) . . ? C35 C40 C39 116.8(6) . . ? C35 C40 C42 121.8(5) . . ? C39 C40 C42 121.4(5) . . ? C51 N3 C43 106.8(4) . . ? C51 N3 C55 111.5(4) . . ? C43 N3 C55 111.0(4) . . ? C51 N3 C47 111.0(4) . . ? C43 N3 C47 110.7(4) . . ? C55 N3 C47 105.9(4) . . ? C44 C43 N3 116.2(4) . . ? C43 C44 C45 109.3(6) . . ? C46 C45 C44 110.1(7) . . ? C48 C47 N3 116.4(4) . . ? C47 C48 C49 109.5(5) . . ? C50 C49 C48 114.7(6) . . ? C52 C51 N3 115.9(4) . . ? C51 C52 C53 111.1(6) . . ? C54' C53 C52 125.1(10) . . ? C54' C53 C54 29.0(7) . . ? C52 C53 C54 101.1(8) . . ? N3 C55 C56 116.6(4) . . ? C55 C56 C57 109.2(4) . . ? C58 C57 C56 113.1(5) . . ? Cl1 C59 Cl2 113.2(4) . . ? Cl1' C59' Cl2' 107.9(6) . . ? Cl3 C60 Cl4 107.4(4) . . ? C61 Cl5 C61 69.0(6) . 2_565 ? Cl5 C61 Cl5 111.0(6) . 2_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.959 _refine_diff_density_min -2.377 _refine_diff_density_rms 0.143