# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Menjon, Babil' _publ_contact_author_email menjon@unizar.es _publ_section_title ; A square-pyramidal organochromium(V) compound ; loop_ _publ_author_name M.Garcia-Monforte P.Alonso A.Arauzo A.Martin B.Menjon C.Rillo # Attachment '- amt622.cif' data_amt622 _database_code_depnum_ccdc_archive 'CCDC 833476' #TrackingRef '- amt622.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H36 Cr F20 N O' _chemical_formula_weight 978.70 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' 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.3583(2) _cell_length_b 19.4978(2) _cell_length_c 22.7303(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8136.22(17) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 19578 _cell_measurement_theta_min 4.1737 _cell_measurement_theta_max 28.7924 _exptl_crystal_description bloc _exptl_crystal_colour brown _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3960 _exptl_absorpt_coefficient_mu 0.408 _exptl_absorpt_correction_T_min 0.8507 _exptl_absorpt_correction_T_max 0.9085 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _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 'Xcalibur, Sapphire3' _diffrn_detector_area_resol_mean 16.0655 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46990 _diffrn_reflns_av_R_equivalents 0.0358 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 4.22 _diffrn_reflns_theta_max 28.86 _diffrn_orient_matrix_UB_11 -0.0232440876 _diffrn_orient_matrix_UB_12 0.0171400140 _diffrn_orient_matrix_UB_13 -0.0201071641 _diffrn_orient_matrix_UB_21 0.0279016941 _diffrn_orient_matrix_UB_22 -0.0008539230 _diffrn_orient_matrix_UB_23 -0.0215683682 _diffrn_orient_matrix_UB_31 -0.0131656325 _diffrn_orient_matrix_UB_32 -0.0320703282 _diffrn_orient_matrix_UB_33 -0.0101772565 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -79.00 44.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - -19.9615 0.0000 90.0000 123 #__ type_ start__ end____ width___ exp.time_ 2 omega 62.00 102.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 179.0000 -120.0000 40 #__ type_ start__ end____ width___ exp.time_ 3 omega -51.00 4.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 -37.0000 -150.0000 55 #__ type_ start__ end____ width___ exp.time_ 4 omega -11.00 95.00 1.0000 60.0000 omega____ theta____ kappa____ phi______ frames - 22.1490 77.0000 -30.0000 106 ; _reflns_number_total 9764 _reflns_number_gt 6594 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) ; _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^)+(0.0869P)^2^+1.0484P] 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 9764 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0788 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1479 _refine_ls_wR_factor_gt 0.1370 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 Cr Cr 0.59700(2) 0.246419(19) 0.800064(15) 0.02076(11) Uani 1 1 d . . . F2 F 0.53804(8) 0.19315(7) 0.67448(6) 0.0286(3) Uani 1 1 d . . . F3 F 0.42059(9) 0.22630(9) 0.61051(7) 0.0406(4) Uani 1 1 d . . . F4 F 0.31862(9) 0.31330(9) 0.65482(8) 0.0483(5) Uani 1 1 d . . . F5 F 0.33292(9) 0.36122(8) 0.76691(9) 0.0468(5) Uani 1 1 d . . . F6 F 0.45528(9) 0.33823(8) 0.82745(7) 0.0371(4) Uani 1 1 d . . . F8 F 0.69101(9) 0.17488(8) 0.90238(6) 0.0348(4) Uani 1 1 d . . . F9 F 0.81677(9) 0.10615(8) 0.90153(7) 0.0449(4) Uani 1 1 d . . . F10 F 0.89464(9) 0.09207(9) 0.79990(8) 0.0491(5) Uani 1 1 d . . . F11 F 0.84397(9) 0.15053(8) 0.69873(7) 0.0418(4) Uani 1 1 d . . . F12 F 0.71848(9) 0.21851(8) 0.69869(6) 0.0323(3) Uani 1 1 d . . . F14 F 0.61666(8) 0.30658(7) 0.66162(6) 0.0313(3) Uani 1 1 d . . . F15 F 0.67805(9) 0.41989(8) 0.62091(6) 0.0388(4) Uani 1 1 d . . . F16 F 0.73800(10) 0.51308(8) 0.69550(7) 0.0419(4) Uani 1 1 d . . . F17 F 0.73664(10) 0.48799(8) 0.81356(7) 0.0441(4) Uani 1 1 d . . . F18 F 0.67593(8) 0.37525(7) 0.85638(6) 0.0319(3) Uani 1 1 d . . . F20 F 0.46983(8) 0.17970(8) 0.87282(6) 0.0338(4) Uani 1 1 d . . . F21 F 0.42466(9) 0.05204(9) 0.89104(7) 0.0469(4) Uani 1 1 d . . . F22 F 0.48439(10) -0.05418(8) 0.82921(9) 0.0532(5) Uani 1 1 d . . . F23 F 0.58692(10) -0.02788(7) 0.74608(8) 0.0469(4) Uani 1 1 d . . . F24 F 0.63383(8) 0.09876(7) 0.72738(6) 0.0294(3) Uani 1 1 d . . . O O 0.58267(10) 0.27059(9) 0.86341(7) 0.0286(4) Uani 1 1 d . . . C1 C 0.50373(13) 0.26622(11) 0.75261(10) 0.0216(5) Uani 1 1 d . . . C2 C 0.49003(13) 0.23860(12) 0.69772(10) 0.0236(5) Uani 1 1 d . . . C3 C 0.43006(15) 0.25446(13) 0.66421(11) 0.0303(6) Uani 1 1 d . . . C4 C 0.37822(14) 0.29748(14) 0.68685(13) 0.0331(6) Uani 1 1 d . . . C5 C 0.38603(14) 0.32298(13) 0.74249(13) 0.0317(6) Uani 1 1 d . . . C6 C 0.44910(15) 0.30886(12) 0.77402(11) 0.0285(5) Uani 1 1 d . . . C7 C 0.69961(13) 0.20140(11) 0.80048(10) 0.0219(5) Uani 1 1 d . . . C8 C 0.72772(14) 0.17125(12) 0.85067(10) 0.0259(5) Uani 1 1 d . . . C9 C 0.79258(14) 0.13509(13) 0.85134(12) 0.0306(6) Uani 1 1 d . . . C10 C 0.83183(14) 0.12792(13) 0.79999(13) 0.0325(6) Uani 1 1 d . . . C11 C 0.80653(15) 0.15737(13) 0.74983(12) 0.0312(6) Uani 1 1 d . . . C12 C 0.74199(14) 0.19307(12) 0.75092(10) 0.0253(5) Uani 1 1 d . . . C13 C 0.64247(13) 0.33385(11) 0.76142(10) 0.0216(5) Uani 1 1 d . . . C14 C 0.64572(13) 0.35000(12) 0.70197(10) 0.0233(5) Uani 1 1 d . . . C15 C 0.67652(14) 0.40873(13) 0.67922(11) 0.0267(5) Uani 1 1 d . . . C16 C 0.70656(14) 0.45599(12) 0.71704(12) 0.0289(5) Uani 1 1 d . . . C17 C 0.70509(14) 0.44313(12) 0.77625(11) 0.0293(6) Uani 1 1 d . . . C18 C 0.67370(13) 0.38360(12) 0.79703(10) 0.0244(5) Uani 1 1 d . . . C19 C 0.55719(13) 0.14567(12) 0.80116(10) 0.0218(5) Uani 1 1 d . . . C20 C 0.50225(13) 0.13005(13) 0.84095(10) 0.0253(5) Uani 1 1 d . . . C21 C 0.47714(14) 0.06368(15) 0.85075(11) 0.0320(6) Uani 1 1 d . . . C22 C 0.50631(16) 0.01062(13) 0.81984(13) 0.0343(6) Uani 1 1 d . . . C23 C 0.55874(15) 0.02394(12) 0.77854(12) 0.0311(6) Uani 1 1 d . . . C24 C 0.58281(13) 0.09026(12) 0.76955(11) 0.0245(5) Uani 1 1 d . . . N N 0.68705(12) 0.34413(12) 0.03113(9) 0.0316(5) Uani 1 1 d . . . C25 C 0.74325(16) 0.29998(15) 0.06229(11) 0.0353(6) Uani 1 1 d . . . H25A H 0.7778 0.3309 0.0826 0.042 Uiso 1 1 calc R . . H25B H 0.7178 0.2731 0.0930 0.042 Uiso 1 1 calc R . . C26 C 0.78708(18) 0.25059(18) 0.02519(14) 0.0478(8) Uani 1 1 d . . . H26A H 0.8171 0.2764 -0.0034 0.057 Uiso 1 1 calc R . . H26B H 0.7538 0.2202 0.0029 0.057 Uiso 1 1 calc R . . C27 C 0.8363(2) 0.20755(19) 0.06499(16) 0.0550(9) Uani 1 1 d . . . H27A H 0.8725 0.2383 0.0837 0.066 Uiso 1 1 calc R . . H27B H 0.8062 0.1875 0.0968 0.066 Uiso 1 1 calc R . . C28 C 0.8760(3) 0.1511(2) 0.03497(18) 0.0765(12) Uani 1 1 d . . . H28A H 0.9068 0.1271 0.0635 0.115 Uiso 1 1 calc R . . H28B H 0.9066 0.1702 0.0036 0.115 Uiso 1 1 calc R . . H28C H 0.8409 0.1189 0.0180 0.115 Uiso 1 1 calc R . . C29 C 0.63290(15) 0.29896(15) -0.00258(10) 0.0322(6) Uani 1 1 d . . . H29A H 0.5965 0.3291 -0.0216 0.039 Uiso 1 1 calc R . . H29B H 0.6596 0.2748 -0.0342 0.039 Uiso 1 1 calc R . . C30 C 0.59277(16) 0.24611(15) 0.03382(11) 0.0360(6) Uani 1 1 d . . . H30A H 0.5652 0.2693 0.0656 0.043 Uiso 1 1 calc R . . H30B H 0.6282 0.2144 0.0522 0.043 Uiso 1 1 calc R . . C31 C 0.54079(16) 0.20603(15) -0.00488(11) 0.0365(6) Uani 1 1 d . . . H31A H 0.5686 0.1849 -0.0375 0.044 Uiso 1 1 calc R . . H31B H 0.5049 0.2381 -0.0223 0.044 Uiso 1 1 calc R . . C32 C 0.50023(19) 0.15003(17) 0.02837(13) 0.0478(8) Uani 1 1 d . . . H32A H 0.4670 0.1263 0.0015 0.072 Uiso 1 1 calc R . . H32B H 0.4723 0.1706 0.0606 0.072 Uiso 1 1 calc R . . H32C H 0.5353 0.1171 0.0445 0.072 Uiso 1 1 calc R . . C33 C 0.72273(17) 0.38947(16) -0.01467(11) 0.0393(7) Uani 1 1 d . . . H33A H 0.6840 0.4160 -0.0347 0.047 Uiso 1 1 calc R . . H33B H 0.7456 0.3595 -0.0446 0.047 Uiso 1 1 calc R . . C34 C 0.78003(19) 0.43964(18) 0.00722(13) 0.0482(8) Uani 1 1 d . . . H34A H 0.8181 0.4149 0.0296 0.058 Uiso 1 1 calc R . . H34B H 0.7574 0.4740 0.0336 0.058 Uiso 1 1 calc R . . C35 C 0.8142(2) 0.47567(17) -0.04656(14) 0.0504(8) Uani 1 1 d . . . H35A H 0.8372 0.4409 -0.0723 0.060 Uiso 1 1 calc R . . H35B H 0.7754 0.4988 -0.0694 0.060 Uiso 1 1 calc R . . C36 C 0.8701(2) 0.52737(18) -0.02873(16) 0.0583(9) Uani 1 1 d . . . H36A H 0.8907 0.5490 -0.0639 0.087 Uiso 1 1 calc R . . H36B H 0.9090 0.5046 -0.0066 0.087 Uiso 1 1 calc R . . H36C H 0.8473 0.5625 -0.0040 0.087 Uiso 1 1 calc R . . C37 C 0.64827(16) 0.38553(14) 0.07901(11) 0.0340(6) Uani 1 1 d . . . H37A H 0.6302 0.3532 0.1093 0.041 Uiso 1 1 calc R . . H37B H 0.6846 0.4157 0.0982 0.041 Uiso 1 1 calc R . . C38 C 0.58469(18) 0.42957(15) 0.05880(12) 0.0404(7) Uani 1 1 d . . . H38A H 0.5464 0.3999 0.0417 0.048 Uiso 1 1 calc R . . H38B H 0.6014 0.4616 0.0278 0.048 Uiso 1 1 calc R . . C39 C 0.55304(19) 0.47022(15) 0.11019(13) 0.0441(7) Uani 1 1 d . . . H39A H 0.5410 0.4381 0.1425 0.053 Uiso 1 1 calc R . . H39B H 0.5905 0.5025 0.1249 0.053 Uiso 1 1 calc R . . C40 C 0.4851(2) 0.51043(19) 0.09391(16) 0.0592(10) Uani 1 1 d . . . H40A H 0.4673 0.5352 0.1285 0.089 Uiso 1 1 calc R . . H40B H 0.4474 0.4788 0.0800 0.089 Uiso 1 1 calc R . . H40C H 0.4968 0.5432 0.0627 0.089 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 0.0223(2) 0.0242(2) 0.01585(18) -0.00215(15) 0.00107(14) 0.00216(16) F2 0.0308(8) 0.0320(7) 0.0229(7) -0.0038(6) 0.0023(6) 0.0008(6) F3 0.0376(9) 0.0553(10) 0.0291(8) 0.0040(7) -0.0100(7) -0.0126(8) F4 0.0279(9) 0.0528(10) 0.0641(11) 0.0215(9) -0.0153(8) -0.0023(8) F5 0.0264(8) 0.0346(9) 0.0795(13) 0.0039(8) 0.0113(8) 0.0106(7) F6 0.0384(9) 0.0356(8) 0.0372(9) -0.0086(7) 0.0078(7) 0.0074(7) F8 0.0407(9) 0.0389(8) 0.0247(7) 0.0027(6) 0.0005(7) 0.0046(7) F9 0.0405(10) 0.0438(9) 0.0502(10) 0.0084(8) -0.0170(8) 0.0074(8) F10 0.0232(8) 0.0444(10) 0.0797(14) -0.0018(9) -0.0022(8) 0.0089(7) F11 0.0307(8) 0.0441(9) 0.0504(10) -0.0082(8) 0.0189(7) 0.0003(7) F12 0.0361(9) 0.0388(8) 0.0220(7) -0.0031(6) 0.0049(6) 0.0014(7) F14 0.0384(9) 0.0381(8) 0.0173(6) -0.0048(6) -0.0027(6) -0.0103(7) F15 0.0451(10) 0.0462(9) 0.0250(7) 0.0097(7) 0.0007(7) -0.0081(8) F16 0.0493(11) 0.0282(8) 0.0482(10) 0.0073(7) -0.0024(8) -0.0103(7) F17 0.0574(11) 0.0311(8) 0.0440(9) -0.0121(7) -0.0132(8) -0.0072(8) F18 0.0388(9) 0.0370(8) 0.0198(7) -0.0060(6) -0.0057(6) 0.0006(7) F20 0.0265(8) 0.0475(9) 0.0275(7) -0.0077(7) 0.0039(6) 0.0029(7) F21 0.0355(9) 0.0666(11) 0.0387(9) 0.0121(8) 0.0078(7) -0.0165(9) F22 0.0504(11) 0.0350(9) 0.0743(13) 0.0156(9) -0.0004(10) -0.0158(8) F23 0.0488(10) 0.0231(8) 0.0688(12) -0.0071(7) 0.0062(9) 0.0015(7) F24 0.0268(8) 0.0277(7) 0.0338(8) -0.0068(6) 0.0078(6) -0.0010(6) O 0.0331(10) 0.0331(9) 0.0197(8) -0.0027(7) 0.0029(7) 0.0008(8) C1 0.0205(11) 0.0220(11) 0.0223(11) 0.0038(9) 0.0023(9) 0.0000(9) C2 0.0205(11) 0.0264(12) 0.0240(11) 0.0028(10) 0.0037(10) -0.0020(9) C3 0.0278(13) 0.0362(14) 0.0269(12) 0.0093(11) -0.0044(10) -0.0105(12) C4 0.0217(12) 0.0317(14) 0.0460(16) 0.0166(12) -0.0057(12) -0.0041(11) C5 0.0201(12) 0.0235(12) 0.0514(16) 0.0061(11) 0.0063(12) 0.0017(10) C6 0.0304(13) 0.0227(12) 0.0324(13) 0.0031(10) 0.0060(11) 0.0000(10) C7 0.0204(11) 0.0207(11) 0.0247(12) -0.0043(9) -0.0014(9) -0.0042(9) C8 0.0263(12) 0.0269(12) 0.0244(12) -0.0028(10) -0.0014(10) -0.0018(10) C9 0.0292(14) 0.0273(13) 0.0353(14) 0.0035(11) -0.0104(11) -0.0029(11) C10 0.0172(12) 0.0255(12) 0.0548(17) -0.0076(12) -0.0006(12) 0.0017(10) C11 0.0274(13) 0.0292(13) 0.0370(14) -0.0089(11) 0.0067(11) -0.0066(11) C12 0.0241(12) 0.0252(11) 0.0266(12) -0.0043(10) 0.0007(10) -0.0051(10) C13 0.0198(11) 0.0238(11) 0.0213(11) -0.0024(9) -0.0001(9) 0.0033(9) C14 0.0245(12) 0.0253(12) 0.0200(11) -0.0029(9) -0.0020(10) 0.0003(10) C15 0.0258(13) 0.0309(13) 0.0236(11) 0.0019(10) -0.0009(10) 0.0013(11) C16 0.0268(13) 0.0205(12) 0.0395(14) 0.0043(10) -0.0020(11) 0.0011(10) C17 0.0284(13) 0.0228(12) 0.0368(14) -0.0111(10) -0.0088(11) 0.0035(11) C18 0.0247(12) 0.0295(12) 0.0189(11) -0.0022(9) -0.0033(10) 0.0081(10) C19 0.0184(11) 0.0257(11) 0.0213(11) 0.0024(9) -0.0053(9) 0.0022(9) C20 0.0195(11) 0.0358(13) 0.0207(11) 0.0021(10) -0.0036(9) 0.0012(11) C21 0.0219(13) 0.0468(16) 0.0272(12) 0.0127(12) -0.0025(10) -0.0066(12) C22 0.0333(15) 0.0269(13) 0.0427(15) 0.0090(11) -0.0090(12) -0.0085(12) C23 0.0274(13) 0.0239(12) 0.0420(14) -0.0021(11) -0.0049(12) 0.0016(11) C24 0.0180(11) 0.0288(12) 0.0266(12) 0.0004(10) 0.0002(9) 0.0004(10) N 0.0352(12) 0.0427(13) 0.0169(9) 0.0048(9) -0.0054(9) -0.0053(10) C25 0.0374(15) 0.0482(16) 0.0202(12) 0.0022(11) -0.0102(11) -0.0008(13) C26 0.0441(18) 0.065(2) 0.0343(15) -0.0075(14) -0.0120(14) 0.0072(16) C27 0.0466(19) 0.065(2) 0.0534(19) -0.0115(17) -0.0250(16) 0.0143(17) C28 0.080(3) 0.086(3) 0.064(2) -0.001(2) -0.024(2) 0.023(3) C29 0.0312(14) 0.0479(16) 0.0175(11) 0.0000(11) -0.0062(10) -0.0036(13) C30 0.0418(16) 0.0471(16) 0.0191(11) 0.0019(11) -0.0010(11) -0.0033(14) C31 0.0369(15) 0.0466(16) 0.0261(13) 0.0005(12) -0.0002(12) -0.0050(13) C32 0.0514(19) 0.0539(19) 0.0381(16) -0.0079(14) 0.0130(15) -0.0134(16) C33 0.0396(16) 0.0568(18) 0.0216(12) 0.0103(12) -0.0061(12) -0.0094(14) C34 0.0512(19) 0.060(2) 0.0336(15) 0.0151(14) -0.0117(14) -0.0170(16) C35 0.058(2) 0.0504(19) 0.0432(17) 0.0094(14) -0.0068(16) -0.0071(16) C36 0.067(2) 0.052(2) 0.056(2) 0.0125(16) 0.0021(18) -0.0133(18) C37 0.0411(16) 0.0399(15) 0.0211(12) 0.0038(11) -0.0044(11) -0.0046(13) C38 0.0496(18) 0.0431(16) 0.0285(14) 0.0030(12) -0.0091(13) 0.0009(14) C39 0.055(2) 0.0387(16) 0.0383(16) 0.0049(13) -0.0082(14) 0.0055(15) C40 0.070(3) 0.053(2) 0.055(2) -0.0001(16) -0.0150(18) 0.0121(19) _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 O 1.5376(17) . ? Cr C1 2.060(2) . ? Cr C7 2.078(2) . ? Cr C13 2.091(2) . ? Cr C19 2.096(2) . ? F2 C2 1.357(3) . ? F3 C3 1.350(3) . ? F4 C4 1.350(3) . ? F5 C5 1.347(3) . ? F6 C6 1.347(3) . ? F8 C8 1.357(3) . ? F9 C9 1.348(3) . ? F10 C10 1.348(3) . ? F11 C11 1.356(3) . ? F12 C12 1.357(3) . ? F14 C14 1.357(3) . ? F15 C15 1.343(3) . ? F16 C16 1.346(3) . ? F17 C17 1.349(3) . ? F18 C18 1.360(3) . ? F20 C20 1.348(3) . ? F21 C21 1.349(3) . ? F22 C22 1.343(3) . ? F23 C23 1.354(3) . ? F24 C24 1.350(3) . ? C1 C2 1.382(3) . ? C1 C6 1.391(3) . ? C2 C3 1.374(4) . ? C3 C4 1.369(4) . ? C4 C5 1.366(4) . ? C5 C6 1.389(4) . ? C7 C12 1.379(3) . ? C7 C8 1.383(3) . ? C8 C9 1.384(4) . ? C9 C10 1.379(4) . ? C10 C11 1.358(4) . ? C11 C12 1.374(4) . ? C13 C18 1.387(3) . ? C13 C14 1.389(3) . ? C14 C15 1.378(3) . ? C15 C16 1.376(4) . ? C16 C17 1.369(4) . ? C17 C18 1.379(4) . ? C19 C24 1.380(3) . ? C19 C20 1.389(3) . ? C20 C21 1.392(4) . ? C21 C22 1.360(4) . ? C22 C23 1.369(4) . ? C23 C24 1.382(3) . ? N C33 1.515(3) . ? N C25 1.519(3) . ? N C37 1.531(3) . ? N C29 1.533(3) . ? C25 C26 1.512(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.530(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.485(5) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.513(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.515(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.523(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.520(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.543(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.495(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.520(4) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.527(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.519(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? 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 O Cr C1 106.89(10) . . ? O Cr C7 106.28(9) . . ? C1 Cr C7 146.60(9) . . ? O Cr C13 102.22(9) . . ? C1 Cr C13 87.66(9) . . ? C7 Cr C13 89.10(9) . . ? O Cr C19 102.50(9) . . ? C1 Cr C19 83.80(9) . . ? C7 Cr C19 85.42(9) . . ? C13 Cr C19 155.23(9) . . ? C2 C1 C6 114.7(2) . . ? C2 C1 Cr 123.43(18) . . ? C6 C1 Cr 121.88(18) . . ? F2 C2 C3 116.8(2) . . ? F2 C2 C1 119.2(2) . . ? C3 C2 C1 124.0(2) . . ? F3 C3 C4 120.0(2) . . ? F3 C3 C2 120.9(2) . . ? C4 C3 C2 119.1(2) . . ? F4 C4 C5 120.1(3) . . ? F4 C4 C3 120.0(3) . . ? C5 C4 C3 119.9(2) . . ? F5 C5 C4 120.4(2) . . ? F5 C5 C6 120.0(3) . . ? C4 C5 C6 119.5(2) . . ? F6 C6 C5 116.8(2) . . ? F6 C6 C1 120.6(2) . . ? C5 C6 C1 122.6(2) . . ? C12 C7 C8 114.4(2) . . ? C12 C7 Cr 123.89(18) . . ? C8 C7 Cr 121.42(17) . . ? F8 C8 C7 120.5(2) . . ? F8 C8 C9 116.4(2) . . ? C7 C8 C9 123.1(2) . . ? F9 C9 C10 120.1(2) . . ? F9 C9 C8 120.4(2) . . ? C10 C9 C8 119.5(2) . . ? F10 C10 C11 120.7(2) . . ? F10 C10 C9 120.0(2) . . ? C11 C10 C9 119.3(2) . . ? F11 C11 C10 120.3(2) . . ? F11 C11 C12 120.1(2) . . ? C10 C11 C12 119.6(2) . . ? F12 C12 C11 116.3(2) . . ? F12 C12 C7 119.5(2) . . ? C11 C12 C7 124.1(2) . . ? C18 C13 C14 113.0(2) . . ? C18 C13 Cr 119.33(17) . . ? C14 C13 Cr 127.63(17) . . ? F14 C14 C15 115.2(2) . . ? F14 C14 C13 119.9(2) . . ? C15 C14 C13 124.8(2) . . ? F15 C15 C16 120.0(2) . . ? F15 C15 C14 120.9(2) . . ? C16 C15 C14 119.1(2) . . ? F16 C16 C17 121.2(2) . . ? F16 C16 C15 119.9(2) . . ? C17 C16 C15 118.9(2) . . ? F17 C17 C16 119.4(2) . . ? F17 C17 C18 120.6(2) . . ? C16 C17 C18 119.9(2) . . ? F18 C18 C17 115.3(2) . . ? F18 C18 C13 120.5(2) . . ? C17 C18 C13 124.1(2) . . ? C24 C19 C20 114.5(2) . . ? C24 C19 Cr 127.50(18) . . ? C20 C19 Cr 117.82(17) . . ? F20 C20 C19 120.9(2) . . ? F20 C20 C21 115.8(2) . . ? C19 C20 C21 123.3(2) . . ? F21 C21 C22 120.3(2) . . ? F21 C21 C20 120.1(3) . . ? C22 C21 C20 119.6(2) . . ? F22 C22 C21 121.0(3) . . ? F22 C22 C23 119.8(3) . . ? C21 C22 C23 119.1(2) . . ? F23 C23 C22 120.0(2) . . ? F23 C23 C24 119.7(2) . . ? C22 C23 C24 120.2(2) . . ? F24 C24 C19 120.7(2) . . ? F24 C24 C23 116.2(2) . . ? C19 C24 C23 123.1(2) . . ? C33 N C25 110.9(2) . . ? C33 N C37 112.5(2) . . ? C25 N C37 106.45(18) . . ? C33 N C29 105.79(18) . . ? C25 N C29 110.4(2) . . ? C37 N C29 110.9(2) . . ? C26 C25 N 117.5(2) . . ? C26 C25 H25A 107.9 . . ? N C25 H25A 107.9 . . ? C26 C25 H25B 107.9 . . ? N C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? C25 C26 C27 109.5(2) . . ? C25 C26 H26A 109.8 . . ? C27 C26 H26A 109.8 . . ? C25 C26 H26B 109.8 . . ? C27 C26 H26B 109.8 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C26 115.1(3) . . ? C28 C27 H27A 108.5 . . ? C26 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? C26 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 N 115.7(2) . . ? C30 C29 H29A 108.4 . . ? N C29 H29A 108.4 . . ? C30 C29 H29B 108.4 . . ? N C29 H29B 108.4 . . ? H29A C29 H29B 107.4 . . ? C29 C30 C31 109.9(2) . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30A 109.7 . . ? C29 C30 H30B 109.7 . . ? C31 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C30 C31 C32 112.9(2) . . ? C30 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? C30 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N C33 C34 116.7(2) . . ? N C33 H33A 108.1 . . ? C34 C33 H33A 108.1 . . ? N C33 H33B 108.1 . . ? C34 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C33 C34 C35 108.4(2) . . ? C33 C34 H34A 110.0 . . ? C35 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? C35 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C36 C35 C34 111.8(3) . . ? C36 C35 H35A 109.3 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 N 116.1(2) . . ? C38 C37 H37A 108.3 . . ? N C37 H37A 108.3 . . ? C38 C37 H37B 108.3 . . ? N C37 H37B 108.3 . . ? H37A C37 H37B 107.4 . . ? C37 C38 C39 110.7(2) . . ? C37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? C40 C39 C38 113.2(3) . . ? C40 C39 H39A 108.9 . . ? C38 C39 H39A 108.9 . . ? C40 C39 H39B 108.9 . . ? C38 C39 H39B 108.9 . . ? H39A C39 H39B 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.914 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.952 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.073