# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 # Attachment '- NJC-new.cif' data_sad #TrackingRef '- NJC-new.cif' #================================================================ # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Sun, Mingtai State Key Laboratory of Supramolecular Structure and Materials School of Chemistry Jilin University Changchun, 130023 P.R. China ; _publ_contact_author_phone 86(431)85168376 _publ_contact_author_fax 86(431)85193421 _publ_contact_author_email smt21@163.com _publ_requested_journal 'New Journal of Chemistry' _publ_requested_coeditor_name ? #=============================================================== # 2. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, structures and ethylene polymerization behavior of half-metallocene chromium(III) catalysts bearing salicylaldiminato ligands ; loop_ _publ_author_name _publ_author_addresst #<--'Last name, first name' 'Mingtai Sun' ; State Key Laboratory of Supramolecular Structure and Materials, School of Chemistry Jilin University Changchun, Jilin. 130023 P.R.China ; 'Ying Mu' ; State Key Laboratory of Supramolecular Structure and Materials, School of Chemistry Jilin University Changchun, Jilin. 130023 P.R.China ; 'Qiaolin Wu' ; State Key Laboratory of Supramolecular Structure and Materials, School of Chemistry Jilin University Changchun, Jilin. 130023 P.R.China ; 'Wei Gao' ; State Key Laboratory of Supramolecular Structure and Materials, School of Chemistry Jilin University Changchun, Jilin. 130023 P.R.China ; 'Ling Ye' ; State Key Laboratory of Supramolecular Structure and Materials, School of Chemistry Jilin University Changchun, Jilin. 130023 P.R.China ; #===END data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 756689' #TrackingRef '- NJC.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H35 Br Cl4 Cr N O' _chemical_formula_weight 639.25 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' 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 12.321(3) _cell_length_b 25.157(5) _cell_length_c 9.3501(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2898.2(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1308 _exptl_absorpt_coefficient_mu 2.160 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7376 _exptl_absorpt_correction_T_max 0.8129 _exptl_absorpt_process_details 'ABSCOR by T.Higashi 8 March, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 28218 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6618 _reflns_number_gt 5021 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0409P)^2^+0.8606P] 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 0.023(9) _refine_ls_number_reflns 6618 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 C20B C 0.1310(16) 0.4575(11) 0.606(4) 0.100(7) Uani 0.51(4) 1 d P A 1 H20A H 0.1157 0.4203 0.5943 0.150 Uiso 0.51(4) 1 calc PR A 1 H20B H 0.0756 0.4781 0.5600 0.150 Uiso 0.51(4) 1 calc PR A 1 H20C H 0.1326 0.4659 0.7063 0.150 Uiso 0.51(4) 1 calc PR A 1 C19B C 0.264(3) 0.5272(9) 0.555(4) 0.116(10) Uani 0.51(4) 1 d P A 1 H19A H 0.3323 0.5347 0.5089 0.173 Uiso 0.51(4) 1 calc PR A 1 H19B H 0.2694 0.5362 0.6546 0.173 Uiso 0.51(4) 1 calc PR A 1 H19C H 0.2079 0.5478 0.5112 0.173 Uiso 0.51(4) 1 calc PR A 1 C20A C 0.1603(16) 0.4813(10) 0.6617(17) 0.071(5) Uani 0.49(4) 1 d P A 2 H20D H 0.1211 0.4494 0.6844 0.106 Uiso 0.49(4) 1 calc PR A 2 H20E H 0.1102 0.5084 0.6329 0.106 Uiso 0.49(4) 1 calc PR A 2 H20F H 0.1997 0.4930 0.7444 0.106 Uiso 0.49(4) 1 calc PR A 2 C19A C 0.3015(18) 0.5231(8) 0.506(2) 0.061(4) Uani 0.49(4) 1 d P A 2 H19D H 0.3483 0.5176 0.4251 0.091 Uiso 0.49(4) 1 calc PR A 2 H19E H 0.3442 0.5334 0.5873 0.091 Uiso 0.49(4) 1 calc PR A 2 H19F H 0.2501 0.5506 0.4844 0.091 Uiso 0.49(4) 1 calc PR A 2 C18 C 0.2393(4) 0.47012(16) 0.5404(5) 0.0530(11) Uani 1 1 d . . . H18A H 0.2293 0.4644 0.4376 0.064 Uiso 0.51(4) 1 calc PR A 1 H18B H 0.1988 0.4572 0.4571 0.064 Uiso 0.49(4) 1 d PR A 2 Br1 Br 0.57432(4) 0.416827(17) 0.88017(4) 0.05420(13) Uani 1 1 d . . . C1 C 0.4269(3) 0.37220(15) 0.1756(4) 0.0446(9) Uani 1 1 d . A . C2 C 0.3309(3) 0.39240(15) 0.1101(4) 0.0477(10) Uani 1 1 d . A . C3 C 0.2891(4) 0.35269(17) 0.0198(4) 0.0464(10) Uani 1 1 d . A . C4 C 0.3572(3) 0.30806(17) 0.0272(4) 0.0448(10) Uani 1 1 d . A . C5 C 0.4436(3) 0.32014(16) 0.1217(4) 0.0472(9) Uani 1 1 d . A . C6 C 0.5035(4) 0.40231(19) 0.2677(5) 0.0639(12) Uani 1 1 d . . . H6A H 0.5371 0.3785 0.3345 0.096 Uiso 1 1 calc R . . H6B H 0.4645 0.4293 0.3188 0.096 Uiso 1 1 calc R . . H6C H 0.5582 0.4186 0.2092 0.096 Uiso 1 1 calc R . . C7 C 0.2880(5) 0.44774(18) 0.1284(6) 0.0768(15) Uani 1 1 d . . . H7A H 0.2910 0.4661 0.0385 0.115 Uiso 1 1 calc R . . H7B H 0.3312 0.4663 0.1975 0.115 Uiso 1 1 calc R . . H7C H 0.2141 0.4462 0.1608 0.115 Uiso 1 1 calc R . . C8 C 0.1922(4) 0.3578(2) -0.0759(5) 0.0743(15) Uani 1 1 d . . . H8A H 0.1442 0.3845 -0.0385 0.111 Uiso 1 1 calc R . . H8B H 0.1547 0.3244 -0.0804 0.111 Uiso 1 1 calc R . . H8C H 0.2154 0.3679 -0.1701 0.111 Uiso 1 1 calc R . . C9 C 0.3446(5) 0.2597(2) -0.0670(5) 0.0693(14) Uani 1 1 d . . . H9A H 0.2771 0.2424 -0.0456 0.104 Uiso 1 1 calc R . . H9B H 0.4035 0.2356 -0.0496 0.104 Uiso 1 1 calc R . . H9C H 0.3452 0.2704 -0.1655 0.104 Uiso 1 1 calc R . . C10 C 0.5415(4) 0.2867(2) 0.1497(6) 0.0708(14) Uani 1 1 d . . . H10A H 0.5260 0.2504 0.1252 0.106 Uiso 1 1 calc R . . H10B H 0.5603 0.2888 0.2492 0.106 Uiso 1 1 calc R . . H10C H 0.6010 0.2993 0.0929 0.106 Uiso 1 1 calc R . . C11 C 0.3232(3) 0.37812(13) 0.5150(4) 0.0337(8) Uani 1 1 d . . . C12 C 0.3978(3) 0.33914(14) 0.5641(4) 0.0357(8) Uani 1 1 d . A . C13 C 0.4699(3) 0.35068(14) 0.6763(4) 0.0386(8) Uani 1 1 d . . . H13 H 0.5172 0.3247 0.7100 0.046 Uiso 1 1 calc R A . C14 C 0.4701(3) 0.40052(14) 0.7356(4) 0.0394(8) Uani 1 1 d . A . C15 C 0.3962(3) 0.43878(15) 0.6925(4) 0.0418(9) Uani 1 1 d . . . H15 H 0.3967 0.4719 0.7366 0.050 Uiso 1 1 calc R A . C16 C 0.3222(3) 0.42871(14) 0.5859(4) 0.0378(8) Uani 1 1 d . A . C17 C 0.3947(3) 0.28542(14) 0.5143(4) 0.0409(9) Uani 1 1 d . . . H17 H 0.4314 0.2606 0.5698 0.049 Uiso 1 1 calc R A . C21 C 0.3354(4) 0.20657(14) 0.3940(5) 0.0547(11) Uani 1 1 d . . . C22 C 0.3104(5) 0.19071(15) 0.2403(5) 0.0702(14) Uani 1 1 d . A . H22A H 0.2958 0.1533 0.2362 0.105 Uiso 1 1 calc R . . H22B H 0.3717 0.1988 0.1807 0.105 Uiso 1 1 calc R . . H22C H 0.2481 0.2100 0.2072 0.105 Uiso 1 1 calc R . . C23 C 0.4369(5) 0.17753(18) 0.4420(6) 0.0876(19) Uani 1 1 d . A . H23A H 0.4457 0.1817 0.5434 0.131 Uiso 1 1 calc R . . H23B H 0.4989 0.1920 0.3937 0.131 Uiso 1 1 calc R . . H23C H 0.4303 0.1404 0.4195 0.131 Uiso 1 1 calc R . . C24 C 0.2393(5) 0.19329(19) 0.4899(6) 0.0787(17) Uani 1 1 d . A . H24A H 0.2195 0.1567 0.4770 0.118 Uiso 1 1 calc R . . H24B H 0.1789 0.2156 0.4653 0.118 Uiso 1 1 calc R . . H24C H 0.2589 0.1992 0.5880 0.118 Uiso 1 1 calc R . . C25 C 0.9217(5) 0.4008(2) 0.1305(7) 0.0916(17) Uani 1 1 d . . . H25 H 0.9636 0.3680 0.1194 0.110 Uiso 1 1 calc R . . Cl1 Cl 0.11073(8) 0.29269(4) 0.22421(11) 0.0497(2) Uani 1 1 d . A . Cl2 Cl 0.9286(2) 0.43547(9) -0.0311(2) 0.1364(7) Uani 1 1 d . . . Cl3 Cl 0.9747(2) 0.43484(11) 0.2715(3) 0.1733(11) Uani 1 1 d . . . Cl4 Cl 0.78974(17) 0.38347(9) 0.1630(3) 0.1300(7) Uani 1 1 d . . . Cr1 Cr 0.28895(4) 0.32270(2) 0.25138(6) 0.03290(13) Uani 1 1 d . . . N1 N 0.3467(3) 0.26716(11) 0.4003(3) 0.0396(7) Uani 1 1 d . A . O1 O 0.2562(2) 0.36888(9) 0.4101(2) 0.0376(6) Uani 1 1 d . A . 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 C20B 0.075(10) 0.107(14) 0.119(17) 0.011(12) 0.002(10) 0.029(10) C19B 0.093(18) 0.051(8) 0.20(3) -0.003(13) -0.030(17) 0.007(10) C20A 0.055(9) 0.088(12) 0.070(8) -0.009(7) 0.006(6) 0.032(8) C19A 0.067(12) 0.034(6) 0.082(9) 0.018(6) -0.008(7) 0.011(6) C18 0.062(3) 0.043(2) 0.054(2) -0.0049(19) -0.010(2) 0.014(2) Br1 0.0572(3) 0.0642(3) 0.04126(19) 0.0021(2) -0.01138(19) -0.0131(2) C1 0.039(2) 0.053(2) 0.0418(18) -0.0025(18) 0.0083(18) -0.020(2) C2 0.049(3) 0.049(2) 0.045(2) 0.012(2) 0.018(2) -0.0043(18) C3 0.045(2) 0.064(3) 0.0300(17) 0.0111(18) 0.0008(17) -0.004(2) C4 0.040(2) 0.058(2) 0.0370(19) -0.0048(18) 0.0096(17) -0.0104(19) C5 0.036(2) 0.055(2) 0.050(2) -0.002(2) 0.0138(19) -0.0030(18) C6 0.054(3) 0.082(3) 0.056(2) -0.011(2) 0.008(2) -0.031(2) C7 0.100(4) 0.052(3) 0.078(3) 0.018(3) 0.020(3) 0.007(3) C8 0.055(3) 0.115(4) 0.052(3) 0.024(3) -0.010(2) -0.011(3) C9 0.082(4) 0.072(3) 0.054(2) -0.017(2) 0.015(3) -0.021(3) C10 0.038(3) 0.081(3) 0.094(4) -0.004(3) 0.008(2) 0.006(2) C11 0.033(2) 0.0353(18) 0.0325(17) 0.0006(15) -0.0005(15) 0.0002(15) C12 0.037(2) 0.0382(18) 0.0319(16) 0.0016(15) 0.0036(15) 0.0000(15) C13 0.041(2) 0.0390(19) 0.0361(17) 0.0059(16) -0.0032(16) 0.0010(16) C14 0.038(2) 0.0497(19) 0.0306(16) 0.0002(17) -0.0024(16) -0.0060(16) C15 0.049(2) 0.0394(19) 0.0371(18) -0.0042(16) 0.0037(17) -0.0049(17) C16 0.040(2) 0.0368(19) 0.0370(18) -0.0019(15) 0.0009(15) -0.0005(15) C17 0.045(2) 0.0372(19) 0.0409(19) 0.0023(17) 0.0004(17) 0.0066(17) C21 0.078(3) 0.0292(18) 0.057(2) -0.002(2) -0.013(2) 0.005(2) C22 0.103(4) 0.038(2) 0.069(3) -0.013(2) -0.018(3) -0.002(2) C23 0.103(5) 0.046(2) 0.114(4) -0.011(3) -0.048(4) 0.025(3) C24 0.107(5) 0.057(3) 0.072(3) 0.014(3) 0.004(3) -0.027(3) C25 0.081(4) 0.074(3) 0.120(5) -0.002(3) 0.012(4) -0.001(3) Cl1 0.0358(5) 0.0625(6) 0.0506(5) 0.0004(5) 0.0001(4) -0.0127(4) Cl2 0.1384(17) 0.1350(16) 0.1357(15) 0.0494(13) 0.0293(14) 0.0064(15) Cl3 0.166(2) 0.180(2) 0.174(2) -0.018(2) -0.043(2) -0.0456(19) Cl4 0.0860(13) 0.1552(17) 0.1490(18) 0.0162(14) 0.0184(12) -0.0208(12) Cr1 0.0300(3) 0.0372(3) 0.0314(3) -0.0010(3) 0.0013(2) -0.0032(2) N1 0.0455(19) 0.0343(15) 0.0390(17) -0.0009(14) -0.0016(14) 0.0019(13) O1 0.0387(14) 0.0389(13) 0.0351(13) -0.0057(11) -0.0049(11) 0.0051(11) _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 C20B C18 1.503(17) . ? C20B H20A 0.9600 . ? C20B H20B 0.9600 . ? C20B H20C 0.9600 . ? C19B C18 1.47(3) . ? C19B H19A 0.9600 . ? C19B H19B 0.9600 . ? C19B H19C 0.9600 . ? C20A C18 1.520(14) . ? C20A H20D 0.9600 . ? C20A H20E 0.9600 . ? C20A H20F 0.9600 . ? C19A C18 1.57(2) . ? C19A H19D 0.9600 . ? C19A H19E 0.9600 . ? C19A H19F 0.9600 . ? C18 C16 1.520(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9801 . ? Br1 C14 1.909(3) . ? C1 C5 1.418(5) . ? C1 C2 1.426(6) . ? C1 C6 1.484(5) . ? C1 Cr1 2.223(4) . ? C2 C3 1.406(6) . ? C2 C7 1.499(6) . ? C2 Cr1 2.255(4) . ? C3 C4 1.403(6) . ? C3 C8 1.498(6) . ? C3 Cr1 2.293(3) . ? C4 C5 1.417(6) . ? C4 C9 1.510(6) . ? C4 Cr1 2.288(4) . ? C5 C10 1.494(6) . ? C5 Cr1 2.260(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.303(4) . ? C11 C12 1.420(5) . ? C11 C16 1.435(5) . ? C12 C13 1.405(5) . ? C12 C17 1.430(5) . ? C13 C14 1.371(5) . ? C13 H13 0.9300 . ? C14 C15 1.385(5) . ? C15 C16 1.375(5) . ? C15 H15 0.9300 . ? C17 N1 1.302(5) . ? C17 H17 0.9300 . ? C21 C23 1.516(7) . ? C21 C22 1.522(6) . ? C21 C24 1.523(7) . ? C21 N1 1.532(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 Cl3 1.702(7) . ? C25 Cl4 1.711(6) . ? C25 Cl2 1.747(7) . ? C25 H25 0.9800 . ? Cl1 Cr1 2.3359(12) . ? Cr1 O1 1.928(2) . ? Cr1 N1 2.097(3) . ? 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 C18 C20B H20A 109.5 . . ? C18 C20B H20B 109.5 . . ? H20A C20B H20B 109.5 . . ? C18 C20B H20C 109.5 . . ? H20A C20B H20C 109.5 . . ? H20B C20B H20C 109.5 . . ? C18 C19B H19A 109.5 . . ? C18 C19B H19B 109.5 . . ? H19A C19B H19B 109.5 . . ? C18 C19B H19C 109.5 . . ? H19A C19B H19C 109.5 . . ? H19B C19B H19C 109.5 . . ? C18 C20A H20D 109.5 . . ? C18 C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18 C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C18 C19A H19D 109.5 . . ? C18 C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18 C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C19B C18 C20B 110.8(11) . . ? C19B C18 C16 120.0(11) . . ? C20B C18 C16 109.7(7) . . ? C19B C18 C20A 83.4(12) . . ? C20B C18 C20A 33.5(8) . . ? C16 C18 C20A 110.4(6) . . ? C19B C18 C19A 24.6(15) . . ? C20B C18 C19A 134.2(10) . . ? C16 C18 C19A 108.1(8) . . ? C20A C18 C19A 108.0(10) . . ? C19B C18 H18A 105.0 . . ? C20B C18 H18A 105.0 . . ? C16 C18 H18A 105.0 . . ? C20A C18 H18A 132.7 . . ? C19A C18 H18A 89.0 . . ? C19B C18 H18B 120.1 . . ? C20B C18 H18B 78.7 . . ? C16 C18 H18B 109.7 . . ? C20A C18 H18B 109.1 . . ? C19A C18 H18B 111.4 . . ? H18A C18 H18B 26.9 . . ? C5 C1 C2 107.3(3) . . ? C5 C1 C6 125.8(4) . . ? C2 C1 C6 126.5(4) . . ? C5 C1 Cr1 73.0(2) . . ? C2 C1 Cr1 72.6(2) . . ? C6 C1 Cr1 125.9(3) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 C7 126.8(4) . . ? C1 C2 C7 125.1(4) . . ? C3 C2 Cr1 73.5(2) . . ? C1 C2 Cr1 70.2(2) . . ? C7 C2 Cr1 125.1(3) . . ? C4 C3 C2 108.7(4) . . ? C4 C3 C8 125.1(4) . . ? C2 C3 C8 126.1(4) . . ? C4 C3 Cr1 72.0(2) . . ? C2 C3 Cr1 70.5(2) . . ? C8 C3 Cr1 126.3(3) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 C9 123.7(4) . . ? C5 C4 C9 127.8(4) . . ? C3 C4 Cr1 72.4(2) . . ? C5 C4 Cr1 70.8(2) . . ? C9 C4 Cr1 128.8(3) . . ? C4 C5 C1 108.1(4) . . ? C4 C5 C10 126.5(4) . . ? C1 C5 C10 125.1(4) . . ? C4 C5 Cr1 72.9(2) . . ? C1 C5 Cr1 70.2(2) . . ? C10 C5 Cr1 127.1(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 122.0(3) . . ? O1 C11 C16 120.0(3) . . ? C12 C11 C16 118.0(3) . . ? C13 C12 C11 120.5(3) . . ? C13 C12 C17 117.1(3) . . ? C11 C12 C17 122.0(3) . . ? C14 C13 C12 119.5(3) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C13 C14 C15 121.1(3) . . ? C13 C14 Br1 119.0(3) . . ? C15 C14 Br1 119.9(3) . . ? C16 C15 C14 121.3(3) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 119.5(3) . . ? C15 C16 C18 121.5(3) . . ? C11 C16 C18 119.0(3) . . ? N1 C17 C12 127.7(3) . . ? N1 C17 H17 116.1 . . ? C12 C17 H17 116.1 . . ? C23 C21 C22 108.7(4) . . ? C23 C21 C24 111.1(4) . . ? C22 C21 C24 109.9(4) . . ? C23 C21 N1 113.1(4) . . ? C22 C21 N1 108.4(3) . . ? C24 C21 N1 105.4(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Cl3 C25 Cl4 110.8(4) . . ? Cl3 C25 Cl2 113.6(3) . . ? Cl4 C25 Cl2 109.1(4) . . ? Cl3 C25 H25 107.7 . . ? Cl4 C25 H25 107.7 . . ? Cl2 C25 H25 107.7 . . ? O1 Cr1 N1 87.78(11) . . ? O1 Cr1 C1 93.91(12) . . ? N1 Cr1 C1 108.98(15) . . ? O1 Cr1 C2 91.74(13) . . ? N1 Cr1 C2 146.00(15) . . ? C1 Cr1 C2 37.12(15) . . ? O1 Cr1 C5 127.37(13) . . ? N1 Cr1 C5 92.93(14) . . ? C1 Cr1 C5 36.87(14) . . ? C2 Cr1 C5 60.97(14) . . ? O1 Cr1 C4 151.57(13) . . ? N1 Cr1 C4 112.11(14) . . ? C1 Cr1 C4 61.14(14) . . ? C2 Cr1 C4 60.30(15) . . ? C5 Cr1 C4 36.31(14) . . ? O1 Cr1 C3 121.93(13) . . ? N1 Cr1 C3 147.79(14) . . ? C1 Cr1 C3 60.93(15) . . ? C2 Cr1 C3 35.99(15) . . ? C5 Cr1 C3 60.14(15) . . ? C4 Cr1 C3 35.67(15) . . ? O1 Cr1 Cl1 94.67(8) . . ? N1 Cr1 Cl1 100.14(9) . . ? C1 Cr1 Cl1 149.90(11) . . ? C2 Cr1 Cl1 113.77(12) . . ? C5 Cr1 Cl1 136.50(11) . . ? C4 Cr1 Cl1 101.17(11) . . ? C3 Cr1 Cl1 90.25(11) . . ? C17 N1 C21 115.1(3) . . ? C17 N1 Cr1 117.6(2) . . ? C21 N1 Cr1 127.3(2) . . ? C11 O1 Cr1 123.6(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.363 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.061 #===END data_complex_7 _database_code_depnum_ccdc_archive 'CCDC 756692' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H36 Cl3 Cr N2 O3' _chemical_formula_weight 570.91 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.839(2) _cell_length_b 11.779(2) _cell_length_c 25.013(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.29(3) _cell_angle_gamma 90.00 _cell_volume 2860.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9199 _exptl_absorpt_correction_T_max 0.9262 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 27517 _diffrn_reflns_av_R_equivalents 0.1476 _diffrn_reflns_av_sigmaI/netI 0.1242 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6519 _reflns_number_gt 3359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0695P)^2^+7.1531P] 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 6519 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1974 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_ref 0.2358 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _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 C1 C 0.0148(6) 0.1881(5) 0.1576(3) 0.0511(15) Uani 1 1 d . . . C2 C 0.0641(6) 0.1599(5) 0.1091(3) 0.0491(16) Uani 1 1 d . . . C3 C 0.1362(6) 0.0561(5) 0.1183(3) 0.0515(16) Uani 1 1 d . . . C4 C 0.1366(7) 0.0219(5) 0.1720(3) 0.0550(17) Uani 1 1 d . . . C5 C 0.0604(7) 0.1048(5) 0.1968(2) 0.0492(15) Uani 1 1 d . . . C6 C -0.0771(8) 0.2857(6) 0.1653(3) 0.077(2) Uani 1 1 d . . . H6A H -0.1715 0.2617 0.1576 0.116 Uiso 1 1 calc R . . H6B H -0.0622 0.3462 0.1412 0.116 Uiso 1 1 calc R . . H6C H -0.0567 0.3119 0.2021 0.116 Uiso 1 1 calc R . . C7 C 0.0355(8) 0.2245(7) 0.0570(3) 0.078(2) Uani 1 1 d . . . H7A H -0.0554 0.2066 0.0387 0.117 Uiso 1 1 calc R . . H7B H 0.1018 0.2040 0.0344 0.117 Uiso 1 1 calc R . . H7C H 0.0417 0.3045 0.0645 0.117 Uiso 1 1 calc R . . C8 C 0.2005(8) -0.0100(6) 0.0773(3) 0.076(2) Uani 1 1 d . . . H8A H 0.2986 -0.0123 0.0884 0.113 Uiso 1 1 calc R . . H8B H 0.1794 0.0261 0.0426 0.113 Uiso 1 1 calc R . . H8C H 0.1647 -0.0860 0.0750 0.113 Uiso 1 1 calc R . . C9 C 0.1931(9) -0.0879(6) 0.1966(4) 0.083(2) Uani 1 1 d . . . H9A H 0.1300 -0.1483 0.1847 0.124 Uiso 1 1 calc R . . H9B H 0.2050 -0.0823 0.2354 0.124 Uiso 1 1 calc R . . H9C H 0.2803 -0.1032 0.1856 0.124 Uiso 1 1 calc R . . C10 C 0.0216(8) 0.0999(7) 0.2522(3) 0.077(2) Uani 1 1 d . . . H10A H 0.0258 0.1747 0.2675 0.116 Uiso 1 1 calc R . . H10B H 0.0844 0.0509 0.2748 0.116 Uiso 1 1 calc R . . H10C H -0.0704 0.0707 0.2497 0.116 Uiso 1 1 calc R . . C11 C 0.4969(6) 0.1477(5) 0.1251(2) 0.0411(14) Uani 1 1 d . . . C12 C 0.5662(6) 0.1550(5) 0.0785(2) 0.0410(14) Uani 1 1 d . . . C13 C 0.6724(6) 0.0803(5) 0.0759(2) 0.0489(15) Uani 1 1 d . . . H13 H 0.7148 0.0800 0.0452 0.059 Uiso 1 1 calc R . . C14 C 0.7181(6) 0.0049(5) 0.1179(3) 0.0494(15) Uani 1 1 d . . . C15 C 0.6642(6) 0.0065(5) 0.1643(3) 0.0511(15) Uani 1 1 d . . . H15 H 0.7005 -0.0400 0.1932 0.061 Uiso 1 1 calc R . . C16 C 0.5547(6) 0.0779(5) 0.1687(2) 0.0455(14) Uani 1 1 d . . . C17 C 0.5110(6) 0.0851(5) 0.2213(2) 0.0488(15) Uani 1 1 d . . . H17 H 0.5680 0.0507 0.2500 0.059 Uiso 1 1 calc R . . C18 C 0.5225(7) 0.2438(5) 0.0330(2) 0.0490(15) Uani 1 1 d . . . C24 C 0.5267(11) 0.3599(6) 0.0580(3) 0.095(3) Uani 1 1 d . . . H24A H 0.5094 0.4160 0.0299 0.142 Uiso 1 1 calc R . . H24B H 0.6158 0.3727 0.0791 0.142 Uiso 1 1 calc R . . H24C H 0.4575 0.3652 0.0809 0.142 Uiso 1 1 calc R . . C25 C 0.6196(9) 0.2444(9) -0.0086(3) 0.104(3) Uani 1 1 d . . . H25A H 0.6160 0.1720 -0.0264 0.156 Uiso 1 1 calc R . . H25B H 0.7119 0.2588 0.0092 0.156 Uiso 1 1 calc R . . H25C H 0.5920 0.3027 -0.0350 0.156 Uiso 1 1 calc R . . C26 C 0.3812(8) 0.2156(7) 0.0030(3) 0.088(3) Uani 1 1 d . . . H26A H 0.3154 0.2201 0.0274 0.132 Uiso 1 1 calc R . . H26B H 0.3815 0.1401 -0.0114 0.132 Uiso 1 1 calc R . . H26C H 0.3567 0.2687 -0.0261 0.132 Uiso 1 1 calc R . . C27 C 0.3905(7) 0.1511(6) 0.2907(2) 0.0595(18) Uani 1 1 d . . . H27 H 0.2986 0.1816 0.2923 0.071 Uiso 1 1 calc R . . C28 C 0.4942(9) 0.2389(7) 0.3147(3) 0.079(2) Uani 1 1 d . . . H28A H 0.5853 0.2077 0.3180 0.118 Uiso 1 1 calc R . . H28B H 0.4760 0.2607 0.3499 0.118 Uiso 1 1 calc R . . H28C H 0.4872 0.3044 0.2915 0.118 Uiso 1 1 calc R . . C29 C 0.4059(10) 0.0413(7) 0.3232(3) 0.091(3) Uani 1 1 d . . . H29A H 0.3424 -0.0142 0.3057 0.137 Uiso 1 1 calc R . . H29B H 0.3866 0.0554 0.3591 0.137 Uiso 1 1 calc R . . H29C H 0.4983 0.0134 0.3255 0.137 Uiso 1 1 calc R . . C30 C 0.979(2) 0.3861(17) 0.9013(8) 0.294(15) Uani 1 1 d . . . H30A H 0.9664 0.4166 0.8648 0.353 Uiso 1 1 calc R . . H30B H 1.0033 0.3070 0.8977 0.353 Uiso 1 1 calc R . . Cl1 Cl 0.24979(19) 0.37391(13) 0.20028(7) 0.0608(5) Uani 1 1 d . . . Cl2 Cl 1.1252(4) 0.4454(3) 0.9310(2) 0.205(2) Uani 1 1 d . . . Cl3 Cl 0.8478(6) 0.3811(7) 0.9128(3) 0.287(3) Uani 1 1 d . . . Cr1 Cr 0.24823(10) 0.18737(8) 0.17296(4) 0.0385(3) Uani 1 1 d . . . N1 N 0.4019(5) 0.1339(4) 0.23261(18) 0.0440(12) Uani 1 1 d . . . N2 N 0.8245(6) -0.0768(5) 0.1110(3) 0.0632(16) Uani 1 1 d . . . O1 O 0.3859(4) 0.2060(3) 0.12626(15) 0.0465(10) Uani 1 1 d . . . O2 O 0.8757(5) -0.0744(4) 0.0700(2) 0.0738(14) Uani 1 1 d . . . O3 O 0.8591(6) -0.1454(5) 0.1478(2) 0.0900(18) 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 C1 0.036(3) 0.048(3) 0.069(4) -0.012(3) 0.008(3) -0.005(3) C2 0.036(4) 0.056(4) 0.056(4) -0.007(3) 0.009(3) -0.003(3) C3 0.042(4) 0.052(4) 0.064(4) -0.021(3) 0.020(3) -0.016(3) C4 0.049(4) 0.045(3) 0.072(5) -0.003(3) 0.014(3) -0.005(3) C5 0.042(4) 0.055(4) 0.052(4) -0.002(3) 0.012(3) -0.007(3) C6 0.054(5) 0.075(5) 0.102(6) -0.009(4) 0.015(4) 0.012(4) C7 0.049(5) 0.112(7) 0.069(5) 0.017(4) -0.004(4) 0.003(4) C8 0.074(5) 0.078(5) 0.081(5) -0.035(4) 0.032(4) -0.012(4) C9 0.084(6) 0.048(4) 0.118(7) 0.010(4) 0.022(5) 0.001(4) C10 0.072(6) 0.106(6) 0.060(4) -0.001(4) 0.031(4) -0.012(5) C11 0.035(3) 0.043(3) 0.044(3) -0.002(3) 0.002(3) -0.007(3) C12 0.035(3) 0.048(3) 0.040(3) -0.008(3) 0.006(3) -0.004(3) C13 0.043(4) 0.061(4) 0.043(3) -0.013(3) 0.008(3) -0.010(3) C14 0.033(3) 0.051(4) 0.063(4) -0.010(3) 0.005(3) -0.001(3) C15 0.043(4) 0.051(4) 0.058(4) 0.007(3) 0.005(3) -0.004(3) C16 0.035(3) 0.049(3) 0.054(4) 0.002(3) 0.009(3) 0.002(3) C17 0.044(4) 0.050(3) 0.052(4) 0.008(3) 0.007(3) 0.004(3) C18 0.051(4) 0.062(4) 0.036(3) 0.005(3) 0.012(3) -0.003(3) C24 0.153(9) 0.052(4) 0.080(6) 0.010(4) 0.021(6) -0.012(5) C25 0.085(7) 0.156(9) 0.084(6) 0.050(6) 0.050(5) 0.037(6) C26 0.063(5) 0.109(7) 0.083(6) 0.020(5) -0.015(4) -0.001(5) C27 0.053(4) 0.079(5) 0.047(4) 0.010(3) 0.009(3) 0.011(4) C28 0.088(6) 0.093(6) 0.049(4) -0.012(4) -0.005(4) 0.005(5) C29 0.102(7) 0.111(7) 0.065(5) 0.035(5) 0.026(5) 0.014(5) C30 0.35(3) 0.27(2) 0.32(2) -0.17(2) 0.25(2) -0.22(2) Cl1 0.0668(12) 0.0460(9) 0.0661(10) -0.0097(8) 0.0002(9) -0.0026(8) Cl2 0.131(3) 0.145(3) 0.322(6) 0.072(4) -0.013(3) -0.004(3) Cl3 0.138(4) 0.345(9) 0.372(9) 0.045(7) 0.020(5) -0.022(5) Cr1 0.0355(5) 0.0402(5) 0.0397(5) -0.0003(4) 0.0058(4) -0.0002(4) N1 0.042(3) 0.047(3) 0.042(3) 0.009(2) 0.005(2) -0.001(2) N2 0.039(3) 0.063(4) 0.087(4) -0.018(4) 0.009(3) 0.003(3) O1 0.039(2) 0.055(2) 0.047(2) 0.0090(19) 0.0099(19) 0.0067(19) O2 0.046(3) 0.092(4) 0.087(4) -0.024(3) 0.021(3) 0.006(3) O3 0.083(4) 0.085(4) 0.104(4) 0.011(3) 0.020(4) 0.039(3) _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 C1 C5 1.407(9) . ? C1 C2 1.419(8) . ? C1 C6 1.494(9) . ? C1 Cr1 2.267(6) . ? C2 C3 1.413(9) . ? C2 C7 1.495(9) . ? C2 Cr1 2.238(6) . ? C3 C4 1.402(9) . ? C3 C8 1.505(8) . ? C3 Cr1 2.234(6) . ? C4 C5 1.431(9) . ? C4 C9 1.500(9) . ? C4 Cr1 2.235(6) . ? C5 C10 1.497(8) . ? C5 Cr1 2.252(6) . ? C11 O1 1.294(7) . ? C11 C16 1.410(8) . ? C11 C12 1.447(8) . ? C12 C13 1.376(8) . ? C12 C18 1.553(8) . ? C13 C14 1.395(9) . ? C14 C15 1.352(8) . ? C14 N2 1.453(8) . ? C15 C16 1.385(8) . ? C16 C17 1.449(8) . ? C17 N1 1.289(7) . ? C18 C24 1.500(9) . ? C18 C26 1.507(10) . ? C18 C25 1.523(9) . ? C27 N1 1.490(7) . ? C27 C28 1.507(10) . ? C27 C29 1.523(10) . ? C30 Cl3 1.367(18) . ? C30 Cl2 1.66(2) . ? Cl1 Cr1 2.3005(18) . ? Cr1 O1 1.939(4) . ? Cr1 N1 2.045(5) . ? N2 O2 1.214(7) . ? N2 O3 1.230(7) . ? 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 C5 C1 C2 108.5(5) . . ? C5 C1 C6 125.3(6) . . ? C2 C1 C6 126.1(6) . . ? C5 C1 Cr1 71.3(4) . . ? C2 C1 Cr1 70.5(3) . . ? C6 C1 Cr1 126.8(5) . . ? C3 C2 C1 107.2(6) . . ? C3 C2 C7 126.9(6) . . ? C1 C2 C7 125.7(6) . . ? C3 C2 Cr1 71.4(4) . . ? C1 C2 Cr1 72.8(3) . . ? C7 C2 Cr1 124.4(4) . . ? C4 C3 C2 109.1(5) . . ? C4 C3 C8 124.5(7) . . ? C2 C3 C8 126.3(6) . . ? C4 C3 Cr1 71.8(4) . . ? C2 C3 Cr1 71.7(3) . . ? C8 C3 Cr1 123.7(4) . . ? C3 C4 C5 107.4(6) . . ? C3 C4 C9 125.8(6) . . ? C5 C4 C9 126.5(6) . . ? C3 C4 Cr1 71.7(3) . . ? C5 C4 Cr1 72.0(3) . . ? C9 C4 Cr1 126.7(5) . . ? C1 C5 C4 107.8(5) . . ? C1 C5 C10 124.8(6) . . ? C4 C5 C10 127.2(6) . . ? C1 C5 Cr1 72.4(3) . . ? C4 C5 Cr1 70.8(3) . . ? C10 C5 Cr1 127.2(5) . . ? O1 C11 C16 121.9(5) . . ? O1 C11 C12 119.7(5) . . ? C16 C11 C12 118.4(5) . . ? C13 C12 C11 117.4(5) . . ? C13 C12 C18 121.3(5) . . ? C11 C12 C18 121.3(5) . . ? C12 C13 C14 121.8(6) . . ? C15 C14 C13 121.0(6) . . ? C15 C14 N2 120.1(6) . . ? C13 C14 N2 118.9(6) . . ? C14 C15 C16 119.7(6) . . ? C15 C16 C11 120.9(6) . . ? C15 C16 C17 117.1(6) . . ? C11 C16 C17 121.7(5) . . ? N1 C17 C16 127.2(6) . . ? C24 C18 C26 111.7(7) . . ? C24 C18 C25 107.6(7) . . ? C26 C18 C25 106.8(6) . . ? C24 C18 C12 108.9(5) . . ? C26 C18 C12 109.9(5) . . ? C25 C18 C12 111.9(6) . . ? N1 C27 C28 109.2(5) . . ? N1 C27 C29 112.9(6) . . ? C28 C27 C29 111.6(6) . . ? Cl3 C30 Cl2 134.5(12) . . ? O1 Cr1 N1 88.17(18) . . ? O1 Cr1 C3 91.88(19) . . ? N1 Cr1 C3 117.9(2) . . ? O1 Cr1 C4 118.8(2) . . ? N1 Cr1 C4 92.5(2) . . ? C3 Cr1 C4 36.6(2) . . ? O1 Cr1 C2 98.6(2) . . ? N1 Cr1 C2 153.5(2) . . ? C3 Cr1 C2 36.9(2) . . ? C4 Cr1 C2 61.7(2) . . ? O1 Cr1 C5 153.0(2) . . ? N1 Cr1 C5 102.5(2) . . ? C3 Cr1 C5 61.2(2) . . ? C4 Cr1 C5 37.2(2) . . ? C2 Cr1 C5 61.4(2) . . ? O1 Cr1 C1 133.2(2) . . ? N1 Cr1 C1 137.3(2) . . ? C3 Cr1 C1 60.8(2) . . ? C4 Cr1 C1 61.2(2) . . ? C2 Cr1 C1 36.7(2) . . ? C5 Cr1 C1 36.3(2) . . ? O1 Cr1 Cl1 95.69(13) . . ? N1 Cr1 Cl1 96.24(14) . . ? C3 Cr1 Cl1 145.28(19) . . ? C4 Cr1 Cl1 144.66(18) . . ? C2 Cr1 Cl1 108.43(17) . . ? C5 Cr1 Cl1 107.49(17) . . ? C1 Cr1 Cl1 90.26(16) . . ? C17 N1 C27 118.2(5) . . ? C17 N1 Cr1 121.4(4) . . ? C27 N1 Cr1 120.5(4) . . ? O2 N2 O3 123.0(6) . . ? O2 N2 C14 119.3(7) . . ? O3 N2 C14 117.7(6) . . ? C11 O1 Cr1 128.8(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.736 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.077 #===END data_complex_8 _database_code_depnum_ccdc_archive 'CCDC 756693' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 Cl3 Cr N2 O3' _chemical_formula_weight 604.92 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.0986(18) _cell_length_b 12.398(3) _cell_length_c 26.249(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.29(3) _cell_angle_gamma 90.00 _cell_volume 2952.6(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9218 _exptl_absorpt_correction_T_max 0.9280 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean '100x100 microns' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 27679 _diffrn_reflns_av_R_equivalents 0.1961 _diffrn_reflns_av_sigmaI/netI 0.1660 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6634 _reflns_number_gt 2929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.1119P)^2^+0.6444P] 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 6634 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2201 _refine_ls_R_factor_gt 0.1000 _refine_ls_wR_factor_ref 0.2617 _refine_ls_wR_factor_gt 0.2035 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 C1 C 0.3522(8) 0.9788(6) 0.8634(3) 0.0547(18) Uani 1 1 d . . . C2 C 0.3995(8) 0.9949(5) 0.8145(2) 0.0504(17) Uani 1 1 d . . . C3 C 0.4869(7) 0.9060(5) 0.8026(2) 0.0465(16) Uani 1 1 d . . . C4 C 0.4932(7) 0.8363(5) 0.8454(2) 0.0477(16) Uani 1 1 d . . . C5 C 0.4101(7) 0.8824(6) 0.8823(2) 0.0503(17) Uani 1 1 d . . . C6 C 0.2623(8) 1.0576(7) 0.8923(3) 0.079(3) Uani 1 1 d . . . H6A H 0.2196 1.0208 0.9198 0.119 Uiso 1 1 calc R . . H6B H 0.1854 1.0874 0.8695 0.119 Uiso 1 1 calc R . . H6C H 0.3250 1.1146 0.9059 0.119 Uiso 1 1 calc R . . C7 C 0.3750(10) 1.0950(6) 0.7822(3) 0.083(3) Uani 1 1 d . . . H7A H 0.4319 1.1534 0.7975 0.125 Uiso 1 1 calc R . . H7B H 0.2723 1.1137 0.7802 0.125 Uiso 1 1 calc R . . H7C H 0.4051 1.0816 0.7485 0.125 Uiso 1 1 calc R . . C8 C 0.5764(8) 0.8903(7) 0.7566(3) 0.070(2) Uani 1 1 d . . . H8A H 0.5598 0.9500 0.7336 0.104 Uiso 1 1 calc R . . H8B H 0.5468 0.8246 0.7394 0.104 Uiso 1 1 calc R . . H8C H 0.6792 0.8865 0.7677 0.104 Uiso 1 1 calc R . . C9 C 0.5849(9) 0.7360(6) 0.8509(3) 0.078(2) Uani 1 1 d . . . H9A H 0.6092 0.7217 0.8865 0.117 Uiso 1 1 calc R . . H9B H 0.6738 0.7458 0.8340 0.117 Uiso 1 1 calc R . . H9C H 0.5304 0.6763 0.8358 0.117 Uiso 1 1 calc R . . C10 C 0.3925(9) 0.8346(7) 0.9337(2) 0.079(3) Uani 1 1 d . . . H10A H 0.4764 0.8530 0.9564 0.118 Uiso 1 1 calc R . . H10B H 0.3853 0.7576 0.9308 0.118 Uiso 1 1 calc R . . H10C H 0.3047 0.8625 0.9470 0.118 Uiso 1 1 calc R . . C11 C -0.0022(7) 0.8779(5) 0.8682(2) 0.0392(15) Uani 1 1 d . . . C12 C -0.0621(7) 0.9562(5) 0.8327(2) 0.0430(15) Uani 1 1 d . . . C13 C -0.1744(7) 1.0255(5) 0.8455(2) 0.0474(16) Uani 1 1 d . . . H13 H -0.2129 1.0765 0.8222 0.057 Uiso 1 1 calc R . . C14 C -0.2273(7) 1.0172(5) 0.8931(2) 0.0462(16) Uani 1 1 d . . . C15 C -0.1760(7) 0.9402(5) 0.9276(2) 0.0471(16) Uani 1 1 d . . . H15 H -0.2168 0.9355 0.9590 0.057 Uiso 1 1 calc R . . C16 C -0.0657(7) 0.8700(5) 0.9169(2) 0.0406(15) Uani 1 1 d . . . C17 C -0.0176(7) 0.9604(5) 0.7805(2) 0.0439(15) Uani 1 1 d . . . H17 H -0.0760 1.0022 0.7576 0.053 Uiso 1 1 calc R . . C18 C 0.0876(8) 0.9083(7) 0.7039(2) 0.063(2) Uani 1 1 d . . . C19 C 0.2408(8) 0.8835(7) 0.6876(2) 0.068(2) Uani 1 1 d . . . H19A H 0.3069 0.9407 0.6985 0.102 Uiso 1 1 calc R . . H19B H 0.2371 0.8772 0.6511 0.102 Uiso 1 1 calc R . . H19C H 0.2752 0.8169 0.7028 0.102 Uiso 1 1 calc R . . C20 C 0.0330(12) 1.0134(9) 0.6792(3) 0.120(4) Uani 1 1 d . . . H20A H -0.0715 1.0195 0.6815 0.180 Uiso 1 1 calc R . . H20B H 0.0543 1.0138 0.6439 0.180 Uiso 1 1 calc R . . H20C H 0.0817 1.0731 0.6965 0.180 Uiso 1 1 calc R . . C21 C -0.0193(10) 0.8168(9) 0.6885(3) 0.102(4) Uani 1 1 d . . . H21A H 0.0099 0.7527 0.7072 0.153 Uiso 1 1 calc R . . H21B H -0.0178 0.8033 0.6526 0.153 Uiso 1 1 calc R . . H21C H -0.1171 0.8369 0.6962 0.153 Uiso 1 1 calc R . . C22 C -0.0054(7) 0.7894(6) 0.9555(2) 0.0473(16) Uani 1 1 d . . . C23 C 0.0341(8) 0.6874(6) 0.9415(3) 0.0574(19) Uani 1 1 d . . . H23 H 0.0229 0.6663 0.9074 0.069 Uiso 1 1 calc R . . C24 C 0.0910(9) 0.6160(7) 0.9785(3) 0.073(2) Uani 1 1 d . . . H24 H 0.1163 0.5465 0.9691 0.087 Uiso 1 1 calc R . . C25 C 0.1104(9) 0.6462(8) 1.0286(3) 0.075(2) Uani 1 1 d . . . H25 H 0.1512 0.5985 1.0531 0.090 Uiso 1 1 calc R . . C26 C 0.0689(10) 0.7473(7) 1.0423(3) 0.075(3) Uani 1 1 d . . . H26 H 0.0781 0.7678 1.0764 0.091 Uiso 1 1 calc R . . C27 C 0.0136(8) 0.8194(6) 1.0056(2) 0.0584(19) Uani 1 1 d . . . H27 H -0.0110 0.8890 1.0151 0.070 Uiso 1 1 calc R . . C28 C 0.5344(13) 0.6398(10) 0.0499(6) 0.149(5) Uani 1 1 d . . . H28A H 0.4579 0.6129 0.0255 0.178 Uiso 1 1 calc R . . H28B H 0.4994 0.7065 0.0641 0.178 Uiso 1 1 calc R . . Cl1 Cl 0.26886(19) 0.67643(13) 0.78049(6) 0.0550(5) Uani 1 1 d . . . Cl2 Cl 0.5651(8) 0.5468(5) 0.0983(2) 0.277(3) Uani 1 1 d . . . Cl3 Cl 0.6835(4) 0.6646(4) 0.0204(2) 0.200(2) Uani 1 1 d . . . Cr1 Cr 0.25649(11) 0.84821(8) 0.81327(3) 0.0384(3) Uani 1 1 d . . . N1 N 0.0916(5) 0.9137(4) 0.76259(17) 0.0413(12) Uani 1 1 d . . . N2 N -0.3403(6) 1.0931(6) 0.9060(2) 0.0604(16) Uani 1 1 d . . . O2 O -0.3772(6) 1.1657(5) 0.8766(2) 0.0727(15) Uani 1 1 d . . . O3 O -0.3938(5) 1.0797(5) 0.94740(19) 0.0772(17) Uani 1 1 d . . . O1 O 0.1023(4) 0.8148(3) 0.85690(14) 0.0438(11) 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 C1 0.061(4) 0.049(5) 0.056(4) -0.014(4) 0.013(4) -0.006(3) C2 0.061(4) 0.038(4) 0.052(4) 0.000(3) 0.005(3) -0.010(3) C3 0.047(4) 0.045(4) 0.047(4) -0.009(3) 0.006(3) -0.011(3) C4 0.053(4) 0.039(4) 0.049(4) -0.009(3) -0.004(3) -0.008(3) C5 0.053(4) 0.053(5) 0.045(4) -0.005(3) 0.006(3) -0.012(3) C6 0.066(5) 0.075(6) 0.099(6) -0.048(5) 0.008(5) -0.009(4) C7 0.095(7) 0.052(5) 0.102(7) 0.014(5) -0.003(5) -0.005(5) C8 0.059(5) 0.095(6) 0.058(4) -0.009(4) 0.028(4) -0.013(4) C9 0.072(5) 0.061(5) 0.098(6) -0.007(5) -0.011(5) 0.012(4) C10 0.077(5) 0.115(8) 0.044(4) 0.009(4) 0.000(4) -0.021(5) C11 0.044(4) 0.040(4) 0.034(3) 0.000(3) 0.006(3) -0.013(3) C12 0.047(4) 0.044(4) 0.039(3) -0.005(3) 0.010(3) -0.005(3) C13 0.050(4) 0.051(4) 0.041(3) -0.003(3) 0.001(3) -0.004(3) C14 0.043(4) 0.053(4) 0.045(4) -0.015(3) 0.015(3) -0.005(3) C15 0.049(4) 0.057(4) 0.036(3) -0.011(3) 0.012(3) -0.007(3) C16 0.055(4) 0.039(4) 0.030(3) -0.001(3) 0.012(3) -0.014(3) C17 0.056(4) 0.040(4) 0.037(3) 0.009(3) 0.012(3) 0.009(3) C18 0.061(5) 0.099(6) 0.030(3) 0.005(4) 0.011(3) 0.026(4) C19 0.067(5) 0.099(6) 0.042(4) 0.007(4) 0.025(4) 0.018(5) C20 0.150(9) 0.159(10) 0.057(5) 0.060(6) 0.046(6) 0.093(8) C21 0.077(6) 0.181(11) 0.049(5) -0.036(6) 0.006(4) -0.021(7) C22 0.053(4) 0.053(4) 0.036(3) 0.001(3) 0.009(3) -0.020(3) C23 0.078(5) 0.047(5) 0.048(4) 0.003(3) 0.011(4) -0.017(4) C24 0.090(6) 0.053(5) 0.078(6) 0.012(4) 0.026(5) -0.013(4) C25 0.082(6) 0.088(7) 0.055(5) 0.022(5) 0.001(4) -0.022(5) C26 0.105(7) 0.081(7) 0.040(4) 0.008(4) 0.005(4) -0.035(5) C27 0.076(5) 0.060(5) 0.039(4) -0.004(3) 0.003(4) -0.020(4) C28 0.122(10) 0.098(9) 0.235(16) 0.000(10) 0.076(10) 0.014(7) Cl1 0.0616(11) 0.0443(11) 0.0602(10) -0.0140(8) 0.0116(9) -0.0063(8) Cl2 0.356(8) 0.238(6) 0.263(6) 0.075(5) 0.184(6) 0.059(6) Cl3 0.139(3) 0.169(4) 0.302(6) 0.085(4) 0.086(4) 0.046(3) Cr1 0.0451(6) 0.0374(6) 0.0338(5) -0.0010(5) 0.0105(4) -0.0005(5) N1 0.048(3) 0.045(3) 0.032(3) 0.000(2) 0.013(2) 0.005(3) N2 0.054(4) 0.070(5) 0.058(4) -0.026(3) 0.014(3) -0.004(3) O2 0.074(4) 0.069(4) 0.078(4) -0.007(3) 0.019(3) 0.017(3) O3 0.066(3) 0.114(5) 0.056(3) -0.022(3) 0.026(3) 0.010(3) O1 0.049(3) 0.049(3) 0.035(2) 0.0054(19) 0.016(2) 0.005(2) _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 C1 C5 1.383(10) . ? C1 C2 1.400(9) . ? C1 C6 1.513(9) . ? C1 Cr1 2.223(7) . ? C2 C3 1.407(9) . ? C2 C7 1.510(9) . ? C2 Cr1 2.235(6) . ? C3 C4 1.414(9) . ? C3 C8 1.519(9) . ? C3 Cr1 2.252(6) . ? C4 C5 1.395(9) . ? C4 C9 1.498(9) . ? C4 Cr1 2.258(6) . ? C5 C10 1.493(9) . ? C5 Cr1 2.244(6) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 O1 1.283(7) . ? C11 C12 1.425(8) . ? C11 C16 1.446(8) . ? C12 C13 1.395(9) . ? C12 C17 1.459(8) . ? C13 C14 1.376(8) . ? C13 H13 0.9300 . ? C14 C15 1.374(9) . ? C14 N2 1.451(9) . ? C15 C16 1.373(9) . ? C15 H15 0.9300 . ? C16 C22 1.496(9) . ? C17 N1 1.270(7) . ? C17 H17 0.9300 . ? C18 C19 1.521(9) . ? C18 C20 1.522(11) . ? C18 C21 1.528(12) . ? C18 N1 1.540(7) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.365(8) . ? C22 C23 1.373(9) . ? C23 C24 1.386(10) . ? C23 H23 0.9300 . ? C24 C25 1.366(10) . ? C24 H24 0.9300 . ? C25 C26 1.365(11) . ? C25 H25 0.9300 . ? C26 C27 1.380(10) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 Cl3 1.642(11) . ? C28 Cl2 1.722(13) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? Cl1 Cr1 2.303(2) . ? Cr1 O1 1.922(4) . ? Cr1 N1 2.093(5) . ? N2 O2 1.216(7) . ? N2 O3 1.235(7) . ? 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 C5 C1 C2 108.5(6) . . ? C5 C1 C6 125.8(7) . . ? C2 C1 C6 125.6(7) . . ? C5 C1 Cr1 72.8(4) . . ? C2 C1 Cr1 72.2(4) . . ? C6 C1 Cr1 124.4(5) . . ? C1 C2 C3 108.0(6) . . ? C1 C2 C7 126.1(7) . . ? C3 C2 C7 125.6(7) . . ? C1 C2 Cr1 71.2(4) . . ? C3 C2 Cr1 72.4(4) . . ? C7 C2 Cr1 126.8(5) . . ? C2 C3 C4 107.0(6) . . ? C2 C3 C8 128.4(6) . . ? C4 C3 C8 124.1(6) . . ? C2 C3 Cr1 71.0(4) . . ? C4 C3 Cr1 72.0(4) . . ? C8 C3 Cr1 128.1(4) . . ? C5 C4 C3 108.0(6) . . ? C5 C4 C9 126.8(7) . . ? C3 C4 C9 124.9(7) . . ? C5 C4 Cr1 71.4(4) . . ? C3 C4 Cr1 71.5(4) . . ? C9 C4 Cr1 126.8(5) . . ? C1 C5 C4 108.5(6) . . ? C1 C5 C10 127.1(7) . . ? C4 C5 C10 124.4(7) . . ? C1 C5 Cr1 71.1(4) . . ? C4 C5 Cr1 72.5(4) . . ? C10 C5 Cr1 123.5(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 121.2(5) . . ? O1 C11 C16 121.0(5) . . ? C12 C11 C16 117.7(6) . . ? C13 C12 C11 120.8(5) . . ? C13 C12 C17 117.7(6) . . ? C11 C12 C17 121.2(6) . . ? C14 C13 C12 119.1(6) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 121.7(6) . . ? C15 C14 N2 120.6(6) . . ? C13 C14 N2 117.7(6) . . ? C16 C15 C14 121.6(6) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C11 119.0(6) . . ? C15 C16 C22 121.4(5) . . ? C11 C16 C22 119.5(6) . . ? N1 C17 C12 127.7(6) . . ? N1 C17 H17 116.2 . . ? C12 C17 H17 116.2 . . ? C19 C18 C20 109.2(7) . . ? C19 C18 C21 110.7(7) . . ? C20 C18 C21 110.0(8) . . ? C19 C18 N1 109.7(5) . . ? C20 C18 N1 111.9(6) . . ? C21 C18 N1 105.3(6) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 119.4(7) . . ? C27 C22 C16 118.9(6) . . ? C23 C22 C16 121.6(6) . . ? C22 C23 C24 119.5(7) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 121.0(8) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C24 119.0(8) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 120.4(7) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C22 C27 C26 120.6(7) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? Cl3 C28 Cl2 112.3(7) . . ? Cl3 C28 H28A 109.1 . . ? Cl2 C28 H28A 109.1 . . ? Cl3 C28 H28B 109.1 . . ? Cl2 C28 H28B 109.1 . . ? H28A C28 H28B 107.9 . . ? O1 Cr1 N1 86.67(18) . . ? O1 Cr1 C1 94.3(2) . . ? N1 Cr1 C1 108.9(2) . . ? O1 Cr1 C2 128.1(2) . . ? N1 Cr1 C2 94.7(2) . . ? C1 Cr1 C2 36.6(2) . . ? O1 Cr1 C5 89.9(2) . . ? N1 Cr1 C5 144.4(2) . . ? C1 Cr1 C5 36.1(2) . . ? C2 Cr1 C5 60.5(2) . . ? O1 Cr1 C3 150.5(2) . . ? N1 Cr1 C3 115.3(2) . . ? C1 Cr1 C3 61.0(2) . . ? C2 Cr1 C3 36.6(2) . . ? C5 Cr1 C3 60.7(2) . . ? O1 Cr1 C4 118.8(2) . . ? N1 Cr1 C4 151.8(2) . . ? C1 Cr1 C4 60.4(2) . . ? C2 Cr1 C4 60.6(2) . . ? C5 Cr1 C4 36.1(2) . . ? C3 Cr1 C4 36.5(2) . . ? O1 Cr1 Cl1 94.66(14) . . ? N1 Cr1 Cl1 100.01(15) . . ? C1 Cr1 Cl1 150.1(2) . . ? C2 Cr1 Cl1 135.48(19) . . ? C5 Cr1 Cl1 115.6(2) . . ? C3 Cr1 Cl1 100.12(18) . . ? C4 Cr1 Cl1 90.42(17) . . ? C17 N1 C18 115.4(5) . . ? C17 N1 Cr1 119.0(4) . . ? C18 N1 Cr1 125.6(4) . . ? O2 N2 O3 123.3(6) . . ? O2 N2 C14 119.9(6) . . ? O3 N2 C14 116.8(7) . . ? C11 O1 Cr1 126.4(4) . . ? 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 C5 C1 C2 C3 0.7(8) . . . . ? C6 C1 C2 C3 176.6(6) . . . . ? Cr1 C1 C2 C3 -63.5(5) . . . . ? C5 C1 C2 C7 -173.4(7) . . . . ? C6 C1 C2 C7 2.5(11) . . . . ? Cr1 C1 C2 C7 122.4(7) . . . . ? C5 C1 C2 Cr1 64.2(5) . . . . ? C6 C1 C2 Cr1 -119.9(7) . . . . ? C1 C2 C3 C4 -0.7(7) . . . . ? C7 C2 C3 C4 173.5(6) . . . . ? Cr1 C2 C3 C4 -63.4(4) . . . . ? C1 C2 C3 C8 -173.2(6) . . . . ? C7 C2 C3 C8 1.0(11) . . . . ? Cr1 C2 C3 C8 124.1(7) . . . . ? C1 C2 C3 Cr1 62.7(5) . . . . ? C7 C2 C3 Cr1 -123.1(7) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C8 C3 C4 C5 173.2(6) . . . . ? Cr1 C3 C4 C5 -62.4(4) . . . . ? C2 C3 C4 C9 -174.7(6) . . . . ? C8 C3 C4 C9 -1.8(10) . . . . ? Cr1 C3 C4 C9 122.5(6) . . . . ? C2 C3 C4 Cr1 62.8(4) . . . . ? C8 C3 C4 Cr1 -124.3(6) . . . . ? C2 C1 C5 C4 -0.5(8) . . . . ? C6 C1 C5 C4 -176.3(6) . . . . ? Cr1 C1 C5 C4 63.3(5) . . . . ? C2 C1 C5 C10 177.9(7) . . . . ? C6 C1 C5 C10 2.1(11) . . . . ? Cr1 C1 C5 C10 -118.3(7) . . . . ? C2 C1 C5 Cr1 -63.8(5) . . . . ? C6 C1 C5 Cr1 120.4(7) . . . . ? C3 C4 C5 C1 0.1(7) . . . . ? C9 C4 C5 C1 175.1(7) . . . . ? Cr1 C4 C5 C1 -62.4(5) . . . . ? C3 C4 C5 C10 -178.4(6) . . . . ? C9 C4 C5 C10 -3.4(11) . . . . ? Cr1 C4 C5 C10 119.1(7) . . . . ? C3 C4 C5 Cr1 62.5(4) . . . . ? C9 C4 C5 Cr1 -122.5(7) . . . . ? O1 C11 C12 C13 -179.1(6) . . . . ? C16 C11 C12 C13 2.4(9) . . . . ? O1 C11 C12 C17 6.3(9) . . . . ? C16 C11 C12 C17 -172.2(6) . . . . ? C11 C12 C13 C14 -0.2(9) . . . . ? C17 C12 C13 C14 174.6(6) . . . . ? C12 C13 C14 C15 -2.2(10) . . . . ? C12 C13 C14 N2 177.8(6) . . . . ? C13 C14 C15 C16 2.2(10) . . . . ? N2 C14 C15 C16 -177.8(6) . . . . ? C14 C15 C16 C11 0.2(9) . . . . ? C14 C15 C16 C22 177.3(6) . . . . ? O1 C11 C16 C15 179.1(5) . . . . ? C12 C11 C16 C15 -2.5(8) . . . . ? O1 C11 C16 C22 2.0(9) . . . . ? C12 C11 C16 C22 -179.6(5) . . . . ? C13 C12 C17 N1 171.5(6) . . . . ? C11 C12 C17 N1 -13.7(10) . . . . ? C15 C16 C22 C27 -39.1(9) . . . . ? C11 C16 C22 C27 138.0(6) . . . . ? C15 C16 C22 C23 142.4(7) . . . . ? C11 C16 C22 C23 -40.5(9) . . . . ? C27 C22 C23 C24 0.8(10) . . . . ? C16 C22 C23 C24 179.3(6) . . . . ? C22 C23 C24 C25 -1.0(11) . . . . ? C23 C24 C25 C26 1.9(12) . . . . ? C24 C25 C26 C27 -2.5(13) . . . . ? C23 C22 C27 C26 -1.4(11) . . . . ? C16 C22 C27 C26 -180.0(7) . . . . ? C25 C26 C27 C22 2.3(12) . . . . ? C5 C1 Cr1 O1 83.8(4) . . . . ? C2 C1 Cr1 O1 -159.6(4) . . . . ? C6 C1 Cr1 O1 -38.1(7) . . . . ? C5 C1 Cr1 N1 171.8(4) . . . . ? C2 C1 Cr1 N1 -71.6(4) . . . . ? C6 C1 Cr1 N1 49.8(7) . . . . ? C5 C1 Cr1 C2 -116.6(6) . . . . ? C6 C1 Cr1 C2 121.4(9) . . . . ? C2 C1 Cr1 C5 116.6(6) . . . . ? C6 C1 Cr1 C5 -122.0(8) . . . . ? C5 C1 Cr1 C3 -79.2(4) . . . . ? C2 C1 Cr1 C3 37.5(4) . . . . ? C6 C1 Cr1 C3 158.9(7) . . . . ? C5 C1 Cr1 C4 -37.0(4) . . . . ? C2 C1 Cr1 C4 79.6(4) . . . . ? C6 C1 Cr1 C4 -159.0(8) . . . . ? C5 C1 Cr1 Cl1 -23.3(6) . . . . ? C2 C1 Cr1 Cl1 93.3(5) . . . . ? C6 C1 Cr1 Cl1 -145.3(5) . . . . ? C1 C2 Cr1 O1 26.3(5) . . . . ? C3 C2 Cr1 O1 143.0(4) . . . . ? C7 C2 Cr1 O1 -95.2(7) . . . . ? C1 C2 Cr1 N1 115.8(4) . . . . ? C3 C2 Cr1 N1 -127.5(4) . . . . ? C7 C2 Cr1 N1 -5.7(7) . . . . ? C3 C2 Cr1 C1 116.8(6) . . . . ? C7 C2 Cr1 C1 -121.5(9) . . . . ? C1 C2 Cr1 C5 -37.2(4) . . . . ? C3 C2 Cr1 C5 79.6(4) . . . . ? C7 C2 Cr1 C5 -158.7(8) . . . . ? C1 C2 Cr1 C3 -116.8(6) . . . . ? C7 C2 Cr1 C3 121.7(8) . . . . ? C1 C2 Cr1 C4 -78.9(4) . . . . ? C3 C2 Cr1 C4 37.9(4) . . . . ? C7 C2 Cr1 C4 159.6(7) . . . . ? C1 C2 Cr1 Cl1 -134.8(4) . . . . ? C3 C2 Cr1 Cl1 -18.0(5) . . . . ? C7 C2 Cr1 Cl1 103.7(7) . . . . ? C1 C5 Cr1 O1 -97.5(4) . . . . ? C4 C5 Cr1 O1 145.2(4) . . . . ? C10 C5 Cr1 O1 25.0(7) . . . . ? C1 C5 Cr1 N1 -13.4(6) . . . . ? C4 C5 Cr1 N1 -130.7(4) . . . . ? C10 C5 Cr1 N1 109.1(7) . . . . ? C4 C5 Cr1 C1 -117.3(6) . . . . ? C10 C5 Cr1 C1 122.6(8) . . . . ? C1 C5 Cr1 C2 37.7(4) . . . . ? C4 C5 Cr1 C2 -79.6(4) . . . . ? C10 C5 Cr1 C2 160.3(7) . . . . ? C1 C5 Cr1 C3 79.9(4) . . . . ? C4 C5 Cr1 C3 -37.4(4) . . . . ? C10 C5 Cr1 C3 -157.5(7) . . . . ? C1 C5 Cr1 C4 117.3(6) . . . . ? C10 C5 Cr1 C4 -120.1(8) . . . . ? C1 C5 Cr1 Cl1 167.4(3) . . . . ? C4 C5 Cr1 Cl1 50.1(4) . . . . ? C10 C5 Cr1 Cl1 -70.1(7) . . . . ? C2 C3 Cr1 O1 -73.8(6) . . . . ? C4 C3 Cr1 O1 42.1(6) . . . . ? C8 C3 Cr1 O1 161.8(5) . . . . ? C2 C3 Cr1 N1 61.0(4) . . . . ? C4 C3 Cr1 N1 177.0(3) . . . . ? C8 C3 Cr1 N1 -63.4(7) . . . . ? C2 C3 Cr1 C1 -37.5(4) . . . . ? C4 C3 Cr1 C1 78.4(4) . . . . ? C8 C3 Cr1 C1 -161.9(7) . . . . ? C4 C3 Cr1 C2 115.9(5) . . . . ? C8 C3 Cr1 C2 -124.4(8) . . . . ? C2 C3 Cr1 C5 -79.0(4) . . . . ? C4 C3 Cr1 C5 36.9(4) . . . . ? C8 C3 Cr1 C5 156.6(7) . . . . ? C2 C3 Cr1 C4 -115.9(5) . . . . ? C8 C3 Cr1 C4 119.6(8) . . . . ? C2 C3 Cr1 Cl1 167.3(3) . . . . ? C4 C3 Cr1 Cl1 -76.8(4) . . . . ? C8 C3 Cr1 Cl1 42.9(6) . . . . ? C5 C4 Cr1 O1 -40.7(5) . . . . ? C3 C4 Cr1 O1 -157.9(3) . . . . ? C9 C4 Cr1 O1 81.9(7) . . . . ? C5 C4 Cr1 N1 111.4(5) . . . . ? C3 C4 Cr1 N1 -5.8(6) . . . . ? C9 C4 Cr1 N1 -126.1(6) . . . . ? C5 C4 Cr1 C1 37.0(4) . . . . ? C3 C4 Cr1 C1 -80.2(4) . . . . ? C9 C4 Cr1 C1 159.5(7) . . . . ? C5 C4 Cr1 C2 79.3(4) . . . . ? C3 C4 Cr1 C2 -37.9(4) . . . . ? C9 C4 Cr1 C2 -158.2(7) . . . . ? C3 C4 Cr1 C5 -117.2(6) . . . . ? C9 C4 Cr1 C5 122.5(8) . . . . ? C5 C4 Cr1 C3 117.2(6) . . . . ? C9 C4 Cr1 C3 -120.3(8) . . . . ? C5 C4 Cr1 Cl1 -136.2(4) . . . . ? C3 C4 Cr1 Cl1 106.6(4) . . . . ? C9 C4 Cr1 Cl1 -13.7(6) . . . . ? C12 C17 N1 C18 164.4(7) . . . . ? C12 C17 N1 Cr1 -14.1(9) . . . . ? C19 C18 N1 C17 162.5(7) . . . . ? C20 C18 N1 C17 41.1(9) . . . . ? C21 C18 N1 C17 -78.3(8) . . . . ? C19 C18 N1 Cr1 -19.0(9) . . . . ? C20 C18 N1 Cr1 -140.4(6) . . . . ? C21 C18 N1 Cr1 100.2(6) . . . . ? O1 Cr1 N1 C17 34.4(5) . . . . ? C1 Cr1 N1 C17 -59.0(5) . . . . ? C2 Cr1 N1 C17 -93.6(5) . . . . ? C5 Cr1 N1 C17 -50.7(7) . . . . ? C3 Cr1 N1 C17 -125.1(5) . . . . ? C4 Cr1 N1 C17 -121.3(6) . . . . ? Cl1 Cr1 N1 C17 128.6(5) . . . . ? O1 Cr1 N1 C18 -144.0(5) . . . . ? C1 Cr1 N1 C18 122.6(5) . . . . ? C2 Cr1 N1 C18 88.0(6) . . . . ? C5 Cr1 N1 C18 130.9(6) . . . . ? C3 Cr1 N1 C18 56.5(6) . . . . ? C4 Cr1 N1 C18 60.3(7) . . . . ? Cl1 Cr1 N1 C18 -49.8(5) . . . . ? C15 C14 N2 O2 174.7(6) . . . . ? C13 C14 N2 O2 -5.3(9) . . . . ? C15 C14 N2 O3 -5.0(9) . . . . ? C13 C14 N2 O3 175.0(6) . . . . ? C12 C11 O1 Cr1 32.2(8) . . . . ? C16 C11 O1 Cr1 -149.4(4) . . . . ? N1 Cr1 O1 C11 -45.5(5) . . . . ? C1 Cr1 O1 C11 63.3(5) . . . . ? C2 Cr1 O1 C11 47.9(5) . . . . ? C5 Cr1 O1 C11 99.1(5) . . . . ? C3 Cr1 O1 C11 94.6(6) . . . . ? C4 Cr1 O1 C11 121.7(5) . . . . ? Cl1 Cr1 O1 C11 -145.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.474 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.084 #===END #=============================================================== #3. CIF files data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 776252' #TrackingRef '- NJC-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H21 Cl Cr N O' _chemical_formula_weight 390.84 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' 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 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 12.378(3) _cell_length_b 16.829(3) _cell_length_c 17.805(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3709.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.769 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27958 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4231 _reflns_number_gt 3498 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.0426P)^2^+1.3188P] 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 4231 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.19554(2) 0.082060(15) 0.483926(14) 0.02557(9) Uani 1 1 d . . . Cl1 Cl 0.07304(4) 0.16262(3) 0.42320(3) 0.04199(13) Uani 1 1 d . . . O1 O 0.15404(10) 0.10427(8) 0.58508(6) 0.0351(3) Uani 1 1 d . . . N1 N 0.30763(11) 0.17026(9) 0.48831(8) 0.0308(3) Uani 1 1 d . . . C1 C 0.2688(2) -0.03645(13) 0.50766(13) 0.0529(6) Uani 1 1 d . . . H1 H 0.3137 -0.0504 0.5510 0.064 Uiso 1 1 calc R . . C2 C 0.15751(19) -0.04701(12) 0.50139(14) 0.0519(5) Uani 1 1 d . . . H2 H 0.1101 -0.0686 0.5405 0.062 Uiso 1 1 calc R . . C3 C 0.1269(2) -0.02795(13) 0.43008(16) 0.0598(6) Uani 1 1 d . . . H3 H 0.0537 -0.0331 0.4098 0.072 Uiso 1 1 calc R . . C4 C 0.2170(2) -0.00618(14) 0.38952(12) 0.0598(7) Uani 1 1 d . . . H4 H 0.2184 0.0066 0.3358 0.072 Uiso 1 1 calc R . . C5 C 0.30615(18) -0.01202(13) 0.43582(16) 0.0573(6) Uani 1 1 d . . . H5 H 0.3817 -0.0046 0.4209 0.069 Uiso 1 1 calc R . . C6 C 0.17935(13) 0.16215(10) 0.63095(9) 0.0291(3) Uani 1 1 d . . . C7 C 0.25342(14) 0.22288(10) 0.61088(9) 0.0312(4) Uani 1 1 d . . . C8 C 0.27433(16) 0.28624(12) 0.66068(11) 0.0412(4) Uani 1 1 d . . . H8 H 0.3225 0.3261 0.6468 0.049 Uiso 1 1 calc R . . C9 C 0.22477(19) 0.28964(13) 0.72876(11) 0.0492(5) Uani 1 1 d . . . H9 H 0.2366 0.3326 0.7605 0.059 Uiso 1 1 calc R . . C10 C 0.15643(17) 0.22852(12) 0.75048(11) 0.0445(5) Uani 1 1 d . . . H10 H 0.1245 0.2309 0.7977 0.053 Uiso 1 1 calc R . . C11 C 0.13363(14) 0.16380(11) 0.70467(9) 0.0330(4) Uani 1 1 d . . . C12 C 0.31349(13) 0.22169(11) 0.54169(10) 0.0321(4) Uani 1 1 d . . . H12 H 0.3624 0.2630 0.5347 0.039 Uiso 1 1 calc R . . C13 C 0.06478(14) 0.09800(11) 0.73323(9) 0.0332(4) Uani 1 1 d . . . C14 C -0.02409(17) 0.11427(13) 0.77886(11) 0.0471(5) Uani 1 1 d . . . H14 H -0.0420 0.1668 0.7893 0.056 Uiso 1 1 calc R . . C15 C -0.08589(17) 0.05396(16) 0.80878(13) 0.0555(6) Uani 1 1 d . . . H15 H -0.1440 0.0663 0.8398 0.067 Uiso 1 1 calc R . . C16 C -0.06258(17) -0.02391(14) 0.79330(11) 0.0498(5) Uani 1 1 d . . . H16 H -0.1053 -0.0643 0.8130 0.060 Uiso 1 1 calc R . . C17 C 0.02515(17) -0.04203(13) 0.74810(11) 0.0455(5) Uani 1 1 d . . . H17 H 0.0417 -0.0948 0.7375 0.055 Uiso 1 1 calc R . . C18 C 0.08797(16) 0.01830(12) 0.71880(10) 0.0392(4) Uani 1 1 d . . . H18 H 0.1470 0.0055 0.6888 0.047 Uiso 1 1 calc R . . C19 C 0.38312(16) 0.18207(12) 0.42355(11) 0.0422(5) Uani 1 1 d . . . H19 H 0.3610 0.1457 0.3834 0.051 Uiso 1 1 calc R . . C20 C 0.3782(2) 0.26602(15) 0.39237(13) 0.0646(7) Uani 1 1 d . . . H20A H 0.3041 0.2815 0.3862 0.097 Uiso 1 1 calc R . . H20B H 0.4142 0.2678 0.3446 0.097 Uiso 1 1 calc R . . H20C H 0.4132 0.3018 0.4266 0.097 Uiso 1 1 calc R . . C21 C 0.49679(18) 0.15943(16) 0.44710(16) 0.0672(7) Uani 1 1 d . . . H21A H 0.5214 0.1952 0.4854 0.101 Uiso 1 1 calc R . . H21B H 0.5441 0.1626 0.4045 0.101 Uiso 1 1 calc R . . H21C H 0.4968 0.1061 0.4663 0.101 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 0.02731(14) 0.02501(15) 0.02440(14) -0.00206(10) 0.00126(10) -0.00193(10) Cl1 0.0393(2) 0.0404(3) 0.0462(3) 0.0078(2) -0.00233(19) 0.00598(19) O1 0.0428(7) 0.0368(7) 0.0256(6) -0.0058(5) 0.0049(5) -0.0110(6) N1 0.0290(7) 0.0311(7) 0.0322(7) -0.0020(6) 0.0023(6) -0.0038(6) C1 0.0664(14) 0.0384(11) 0.0540(12) -0.0060(10) -0.0184(11) 0.0206(10) C2 0.0596(13) 0.0264(10) 0.0697(14) -0.0002(10) 0.0212(11) -0.0030(9) C3 0.0583(13) 0.0343(11) 0.0866(18) -0.0211(11) -0.0248(13) 0.0009(10) C4 0.105(2) 0.0385(12) 0.0356(10) -0.0121(9) -0.0003(12) 0.0127(13) C5 0.0465(12) 0.0363(11) 0.0890(18) -0.0162(11) 0.0282(12) 0.0007(9) C6 0.0295(8) 0.0315(9) 0.0263(8) -0.0027(7) -0.0031(6) 0.0036(7) C7 0.0330(8) 0.0299(8) 0.0307(8) -0.0021(7) -0.0034(7) 0.0015(7) C8 0.0485(11) 0.0344(10) 0.0407(10) -0.0068(8) -0.0041(8) -0.0045(8) C9 0.0682(14) 0.0386(11) 0.0406(10) -0.0162(9) -0.0029(10) -0.0031(10) C10 0.0569(12) 0.0470(11) 0.0298(8) -0.0104(8) 0.0047(8) 0.0028(10) C11 0.0350(9) 0.0371(9) 0.0270(8) -0.0029(7) -0.0003(7) 0.0060(7) C12 0.0297(8) 0.0299(9) 0.0368(9) -0.0019(7) 0.0003(7) -0.0059(7) C13 0.0352(9) 0.0417(10) 0.0227(7) 0.0014(7) -0.0003(7) 0.0054(7) C14 0.0496(11) 0.0479(12) 0.0438(11) 0.0067(9) 0.0140(9) 0.0137(9) C15 0.0460(11) 0.0684(15) 0.0520(12) 0.0148(11) 0.0190(10) 0.0100(11) C16 0.0481(11) 0.0585(14) 0.0430(11) 0.0161(10) 0.0007(9) -0.0076(10) C17 0.0574(12) 0.0423(11) 0.0367(9) 0.0027(9) -0.0003(9) -0.0007(9) C18 0.0420(10) 0.0454(11) 0.0301(8) -0.0017(8) 0.0041(7) 0.0039(8) C19 0.0441(10) 0.0432(11) 0.0394(10) -0.0103(8) 0.0146(8) -0.0148(9) C20 0.0940(18) 0.0534(14) 0.0463(12) 0.0038(11) 0.0166(12) -0.0244(13) C21 0.0379(11) 0.0771(17) 0.0865(18) -0.0288(15) 0.0195(12) -0.0050(11) _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 1.9099(12) . ? Cr1 N1 2.0334(15) . ? Cr1 C1 2.231(2) . ? Cr1 C2 2.244(2) . ? Cr1 C3 2.251(2) . ? Cr1 C4 2.259(2) . ? Cr1 C5 2.262(2) . ? Cr1 Cl1 2.3035(6) . ? O1 C6 1.309(2) . ? N1 C12 1.287(2) . ? N1 C19 1.497(2) . ? C1 C2 1.394(3) . ? C1 C5 1.421(3) . ? C2 C3 1.363(3) . ? C3 C4 1.378(4) . ? C4 C5 1.381(3) . ? C6 C7 1.419(2) . ? C6 C11 1.430(2) . ? C7 C8 1.411(2) . ? C7 C12 1.439(2) . ? C8 C9 1.360(3) . ? C9 C10 1.387(3) . ? C10 C11 1.390(3) . ? C11 C13 1.487(3) . ? C13 C14 1.395(2) . ? C13 C18 1.396(3) . ? C14 C15 1.378(3) . ? C15 C16 1.370(3) . ? C16 C17 1.386(3) . ? C17 C18 1.381(3) . ? C19 C21 1.517(3) . ? C19 C20 1.519(3) . ? 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 N1 90.25(5) . . ? O1 Cr1 C1 96.06(7) . . ? N1 Cr1 C1 111.58(8) . . ? O1 Cr1 C2 90.13(7) . . ? N1 Cr1 C2 147.60(8) . . ? C1 Cr1 C2 36.28(9) . . ? O1 Cr1 C3 117.46(9) . . ? N1 Cr1 C3 150.93(9) . . ? C1 Cr1 C3 59.93(9) . . ? C2 Cr1 C3 35.31(9) . . ? O1 Cr1 C4 149.56(8) . . ? N1 Cr1 C4 115.36(8) . . ? C1 Cr1 C4 60.36(8) . . ? C2 Cr1 C4 59.43(9) . . ? C3 Cr1 C4 35.57(9) . . ? O1 Cr1 C5 131.07(9) . . ? N1 Cr1 C5 96.46(7) . . ? C1 Cr1 C5 36.87(9) . . ? C2 Cr1 C5 60.13(8) . . ? C3 Cr1 C5 59.42(9) . . ? C4 Cr1 C5 35.58(9) . . ? O1 Cr1 Cl1 98.65(4) . . ? N1 Cr1 Cl1 92.15(5) . . ? C1 Cr1 Cl1 151.95(6) . . ? C2 Cr1 Cl1 119.78(7) . . ? C3 Cr1 Cl1 92.05(6) . . ? C4 Cr1 Cl1 96.61(7) . . ? C5 Cr1 Cl1 129.26(8) . . ? C6 O1 Cr1 132.03(11) . . ? C12 N1 C19 116.37(15) . . ? C12 N1 Cr1 123.88(12) . . ? C19 N1 Cr1 119.55(11) . . ? C2 C1 C5 106.6(2) . . ? C2 C1 Cr1 72.36(12) . . ? C5 C1 Cr1 72.73(12) . . ? C3 C2 C1 108.6(2) . . ? C3 C2 Cr1 72.63(13) . . ? C1 C2 Cr1 71.36(12) . . ? C2 C3 C4 109.0(2) . . ? C2 C3 Cr1 72.07(12) . . ? C4 C3 Cr1 72.51(13) . . ? C3 C4 C5 108.3(2) . . ? C3 C4 Cr1 71.91(12) . . ? C5 C4 Cr1 72.33(12) . . ? C4 C5 C1 107.3(2) . . ? C4 C5 Cr1 72.09(12) . . ? C1 C5 Cr1 70.40(12) . . ? O1 C6 C7 122.24(14) . . ? O1 C6 C11 119.50(15) . . ? C7 C6 C11 118.23(15) . . ? C8 C7 C6 120.31(16) . . ? C8 C7 C12 116.99(16) . . ? C6 C7 C12 122.65(15) . . ? C9 C8 C7 120.62(19) . . ? C8 C9 C10 119.51(18) . . ? C9 C10 C11 122.78(18) . . ? C10 C11 C6 118.28(17) . . ? C10 C11 C13 119.95(16) . . ? C6 C11 C13 121.76(15) . . ? N1 C12 C7 127.75(16) . . ? C14 C13 C18 117.27(18) . . ? C14 C13 C11 120.34(17) . . ? C18 C13 C11 122.34(16) . . ? C15 C14 C13 121.2(2) . . ? C16 C15 C14 120.65(19) . . ? C15 C16 C17 119.5(2) . . ? C18 C17 C16 119.9(2) . . ? C17 C18 C13 121.41(18) . . ? N1 C19 C21 109.44(18) . . ? N1 C19 C20 112.31(17) . . ? C21 C19 C20 111.8(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.329 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.048 #===END data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 776253' #TrackingRef '- NJC-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H33 Cl Cr N O' _chemical_formula_weight 474.99 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' 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 7.7239(15) _cell_length_b 16.784(3) _cell_length_c 20.079(4) _cell_angle_alpha 80.09(3) _cell_angle_beta 80.03(3) _cell_angle_gamma 85.18(3) _cell_volume 2521.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23908 _diffrn_reflns_av_R_equivalents 0.1368 _diffrn_reflns_av_sigmaI/netI 0.1920 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 10952 _reflns_number_gt 4837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1077P)^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 10952 _refine_ls_number_parameters 575 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2172 _refine_ls_R_factor_gt 0.0951 _refine_ls_wR_factor_ref 0.2500 _refine_ls_wR_factor_gt 0.1901 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Cr1 Cr 0.43210(13) 0.36048(6) 0.27932(5) 0.0319(3) Uani 1 1 d . . . Cr2 Cr 0.15287(13) 0.16585(6) 0.69692(5) 0.0330(3) Uani 1 1 d . . . Cl1 Cl 0.2733(3) 0.25561(11) 0.34472(9) 0.0558(5) Uani 1 1 d . . . Cl2 Cl 0.0314(3) 0.29217(11) 0.65628(11) 0.0606(6) Uani 1 1 d . . . O1 O 0.2605(5) 0.3868(2) 0.2192(2) 0.0352(10) Uani 1 1 d . . . O2 O -0.0674(6) 0.1257(3) 0.7473(2) 0.0406(11) Uani 1 1 d . . . N1 N 0.3176(6) 0.4576(3) 0.3280(2) 0.0341(12) Uani 1 1 d . . . N2 N 0.1150(7) 0.1021(3) 0.6191(3) 0.0372(13) Uani 1 1 d . . . C1 C 0.7153(8) 0.3951(4) 0.2696(4) 0.0466(17) Uani 1 1 d . . . C2 C 0.7088(9) 0.3140(4) 0.2984(4) 0.052(2) Uani 1 1 d . . . C3 C 0.6586(9) 0.2722(5) 0.2492(5) 0.068(3) Uani 1 1 d . . . C4 C 0.6316(10) 0.3281(6) 0.1922(4) 0.065(3) Uani 1 1 d . . . C5 C 0.6635(10) 0.4062(5) 0.2049(4) 0.057(2) Uani 1 1 d . . . C6 C 0.7797(11) 0.4629(5) 0.2987(5) 0.080(3) Uani 1 1 d . . . H6A H 0.8496 0.4973 0.2626 0.119 Uiso 1 1 calc R . . H6B H 0.8498 0.4402 0.3332 0.119 Uiso 1 1 calc R . . H6C H 0.6805 0.4941 0.3187 0.119 Uiso 1 1 calc R . . C7 C 0.7633(13) 0.2749(6) 0.3655(5) 0.096(3) Uani 1 1 d . . . H7A H 0.8831 0.2537 0.3574 0.145 Uiso 1 1 calc R . . H7B H 0.6881 0.2317 0.3864 0.145 Uiso 1 1 calc R . . H7C H 0.7534 0.3145 0.3954 0.145 Uiso 1 1 calc R . . C8 C 0.6441(13) 0.1820(5) 0.2592(8) 0.136(6) Uani 1 1 d . . . H8A H 0.6016 0.1624 0.3065 0.204 Uiso 1 1 calc R . . H8B H 0.7578 0.1564 0.2460 0.204 Uiso 1 1 calc R . . H8C H 0.5636 0.1696 0.2314 0.204 Uiso 1 1 calc R . . C9 C 0.5804(13) 0.3099(9) 0.1269(5) 0.144(6) Uani 1 1 d . . . H9A H 0.6394 0.3449 0.0883 0.216 Uiso 1 1 calc R . . H9B H 0.4554 0.3189 0.1289 0.216 Uiso 1 1 calc R . . H9C H 0.6141 0.2545 0.1224 0.216 Uiso 1 1 calc R . . C10 C 0.6652(13) 0.4827(7) 0.1548(5) 0.113(4) Uani 1 1 d . . . H10A H 0.6604 0.5281 0.1784 0.170 Uiso 1 1 calc R . . H10B H 0.5651 0.4866 0.1317 0.170 Uiso 1 1 calc R . . H10C H 0.7713 0.4828 0.1218 0.170 Uiso 1 1 calc R . . C11 C 0.2283(7) 0.4607(4) 0.1889(3) 0.0333(14) Uani 1 1 d . . . C12 C 0.2359(9) 0.5293(4) 0.2195(3) 0.0396(16) Uani 1 1 d . . . C13 C 0.2004(10) 0.6072(4) 0.1858(4) 0.057(2) Uani 1 1 d . . . H13 H 0.1991 0.6516 0.2080 0.069 Uiso 1 1 calc R . . C14 C 0.1671(12) 0.6184(5) 0.1189(4) 0.067(2) Uani 1 1 d . . . H14 H 0.1525 0.6704 0.0948 0.080 Uiso 1 1 calc R . . C15 C 0.1557(11) 0.5510(5) 0.0884(4) 0.061(2) Uani 1 1 d . . . H15 H 0.1296 0.5588 0.0442 0.073 Uiso 1 1 calc R . . C16 C 0.1819(9) 0.4727(4) 0.1218(3) 0.0471(18) Uani 1 1 d . . . C17 C 0.2557(9) 0.5214(4) 0.2913(3) 0.0389(15) Uani 1 1 d . . . H17 H 0.2206 0.5663 0.3128 0.047 Uiso 1 1 calc R . . C18 C 0.1681(10) 0.4020(5) 0.0870(3) 0.0475(19) Uani 1 1 d . . . C19 C 0.0800(10) 0.3350(5) 0.1213(4) 0.054(2) Uani 1 1 d . . . H19 H 0.0287 0.3333 0.1669 0.065 Uiso 1 1 calc R . . C20 C 0.0672(12) 0.2698(5) 0.0882(4) 0.068(2) Uani 1 1 d . . . H20 H 0.0101 0.2243 0.1120 0.082 Uiso 1 1 calc R . . C21 C 0.1378(17) 0.2728(7) 0.0215(5) 0.101(4) Uani 1 1 d . . . H21 H 0.1278 0.2295 -0.0007 0.122 Uiso 1 1 calc R . . C22 C 0.2224(17) 0.3379(7) -0.0131(5) 0.101(4) Uani 1 1 d . . . H22 H 0.2683 0.3394 -0.0592 0.121 Uiso 1 1 calc R . . C23 C 0.2426(13) 0.4025(6) 0.0184(4) 0.075(3) Uani 1 1 d . . . H23 H 0.3055 0.4462 -0.0058 0.090 Uiso 1 1 calc R . . C24 C 0.2916(9) 0.4591(4) 0.4045(3) 0.0422(17) Uani 1 1 d . . . C25 C 0.4234(10) 0.3974(4) 0.4360(3) 0.055(2) Uani 1 1 d . . . H25A H 0.4120 0.3454 0.4239 0.082 Uiso 1 1 calc R . . H25B H 0.4003 0.3936 0.4850 0.082 Uiso 1 1 calc R . . H25C H 0.5407 0.4144 0.4190 0.082 Uiso 1 1 calc R . . C26 C 0.1016(11) 0.4334(6) 0.4335(4) 0.072(3) Uani 1 1 d . . . H26A H 0.0189 0.4732 0.4146 0.107 Uiso 1 1 calc R . . H26B H 0.0817 0.4292 0.4824 0.107 Uiso 1 1 calc R . . H26C H 0.0863 0.3819 0.4213 0.107 Uiso 1 1 calc R . . C27 C 0.3176(12) 0.5420(4) 0.4224(4) 0.065(2) Uani 1 1 d . . . H27A H 0.4304 0.5603 0.3996 0.097 Uiso 1 1 calc R . . H27B H 0.3119 0.5375 0.4711 0.097 Uiso 1 1 calc R . . H27C H 0.2266 0.5803 0.4079 0.097 Uiso 1 1 calc R . . C28 C 0.4223(9) 0.1069(4) 0.7065(4) 0.0466(18) Uani 1 1 d . . . C29 C 0.4421(9) 0.1913(5) 0.6912(4) 0.055(2) Uani 1 1 d . . . C30 C 0.3393(10) 0.2257(4) 0.7471(4) 0.055(2) Uani 1 1 d . . . C31 C 0.2598(9) 0.1626(4) 0.7942(3) 0.0457(18) Uani 1 1 d . . . C32 C 0.3117(9) 0.0885(4) 0.7692(3) 0.0393(16) Uani 1 1 d . . . C33 C 0.5138(11) 0.0428(5) 0.6647(5) 0.075(3) Uani 1 1 d . . . H33A H 0.5787 0.0036 0.6929 0.112 Uiso 1 1 calc R . . H33B H 0.5929 0.0683 0.6261 0.112 Uiso 1 1 calc R . . H33C H 0.4270 0.0164 0.6487 0.112 Uiso 1 1 calc R . . C34 C 0.5677(13) 0.2363(6) 0.6352(5) 0.096(3) Uani 1 1 d . . . H34A H 0.6717 0.2449 0.6527 0.144 Uiso 1 1 calc R . . H34B H 0.5132 0.2877 0.6186 0.144 Uiso 1 1 calc R . . H34C H 0.5991 0.2054 0.5985 0.144 Uiso 1 1 calc R . . C35 C 0.3286(13) 0.3133(5) 0.7541(5) 0.085(3) Uani 1 1 d . . . H35A H 0.2277 0.3244 0.7871 0.127 Uiso 1 1 calc R . . H35B H 0.3180 0.3459 0.7106 0.127 Uiso 1 1 calc R . . H35C H 0.4332 0.3258 0.7690 0.127 Uiso 1 1 calc R . . C36 C 0.1417(12) 0.1705(6) 0.8622(4) 0.074(3) Uani 1 1 d . . . H36A H 0.2050 0.1497 0.8993 0.111 Uiso 1 1 calc R . . H36B H 0.0390 0.1403 0.8666 0.111 Uiso 1 1 calc R . . H36C H 0.1066 0.2265 0.8636 0.111 Uiso 1 1 calc R . . C37 C 0.2700(11) 0.0056(4) 0.8067(4) 0.063(2) Uani 1 1 d . . . H37A H 0.2414 -0.0267 0.7755 0.094 Uiso 1 1 calc R . . H37B H 0.1714 0.0096 0.8426 0.094 Uiso 1 1 calc R . . H37C H 0.3703 -0.0193 0.8262 0.094 Uiso 1 1 calc R . . C38 C -0.1065(9) 0.0494(4) 0.7558(4) 0.0422(17) Uani 1 1 d . . . C39 C -0.0530(9) 0.0020(4) 0.7036(4) 0.0420(17) Uani 1 1 d . . . C40 C -0.1010(10) -0.0797(4) 0.7135(4) 0.0520(19) Uani 1 1 d . . . H40 H -0.0689 -0.1101 0.6782 0.062 Uiso 1 1 calc R . . C41 C -0.1927(11) -0.1134(5) 0.7738(5) 0.063(2) Uani 1 1 d . . . H41 H -0.2210 -0.1673 0.7809 0.075 Uiso 1 1 calc R . . C42 C -0.2436(10) -0.0668(5) 0.8244(4) 0.061(2) Uani 1 1 d . . . H42 H -0.3040 -0.0912 0.8661 0.073 Uiso 1 1 calc R . . C43 C -0.2108(10) 0.0135(4) 0.8175(4) 0.0493(18) Uani 1 1 d . . . C44 C 0.0367(8) 0.0360(4) 0.6370(3) 0.0381(15) Uani 1 1 d . . . H44 H 0.0375 0.0056 0.6023 0.046 Uiso 1 1 calc R . . C45 C -0.2686(11) 0.0615(6) 0.8739(4) 0.062(2) Uani 1 1 d . . . C46 C -0.3452(10) 0.1396(6) 0.8644(5) 0.067(2) Uani 1 1 d . . . H46 H -0.3586 0.1640 0.8202 0.080 Uiso 1 1 calc R . . C47 C -0.4022(14) 0.1824(8) 0.9175(7) 0.104(4) Uani 1 1 d . . . H47 H -0.4531 0.2346 0.9092 0.125 Uiso 1 1 calc R . . C48 C -0.383(2) 0.1472(11) 0.9822(7) 0.133(6) Uani 1 1 d . . . H48 H -0.4218 0.1751 1.0187 0.160 Uiso 1 1 calc R . . C49 C -0.306(3) 0.0710(11) 0.9933(6) 0.163(7) Uani 1 1 d . . . H49 H -0.2876 0.0482 1.0373 0.196 Uiso 1 1 calc R . . C50 C -0.2556(17) 0.0274(7) 0.9410(5) 0.106(4) Uani 1 1 d . . . H50 H -0.2119 -0.0259 0.9505 0.127 Uiso 1 1 calc R . . C51 C 0.1686(10) 0.1298(5) 0.5421(3) 0.0488(18) Uani 1 1 d . . . C52 C 0.3132(11) 0.1891(5) 0.5312(4) 0.068(2) Uani 1 1 d . . . H52A H 0.2725 0.2334 0.5556 0.102 Uiso 1 1 calc R . . H52B H 0.3431 0.2095 0.4832 0.102 Uiso 1 1 calc R . . H52C H 0.4153 0.1620 0.5480 0.102 Uiso 1 1 calc R . . C53 C 0.2410(12) 0.0598(5) 0.5036(4) 0.076(3) Uani 1 1 d . . . H53A H 0.3317 0.0291 0.5256 0.114 Uiso 1 1 calc R . . H53B H 0.2889 0.0811 0.4572 0.114 Uiso 1 1 calc R . . H53C H 0.1476 0.0254 0.5038 0.114 Uiso 1 1 calc R . . C54 C 0.0034(11) 0.1702(6) 0.5163(4) 0.074(3) Uani 1 1 d . . . H54A H -0.0809 0.1301 0.5196 0.112 Uiso 1 1 calc R . . H54B H 0.0332 0.1951 0.4693 0.112 Uiso 1 1 calc R . . H54C H -0.0463 0.2107 0.5436 0.112 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 0.0321(6) 0.0290(6) 0.0351(6) -0.0038(4) -0.0089(5) -0.0011(4) Cr2 0.0322(6) 0.0274(6) 0.0392(6) -0.0039(4) -0.0073(5) -0.0013(4) Cl1 0.0758(14) 0.0493(11) 0.0429(10) 0.0008(8) -0.0073(10) -0.0283(9) Cl2 0.0669(13) 0.0371(10) 0.0739(13) 0.0013(9) -0.0185(11) 0.0120(9) O1 0.038(3) 0.036(3) 0.031(2) -0.0048(19) -0.008(2) 0.0018(19) O2 0.044(3) 0.038(3) 0.040(3) -0.005(2) -0.006(2) -0.009(2) N1 0.031(3) 0.040(3) 0.032(3) -0.007(2) -0.003(2) -0.007(2) N2 0.029(3) 0.045(3) 0.036(3) -0.005(3) -0.001(3) -0.003(2) C1 0.025(4) 0.054(5) 0.059(5) -0.013(4) 0.001(3) -0.008(3) C2 0.035(4) 0.048(5) 0.074(5) -0.002(4) -0.023(4) 0.000(3) C3 0.033(4) 0.046(5) 0.132(8) -0.035(5) -0.018(5) 0.011(4) C4 0.035(4) 0.108(8) 0.062(5) -0.047(5) -0.014(4) 0.019(5) C5 0.037(4) 0.072(6) 0.050(5) 0.004(4) 0.006(4) 0.001(4) C6 0.049(5) 0.080(7) 0.114(8) -0.035(6) 0.007(5) -0.028(4) C7 0.077(7) 0.101(8) 0.108(8) 0.021(6) -0.053(6) 0.014(6) C8 0.065(7) 0.043(6) 0.311(18) -0.077(9) -0.029(9) 0.027(5) C9 0.068(7) 0.298(17) 0.100(8) -0.143(10) -0.034(6) 0.065(9) C10 0.068(7) 0.145(10) 0.090(7) 0.071(7) 0.003(6) -0.014(6) C11 0.016(3) 0.050(4) 0.029(3) -0.006(3) 0.007(3) 0.001(3) C12 0.046(4) 0.029(4) 0.045(4) 0.002(3) -0.016(3) -0.003(3) C13 0.070(6) 0.038(4) 0.065(5) -0.004(4) -0.019(5) 0.003(4) C14 0.089(7) 0.047(5) 0.057(5) 0.014(4) -0.021(5) 0.005(4) C15 0.073(6) 0.062(5) 0.045(4) 0.005(4) -0.019(4) 0.012(4) C16 0.045(4) 0.056(5) 0.040(4) -0.008(3) -0.012(3) 0.010(3) C17 0.042(4) 0.032(4) 0.043(4) -0.008(3) -0.006(3) -0.001(3) C18 0.049(5) 0.059(5) 0.036(4) -0.011(4) -0.017(4) 0.017(4) C19 0.051(5) 0.068(6) 0.048(4) -0.020(4) -0.015(4) 0.005(4) C20 0.082(6) 0.063(6) 0.069(6) -0.022(5) -0.028(5) 0.003(5) C21 0.172(12) 0.085(8) 0.062(7) -0.042(6) -0.056(7) 0.047(8) C22 0.166(12) 0.099(9) 0.034(5) -0.017(6) -0.018(6) 0.031(8) C23 0.109(8) 0.076(6) 0.035(4) -0.007(4) -0.009(5) 0.019(5) C24 0.052(4) 0.050(4) 0.029(3) -0.014(3) -0.008(3) -0.010(3) C25 0.074(6) 0.062(5) 0.031(4) -0.001(3) -0.020(4) -0.013(4) C26 0.074(6) 0.103(7) 0.044(5) -0.025(5) -0.001(5) -0.031(5) C27 0.090(6) 0.060(5) 0.056(5) -0.028(4) -0.024(5) 0.001(4) C28 0.044(4) 0.043(4) 0.060(5) -0.011(4) -0.030(4) 0.007(3) C29 0.038(4) 0.065(5) 0.066(5) -0.006(4) -0.018(4) -0.013(4) C30 0.059(5) 0.040(4) 0.073(6) -0.009(4) -0.030(5) -0.014(4) C31 0.044(4) 0.058(5) 0.040(4) -0.019(4) -0.010(3) 0.003(3) C32 0.041(4) 0.037(4) 0.040(4) 0.000(3) -0.014(3) -0.001(3) C33 0.059(5) 0.082(6) 0.093(7) -0.043(5) -0.029(5) 0.037(5) C34 0.080(7) 0.113(9) 0.095(7) 0.012(6) -0.013(6) -0.068(6) C35 0.096(7) 0.046(5) 0.129(9) -0.033(5) -0.036(7) -0.018(5) C36 0.083(7) 0.093(7) 0.057(5) -0.033(5) -0.021(5) -0.006(5) C37 0.076(6) 0.042(4) 0.071(5) 0.011(4) -0.035(5) 0.002(4) C38 0.039(4) 0.038(4) 0.052(4) 0.006(3) -0.022(4) -0.009(3) C39 0.042(4) 0.038(4) 0.049(4) -0.003(3) -0.018(4) -0.006(3) C40 0.053(5) 0.034(4) 0.070(5) -0.005(4) -0.015(4) -0.006(3) C41 0.063(6) 0.036(4) 0.086(6) 0.013(4) -0.019(5) -0.011(4) C42 0.054(5) 0.064(6) 0.060(5) 0.017(4) -0.013(4) -0.018(4) C43 0.046(4) 0.047(5) 0.054(5) 0.005(4) -0.016(4) -0.009(3) C44 0.032(4) 0.047(4) 0.037(4) -0.014(3) -0.005(3) -0.002(3) C45 0.055(5) 0.079(6) 0.054(5) 0.000(4) -0.011(4) -0.025(4) C46 0.042(5) 0.091(7) 0.069(6) -0.026(5) 0.001(4) -0.001(5) C47 0.082(8) 0.129(10) 0.110(9) -0.066(8) 0.016(7) -0.021(7) C48 0.146(13) 0.184(16) 0.072(9) -0.068(10) 0.042(8) -0.049(11) C49 0.27(2) 0.171(16) 0.044(7) -0.015(9) -0.004(10) -0.036(15) C50 0.162(12) 0.101(8) 0.041(5) 0.009(5) -0.001(6) -0.010(8) C51 0.048(4) 0.067(5) 0.027(4) -0.003(3) 0.004(3) -0.008(4) C52 0.073(6) 0.075(6) 0.055(5) 0.010(4) -0.015(5) -0.027(5) C53 0.078(7) 0.095(7) 0.055(5) -0.026(5) 0.006(5) -0.013(5) C54 0.057(6) 0.114(8) 0.046(5) 0.005(5) -0.013(4) 0.001(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 Cr1 O1 1.919(4) . ? Cr1 N1 2.098(5) . ? Cr1 C5 2.220(8) . ? Cr1 C4 2.232(8) . ? Cr1 C3 2.265(7) . ? Cr1 C1 2.277(7) . ? Cr1 C2 2.285(6) . ? Cr1 Cl1 2.310(2) . ? Cr2 O2 1.933(5) . ? Cr2 N2 2.112(5) . ? Cr2 C32 2.236(6) . ? Cr2 C31 2.240(6) . ? Cr2 C28 2.252(6) . ? Cr2 C30 2.279(6) . ? Cr2 C29 2.289(7) . ? Cr2 Cl2 2.319(2) . ? O1 C11 1.308(7) . ? O2 C38 1.316(7) . ? N1 C17 1.297(7) . ? N1 C24 1.518(7) . ? N2 C44 1.276(8) . ? N2 C51 1.529(8) . ? C1 C2 1.385(10) . ? C1 C5 1.403(10) . ? C1 C6 1.520(10) . ? C2 C3 1.426(10) . ? C2 C7 1.506(10) . ? C3 C4 1.384(12) . ? C3 C8 1.504(11) . ? C4 C5 1.427(11) . ? C4 C9 1.518(10) . ? C5 C10 1.488(11) . ? C11 C12 1.405(9) . ? C11 C16 1.430(8) . ? C12 C13 1.394(9) . ? C12 C17 1.459(8) . ? C13 C14 1.389(10) . ? C14 C15 1.391(10) . ? C15 C16 1.383(10) . ? C16 C18 1.497(9) . ? C18 C19 1.378(10) . ? C18 C23 1.396(10) . ? C19 C20 1.393(10) . ? C20 C21 1.349(13) . ? C21 C22 1.344(15) . ? C22 C23 1.377(13) . ? C24 C25 1.526(9) . ? C24 C27 1.534(9) . ? C24 C26 1.550(10) . ? C28 C32 1.397(10) . ? C28 C29 1.411(10) . ? C28 C33 1.529(10) . ? C29 C30 1.436(11) . ? C29 C34 1.493(11) . ? C30 C31 1.398(10) . ? C30 C35 1.494(10) . ? C31 C32 1.423(9) . ? C31 C36 1.525(10) . ? C32 C37 1.495(9) . ? C38 C39 1.409(9) . ? C38 C43 1.423(10) . ? C39 C40 1.421(9) . ? C39 C44 1.442(9) . ? C40 C41 1.349(11) . ? C41 C42 1.372(11) . ? C42 C43 1.371(10) . ? C43 C45 1.487(11) . ? C45 C46 1.387(11) . ? C45 C50 1.387(11) . ? C46 C47 1.377(12) . ? C47 C48 1.359(17) . ? C48 C49 1.364(19) . ? C49 C50 1.366(16) . ? C51 C52 1.521(10) . ? C51 C54 1.523(10) . ? C51 C53 1.531(10) . ? 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 N1 87.27(18) . . ? O1 Cr1 C5 97.4(2) . . ? N1 Cr1 C5 107.0(3) . . ? O1 Cr1 C4 89.9(2) . . ? N1 Cr1 C4 143.4(3) . . ? C5 Cr1 C4 37.4(3) . . ? O1 Cr1 C3 117.1(3) . . ? N1 Cr1 C3 153.0(2) . . ? C5 Cr1 C3 60.9(3) . . ? C4 Cr1 C3 35.8(3) . . ? O1 Cr1 C1 132.3(2) . . ? N1 Cr1 C1 95.8(2) . . ? C5 Cr1 C1 36.3(3) . . ? C4 Cr1 C1 60.5(3) . . ? C3 Cr1 C1 59.7(3) . . ? O1 Cr1 C2 150.5(2) . . ? N1 Cr1 C2 116.7(2) . . ? C5 Cr1 C2 60.7(3) . . ? C4 Cr1 C2 60.6(3) . . ? C3 Cr1 C2 36.5(3) . . ? C1 Cr1 C2 35.3(2) . . ? O1 Cr1 Cl1 92.14(15) . . ? N1 Cr1 Cl1 100.40(16) . . ? C5 Cr1 Cl1 151.3(2) . . ? C4 Cr1 Cl1 116.1(3) . . ? C3 Cr1 Cl1 90.7(2) . . ? C1 Cr1 Cl1 133.4(2) . . ? C2 Cr1 Cl1 99.5(2) . . ? O2 Cr2 N2 87.06(19) . . ? O2 Cr2 C32 93.1(2) . . ? N2 Cr2 C32 110.3(2) . . ? O2 Cr2 C31 91.3(2) . . ? N2 Cr2 C31 147.3(2) . . ? C32 Cr2 C31 37.1(2) . . ? O2 Cr2 C28 125.7(2) . . ? N2 Cr2 C28 94.3(2) . . ? C32 Cr2 C28 36.3(3) . . ? C31 Cr2 C28 60.7(2) . . ? O2 Cr2 C30 121.8(3) . . ? N2 Cr2 C30 148.9(3) . . ? C32 Cr2 C30 61.0(2) . . ? C31 Cr2 C30 36.0(3) . . ? C28 Cr2 C30 60.5(3) . . ? O2 Cr2 C29 151.3(2) . . ? N2 Cr2 C29 112.3(3) . . ? C32 Cr2 C29 60.9(3) . . ? C31 Cr2 C29 60.8(3) . . ? C28 Cr2 C29 36.2(3) . . ? C30 Cr2 C29 36.7(3) . . ? O2 Cr2 Cl2 94.74(15) . . ? N2 Cr2 Cl2 99.52(15) . . ? C32 Cr2 Cl2 149.47(18) . . ? C31 Cr2 Cl2 113.20(19) . . ? C28 Cr2 Cl2 137.9(2) . . ? C30 Cr2 Cl2 90.07(19) . . ? C29 Cr2 Cl2 102.3(2) . . ? C11 O1 Cr1 122.6(4) . . ? C38 O2 Cr2 123.5(4) . . ? C17 N1 C24 115.5(5) . . ? C17 N1 Cr1 118.8(4) . . ? C24 N1 Cr1 125.6(4) . . ? C44 N2 C51 116.5(5) . . ? C44 N2 Cr2 117.9(4) . . ? C51 N2 Cr2 125.5(4) . . ? C2 C1 C5 109.4(6) . . ? C2 C1 C6 127.3(7) . . ? C5 C1 C6 123.1(7) . . ? C2 C1 Cr1 72.6(4) . . ? C5 C1 Cr1 69.6(4) . . ? C6 C1 Cr1 127.2(5) . . ? C1 C2 C3 107.1(7) . . ? C1 C2 C7 127.0(7) . . ? C3 C2 C7 125.6(8) . . ? C1 C2 Cr1 72.0(4) . . ? C3 C2 Cr1 71.0(4) . . ? C7 C2 Cr1 127.3(6) . . ? C4 C3 C2 108.5(7) . . ? C4 C3 C8 127.3(9) . . ? C2 C3 C8 124.1(9) . . ? C4 C3 Cr1 70.8(4) . . ? C2 C3 Cr1 72.5(4) . . ? C8 C3 Cr1 123.8(6) . . ? C3 C4 C5 107.9(7) . . ? C3 C4 C9 126.4(10) . . ? C5 C4 C9 125.7(10) . . ? C3 C4 Cr1 73.4(5) . . ? C5 C4 Cr1 70.8(4) . . ? C9 C4 Cr1 122.3(5) . . ? C1 C5 C4 106.9(7) . . ? C1 C5 C10 126.7(8) . . ? C4 C5 C10 125.9(9) . . ? C1 C5 Cr1 74.1(4) . . ? C4 C5 Cr1 71.8(5) . . ? C10 C5 Cr1 125.7(6) . . ? O1 C11 C12 123.0(5) . . ? O1 C11 C16 118.9(6) . . ? C12 C11 C16 118.1(6) . . ? C13 C12 C11 121.5(6) . . ? C13 C12 C17 116.8(6) . . ? C11 C12 C17 121.1(6) . . ? C14 C13 C12 119.8(7) . . ? C13 C14 C15 119.3(7) . . ? C16 C15 C14 122.2(7) . . ? C15 C16 C11 118.9(6) . . ? C15 C16 C18 120.4(6) . . ? C11 C16 C18 120.7(6) . . ? N1 C17 C12 126.1(6) . . ? C19 C18 C23 118.1(7) . . ? C19 C18 C16 121.2(6) . . ? C23 C18 C16 120.7(8) . . ? C18 C19 C20 120.6(8) . . ? C21 C20 C19 119.9(10) . . ? C22 C21 C20 120.4(9) . . ? C21 C22 C23 121.4(9) . . ? C22 C23 C18 119.5(10) . . ? N1 C24 C25 108.6(5) . . ? N1 C24 C27 113.7(6) . . ? C25 C24 C27 108.3(5) . . ? N1 C24 C26 106.3(5) . . ? C25 C24 C26 109.7(6) . . ? C27 C24 C26 110.3(6) . . ? C32 C28 C29 109.5(7) . . ? C32 C28 C33 123.5(7) . . ? C29 C28 C33 126.9(8) . . ? C32 C28 Cr2 71.2(4) . . ? C29 C28 Cr2 73.3(4) . . ? C33 C28 Cr2 124.6(4) . . ? C28 C29 C30 106.6(7) . . ? C28 C29 C34 127.9(8) . . ? C30 C29 C34 124.7(8) . . ? C28 C29 Cr2 70.5(4) . . ? C30 C29 Cr2 71.3(4) . . ? C34 C29 Cr2 131.1(5) . . ? C31 C30 C29 107.9(6) . . ? C31 C30 C35 126.9(8) . . ? C29 C30 C35 125.1(8) . . ? C31 C30 Cr2 70.5(4) . . ? C29 C30 Cr2 72.1(4) . . ? C35 C30 Cr2 125.3(5) . . ? C30 C31 C32 108.6(6) . . ? C30 C31 C36 126.4(7) . . ? C32 C31 C36 125.0(7) . . ? C30 C31 Cr2 73.5(4) . . ? C32 C31 Cr2 71.3(3) . . ? C36 C31 Cr2 122.6(5) . . ? C28 C32 C31 107.3(6) . . ? C28 C32 C37 126.4(7) . . ? C31 C32 C37 126.0(7) . . ? C28 C32 Cr2 72.5(4) . . ? C31 C32 Cr2 71.6(4) . . ? C37 C32 Cr2 125.9(5) . . ? O2 C38 C39 121.4(6) . . ? O2 C38 C43 120.5(7) . . ? C39 C38 C43 118.1(6) . . ? C38 C39 C40 120.2(7) . . ? C38 C39 C44 121.7(6) . . ? C40 C39 C44 117.9(6) . . ? C41 C40 C39 120.4(7) . . ? C40 C41 C42 118.9(8) . . ? C43 C42 C41 124.1(8) . . ? C42 C43 C38 118.1(7) . . ? C42 C43 C45 122.2(8) . . ? C38 C43 C45 119.6(7) . . ? N2 C44 C39 128.8(6) . . ? C46 C45 C50 116.0(9) . . ? C46 C45 C43 123.7(7) . . ? C50 C45 C43 120.2(9) . . ? C47 C46 C45 122.9(10) . . ? C48 C47 C46 119.0(12) . . ? C47 C48 C49 119.7(12) . . ? C48 C49 C50 121.2(12) . . ? C49 C50 C45 121.0(12) . . ? C52 C51 C54 111.5(7) . . ? C52 C51 N2 108.7(6) . . ? C54 C51 N2 106.1(6) . . ? C52 C51 C53 107.5(7) . . ? C54 C51 C53 110.4(6) . . ? N2 C51 C53 112.8(6) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.408 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.096 #===END data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 776254' #TrackingRef '- NJC-new.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Cl3 Cr N2 O3' _chemical_formula_weight 520.77 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.365(2) _cell_length_b 18.149(4) _cell_length_c 12.445(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.76(3) _cell_angle_gamma 90.00 _cell_volume 2400.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Rigaku R-AXIS RAPID IP diffractometer' _diffrn_measurement_method 'Oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18085 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0548 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4172 _reflns_number_gt 2499 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _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^)+(0.1306P)^2^+0.1907P] 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 4172 _refine_ls_number_parameters 282 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.1953 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Cr1 Cr 0.78039(8) 0.12867(4) 0.97467(7) 0.0624(3) Uani 1 1 d . . . Cl1 Cl 0.95023(15) 0.13825(9) 0.91550(13) 0.0858(5) Uani 1 1 d . . . Cl2 Cl 0.9007(4) 0.9481(3) 0.3816(4) 0.251(2) Uani 1 1 d . . . Cl3 Cl 0.7076(4) 0.8588(3) 0.2332(4) 0.2273(19) Uani 1 1 d . . . O1 O 0.6948(3) 0.21494(19) 0.9000(3) 0.0716(10) Uani 1 1 d . . . O2 O 0.7373(7) 0.5216(3) 1.1319(5) 0.147(2) Uani 1 1 d . . . O3 O 0.6000(6) 0.5447(3) 0.9658(5) 0.1125(16) Uani 1 1 d . . . N1 N 0.8651(3) 0.1873(2) 1.1189(3) 0.0584(10) Uani 1 1 d . . . N2 N 0.6713(7) 0.5025(3) 1.0347(5) 0.0946(16) Uani 1 1 d . . . C1 C 0.7406(12) 0.0163(5) 0.9029(11) 0.125(3) Uani 1 1 d . . . H1 H 0.7787 -0.0076 0.8526 0.150 Uiso 1 1 calc R . . C2 C 0.6292(12) 0.0545(5) 0.8688(9) 0.131(4) Uani 1 1 d . . . H2 H 0.5729 0.0631 0.7895 0.158 Uiso 1 1 calc R . . C3 C 0.6058(9) 0.0729(5) 0.9693(15) 0.139(4) Uani 1 1 d . . . H3A H 0.5301 0.0973 0.9719 0.167 Uiso 1 1 calc R . . C4 C 0.6995(10) 0.0450(6) 1.0605(8) 0.115(3) Uani 1 1 d . . . H4 H 0.7039 0.0465 1.1405 0.138 Uiso 1 1 calc R . . C5 C 0.7820(9) 0.0114(4) 1.0221(10) 0.122(3) Uani 1 1 d . . . H5 H 0.8564 -0.0159 1.0701 0.146 Uiso 1 1 calc R . . C6 C 0.6899(4) 0.2821(3) 0.9330(4) 0.0547(11) Uani 1 1 d . . . C7 C 0.6067(4) 0.3328(3) 0.8559(4) 0.0571(12) Uani 1 1 d . . . C8 C 0.6052(5) 0.4049(3) 0.8926(5) 0.0650(13) Uani 1 1 d . . . H8 H 0.5538 0.4392 0.8420 0.078 Uiso 1 1 calc R . . C9 C 0.6770(6) 0.4267(3) 1.0005(5) 0.0713(14) Uani 1 1 d . . . C10 C 0.7581(6) 0.3785(3) 1.0785(5) 0.0670(13) Uani 1 1 d . . . H10 H 0.8067 0.3946 1.1518 0.080 Uiso 1 1 calc R . . C11 C 0.7660(4) 0.3062(3) 1.0461(4) 0.0553(11) Uani 1 1 d . . . C12 C 0.8489(4) 0.2571(3) 1.1306(4) 0.0596(12) Uani 1 1 d . . . H12 H 0.8958 0.2779 1.2012 0.071 Uiso 1 1 calc R . . C13 C 0.5186(4) 0.3102(3) 0.7408(4) 0.0577(12) Uani 1 1 d . . . C14 C 0.5508(5) 0.2577(3) 0.6743(4) 0.0706(14) Uani 1 1 d . . . H14 H 0.6300 0.2360 0.7023 0.085 Uiso 1 1 calc R . . C15 C 0.4676(6) 0.2374(4) 0.5680(5) 0.0863(18) Uani 1 1 d . . . H15 H 0.4904 0.2022 0.5247 0.104 Uiso 1 1 calc R . . C16 C 0.3504(6) 0.2697(4) 0.5263(5) 0.0922(19) Uani 1 1 d . . . H16 H 0.2936 0.2557 0.4548 0.111 Uiso 1 1 calc R . . C17 C 0.3172(6) 0.3215(4) 0.5884(6) 0.0907(19) Uani 1 1 d . . . H17 H 0.2391 0.3443 0.5584 0.109 Uiso 1 1 calc R . . C18 C 0.3984(5) 0.3403(3) 0.6952(5) 0.0766(15) Uani 1 1 d . . . H18 H 0.3727 0.3741 0.7386 0.092 Uiso 1 1 calc R . . C19 C 0.9599(5) 0.1491(3) 1.2195(5) 0.0717(15) Uani 1 1 d . . . H19 H 0.9655 0.0978 1.1974 0.086 Uiso 1 1 calc R . . C20 C 1.0888(6) 0.1828(5) 1.2505(7) 0.116(3) Uani 1 1 d . . . H20A H 1.1067 0.1914 1.1817 0.173 Uiso 1 1 calc R . . H20B H 1.1504 0.1497 1.2997 0.173 Uiso 1 1 calc R . . H20C H 1.0914 0.2286 1.2897 0.173 Uiso 1 1 calc R . . C21 C 0.9166(8) 0.1486(5) 1.3236(6) 0.112(3) Uani 1 1 d . . . H21A H 0.9079 0.1984 1.3458 0.168 Uiso 1 1 calc R . . H21B H 0.9779 0.1234 1.3865 0.168 Uiso 1 1 calc R . . H21C H 0.8371 0.1238 1.3033 0.168 Uiso 1 1 calc R . . C22 C 0.8040(16) 0.8665(7) 0.3658(11) 0.193(6) Uani 1 1 d . . . H22A H 0.8573 0.8232 0.3870 0.231 Uiso 1 1 calc R . . H22B H 0.7564 0.8698 0.4167 0.231 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 0.0639(5) 0.0453(5) 0.0680(6) -0.0002(4) 0.0112(4) 0.0065(4) Cl1 0.0816(10) 0.1024(12) 0.0736(10) 0.0059(8) 0.0279(8) 0.0190(8) Cl2 0.239(4) 0.199(4) 0.224(4) 0.048(3) -0.031(3) -0.077(3) Cl3 0.214(4) 0.231(5) 0.176(4) -0.009(3) -0.006(3) -0.007(3) O1 0.072(2) 0.052(2) 0.069(2) -0.0092(17) -0.0011(18) 0.0183(17) O2 0.246(7) 0.053(3) 0.112(4) -0.017(3) 0.026(5) 0.009(4) O3 0.163(5) 0.050(2) 0.122(4) 0.014(3) 0.048(4) 0.022(3) N1 0.053(2) 0.055(3) 0.062(2) 0.0102(19) 0.014(2) 0.0105(19) N2 0.145(5) 0.047(3) 0.089(4) -0.002(3) 0.037(4) 0.003(3) C1 0.151(8) 0.062(5) 0.167(10) -0.034(5) 0.064(8) -0.024(5) C2 0.137(8) 0.079(6) 0.123(7) -0.002(5) -0.021(6) -0.051(6) C3 0.077(5) 0.080(6) 0.250(14) -0.004(8) 0.045(8) -0.027(4) C4 0.109(6) 0.100(6) 0.135(7) -0.003(5) 0.041(6) -0.038(5) C5 0.119(7) 0.060(4) 0.149(8) 0.022(5) 0.001(6) -0.013(4) C6 0.051(3) 0.049(3) 0.063(3) 0.000(2) 0.018(2) 0.003(2) C7 0.060(3) 0.054(3) 0.060(3) 0.007(2) 0.024(3) 0.009(2) C8 0.077(3) 0.048(3) 0.071(3) 0.011(2) 0.026(3) 0.012(2) C9 0.096(4) 0.046(3) 0.073(4) -0.003(3) 0.032(3) -0.001(3) C10 0.087(4) 0.049(3) 0.060(3) -0.006(2) 0.020(3) -0.004(3) C11 0.058(3) 0.046(3) 0.059(3) 0.002(2) 0.017(2) 0.004(2) C12 0.057(3) 0.058(3) 0.056(3) -0.003(2) 0.010(2) -0.003(2) C13 0.059(3) 0.058(3) 0.056(3) 0.011(2) 0.019(2) 0.008(2) C14 0.064(3) 0.085(4) 0.062(3) 0.001(3) 0.021(3) 0.007(3) C15 0.082(4) 0.105(5) 0.067(4) -0.010(3) 0.019(3) 0.000(4) C16 0.090(5) 0.104(5) 0.062(4) 0.002(3) 0.002(3) -0.006(4) C17 0.068(4) 0.089(5) 0.090(5) 0.013(4) -0.002(3) 0.015(3) C18 0.067(3) 0.067(4) 0.087(4) 0.009(3) 0.016(3) 0.017(3) C19 0.075(3) 0.065(3) 0.069(3) 0.010(3) 0.018(3) 0.019(3) C20 0.064(4) 0.125(7) 0.125(6) 0.017(5) -0.006(4) 0.010(4) C21 0.142(7) 0.118(6) 0.081(4) 0.042(4) 0.046(5) 0.043(5) C22 0.310(19) 0.157(11) 0.139(10) -0.024(7) 0.113(12) 0.000(10) _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 1.903(4) . ? Cr1 N1 2.013(4) . ? Cr1 C5 2.207(7) . ? Cr1 C3 2.207(7) . ? Cr1 C1 2.208(7) . ? Cr1 C2 2.213(7) . ? Cr1 C4 2.233(8) . ? Cr1 Cl1 2.3034(17) . ? Cl2 C22 1.813(14) . ? Cl3 C22 1.631(14) . ? O1 C6 1.294(6) . ? O2 N2 1.225(8) . ? O3 N2 1.220(7) . ? N1 C12 1.297(6) . ? N1 C19 1.500(7) . ? N2 C9 1.448(7) . ? C1 C2 1.371(14) . ? C1 C5 1.392(13) . ? C2 C3 1.408(14) . ? C3 C4 1.349(13) . ? C4 C5 1.339(12) . ? C6 C7 1.421(7) . ? C6 C11 1.434(7) . ? C7 C8 1.388(7) . ? C7 C13 1.485(7) . ? C8 C9 1.360(8) . ? C9 C10 1.386(8) . ? C10 C11 1.386(7) . ? C11 C12 1.444(7) . ? C13 C18 1.392(7) . ? C13 C14 1.393(7) . ? C14 C15 1.375(8) . ? C15 C16 1.377(9) . ? C16 C17 1.353(9) . ? C17 C18 1.365(8) . ? C19 C20 1.505(9) . ? C19 C21 1.539(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 O1 Cr1 N1 90.05(15) . . ? O1 Cr1 C5 151.5(3) . . ? N1 Cr1 C5 108.3(3) . . ? O1 Cr1 C3 93.7(3) . . ? N1 Cr1 C3 114.2(4) . . ? C5 Cr1 C3 59.2(4) . . ? O1 Cr1 C1 124.5(4) . . ? N1 Cr1 C1 144.4(4) . . ? C5 Cr1 C1 36.8(3) . . ? C3 Cr1 C1 60.7(4) . . ? O1 Cr1 C2 93.2(3) . . ? N1 Cr1 C2 151.3(4) . . ? C5 Cr1 C2 60.2(3) . . ? C3 Cr1 C2 37.2(4) . . ? C1 Cr1 C2 36.1(4) . . ? O1 Cr1 C4 124.6(3) . . ? N1 Cr1 C4 94.6(3) . . ? C5 Cr1 C4 35.1(3) . . ? C3 Cr1 C4 35.4(3) . . ? C1 Cr1 C4 60.4(4) . . ? C2 Cr1 C4 60.4(4) . . ? O1 Cr1 Cl1 97.05(13) . . ? N1 Cr1 Cl1 93.16(12) . . ? C5 Cr1 Cl1 103.3(3) . . ? C3 Cr1 Cl1 150.6(4) . . ? C1 Cr1 Cl1 90.9(3) . . ? C2 Cr1 Cl1 114.7(4) . . ? C4 Cr1 Cl1 137.5(3) . . ? C6 O1 Cr1 133.8(3) . . ? C12 N1 C19 116.4(4) . . ? C12 N1 Cr1 125.1(3) . . ? C19 N1 Cr1 118.4(3) . . ? O3 N2 O2 122.5(6) . . ? O3 N2 C9 118.6(6) . . ? O2 N2 C9 118.9(6) . . ? C2 C1 C5 106.7(9) . . ? C2 C1 Cr1 72.1(5) . . ? C5 C1 Cr1 71.6(4) . . ? C1 C2 C3 106.8(9) . . ? C1 C2 Cr1 71.7(5) . . ? C3 C2 Cr1 71.2(5) . . ? C4 C3 C2 108.5(9) . . ? C4 C3 Cr1 73.4(5) . . ? C2 C3 Cr1 71.7(5) . . ? C5 C4 C3 108.3(9) . . ? C5 C4 Cr1 71.4(5) . . ? C3 C4 Cr1 71.2(5) . . ? C4 C5 C1 109.7(9) . . ? C4 C5 Cr1 73.5(5) . . ? C1 C5 Cr1 71.7(4) . . ? O1 C6 C7 119.2(5) . . ? O1 C6 C11 121.4(4) . . ? C7 C6 C11 119.4(4) . . ? C8 C7 C6 118.1(5) . . ? C8 C7 C13 119.7(4) . . ? C6 C7 C13 122.2(4) . . ? C9 C8 C7 121.8(5) . . ? C8 C9 C10 121.7(5) . . ? C8 C9 N2 119.6(5) . . ? C10 C9 N2 118.8(6) . . ? C11 C10 C9 119.3(5) . . ? C10 C11 C6 119.7(5) . . ? C10 C11 C12 117.7(5) . . ? C6 C11 C12 122.5(4) . . ? N1 C12 C11 127.1(5) . . ? C18 C13 C14 116.9(5) . . ? C18 C13 C7 120.9(5) . . ? C14 C13 C7 122.2(4) . . ? C15 C14 C13 121.2(5) . . ? C14 C15 C16 119.5(6) . . ? C17 C16 C15 120.5(6) . . ? C16 C17 C18 120.1(6) . . ? C17 C18 C13 121.7(6) . . ? N1 C19 C20 111.9(5) . . ? N1 C19 C21 110.9(5) . . ? C20 C19 C21 111.1(6) . . ? Cl3 C22 Cl2 110.1(7) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.582 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.072