# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guo-Xin Jin' _publ_contact_author_email GXJIN@FUDAN.EDU.CN _publ_section_title ; Half-Sandwich Chromium(III) Complexes Bearing ?-Ketoiminato and ?-Diketiminate Ligands as Catalysts for Ethylene Polymerization ; loop_ _publ_author_name 'Guo-Xin Jin' 'Yuan-Biao Huang' # Attachment 'cif of complex 1c.cif' data_f80517b _database_code_depnum_ccdc_archive 'CCDC 705206' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _choiety ? _chemical_formula_sum emical_formula_m _chemical_formula_weight 410.91 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.976(6) _cell_length_b 9.965(6) _cell_length_c 12.294(8) _cell_angle_alpha 83.284(9) _cell_angle_beta 81.187(9) _cell_angle_gamma 81.543(10) _cell_volume 1069.8(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 867 _cell_measurement_theta_min 2.316 _cell_measurement_theta_max 19.714 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.276 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 434 _exptl_absorpt_coefficient_mu 0.669 _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4472 _diffrn_reflns_av_R_equivalents 0.0749 _diffrn_reflns_av_sigmaI/netI 0.1635 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.01 _reflns_number_total 3714 _reflns_number_gt 1608 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0746P)^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 3714 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1221 _refine_ls_R_factor_gt 0.0551 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1341 _refine_ls_goodness_of_fit_ref 0.777 _refine_ls_restrained_S_all 0.777 _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 0.22990(10) 0.14392(8) 0.13630(7) 0.0504(3) Uani 1 1 d . . . Cl1 Cl 0.09980(19) -0.04139(14) 0.17502(13) 0.0820(6) Uani 1 1 d . . . N1 N 0.1426(4) 0.2295(4) 0.2795(3) 0.0380(10) Uani 1 1 d . . . O1 O 0.4012(4) 0.0527(3) 0.2043(3) 0.0553(10) Uani 1 1 d . . . C1 C 0.5148(6) -0.1115(5) 0.3375(5) 0.0700(17) Uani 1 1 d . . . H1A H 0.5036 -0.1916 0.3048 0.105 Uiso 1 1 calc R . . H1B H 0.5043 -0.1304 0.4165 0.105 Uiso 1 1 calc R . . H1C H 0.6134 -0.0849 0.3108 0.105 Uiso 1 1 calc R . . C2 C 0.3893(6) 0.0068(5) 0.3058(5) 0.0510(14) Uani 1 1 d . . . C3 C 0.2800(6) 0.0526(5) 0.3862(4) 0.0492(14) Uani 1 1 d . . . H3 H 0.2792 0.0048 0.4559 0.059 Uiso 1 1 calc R . . C4 C 0.1671(6) 0.1656(5) 0.3749(4) 0.0459(13) Uani 1 1 d . . . C5 C 0.0793(6) 0.2142(6) 0.4807(4) 0.0742(18) Uani 1 1 d . . . H5A H 0.0649 0.3120 0.4746 0.111 Uiso 1 1 calc R . . H5B H 0.1349 0.1799 0.5411 0.111 Uiso 1 1 calc R . . H5C H -0.0180 0.1815 0.4938 0.111 Uiso 1 1 calc R . . C6 C 0.0482(5) 0.3618(5) 0.2755(3) 0.0368(12) Uani 1 1 d . . . C7 C 0.1147(6) 0.4785(5) 0.2809(4) 0.0392(12) Uani 1 1 d . . . C8 C 0.0219(7) 0.6028(5) 0.2765(4) 0.0536(14) Uani 1 1 d . . . H8 H 0.0641 0.6821 0.2788 0.064 Uiso 1 1 calc R . . C9 C -0.1316(7) 0.6123(6) 0.2688(4) 0.0587(16) Uani 1 1 d . . . H9 H -0.1919 0.6966 0.2669 0.070 Uiso 1 1 calc R . . C10 C -0.1929(6) 0.4968(6) 0.2639(5) 0.0613(16) Uani 1 1 d . . . H10 H -0.2958 0.5034 0.2580 0.074 Uiso 1 1 calc R . . C11 C -0.1064(6) 0.3691(5) 0.2676(4) 0.0477(14) Uani 1 1 d . . . C12 C -0.1849(6) 0.2455(6) 0.2628(5) 0.0715(18) Uani 1 1 d . . . H12 H -0.1076 0.1650 0.2611 0.086 Uiso 1 1 calc R . . C13 C -0.3027(9) 0.2244(8) 0.3665(6) 0.122(3) Uani 1 1 d . . . H13A H -0.2522 0.2091 0.4311 0.183 Uiso 1 1 calc R . . H13B H -0.3523 0.1469 0.3612 0.183 Uiso 1 1 calc R . . H13C H -0.3768 0.3041 0.3718 0.183 Uiso 1 1 calc R . . C14 C -0.2658(8) 0.2538(7) 0.1612(6) 0.109(3) Uani 1 1 d . . . H14A H -0.3366 0.3359 0.1581 0.164 Uiso 1 1 calc R . . H14B H -0.3195 0.1763 0.1660 0.164 Uiso 1 1 calc R . . H14C H -0.1922 0.2544 0.0958 0.164 Uiso 1 1 calc R . . C15 C 0.2811(6) 0.4776(5) 0.2863(5) 0.0550(15) Uani 1 1 d . . . H15 H 0.3331 0.3861 0.2732 0.066 Uiso 1 1 calc R . . C16 C 0.3535(7) 0.5770(6) 0.2024(6) 0.093(2) Uani 1 1 d . . . H16A H 0.3269 0.5680 0.1312 0.139 Uiso 1 1 calc R . . H16B H 0.4620 0.5593 0.1999 0.139 Uiso 1 1 calc R . . H16C H 0.3183 0.6678 0.2221 0.139 Uiso 1 1 calc R . . C17 C 0.3048(7) 0.5066(8) 0.4009(6) 0.121(3) Uani 1 1 d . . . H17A H 0.4118 0.4968 0.4054 0.181 Uiso 1 1 calc R . . H17B H 0.2576 0.4434 0.4556 0.181 Uiso 1 1 calc R . . H17C H 0.2601 0.5979 0.4138 0.181 Uiso 1 1 calc R . . C18 C 0.1762(13) 0.3274(8) 0.0218(5) 0.093(3) Uani 1 1 d . . . H18 H 0.1113 0.4036 0.0447 0.111 Uiso 1 1 calc R . . C19 C 0.1369(11) 0.2168(14) -0.0192(7) 0.111(3) Uani 1 1 d . . . H19 H 0.0394 0.2024 -0.0277 0.133 Uiso 1 1 calc R . . C20 C 0.270(2) 0.1317(9) -0.0454(6) 0.129(5) Uani 1 1 d . . . H20 H 0.2774 0.0488 -0.0750 0.154 Uiso 1 1 calc R . . C21 C 0.3829(11) 0.1869(13) -0.0216(7) 0.105(3) Uani 1 1 d . . . H21 H 0.4846 0.1496 -0.0340 0.126 Uiso 1 1 calc R . . C22 C 0.3333(14) 0.3020(11) 0.0221(6) 0.098(2) Uani 1 1 d . . . H22 H 0.3924 0.3568 0.0486 0.118 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 0.0695(7) 0.0415(5) 0.0398(5) -0.0061(4) -0.0119(4) 0.0004(4) Cl1 0.1212(14) 0.0496(9) 0.0872(12) -0.0047(8) -0.0407(10) -0.0252(9) N1 0.040(3) 0.035(2) 0.039(2) -0.0049(19) -0.0097(19) -0.001(2) O1 0.059(2) 0.055(2) 0.045(2) -0.0069(18) -0.0034(18) 0.0146(19) C1 0.069(4) 0.055(4) 0.078(4) -0.004(3) -0.018(3) 0.022(3) C2 0.055(4) 0.046(3) 0.053(4) -0.009(3) -0.015(3) -0.001(3) C3 0.060(4) 0.048(3) 0.038(3) 0.002(3) -0.011(3) 0.001(3) C4 0.049(4) 0.047(3) 0.040(3) -0.007(3) -0.009(3) 0.004(3) C5 0.085(5) 0.090(5) 0.037(3) -0.004(3) -0.005(3) 0.018(4) C6 0.039(3) 0.040(3) 0.029(3) -0.003(2) -0.007(2) 0.003(3) C7 0.047(3) 0.031(3) 0.038(3) 0.000(2) -0.007(2) 0.001(3) C8 0.056(4) 0.041(3) 0.063(4) -0.009(3) 0.000(3) -0.006(3) C9 0.058(4) 0.051(4) 0.055(4) -0.003(3) 0.001(3) 0.020(3) C10 0.037(4) 0.072(4) 0.074(4) -0.012(3) -0.009(3) 0.000(3) C11 0.048(4) 0.043(3) 0.049(3) 0.007(3) -0.015(3) 0.003(3) C12 0.054(4) 0.065(4) 0.103(5) -0.013(4) -0.026(4) -0.013(3) C13 0.137(7) 0.128(7) 0.113(7) 0.021(5) -0.022(6) -0.077(6) C14 0.105(6) 0.126(6) 0.115(6) -0.038(5) -0.029(5) -0.041(5) C15 0.043(4) 0.042(3) 0.078(4) -0.008(3) -0.006(3) 0.001(3) C16 0.063(4) 0.078(5) 0.135(7) -0.008(4) -0.001(4) -0.018(4) C17 0.068(5) 0.192(8) 0.121(7) -0.077(6) -0.038(4) -0.003(5) C18 0.139(8) 0.072(6) 0.041(4) 0.005(3) 0.010(5) 0.040(6) C19 0.129(8) 0.165(9) 0.055(5) 0.026(6) -0.044(5) -0.066(7) C20 0.267(16) 0.072(6) 0.038(4) -0.013(4) -0.007(7) -0.005(9) C21 0.116(8) 0.111(9) 0.056(6) 0.028(5) 0.015(5) 0.029(7) C22 0.145(9) 0.095(7) 0.056(5) 0.020(5) -0.013(5) -0.046(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cr1 O1 1.922(3) . ? Cr1 N1 2.042(4) . ? Cr1 C22 2.197(7) . ? Cr1 C19 2.206(7) . ? Cr1 C18 2.214(6) . ? Cr1 C20 2.222(8) . ? Cr1 C21 2.236(8) . ? Cr1 Cl1 2.293(2) . ? N1 C4 1.301(6) . ? N1 C6 1.458(5) . ? O1 C2 1.272(6) . ? C1 C2 1.564(6) . ? C2 C3 1.350(6) . ? C3 C4 1.409(6) . ? C4 C5 1.506(7) . ? C6 C7 1.395(6) . ? C6 C11 1.397(6) . ? C7 C8 1.388(6) . ? C7 C15 1.504(7) . ? C8 C9 1.384(7) . ? C9 C10 1.358(7) . ? C10 C11 1.390(7) . ? C11 C12 1.518(7) . ? C12 C14 1.526(8) . ? C12 C13 1.541(9) . ? C15 C16 1.487(7) . ? C15 C17 1.522(8) . ? C18 C19 1.375(10) . ? C18 C22 1.397(10) . ? C19 C20 1.374(11) . ? C20 C21 1.310(12) . ? C21 C22 1.313(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 89.98(15) . . ? O1 Cr1 C22 101.7(3) . . ? N1 Cr1 C22 107.1(3) . . ? O1 Cr1 C19 146.9(4) . . ? N1 Cr1 C19 121.0(4) . . ? C22 Cr1 C19 60.4(3) . . ? O1 Cr1 C18 138.1(4) . . ? N1 Cr1 C18 96.8(2) . . ? C22 Cr1 C18 36.9(3) . . ? C19 Cr1 C18 36.3(3) . . ? O1 Cr1 C20 111.2(4) . . ? N1 Cr1 C20 155.8(3) . . ? C22 Cr1 C20 58.5(3) . . ? C19 Cr1 C20 36.2(3) . . ? C18 Cr1 C20 59.7(3) . . ? O1 Cr1 C21 90.3(3) . . ? N1 Cr1 C21 140.2(4) . . ? C22 Cr1 C21 34.4(3) . . ? C19 Cr1 C21 58.8(3) . . ? C18 Cr1 C21 59.0(3) . . ? C20 Cr1 C21 34.2(3) . . ? O1 Cr1 Cl1 93.25(12) . . ? N1 Cr1 Cl1 95.64(12) . . ? C22 Cr1 Cl1 152.6(2) . . ? C19 Cr1 Cl1 95.0(3) . . ? C18 Cr1 Cl1 126.8(4) . . ? C20 Cr1 Cl1 94.8(3) . . ? C21 Cr1 Cl1 124.1(4) . . ? C4 N1 C6 119.4(4) . . ? C4 N1 Cr1 120.7(3) . . ? C6 N1 Cr1 120.0(3) . . ? C2 O1 Cr1 122.4(3) . . ? O1 C2 C3 125.5(5) . . ? O1 C2 C1 115.7(5) . . ? C3 C2 C1 118.7(5) . . ? C2 C3 C4 126.5(5) . . ? N1 C4 C3 122.8(4) . . ? N1 C4 C5 120.9(4) . . ? C3 C4 C5 116.3(5) . . ? C7 C6 C11 121.4(4) . . ? C7 C6 N1 119.0(4) . . ? C11 C6 N1 119.6(4) . . ? C8 C7 C6 117.6(5) . . ? C8 C7 C15 118.5(5) . . ? C6 C7 C15 123.9(4) . . ? C9 C8 C7 122.0(5) . . ? C10 C9 C8 119.1(5) . . ? C9 C10 C11 121.9(5) . . ? C10 C11 C6 118.1(5) . . ? C10 C11 C12 118.3(5) . . ? C6 C11 C12 123.7(4) . . ? C11 C12 C14 113.6(5) . . ? C11 C12 C13 110.8(5) . . ? C14 C12 C13 108.1(5) . . ? C16 C15 C7 113.4(5) . . ? C16 C15 C17 108.9(5) . . ? C7 C15 C17 110.4(5) . . ? C19 C18 C22 106.0(7) . . ? C19 C18 Cr1 71.5(4) . . ? C22 C18 Cr1 70.9(4) . . ? C20 C19 C18 106.8(8) . . ? C20 C19 Cr1 72.6(5) . . ? C18 C19 Cr1 72.2(4) . . ? C21 C20 C19 108.6(9) . . ? C21 C20 Cr1 73.5(5) . . ? C19 C20 Cr1 71.3(4) . . ? C20 C21 C22 110.7(10) . . ? C20 C21 Cr1 72.3(6) . . ? C22 C21 Cr1 71.2(5) . . ? C21 C22 C18 107.8(9) . . ? C21 C22 Cr1 74.4(5) . . ? C18 C22 Cr1 72.2(4) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.365 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.068 # Attachment 'cif of complex 2.cif' data_f80521d _database_code_depnum_ccdc_archive 'CCDC 705207' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H22 Cl Cr N2' _chemical_formula_weight 401.87 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' 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 14.033(5) _cell_length_b 23.567(8) _cell_length_c 12.120(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.023(5) _cell_angle_gamma 90.00 _cell_volume 4008(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 918 _cell_measurement_theta_min 2.254 _cell_measurement_theta_max 18.983 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1672 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8708 _exptl_absorpt_correction_T_max 0.9323 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16489 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.1157 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7065 _reflns_number_gt 3525 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^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 7065 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 0.786 _refine_ls_restrained_S_all 0.786 _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 0.24357(4) 0.55020(2) 0.61694(5) 0.04882(19) Uani 1 1 d . . . Cl1 Cl 0.17583(7) 0.63098(4) 0.54175(9) 0.0638(3) Uani 1 1 d . . . N1 N 0.19515(19) 0.49476(11) 0.5051(2) 0.0455(8) Uani 1 1 d . . . N2 N 0.1361(2) 0.53130(13) 0.7181(3) 0.0502(8) Uani 1 1 d . . . C1 C 0.0974(3) 0.41774(16) 0.4267(3) 0.0679(12) Uani 1 1 d . . . H1A H 0.1416 0.4218 0.3668 0.102 Uiso 1 1 calc R . . H1B H 0.0339 0.4250 0.4007 0.102 Uiso 1 1 calc R . . H1C H 0.1009 0.3798 0.4555 0.102 Uiso 1 1 calc R . . C2 C 0.1219(3) 0.45927(15) 0.5162(3) 0.0501(10) Uani 1 1 d . . . C3 C 0.0637(3) 0.45867(16) 0.6085(4) 0.0563(11) Uani 1 1 d . . . H3A H 0.0139 0.4326 0.6066 0.068 Uiso 1 1 calc R . . C4 C 0.0692(3) 0.49121(17) 0.7022(3) 0.0531(10) Uani 1 1 d . . . C5 C -0.0064(3) 0.48225(18) 0.7894(3) 0.0771(13) Uani 1 1 d . . . H5A H 0.0048 0.5076 0.8501 0.116 Uiso 1 1 calc R . . H5B H -0.0040 0.4437 0.8150 0.116 Uiso 1 1 calc R . . H5C H -0.0681 0.4898 0.7583 0.116 Uiso 1 1 calc R . . C6 C 0.2525(2) 0.49191(15) 0.4077(3) 0.0461(10) Uani 1 1 d . . . C7 C 0.2560(3) 0.53833(15) 0.3376(3) 0.0517(10) Uani 1 1 d . . . H7A H 0.2168 0.5695 0.3501 0.062 Uiso 1 1 calc R . . C8 C 0.3177(3) 0.53821(18) 0.2496(3) 0.0629(12) Uani 1 1 d . . . H8A H 0.3205 0.5695 0.2031 0.075 Uiso 1 1 calc R . . C9 C 0.3753(3) 0.4921(2) 0.2298(4) 0.0688(13) Uani 1 1 d . . . H9A H 0.4168 0.4922 0.1700 0.083 Uiso 1 1 calc R . . C10 C 0.3715(3) 0.44610(17) 0.2985(4) 0.0643(12) Uani 1 1 d . . . H10A H 0.4100 0.4147 0.2849 0.077 Uiso 1 1 calc R . . C11 C 0.3109(3) 0.44611(15) 0.3876(3) 0.0546(10) Uani 1 1 d . . . H11A H 0.3093 0.4149 0.4346 0.066 Uiso 1 1 calc R . . C12 C 0.1351(3) 0.56294(19) 0.8173(4) 0.0584(11) Uani 1 1 d . . . C13 C 0.1692(3) 0.5392(2) 0.9141(4) 0.0852(15) Uani 1 1 d . . . H13A H 0.1910 0.5019 0.9137 0.102 Uiso 1 1 calc R . . C14 C 0.1715(4) 0.5698(4) 1.0110(5) 0.121(2) Uani 1 1 d . . . H14A H 0.1931 0.5531 1.0758 0.146 Uiso 1 1 calc R . . C15 C 0.1416(5) 0.6251(4) 1.0106(6) 0.125(3) Uani 1 1 d . . . H15A H 0.1444 0.6467 1.0749 0.150 Uiso 1 1 calc R . . C16 C 0.1073(4) 0.6486(3) 0.9146(6) 0.115(2) Uani 1 1 d . . . H16A H 0.0868 0.6861 0.9143 0.137 Uiso 1 1 calc R . . C17 C 0.1032(3) 0.6175(2) 0.8194(4) 0.0789(14) Uani 1 1 d . . . H17A H 0.0783 0.6337 0.7557 0.095 Uiso 1 1 calc R . . C18 C 0.3545(3) 0.5195(3) 0.7358(5) 0.0853(15) Uani 1 1 d . . . H18A H 0.3436 0.4938 0.7980 0.102 Uiso 1 1 calc R . . C19 C 0.3527(3) 0.5786(3) 0.7404(5) 0.0867(16) Uani 1 1 d . . . H19A H 0.3407 0.6017 0.8062 0.104 Uiso 1 1 calc R . . C20 C 0.3810(3) 0.5982(2) 0.6390(5) 0.0848(15) Uani 1 1 d . . . H20A H 0.3911 0.6382 0.6198 0.102 Uiso 1 1 calc R . . C21 C 0.3996(3) 0.5524(3) 0.5705(4) 0.0741(13) Uani 1 1 d . . . H21A H 0.4256 0.5542 0.4955 0.089 Uiso 1 1 calc R . . C22 C 0.3830(3) 0.5038(2) 0.6315(5) 0.0762(13) Uani 1 1 d . . . H22A H 0.3951 0.4649 0.6068 0.091 Uiso 1 1 calc R . . Cr2 Cr 0.67018(4) 0.71175(2) 0.21027(5) 0.04696(19) Uani 1 1 d . . . Cl2 Cl 0.69270(8) 0.65118(5) 0.35623(9) 0.0771(4) Uani 1 1 d . . . N3 N 0.5673(2) 0.66684(12) 0.1369(2) 0.0476(8) Uani 1 1 d . . . N4 N 0.76854(19) 0.67636(12) 0.1136(2) 0.0453(8) Uani 1 1 d . . . C23 C 0.4930(3) 0.59475(18) 0.0176(3) 0.0822(14) Uani 1 1 d . . . H23A H 0.4362 0.6092 0.0516 0.123 Uiso 1 1 calc R . . H23B H 0.4991 0.5550 0.0337 0.123 Uiso 1 1 calc R . . H23C H 0.4893 0.6001 -0.0608 0.123 Uiso 1 1 calc R . . C24 C 0.5791(3) 0.62624(16) 0.0626(3) 0.0503(10) Uani 1 1 d . . . C25 C 0.6669(3) 0.61042(15) 0.0206(3) 0.0521(10) Uani 1 1 d . . . H25A H 0.6666 0.5801 -0.0286 0.063 Uiso 1 1 calc R . . C26 C 0.7555(3) 0.63433(15) 0.0432(3) 0.0487(10) Uani 1 1 d . . . C27 C 0.8390(3) 0.61083(16) -0.0222(3) 0.0693(12) Uani 1 1 d . . . H27A H 0.8964 0.6300 -0.0006 0.104 Uiso 1 1 calc R . . H27B H 0.8281 0.6167 -0.0995 0.104 Uiso 1 1 calc R . . H27C H 0.8454 0.5710 -0.0077 0.104 Uiso 1 1 calc R . . C28 C 0.4739(3) 0.68080(16) 0.1765(4) 0.0569(11) Uani 1 1 d . . . C29 C 0.4121(3) 0.7135(2) 0.1130(4) 0.0839(14) Uani 1 1 d . . . H29A H 0.4288 0.7235 0.0414 0.101 Uiso 1 1 calc R . . C30 C 0.3254(4) 0.7310(2) 0.1569(6) 0.112(2) Uani 1 1 d . . . H30A H 0.2840 0.7531 0.1152 0.134 Uiso 1 1 calc R . . C31 C 0.3017(4) 0.7155(3) 0.2621(7) 0.120(2) Uani 1 1 d . . . H31A H 0.2438 0.7273 0.2913 0.144 Uiso 1 1 calc R . . C32 C 0.3612(4) 0.6830(2) 0.3251(5) 0.0939(17) Uani 1 1 d . . . H32A H 0.3438 0.6729 0.3966 0.113 Uiso 1 1 calc R . . C33 C 0.4479(3) 0.66515(17) 0.2815(4) 0.0667(12) Uani 1 1 d . . . H33A H 0.4884 0.6426 0.3236 0.080 Uiso 1 1 calc R . . C34 C 0.8640(3) 0.69716(16) 0.1313(3) 0.0531(10) Uani 1 1 d . . . C35 C 0.9141(3) 0.67850(18) 0.2228(4) 0.0692(12) Uani 1 1 d . . . H35A H 0.8888 0.6506 0.2685 0.083 Uiso 1 1 calc R . . C36 C 1.0028(3) 0.7022(2) 0.2452(4) 0.0892(16) Uani 1 1 d . . . H36A H 1.0376 0.6899 0.3059 0.107 Uiso 1 1 calc R . . C37 C 1.0388(3) 0.7437(2) 0.1779(5) 0.0962(18) Uani 1 1 d . . . H37A H 1.0971 0.7603 0.1948 0.115 Uiso 1 1 calc R . . C38 C 0.9897(3) 0.76102(19) 0.0858(5) 0.0815(15) Uani 1 1 d . . . H38A H 1.0156 0.7884 0.0394 0.098 Uiso 1 1 calc R . . C39 C 0.9027(3) 0.73772(17) 0.0627(4) 0.0671(12) Uani 1 1 d . . . H39A H 0.8693 0.7493 0.0003 0.080 Uiso 1 1 calc R . . C40 C 0.7428(3) 0.79329(16) 0.2545(4) 0.0693(13) Uani 1 1 d . . . H40A H 0.8104 0.7975 0.2732 0.083 Uiso 1 1 calc R . . C41 C 0.7041(3) 0.79928(15) 0.1503(4) 0.0641(12) Uani 1 1 d . . . H41A H 0.7397 0.8084 0.0831 0.077 Uiso 1 1 calc R . . C42 C 0.6058(3) 0.79503(15) 0.1582(4) 0.0663(12) Uani 1 1 d . . . H42A H 0.5601 0.8007 0.0980 0.080 Uiso 1 1 calc R . . C43 C 0.5835(3) 0.78626(16) 0.2682(5) 0.0742(14) Uani 1 1 d . . . H43A H 0.5191 0.7844 0.2992 0.089 Uiso 1 1 calc R . . C44 C 0.6694(4) 0.78507(16) 0.3294(4) 0.0754(13) Uani 1 1 d . . . H44A H 0.6754 0.7828 0.4098 0.091 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 0.0389(3) 0.0475(4) 0.0601(4) -0.0030(3) 0.0007(3) -0.0017(3) Cl1 0.0636(7) 0.0478(6) 0.0799(8) 0.0058(6) 0.0172(6) 0.0075(5) N1 0.0395(18) 0.0373(18) 0.060(2) 0.0060(16) -0.0025(16) -0.0033(15) N2 0.0451(19) 0.053(2) 0.053(2) 0.0049(17) -0.0022(16) 0.0042(16) C1 0.052(3) 0.055(3) 0.096(3) -0.009(3) -0.007(2) -0.013(2) C2 0.039(2) 0.039(2) 0.073(3) 0.006(2) -0.008(2) 0.0061(19) C3 0.042(2) 0.049(3) 0.077(3) 0.007(2) 0.000(2) -0.009(2) C4 0.040(2) 0.054(3) 0.065(3) 0.017(2) 0.000(2) 0.003(2) C5 0.056(3) 0.098(4) 0.077(3) 0.021(3) 0.013(2) -0.006(2) C6 0.047(2) 0.038(2) 0.053(3) -0.003(2) -0.004(2) -0.0047(19) C7 0.057(3) 0.042(2) 0.055(3) -0.001(2) -0.006(2) 0.000(2) C8 0.080(3) 0.057(3) 0.051(3) 0.005(2) -0.002(2) -0.012(3) C9 0.073(3) 0.068(3) 0.065(3) -0.018(3) 0.016(2) -0.013(3) C10 0.068(3) 0.052(3) 0.073(3) -0.010(3) 0.010(3) 0.005(2) C11 0.062(3) 0.038(2) 0.064(3) 0.000(2) 0.001(2) -0.001(2) C12 0.056(3) 0.067(3) 0.052(3) 0.003(3) 0.007(2) -0.006(2) C13 0.080(3) 0.107(4) 0.069(4) 0.015(3) 0.003(3) -0.009(3) C14 0.117(5) 0.187(7) 0.060(4) -0.002(5) 0.002(3) -0.043(5) C15 0.144(6) 0.165(7) 0.066(5) -0.044(5) 0.024(4) -0.051(6) C16 0.133(5) 0.116(5) 0.095(5) -0.032(5) 0.039(4) -0.012(4) C17 0.093(4) 0.082(4) 0.062(3) -0.011(3) 0.021(3) 0.004(3) C18 0.046(3) 0.128(5) 0.081(4) 0.026(4) -0.015(3) 0.006(3) C19 0.051(3) 0.116(5) 0.093(4) -0.046(4) -0.016(3) -0.005(3) C20 0.049(3) 0.085(4) 0.120(5) -0.008(4) -0.011(3) -0.024(3) C21 0.036(2) 0.102(4) 0.084(4) -0.012(4) 0.009(2) -0.007(3) C22 0.048(3) 0.075(4) 0.105(4) -0.011(4) -0.013(3) 0.012(3) Cr2 0.0563(4) 0.0370(4) 0.0476(4) -0.0019(3) -0.0021(3) -0.0045(3) Cl2 0.0978(9) 0.0767(8) 0.0569(7) 0.0191(6) -0.0039(6) 0.0014(7) N3 0.050(2) 0.048(2) 0.0443(19) -0.0031(17) 0.0067(16) -0.0080(16) N4 0.047(2) 0.0363(18) 0.052(2) 0.0000(16) -0.0001(16) -0.0050(15) C23 0.077(3) 0.088(3) 0.082(3) -0.030(3) 0.011(3) -0.039(3) C24 0.062(3) 0.043(2) 0.046(2) 0.002(2) 0.002(2) -0.015(2) C25 0.068(3) 0.039(2) 0.049(2) -0.006(2) 0.002(2) -0.009(2) C26 0.060(3) 0.037(2) 0.049(3) 0.009(2) 0.002(2) 0.002(2) C27 0.071(3) 0.055(3) 0.082(3) -0.005(2) 0.010(2) 0.003(2) C28 0.057(3) 0.049(3) 0.064(3) -0.004(2) 0.002(2) -0.013(2) C29 0.058(3) 0.093(4) 0.100(4) 0.004(3) -0.005(3) -0.009(3) C30 0.057(4) 0.121(5) 0.157(6) 0.006(5) -0.009(4) 0.006(3) C31 0.060(4) 0.131(6) 0.169(7) -0.011(5) 0.031(4) 0.001(4) C32 0.081(4) 0.097(4) 0.103(4) -0.011(4) 0.039(3) -0.022(3) C33 0.064(3) 0.063(3) 0.074(3) -0.006(3) 0.013(3) -0.011(2) C34 0.048(3) 0.042(2) 0.069(3) -0.007(2) 0.002(2) 0.001(2) C35 0.056(3) 0.067(3) 0.085(4) 0.001(3) -0.008(3) 0.004(2) C36 0.063(3) 0.105(4) 0.099(4) -0.020(4) -0.019(3) 0.012(3) C37 0.054(3) 0.092(4) 0.143(6) -0.033(4) -0.002(4) -0.010(3) C38 0.063(3) 0.060(3) 0.122(5) -0.004(3) 0.020(3) -0.011(3) C39 0.058(3) 0.056(3) 0.087(3) 0.003(3) 0.002(2) -0.008(2) C40 0.071(3) 0.042(3) 0.095(4) -0.021(3) -0.013(3) -0.014(2) C41 0.085(4) 0.028(2) 0.078(4) 0.002(2) 0.014(3) -0.006(2) C42 0.073(3) 0.035(2) 0.091(4) 0.003(2) -0.012(3) 0.005(2) C43 0.078(4) 0.046(3) 0.099(4) -0.018(3) 0.023(3) 0.001(2) C44 0.115(4) 0.050(3) 0.061(3) -0.019(2) -0.001(3) -0.005(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 Cr1 N2 1.995(3) . ? Cr1 N1 2.001(3) . ? Cr1 C18 2.241(4) . ? Cr1 C19 2.243(4) . ? Cr1 C22 2.248(4) . ? Cr1 C20 2.253(4) . ? Cr1 C21 2.262(4) . ? Cr1 Cl1 2.3145(13) . ? N1 C2 1.332(4) . ? N1 C6 1.430(4) . ? N2 C4 1.345(4) . ? N2 C12 1.415(5) . ? C1 C2 1.500(5) . ? C2 C3 1.386(5) . ? C3 C4 1.373(5) . ? C4 C5 1.513(5) . ? C6 C11 1.377(5) . ? C6 C7 1.386(5) . ? C7 C8 1.374(5) . ? C8 C9 1.376(5) . ? C9 C10 1.368(5) . ? C10 C11 1.374(5) . ? C12 C17 1.361(5) . ? C12 C13 1.385(5) . ? C13 C14 1.378(7) . ? C14 C15 1.371(8) . ? C15 C16 1.375(8) . ? C16 C17 1.369(6) . ? C18 C22 1.378(6) . ? C18 C19 1.393(6) . ? C19 C20 1.372(6) . ? C20 C21 1.387(6) . ? C21 C22 1.383(6) . ? Cr2 N4 1.994(3) . ? Cr2 N3 1.999(3) . ? Cr2 C41 2.238(4) . ? Cr2 C40 2.240(4) . ? Cr2 C43 2.249(4) . ? Cr2 C42 2.251(4) . ? Cr2 C44 2.252(4) . ? Cr2 Cl2 2.2948(13) . ? N3 C24 1.325(4) . ? N3 C28 1.434(4) . ? N4 C26 1.320(4) . ? N4 C34 1.443(4) . ? C23 C24 1.519(5) . ? C24 C25 1.383(5) . ? C25 C26 1.392(5) . ? C26 C27 1.520(5) . ? C28 C33 1.374(5) . ? C28 C29 1.391(5) . ? C29 C30 1.391(6) . ? C30 C31 1.367(7) . ? C31 C32 1.366(7) . ? C32 C33 1.393(6) . ? C34 C39 1.378(5) . ? C34 C35 1.384(5) . ? C35 C36 1.391(6) . ? C36 C37 1.370(6) . ? C37 C38 1.374(6) . ? C38 C39 1.368(5) . ? C40 C41 1.381(5) . ? C40 C44 1.388(5) . ? C41 C42 1.386(5) . ? C42 C43 1.385(5) . ? C43 C44 1.414(6) . ? 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 N2 Cr1 N1 90.80(13) . . ? N2 Cr1 C18 93.33(16) . . ? N1 Cr1 C18 117.4(2) . . ? N2 Cr1 C19 99.96(19) . . ? N1 Cr1 C19 151.41(17) . . ? C18 Cr1 C19 36.20(17) . . ? N2 Cr1 C22 120.11(18) . . ? N1 Cr1 C22 91.76(15) . . ? C18 Cr1 C22 35.74(15) . . ? C19 Cr1 C22 59.92(17) . . ? N2 Cr1 C20 133.4(2) . . ? N1 Cr1 C20 134.3(2) . . ? C18 Cr1 C20 59.39(19) . . ? C19 Cr1 C20 35.54(16) . . ? C22 Cr1 C20 59.32(17) . . ? N2 Cr1 C21 152.96(16) . . ? N1 Cr1 C21 100.08(16) . . ? C18 Cr1 C21 59.67(17) . . ? C19 Cr1 C21 59.88(17) . . ? C22 Cr1 C21 35.72(15) . . ? C20 Cr1 C21 35.77(15) . . ? N2 Cr1 Cl1 96.62(9) . . ? N1 Cr1 Cl1 97.53(9) . . ? C18 Cr1 Cl1 143.47(18) . . ? C19 Cr1 Cl1 107.31(18) . . ? C22 Cr1 Cl1 142.00(16) . . ? C20 Cr1 Cl1 89.14(14) . . ? C21 Cr1 Cl1 106.28(15) . . ? C2 N1 C6 119.2(3) . . ? C2 N1 Cr1 127.1(3) . . ? C6 N1 Cr1 113.5(2) . . ? C4 N2 C12 119.0(3) . . ? C4 N2 Cr1 126.6(3) . . ? C12 N2 Cr1 114.3(2) . . ? N1 C2 C3 122.9(4) . . ? N1 C2 C1 120.9(4) . . ? C3 C2 C1 116.2(3) . . ? C4 C3 C2 129.0(4) . . ? N2 C4 C3 123.4(4) . . ? N2 C4 C5 119.2(4) . . ? C3 C4 C5 117.4(4) . . ? C11 C6 C7 119.2(4) . . ? C11 C6 N1 121.2(3) . . ? C7 C6 N1 119.3(3) . . ? C8 C7 C6 119.8(4) . . ? C7 C8 C9 120.5(4) . . ? C10 C9 C8 119.8(4) . . ? C9 C10 C11 120.2(4) . . ? C10 C11 C6 120.5(4) . . ? C17 C12 C13 118.7(5) . . ? C17 C12 N2 121.1(4) . . ? C13 C12 N2 120.2(4) . . ? C14 C13 C12 121.2(6) . . ? C15 C14 C13 119.2(7) . . ? C14 C15 C16 119.5(7) . . ? C17 C16 C15 120.8(6) . . ? C12 C17 C16 120.5(5) . . ? C22 C18 C19 108.1(5) . . ? C22 C18 Cr1 72.4(3) . . ? C19 C18 Cr1 72.0(3) . . ? C20 C19 C18 107.2(5) . . ? C20 C19 Cr1 72.6(3) . . ? C18 C19 Cr1 71.8(3) . . ? C19 C20 C21 109.2(5) . . ? C19 C20 Cr1 71.8(3) . . ? C21 C20 Cr1 72.5(2) . . ? C22 C21 C20 107.0(5) . . ? C22 C21 Cr1 71.6(2) . . ? C20 C21 Cr1 71.7(2) . . ? C18 C22 C21 108.5(5) . . ? C18 C22 Cr1 71.8(3) . . ? C21 C22 Cr1 72.7(2) . . ? N4 Cr2 N3 90.99(12) . . ? N4 Cr2 C41 92.72(14) . . ? N3 Cr2 C41 119.81(16) . . ? N4 Cr2 C40 100.62(16) . . ? N3 Cr2 C40 152.77(15) . . ? C41 Cr2 C40 35.93(14) . . ? N4 Cr2 C43 152.23(15) . . ? N3 Cr2 C43 99.31(16) . . ? C41 Cr2 C43 59.78(15) . . ? C40 Cr2 C43 60.10(16) . . ? N4 Cr2 C42 118.54(16) . . ? N3 Cr2 C42 92.71(14) . . ? C41 Cr2 C42 35.96(13) . . ? C40 Cr2 C42 60.10(16) . . ? C43 Cr2 C42 35.87(14) . . ? N4 Cr2 C44 134.55(17) . . ? N3 Cr2 C44 133.45(17) . . ? C41 Cr2 C44 60.14(16) . . ? C40 Cr2 C44 35.99(14) . . ? C43 Cr2 C44 36.64(15) . . ? C42 Cr2 C44 60.56(16) . . ? N4 Cr2 Cl2 95.61(9) . . ? N3 Cr2 Cl2 96.47(9) . . ? C41 Cr2 Cl2 142.59(14) . . ? C40 Cr2 Cl2 106.67(14) . . ? C43 Cr2 Cl2 108.62(15) . . ? C42 Cr2 Cl2 144.46(13) . . ? C44 Cr2 Cl2 89.07(13) . . ? C24 N3 C28 120.6(3) . . ? C24 N3 Cr2 126.4(3) . . ? C28 N3 Cr2 112.9(2) . . ? C26 N4 C34 118.7(3) . . ? C26 N4 Cr2 126.7(2) . . ? C34 N4 Cr2 114.4(2) . . ? N3 C24 C25 123.8(3) . . ? N3 C24 C23 119.8(4) . . ? C25 C24 C23 116.4(4) . . ? C24 C25 C26 127.9(4) . . ? N4 C26 C25 123.6(3) . . ? N4 C26 C27 120.2(3) . . ? C25 C26 C27 116.1(3) . . ? C33 C28 C29 119.7(4) . . ? C33 C28 N3 119.4(4) . . ? C29 C28 N3 120.7(4) . . ? C28 C29 C30 119.8(5) . . ? C31 C30 C29 119.4(6) . . ? C32 C31 C30 121.5(6) . . ? C31 C32 C33 119.4(5) . . ? C28 C33 C32 120.1(5) . . ? C39 C34 C35 120.3(4) . . ? C39 C34 N4 120.8(4) . . ? C35 C34 N4 118.8(4) . . ? C34 C35 C36 118.9(4) . . ? C37 C36 C35 120.0(5) . . ? C36 C37 C38 120.8(5) . . ? C39 C38 C37 119.6(5) . . ? C38 C39 C34 120.4(4) . . ? C41 C40 C44 108.7(4) . . ? C41 C40 Cr2 72.0(2) . . ? C44 C40 Cr2 72.5(2) . . ? C40 C41 C42 108.7(4) . . ? C40 C41 Cr2 72.1(2) . . ? C42 C41 Cr2 72.5(2) . . ? C43 C42 C41 107.6(4) . . ? C43 C42 Cr2 72.0(2) . . ? C41 C42 Cr2 71.5(2) . . ? C42 C43 C44 108.4(4) . . ? C42 C43 Cr2 72.1(2) . . ? C44 C43 Cr2 71.8(2) . . ? C40 C44 C43 106.7(4) . . ? C40 C44 Cr2 71.6(2) . . ? C43 C44 Cr2 71.6(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.298 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.064