# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Sundermeyer, Jorg' _publ_contact_author_email jsu@staff.uni-marburg.de _publ_section_title ; Sulfinylamine Metathesis at Oxo Metal Species - Convenient Entry into Imido Metal Chemistry ; loop_ _publ_author_name J.Sundermeyer K.Rufanov J.Kipke # Attachment '- NSO.cif.txt' data_gotrif1 _database_code_depnum_ccdc_archive 'CCDC 155134' #TrackingRef '- NSO.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 Cl2 Cr F10 N2' _chemical_formula_weight 485.04 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.8629(8) _cell_length_b 15.2000(14) _cell_length_c 13.2641(14) _cell_angle_alpha 90.00 _cell_angle_beta 101.879(12) _cell_angle_gamma 90.00 _cell_volume 1551.3(1) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 4873 _cell_measurement_theta_min 2.06 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ? _diffrn_ambient_temperature 170(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 'Stoe IPDS' _diffrn_measurement_method Phi-scans _diffrn_detector_area_resol_mean 0.79 _diffrn_standards_number 200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no significant decay observed' _diffrn_reflns_number 10478 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2735 _reflns_number_gt 1846 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe Expose' _computing_cell_refinement 'Stoe Cell' _computing_data_reduction 'Stoe Integrate' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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 w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct_ _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'no hydrogen atoms in the molecule' _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2735 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0727 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.913 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.16653(7) 0.86344(4) 0.34122(4) 0.02415(14) Uani 1 d . . . Cl1 Cl 0.38679(12) 0.94970(6) 0.38940(7) 0.0413(2) Uani 1 d . . . Cl2 Cl 0.11951(14) 0.76079(6) 0.44477(7) 0.0428(2) Uani 1 d . . . N11 N -0.0091(3) 0.92421(18) 0.31922(19) 0.0266(6) Uani 1 d . . . C11 C -0.1624(4) 0.9606(2) 0.2692(2) 0.0226(7) Uani 1 d . . . C12 C -0.2211(4) 1.0404(2) 0.3030(2) 0.0279(8) Uani 1 d . . . F12 F -0.1231(3) 1.08071(14) 0.38335(16) 0.0429(5) Uani 1 d . . . C13 C -0.3785(5) 1.0754(2) 0.2574(3) 0.0338(8) Uani 1 d . . . F13 F -0.4320(3) 1.15041(15) 0.29189(19) 0.0542(6) Uani 1 d . . . C14 C -0.4813(4) 1.0321(2) 0.1755(3) 0.0353(9) Uani 1 d . . . F14 F -0.6382(3) 1.06318(15) 0.13312(19) 0.0535(6) Uani 1 d . . . C15 C -0.4267(4) 0.9538(2) 0.1404(3) 0.0303(8) Uani 1 d . . . F15 F -0.5305(3) 0.91247(15) 0.06098(15) 0.0434(5) Uani 1 d . . . C16 C -0.2711(4) 0.9190(2) 0.1855(2) 0.0264(7) Uani 1 d . . . F16 F -0.2208(3) 0.84175(13) 0.15280(15) 0.0364(5) Uani 1 d . . . N21 N 0.1985(4) 0.81545(19) 0.2357(2) 0.0290(6) Uani 1 d . . . C21 C 0.1757(4) 0.7932(2) 0.1340(2) 0.0256(7) Uani 1 d . . . C22 C 0.2365(4) 0.7112(2) 0.1063(2) 0.0258(7) Uani 1 d . . . F22 F 0.3082(3) 0.65559(13) 0.17972(14) 0.0376(5) Uani 1 d . . . C23 C 0.2234(4) 0.6895(2) 0.0044(3) 0.0293(8) Uani 1 d . . . F23 F 0.2827(3) 0.61181(13) -0.02100(15) 0.0392(5) Uani 1 d . . . C24 C 0.1506(4) 0.7482(2) -0.0719(2) 0.0293(8) Uani 1 d . . . F24 F 0.1421(3) 0.72804(15) -0.17066(14) 0.0440(5) Uani 1 d . . . C25 C 0.0896(4) 0.8288(2) -0.0466(2) 0.0293(8) Uani 1 d . . . F25 F 0.0226(3) 0.88552(14) -0.12131(14) 0.0445(6) Uani 1 d . . . C26 C 0.1015(4) 0.8505(2) 0.0547(2) 0.0259(7) Uani 1 d . . . F26 F 0.0456(3) 0.92921(13) 0.07888(14) 0.0383(5) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0278(3) 0.0257(3) 0.0189(2) -0.0021(2) 0.0047(2) 0.0026(2) Cl1 0.0348(5) 0.0419(6) 0.0450(5) -0.0086(4) 0.0026(4) -0.0061(4) Cl2 0.0640(6) 0.0334(5) 0.0350(5) 0.0081(4) 0.0193(4) 0.0079(5) N11 0.0288(15) 0.0271(15) 0.0253(14) 0.0004(12) 0.0089(12) -0.0011(13) C11 0.0236(16) 0.0216(17) 0.0244(16) 0.0040(13) 0.0088(13) -0.0004(14) C12 0.0288(18) 0.0275(19) 0.0284(17) -0.0031(15) 0.0084(14) -0.0050(15) F12 0.0413(12) 0.0420(13) 0.0454(12) -0.0199(10) 0.0088(10) -0.0011(10) C13 0.0340(19) 0.0203(18) 0.051(2) 0.0015(16) 0.0177(18) 0.0041(16) F13 0.0464(13) 0.0373(14) 0.0810(17) -0.0104(12) 0.0180(12) 0.0129(11) C14 0.0272(19) 0.033(2) 0.046(2) 0.0123(17) 0.0088(17) 0.0018(16) F14 0.0299(11) 0.0511(14) 0.0754(16) 0.0128(12) 0.0014(11) 0.0114(11) C15 0.0265(18) 0.035(2) 0.0282(18) 0.0062(16) 0.0020(14) -0.0078(16) F15 0.0330(11) 0.0537(14) 0.0387(11) -0.0017(10) -0.0034(9) -0.0095(10) C16 0.0312(19) 0.0229(19) 0.0275(17) 0.0008(14) 0.0116(15) -0.0015(15) F16 0.0398(11) 0.0313(12) 0.0383(11) -0.0090(9) 0.0089(9) -0.0002(9) N21 0.0337(15) 0.0305(16) 0.0243(15) -0.0040(12) 0.0095(12) -0.0016(13) C21 0.0258(17) 0.030(2) 0.0228(17) -0.0053(14) 0.0088(14) -0.0051(15) C22 0.0241(17) 0.0294(19) 0.0248(17) -0.0016(14) 0.0073(13) 0.0017(15) F22 0.0450(12) 0.0374(12) 0.0294(10) 0.0004(9) 0.0053(9) 0.0125(10) C23 0.0289(18) 0.030(2) 0.0306(19) -0.0086(16) 0.0110(15) 0.0002(16) F23 0.0446(12) 0.0380(12) 0.0375(11) -0.0118(9) 0.0142(9) 0.0069(10) C24 0.0310(18) 0.040(2) 0.0198(17) -0.0103(15) 0.0107(14) -0.0053(16) F24 0.0581(13) 0.0534(14) 0.0218(11) -0.0084(9) 0.0110(10) 0.0006(12) C25 0.0304(18) 0.034(2) 0.0243(18) 0.0071(15) 0.0083(14) -0.0026(16) F25 0.0615(14) 0.0441(13) 0.0275(11) 0.0078(9) 0.0081(10) 0.0048(11) C26 0.0266(17) 0.0242(19) 0.0283(18) -0.0031(14) 0.0086(14) -0.0021(15) F26 0.0558(13) 0.0253(11) 0.0356(11) -0.0018(9) 0.0133(10) 0.0043(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 N11 1.637(3) . ? Cr1 N21 1.643(3) . ? Cr1 Cl2 2.1604(11) . ? Cr1 Cl1 2.1613(11) . ? N11 C11 1.367(4) . ? C11 C16 1.404(4) . ? C11 C12 1.404(5) . ? C12 F12 1.329(4) . ? C12 C13 1.368(5) . ? C13 F13 1.328(4) . ? C13 C14 1.381(5) . ? C14 F14 1.333(4) . ? C14 C15 1.377(5) . ? C15 F15 1.348(4) . ? C15 C16 1.355(5) . ? C16 F16 1.339(4) . ? N21 C21 1.366(4) . ? C21 C26 1.398(5) . ? C21 C22 1.410(5) . ? C22 F22 1.324(4) . ? C22 C23 1.375(5) . ? C23 F23 1.338(4) . ? C23 C24 1.382(5) . ? C24 F24 1.334(4) . ? C24 C25 1.381(5) . ? C25 F25 1.337(4) . ? C25 C26 1.368(4) . ? C26 F26 1.336(4) . ? 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 N11 Cr1 N21 111.72(14) . . ? N11 Cr1 Cl2 105.81(10) . . ? N21 Cr1 Cl2 107.29(11) . . ? N11 Cr1 Cl1 107.80(10) . . ? N21 Cr1 Cl1 105.51(11) . . ? Cl2 Cr1 Cl1 118.80(5) . . ? C11 N11 Cr1 160.4(2) . . ? N11 C11 C16 122.3(3) . . ? N11 C11 C12 120.6(3) . . ? C16 C11 C12 117.1(3) . . ? F12 C12 C13 119.8(3) . . ? F12 C12 C11 118.7(3) . . ? C13 C12 C11 121.4(3) . . ? F13 C13 C12 120.2(3) . . ? F13 C13 C14 120.3(3) . . ? C12 C13 C14 119.5(3) . . ? F14 C14 C15 119.3(3) . . ? F14 C14 C13 120.3(3) . . ? C15 C14 C13 120.3(3) . . ? F15 C15 C16 120.6(3) . . ? F15 C15 C14 119.1(3) . . ? C16 C15 C14 120.3(3) . . ? F16 C16 C15 120.0(3) . . ? F16 C16 C11 118.6(3) . . ? C15 C16 C11 121.4(3) . . ? C21 N21 Cr1 159.9(3) . . ? N21 C21 C26 122.5(3) . . ? N21 C21 C22 119.6(3) . . ? C26 C21 C22 117.8(3) . . ? F22 C22 C23 120.3(3) . . ? F22 C22 C21 119.2(3) . . ? C23 C22 C21 120.5(3) . . ? F23 C23 C22 119.9(3) . . ? F23 C23 C24 120.0(3) . . ? C22 C23 C24 120.1(3) . . ? F24 C24 C25 119.5(3) . . ? F24 C24 C23 120.0(3) . . ? C25 C24 C23 120.5(3) . . ? F25 C25 C26 120.6(3) . . ? F25 C25 C24 119.7(3) . . ? C26 C25 C24 119.7(3) . . ? F26 C26 C25 119.5(3) . . ? F26 C26 C21 119.0(3) . . ? C25 C26 C21 121.5(3) . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 0.342 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.078 #================================================================ data_jk07 #TrackingRef '- NSO_cif.txt' _database_code_depnum_ccdc_archive 'CCDC 155135' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H4 Cl8 Cr N2' _chemical_formula_weight 511.77 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.2157(6) _cell_length_b 8.5808(5) _cell_length_c 14.6107(8) _cell_angle_alpha 90.00 _cell_angle_beta 96.439(5) _cell_angle_gamma 90.00 _cell_volume 1770.99(16) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 17.503 _cell_measurement_theta_max 20.451 _exptl_crystal_description QUADERFOERMIG _exptl_crystal_colour DUNKELROT _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.919 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 1.848 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6653 _exptl_absorpt_correction_T_max 0.8513 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(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 'Enraf Nonius CAD4' _diffrn_measurement_method Omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 1618 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 24.96 _reflns_number_total 1553 _reflns_number_gt 1401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens 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^)+(0.0375P)^2^+1.9004P] 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 refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1553 _refine_ls_number_parameters 105 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0651 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _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 0.5000 0.19792(5) 0.2500 0.02225(15) Uani 1 2 d S . . N1 N 0.48566(12) 0.3117(2) 0.33821(12) 0.0247(4) Uani 1 1 d . . . Cl1 Cl 0.30198(4) 0.32999(7) 0.40836(4) 0.03289(16) Uani 1 1 d . . . Cl2 Cl 0.38226(4) 0.93564(7) 0.45641(4) 0.03792(17) Uani 1 1 d . . . Cl3 Cl 0.64036(4) 0.55119(7) 0.33600(4) 0.03445(17) Uani 1 1 d . . . Cl4 Cl 0.63002(5) 0.06879(8) 0.28412(4) 0.04230(19) Uani 1 1 d . . . C1 C 0.46707(15) 0.4560(2) 0.37196(13) 0.0218(4) Uani 1 1 d . . . C2 C 0.37929(15) 0.4830(3) 0.40492(14) 0.0230(4) Uani 1 1 d . . . C3 C 0.35328(15) 0.6300(3) 0.43132(14) 0.0260(5) Uani 1 1 d . . . H3A H 0.2933 0.6474 0.4523 0.031 Uiso 1 1 calc R . . C4 C 0.41662(16) 0.7512(2) 0.42656(14) 0.0251(5) Uani 1 1 d . . . C5 C 0.50530(15) 0.7297(3) 0.39780(14) 0.0263(5) Uani 1 1 d . . . H5A H 0.5481 0.8145 0.3963 0.032 Uiso 1 1 calc R . . C6 C 0.52999(15) 0.5822(3) 0.37137(13) 0.0238(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0246(3) 0.0205(3) 0.0218(3) 0.000 0.00292(19) 0.000 N1 0.0216(9) 0.0276(10) 0.0247(9) -0.0020(7) 0.0022(7) -0.0008(7) Cl1 0.0266(3) 0.0277(3) 0.0458(3) 0.0005(2) 0.0102(2) -0.0069(2) Cl2 0.0415(4) 0.0259(3) 0.0465(4) -0.0078(2) 0.0055(3) 0.0027(2) Cl3 0.0213(3) 0.0447(4) 0.0385(3) -0.0124(3) 0.0086(2) -0.0083(2) Cl4 0.0420(4) 0.0462(4) 0.0385(3) 0.0084(3) 0.0040(3) 0.0202(3) C1 0.0229(11) 0.0245(11) 0.0173(9) -0.0011(8) -0.0011(8) -0.0010(8) C2 0.0215(10) 0.0256(11) 0.0217(10) 0.0014(9) 0.0025(8) -0.0048(9) C3 0.0236(11) 0.0294(11) 0.0256(11) 0.0000(9) 0.0055(9) 0.0009(9) C4 0.0303(12) 0.0236(11) 0.0209(10) -0.0016(9) 0.0005(8) 0.0024(9) C5 0.0286(12) 0.0274(12) 0.0224(10) -0.0006(9) 0.0002(8) -0.0074(9) C6 0.0203(11) 0.0315(11) 0.0195(10) -0.0011(9) 0.0020(8) -0.0034(9) _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 N1 1.6476(17) . ? Cr1 N1 1.6477(17) 2_655 ? Cr1 Cl4 2.1646(6) 2_655 ? Cr1 Cl4 2.1646(6) . ? N1 C1 1.370(3) . ? Cl1 C2 1.717(2) . ? Cl2 C4 1.727(2) . ? Cl3 C6 1.727(2) . ? C1 C6 1.405(3) . ? C1 C2 1.406(3) . ? C2 C3 1.381(3) . ? C3 C4 1.382(3) . ? C4 C5 1.385(3) . ? C5 C6 1.380(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 N1 Cr1 N1 107.33(13) . 2_655 ? N1 Cr1 Cl4 107.83(6) . 2_655 ? N1 Cr1 Cl4 107.49(6) 2_655 2_655 ? N1 Cr1 Cl4 107.49(6) . . ? N1 Cr1 Cl4 107.82(6) 2_655 . ? Cl4 Cr1 Cl4 118.42(4) 2_655 . ? C1 N1 Cr1 149.68(15) . . ? N1 C1 C6 123.09(19) . . ? N1 C1 C2 119.14(19) . . ? C6 C1 C2 117.69(19) . . ? C3 C2 C1 121.46(19) . . ? C3 C2 Cl1 119.86(16) . . ? C1 C2 Cl1 118.64(16) . . ? C2 C3 C4 118.5(2) . . ? C3 C4 C5 122.4(2) . . ? C3 C4 Cl2 118.20(17) . . ? C5 C4 Cl2 119.42(17) . . ? C6 C5 C4 118.4(2) . . ? C5 C6 C1 121.5(2) . . ? C5 C6 Cl3 119.56(17) . . ? C1 C6 Cl3 118.90(17) . . ? 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 N1 Cr1 N1 C1 15.1(3) 2_655 . . . ? Cl4 Cr1 N1 C1 -100.5(3) 2_655 . . . ? Cl4 Cr1 N1 C1 130.8(3) . . . . ? Cr1 N1 C1 C6 -68.6(4) . . . . ? Cr1 N1 C1 C2 108.2(3) . . . . ? N1 C1 C2 C3 -173.63(19) . . . . ? C6 C1 C2 C3 3.4(3) . . . . ? N1 C1 C2 Cl1 4.2(3) . . . . ? C6 C1 C2 Cl1 -178.82(15) . . . . ? C1 C2 C3 C4 -1.3(3) . . . . ? Cl1 C2 C3 C4 -179.13(16) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? C2 C3 C4 Cl2 178.11(16) . . . . ? C3 C4 C5 C6 1.3(3) . . . . ? Cl2 C4 C5 C6 -177.88(16) . . . . ? C4 C5 C6 C1 0.9(3) . . . . ? C4 C5 C6 Cl3 -179.50(15) . . . . ? N1 C1 C6 C5 173.73(19) . . . . ? C2 C1 C6 C5 -3.1(3) . . . . ? N1 C1 C6 Cl3 -5.9(3) . . . . ? C2 C1 C6 Cl3 177.26(15) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.96 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.296 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.076 #===END