# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email a.white@imperial.ac.uk _publ_contact_author_name 'Andrew J.P. White' loop_ _publ_author_name G.Britovsek J.Nobbs A.Tomov V.Gibson A.White R.Cariou data_L1 _database_code_depnum_ccdc_archive 'CCDC 859231' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H19 N3 S2' _chemical_formula_sum 'C23 H19 N3 S2' _chemical_formula_weight 401.53 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 5.5776(3) _cell_length_b 7.5976(4) _cell_length_c 22.5774(13) _cell_angle_alpha 90 _cell_angle_beta 92.097(5) _cell_angle_gamma 90 _cell_volume 956.11(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2667 _cell_measurement_theta_min 3.8111 _cell_measurement_theta_max 32.0458 _exptl_crystal_description plates _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 420 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.85709 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7167 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 32.13 _reflns_number_total 2970 _reflns_number_gt 1730 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0389 _refine_ls_wR_factor_obs+ 0.0761 _refine_ls_abs_structure_Flack+ 0.07(7) _refine_ls_R_factor_obs- 0.0396 _refine_ls_wR_factor_obs- 0.0785 _refine_ls_abs_structure_Flack- 0.93(7) ; _chemical_absolute_configuration ad _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^)+(0.0356P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 1286 Friedel pairs' _refine_ls_abs_structure_Flack 0.07(7) _refine_ls_number_reflns 2970 _refine_ls_number_parameters 128 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0816 _refine_ls_wR_factor_gt 0.0761 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.897 _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 N1 N 1.0000 0.1854(3) 0.5000 0.0232(5) Uani 1 2 d S . . C2 C 0.8311(4) 0.0942(3) 0.46995(9) 0.0232(5) Uani 1 1 d . . . C3 C 0.8216(3) -0.0894(3) 0.46926(8) 0.0262(5) Uani 1 1 d . . . H3A H 0.6957 -0.1494 0.4482 0.031 Uiso 1 1 calc R . . C4 C 1.0000 -0.1819(4) 0.5000 0.0309(7) Uani 1 2 d S . . H4A H 1.0000 -0.3070 0.5000 0.037 Uiso 1 2 calc SR . . C7 C 0.6526(3) 0.2003(2) 0.43556(9) 0.0219(5) Uani 1 1 d . . . N7 N 0.4783(3) 0.1321(2) 0.40571(7) 0.0247(4) Uani 1 1 d . . . S8 S 0.69269(9) 0.42997(7) 0.43302(2) 0.02976(14) Uani 1 1 d . . . C9 C 0.3982(3) 0.4469(3) 0.39731(8) 0.0284(5) Uani 1 1 d . . . H9A H 0.2761 0.4748 0.4266 0.034 Uiso 1 1 calc R . . H9B H 0.3955 0.5401 0.3666 0.034 Uiso 1 1 calc R . . C10 C 0.3494(3) 0.2654(3) 0.36909(9) 0.0260(5) Uani 1 1 d . . . H10A H 0.1735 0.2408 0.3700 0.031 Uiso 1 1 calc R . . C11 C 0.4251(3) 0.2542(3) 0.30552(8) 0.0216(4) Uani 1 1 d . . . C12 C 0.6359(3) 0.1728(3) 0.28930(9) 0.0261(5) Uani 1 1 d . . . H12A H 0.7384 0.1203 0.3188 0.031 Uiso 1 1 calc R . . C13 C 0.6981(4) 0.1673(3) 0.23063(9) 0.0310(5) Uani 1 1 d . . . H13A H 0.8415 0.1097 0.2200 0.037 Uiso 1 1 calc R . . C14 C 0.5527(4) 0.2452(3) 0.18737(10) 0.0328(5) Uani 1 1 d . . . H14A H 0.5961 0.2414 0.1471 0.039 Uiso 1 1 calc R . . C15 C 0.3440(4) 0.3287(3) 0.20276(9) 0.0304(5) Uani 1 1 d . . . H15A H 0.2439 0.3830 0.1731 0.036 Uiso 1 1 calc R . . C16 C 0.2809(4) 0.3333(3) 0.26170(9) 0.0257(4) Uani 1 1 d . . . H16A H 0.1375 0.3911 0.2721 0.031 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 N1 0.0219(12) 0.0281(14) 0.0197(13) 0.000 0.0013(10) 0.000 C2 0.0265(11) 0.0270(13) 0.0160(10) -0.0016(8) -0.0026(9) 0.0026(9) C3 0.0302(11) 0.0280(14) 0.0200(10) -0.0029(11) -0.0042(8) -0.0037(11) C4 0.0453(19) 0.0200(15) 0.0268(15) 0.000 -0.0080(14) 0.000 C7 0.0297(12) 0.0209(11) 0.0152(10) 0.0006(8) 0.0039(9) 0.0006(8) N7 0.0231(9) 0.0300(10) 0.0206(10) 0.0034(7) -0.0030(7) -0.0038(7) S8 0.0329(3) 0.0242(2) 0.0317(3) -0.0024(3) -0.0054(2) 0.0002(3) C9 0.0298(10) 0.0334(13) 0.0218(10) -0.0017(11) -0.0025(8) 0.0128(11) C10 0.0205(10) 0.0349(13) 0.0225(10) 0.0003(9) -0.0016(8) 0.0012(9) C11 0.0200(10) 0.0211(10) 0.0236(10) 0.0006(8) -0.0024(8) -0.0037(8) C12 0.0249(11) 0.0248(11) 0.0283(12) -0.0018(9) -0.0035(9) -0.0008(9) C13 0.0293(12) 0.0313(12) 0.0325(13) -0.0065(11) 0.0056(9) -0.0038(10) C14 0.0456(14) 0.0295(12) 0.0237(11) -0.0020(9) 0.0051(10) -0.0106(11) C15 0.0397(12) 0.0231(11) 0.0277(11) 0.0014(10) -0.0091(10) 0.0015(10) C16 0.0287(10) 0.0225(10) 0.0254(10) -0.0033(9) -0.0056(8) 0.0038(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 N1 C2 1.335(2) . ? N1 C2 1.335(2) 2_756 ? C2 C3 1.396(3) . ? C2 C7 1.479(3) . ? C3 C4 1.384(3) . ? C4 C3 1.384(3) 2_756 ? C7 N7 1.272(3) . ? C7 S8 1.761(2) . ? N7 C10 1.477(2) . ? S8 C9 1.8078(19) . ? C9 C10 1.539(3) . ? C10 C11 1.513(3) . ? C11 C16 1.389(3) . ? C11 C12 1.390(3) . ? C12 C13 1.382(3) . ? C13 C14 1.380(3) . ? C14 C15 1.381(3) . ? C15 C16 1.389(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 C2 N1 C2 117.4(3) . 2_756 ? N1 C2 C3 123.4(2) . . ? N1 C2 C7 115.64(19) . . ? C3 C2 C7 120.95(18) . . ? C4 C3 C2 118.4(2) . . ? C3 C4 C3 119.0(3) 2_756 . ? N7 C7 C2 122.86(18) . . ? N7 C7 S8 118.79(16) . . ? C2 C7 S8 118.26(15) . . ? C7 N7 C10 111.34(16) . . ? C7 S8 C9 88.33(11) . . ? C10 C9 S8 105.34(14) . . ? N7 C10 C11 110.20(16) . . ? N7 C10 C9 107.93(16) . . ? C11 C10 C9 113.08(17) . . ? C16 C11 C12 118.59(18) . . ? C16 C11 C10 118.50(17) . . ? C12 C11 C10 122.89(17) . . ? C13 C12 C11 120.69(19) . . ? C14 C13 C12 120.3(2) . . ? C13 C14 C15 119.9(2) . . ? C14 C15 C16 119.9(2) . . ? C11 C16 C15 120.7(2) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.454 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.056 #===END data_[Cr(L2)Cl3] _database_code_depnum_ccdc_archive 'CCDC 859232' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H27 Cl3 Cr N3 S2, C H2 Cl2' _chemical_formula_sum 'C20 H29 Cl5 Cr N3 S2' _chemical_formula_weight 604.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr -0.1635 2.4439 '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(1) 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' _cell_length_a 10.16474(7) _cell_length_b 16.10208(9) _cell_length_c 16.90466(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2766.84(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15504 _cell_measurement_theta_min 2.6102 _cell_measurement_theta_max 71.2486 _exptl_crystal_description plates _exptl_crystal_colour Green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 9.365 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65109 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40641 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 71.37 _reflns_number_total 5359 _reflns_number_gt 4425 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0280 _refine_ls_wR_factor_obs+ 0.0577 _refine_ls_abs_structure_Flack+ 0.000(5) _refine_ls_R_factor_obs- 0.0782 _refine_ls_wR_factor_obs- 0.1787 _refine_ls_abs_structure_Flack- *** ; _chemical_absolute_configuration ad _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^)+(0.0329P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2321 Friedel pairs' _refine_ls_abs_structure_Flack -0.011(5) _refine_ls_number_reflns 5359 _refine_ls_number_parameters 307 _refine_ls_number_restraints 46 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0577 _refine_ls_goodness_of_fit_ref 0.933 _refine_ls_restrained_S_all 0.945 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr Cr 0.66445(5) 0.43214(2) 0.32252(2) 0.02328(10) Uani 1 1 d . . . Cl1 Cl 0.50426(7) 0.34461(4) 0.37449(4) 0.03308(16) Uani 1 1 d . . . Cl2 Cl 0.67125(8) 0.36013(4) 0.20641(4) 0.03324(15) Uani 1 1 d . . . Cl3 Cl 0.81834(7) 0.52916(4) 0.28126(4) 0.03487(16) Uani 1 1 d . . . N1 N 0.6540(2) 0.49034(13) 0.42766(12) 0.0280(5) Uani 1 1 d . . . C2 C 0.5724(3) 0.55396(17) 0.43619(17) 0.0338(7) Uani 1 1 d . . . C3 C 0.5495(3) 0.58938(19) 0.50998(17) 0.0447(8) Uani 1 1 d . . . H3A H 0.4916 0.6353 0.5160 0.054 Uiso 1 1 calc R . . C4 C 0.6140(3) 0.5554(2) 0.57431(18) 0.0463(8) Uani 1 1 d . . . H4A H 0.5994 0.5779 0.6255 0.056 Uiso 1 1 calc R . . C5 C 0.6994(3) 0.48941(18) 0.56538(16) 0.0387(8) Uani 1 1 d . . . H5A H 0.7436 0.4662 0.6097 0.046 Uiso 1 1 calc R . . C6 C 0.7191(3) 0.45770(17) 0.48964(16) 0.0316(7) Uani 1 1 d . . . C7 C 0.5167(3) 0.57880(16) 0.35938(16) 0.0323(6) Uani 1 1 d . . . N7 N 0.5262(2) 0.52846(13) 0.30097(12) 0.0279(5) Uani 1 1 d . . . S8 S 0.45635(9) 0.67803(5) 0.34370(5) 0.0468(2) Uani 1 1 d . . . C9 C 0.4716(3) 0.65903(19) 0.23800(17) 0.0451(8) Uani 1 1 d . . . H9A H 0.3967 0.6842 0.2093 0.054 Uiso 1 1 calc R . . H9B H 0.5542 0.6836 0.2176 0.054 Uiso 1 1 calc R . . C10 C 0.4724(3) 0.56418(18) 0.22618(15) 0.0344(7) Uani 1 1 d . . . H10A H 0.5363 0.5514 0.1829 0.041 Uiso 1 1 calc R . . C11 C 0.3382(3) 0.52580(19) 0.20273(17) 0.0430(7) Uani 1 1 d . . . C12 C 0.2295(3) 0.5471(2) 0.2611(2) 0.0590(10) Uani 1 1 d . . . H12A H 0.1467 0.5220 0.2434 0.089 Uiso 1 1 calc R . . H12B H 0.2192 0.6075 0.2640 0.089 Uiso 1 1 calc R . . H12C H 0.2524 0.5254 0.3135 0.089 Uiso 1 1 calc R . . C13 C 0.3027(4) 0.5611(2) 0.12050(19) 0.0608(10) Uani 1 1 d . . . H13A H 0.2166 0.5397 0.1042 0.091 Uiso 1 1 calc R . . H13B H 0.3695 0.5442 0.0820 0.091 Uiso 1 1 calc R . . H13C H 0.2993 0.6219 0.1232 0.091 Uiso 1 1 calc R . . C14 C 0.3490(3) 0.4312(2) 0.19362(17) 0.0463(8) Uani 1 1 d . . . H14A H 0.2626 0.4083 0.1799 0.070 Uiso 1 1 calc R . . H14B H 0.3792 0.4068 0.2435 0.070 Uiso 1 1 calc R . . H14C H 0.4120 0.4181 0.1516 0.070 Uiso 1 1 calc R . . C17 C 0.7958(3) 0.38535(16) 0.46668(15) 0.0287(6) Uani 1 1 d . . . N17 N 0.8020(2) 0.36447(13) 0.39279(12) 0.0264(5) Uani 1 1 d . . . S18 S 0.86654(8) 0.32032(5) 0.53654(4) 0.03679(18) Uani 1 1 d . . . C19 C 0.8814(3) 0.24120(17) 0.46078(15) 0.0381(7) Uani 1 1 d . . . H19A H 0.9657 0.2110 0.4666 0.046 Uiso 1 1 calc R . . H19B H 0.8085 0.2007 0.4652 0.046 Uiso 1 1 calc R . . C20 C 0.8761(3) 0.28581(16) 0.37948(15) 0.0273(6) Uani 1 1 d . . . H20A H 0.8224 0.2505 0.3431 0.033 Uiso 1 1 calc R . . C21 C 1.0131(3) 0.29734(17) 0.34105(17) 0.0358(7) Uani 1 1 d . . . C22 C 1.0716(3) 0.21069(19) 0.3266(2) 0.0467(8) Uani 1 1 d . . . H22A H 1.0110 0.1780 0.2940 0.070 Uiso 1 1 calc R . . H22B H 1.0852 0.1827 0.3774 0.070 Uiso 1 1 calc R . . H22C H 1.1561 0.2162 0.2992 0.070 Uiso 1 1 calc R . . C23 C 1.1051(3) 0.3494(2) 0.3923(2) 0.0506(9) Uani 1 1 d . . . H23A H 1.0663 0.4044 0.4010 0.076 Uiso 1 1 calc R . . H23B H 1.1901 0.3555 0.3656 0.076 Uiso 1 1 calc R . . H23C H 1.1181 0.3217 0.4434 0.076 Uiso 1 1 calc R . . C24 C 0.9989(3) 0.3378(2) 0.25975(17) 0.0444(8) Uani 1 1 d . . . H24A H 0.9622 0.3938 0.2659 0.067 Uiso 1 1 calc R . . H24B H 0.9399 0.3043 0.2268 0.067 Uiso 1 1 calc R . . H24C H 1.0854 0.3414 0.2344 0.067 Uiso 1 1 calc R . . C30 C 0.9314(9) 0.6471(6) 0.4737(7) 0.110(4) Uani 0.549(3) 1 d PDU A 1 H30A H 0.9243 0.6403 0.5318 0.133 Uiso 0.549(3) 1 calc PR A 1 H30B H 0.9092 0.5934 0.4483 0.133 Uiso 0.549(3) 1 calc PR A 1 Cl4 Cl 0.8209(6) 0.7268(4) 0.4403(6) 0.152(3) Uani 0.549(3) 1 d PDU A 1 Cl5 Cl 1.0889(3) 0.6766(2) 0.4483(2) 0.1495(16) Uani 0.549(3) 1 d PD A 1 C30' C 0.9857(16) 0.6666(12) 0.4067(9) 0.065(4) Uiso 0.275(7) 1 d PDU B 2 H30C H 1.0573 0.7073 0.3983 0.078 Uiso 0.275(7) 1 calc PR B 2 H30D H 0.9714 0.6365 0.3564 0.078 Uiso 0.275(7) 1 calc PR B 2 Cl4' Cl 0.8426(12) 0.7190(8) 0.4324(8) 0.097(3) Uiso 0.275(7) 1 d PDU B 2 Cl5' Cl 1.0331(10) 0.5958(4) 0.4800(4) 0.119(3) Uiso 0.275(7) 1 d PDU B 2 C30" C 1.015(2) 0.6529(19) 0.4094(13) 0.062(6) Uiso 0.176(7) 1 d PDU C 3 H30E H 0.9845 0.6202 0.3634 0.075 Uiso 0.176(7) 1 calc PR C 3 H30F H 1.0691 0.6997 0.3894 0.075 Uiso 0.176(7) 1 calc PR C 3 Cl4" Cl 0.8795(14) 0.6916(9) 0.4617(10) 0.124(4) Uiso 0.176(7) 1 d PDU C 3 Cl5" Cl 1.1117(15) 0.5901(7) 0.4704(6) 0.116(4) Uiso 0.176(7) 1 d PDU C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.0307(2) 0.01963(19) 0.01952(19) 0.00200(16) -0.00080(19) -0.00013(19) Cl1 0.0379(4) 0.0304(3) 0.0309(3) 0.0071(3) 0.0047(3) -0.0050(3) Cl2 0.0404(4) 0.0333(3) 0.0260(3) -0.0058(3) 0.0012(3) -0.0050(3) Cl3 0.0407(4) 0.0267(3) 0.0371(4) 0.0030(3) 0.0008(3) -0.0078(3) N1 0.0345(13) 0.0272(11) 0.0222(10) 0.0003(9) -0.0025(11) 0.0015(11) C2 0.0384(17) 0.0270(16) 0.0361(16) 0.0010(12) -0.0022(13) 0.0021(13) C3 0.056(2) 0.0376(17) 0.0408(17) -0.0143(14) -0.0022(16) 0.0165(15) C4 0.055(2) 0.051(2) 0.0321(16) -0.0141(15) -0.0051(15) 0.0096(16) C5 0.050(2) 0.0418(17) 0.0245(15) -0.0065(12) -0.0089(13) 0.0006(15) C6 0.0391(17) 0.0302(15) 0.0255(14) -0.0002(11) -0.0034(12) -0.0024(13) C7 0.0370(16) 0.0269(14) 0.0330(15) 0.0023(12) 0.0048(13) 0.0026(13) N7 0.0281(13) 0.0257(11) 0.0299(12) 0.0064(9) -0.0010(10) 0.0028(10) S8 0.0646(6) 0.0285(4) 0.0473(5) 0.0016(3) -0.0035(4) 0.0154(4) C9 0.052(2) 0.0400(17) 0.0430(18) 0.0133(14) 0.0002(15) 0.0079(16) C10 0.0406(17) 0.0364(15) 0.0262(14) 0.0096(12) -0.0013(12) 0.0040(14) C11 0.0406(18) 0.0498(18) 0.0386(16) 0.0070(13) -0.0086(15) 0.0041(17) C12 0.0359(19) 0.074(3) 0.068(2) -0.004(2) 0.0035(17) 0.0032(19) C13 0.067(3) 0.062(2) 0.054(2) 0.0126(18) -0.0251(19) 0.009(2) C14 0.0425(18) 0.0511(18) 0.0454(19) 0.0050(15) -0.0082(16) -0.0061(17) C17 0.0319(16) 0.0296(14) 0.0247(14) 0.0031(11) -0.0044(12) -0.0026(12) N17 0.0294(13) 0.0280(11) 0.0217(11) 0.0049(9) -0.0016(9) -0.0004(10) S18 0.0511(5) 0.0349(4) 0.0243(3) 0.0029(3) -0.0082(3) 0.0065(3) C19 0.054(2) 0.0290(15) 0.0316(15) 0.0022(12) -0.0041(14) 0.0078(14) C20 0.0331(16) 0.0246(13) 0.0242(13) -0.0009(11) -0.0067(12) 0.0023(11) C21 0.0350(16) 0.0333(15) 0.0392(16) -0.0001(12) 0.0002(14) 0.0034(13) C22 0.0433(19) 0.0455(19) 0.0511(19) -0.0016(16) -0.0016(17) 0.0161(15) C23 0.0391(19) 0.051(2) 0.061(2) -0.0059(17) -0.0014(16) -0.0029(16) C24 0.0407(17) 0.053(2) 0.0395(17) 0.0059(15) 0.0133(14) 0.0083(16) C30 0.117(8) 0.075(6) 0.139(8) -0.018(6) 0.021(7) -0.012(6) Cl4 0.158(5) 0.106(3) 0.192(5) -0.011(3) -0.046(4) -0.075(3) Cl5 0.134(3) 0.127(3) 0.187(3) -0.052(2) -0.005(2) -0.017(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 Cr N1 2.012(2) . ? Cr N7 2.124(2) . ? Cr N17 2.134(2) . ? Cr Cl2 2.2808(7) . ? Cr Cl3 2.3181(8) . ? Cr Cl1 2.3259(8) . ? N1 C2 1.326(3) . ? N1 C6 1.346(3) . ? C2 C3 1.391(4) . ? C2 C7 1.472(4) . ? C3 C4 1.383(4) . ? C4 C5 1.381(4) . ? C5 C6 1.393(4) . ? C6 C17 1.455(4) . ? C7 N7 1.281(3) . ? C7 S8 1.732(3) . ? N7 C10 1.493(3) . ? S8 C9 1.819(3) . ? C9 C10 1.540(4) . ? C10 C11 1.549(4) . ? C11 C12 1.521(4) . ? C11 C14 1.535(4) . ? C11 C13 1.545(4) . ? C17 N17 1.295(3) . ? C17 S18 1.734(3) . ? N17 C20 1.491(3) . ? S18 C19 1.813(3) . ? C19 C20 1.552(3) . ? C20 C21 1.548(4) . ? C21 C23 1.526(4) . ? C21 C24 1.528(4) . ? C21 C22 1.537(4) . ? C30 Cl5 1.725(9) . ? C30 Cl4 1.798(10) . ? C30' Cl4' 1.737(12) . ? C30' Cl5' 1.752(11) . ? C30" Cl5" 1.744(14) . ? C30" Cl4" 1.755(14) . ? 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 Cr N7 77.08(8) . . ? N1 Cr N17 77.34(9) . . ? N7 Cr N17 154.39(8) . . ? N1 Cr Cl2 176.94(7) . . ? N7 Cr Cl2 104.10(6) . . ? N17 Cr Cl2 101.51(6) . . ? N1 Cr Cl3 89.29(7) . . ? N7 Cr Cl3 84.42(6) . . ? N17 Cr Cl3 93.98(6) . . ? Cl2 Cr Cl3 93.62(3) . . ? N1 Cr Cl1 84.92(7) . . ? N7 Cr Cl1 92.53(6) . . ? N17 Cr Cl1 86.50(6) . . ? Cl2 Cr Cl1 92.19(3) . . ? Cl3 Cr Cl1 173.95(3) . . ? C2 N1 C6 121.6(2) . . ? C2 N1 Cr 119.28(18) . . ? C6 N1 Cr 118.67(18) . . ? N1 C2 C3 121.3(3) . . ? N1 C2 C7 110.8(2) . . ? C3 C2 C7 128.0(3) . . ? C4 C3 C2 117.6(3) . . ? C5 C4 C3 121.1(3) . . ? C4 C5 C6 118.2(3) . . ? N1 C6 C5 120.1(3) . . ? N1 C6 C17 111.6(2) . . ? C5 C6 C17 128.0(3) . . ? N7 C7 C2 118.6(2) . . ? N7 C7 S8 119.5(2) . . ? C2 C7 S8 121.5(2) . . ? C7 N7 C10 112.4(2) . . ? C7 N7 Cr 112.32(18) . . ? C10 N7 Cr 131.98(17) . . ? C7 S8 C9 87.99(13) . . ? C10 C9 S8 107.13(19) . . ? N7 C10 C9 105.9(2) . . ? N7 C10 C11 112.7(2) . . ? C9 C10 C11 115.1(3) . . ? C12 C11 C14 109.9(3) . . ? C12 C11 C13 109.3(3) . . ? C14 C11 C13 107.0(3) . . ? C12 C11 C10 112.6(3) . . ? C14 C11 C10 111.0(3) . . ? C13 C11 C10 106.8(3) . . ? N17 C17 C6 119.4(2) . . ? N17 C17 S18 118.7(2) . . ? C6 C17 S18 121.6(2) . . ? C17 N17 C20 113.0(2) . . ? C17 N17 Cr 111.88(18) . . ? C20 N17 Cr 132.92(16) . . ? C17 S18 C19 88.72(13) . . ? C20 C19 S18 107.31(18) . . ? N17 C20 C21 114.6(2) . . ? N17 C20 C19 106.1(2) . . ? C21 C20 C19 113.3(2) . . ? C23 C21 C24 109.5(3) . . ? C23 C21 C22 110.6(3) . . ? C24 C21 C22 106.3(2) . . ? C23 C21 C20 112.3(2) . . ? C24 C21 C20 110.1(2) . . ? C22 C21 C20 107.8(2) . . ? Cl5 C30 Cl4 107.7(6) . . ? Cl4' C30' Cl5' 111.7(9) . . ? Cl5" C30" Cl4" 110.5(11) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 71.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.387 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.047 #===END data_[Fe(L1)2][FeCl4] _database_code_depnum_ccdc_archive 'CCDC 859233' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H38 Fe N6 S4, C2 H3 N, Cl4 Fe' _chemical_formula_sum 'C48 H41 Cl4 Fe2 N7 S4' _chemical_formula_weight 1097.62 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' S S 0.1246 0.1234 '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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 13.3454(2) _cell_length_b 13.3454(2) _cell_length_c 26.6492(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4746.24(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10776 _cell_measurement_theta_min 3.7272 _cell_measurement_theta_max 28.9107 _exptl_crystal_description 'platy needles' _exptl_crystal_colour 'Dark purple' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.056 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.871 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37723 _diffrn_reflns_av_R_equivalents 0.0977 _diffrn_reflns_av_sigmaI/netI 0.0962 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 29.01 _reflns_number_total 5782 _reflns_number_gt 4149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0460 _refine_ls_wR_factor_obs+ 0.0791 _refine_ls_abs_structure_Flack+ 0.000(19) _refine_ls_R_factor_obs- 0.0553 _refine_ls_wR_factor_obs- 0.1006 _refine_ls_abs_structure_Flack- **** ; _chemical_absolute_configuration ad _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^)+(0.0368P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2371 Friedel pairs' _refine_ls_abs_structure_Flack -0.007(19) _refine_ls_number_reflns 5782 _refine_ls_number_parameters 310 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0810 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0791 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.988 _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 Fe1 Fe 0.51531(3) 0.48469(3) 0.2500 0.01712(15) Uani 1 2 d S . . N1 N 0.42248(19) 0.39180(18) 0.27639(9) 0.0198(6) Uani 1 1 d . . . C2 C 0.4495(3) 0.3319(2) 0.31425(12) 0.0239(8) Uani 1 1 d . . . C3 C 0.3840(3) 0.2607(3) 0.33371(13) 0.0315(9) Uani 1 1 d . . . H3A H 0.4034 0.2191 0.3610 0.038 Uiso 1 1 calc R . . C4 C 0.2902(3) 0.2523(3) 0.31233(14) 0.0368(10) Uani 1 1 d . . . H4A H 0.2451 0.2025 0.3241 0.044 Uiso 1 1 calc R . . C5 C 0.2614(3) 0.3158(3) 0.27390(13) 0.0296(8) Uani 1 1 d . . . H5A H 0.1961 0.3117 0.2598 0.035 Uiso 1 1 calc R . . C6 C 0.3295(2) 0.3846(2) 0.25677(12) 0.0227(7) Uani 1 1 d . . . C7 C 0.5502(3) 0.3582(2) 0.33082(11) 0.0225(8) Uani 1 1 d . . . N7 N 0.59708(19) 0.42504(19) 0.30520(9) 0.0186(6) Uani 1 1 d . . . S8 S 0.60098(8) 0.31831(8) 0.38717(3) 0.0401(3) Uani 1 1 d . . . C9 C 0.7150(3) 0.3859(3) 0.37226(12) 0.0343(9) Uani 1 1 d . . . H9A H 0.7403 0.4216 0.4023 0.041 Uiso 1 1 calc R . . H9B H 0.7675 0.3391 0.3605 0.041 Uiso 1 1 calc R . . C10 C 0.6883(3) 0.4609(3) 0.33081(12) 0.0269(8) Uani 1 1 d . . . H10A H 0.6713 0.5258 0.3475 0.032 Uiso 1 1 calc R . . C11 C 0.7768(2) 0.4800(3) 0.29669(11) 0.0231(7) Uani 1 1 d . . . C12 C 0.8130(3) 0.4059(3) 0.26485(12) 0.0298(8) Uani 1 1 d . . . H12A H 0.7811 0.3423 0.2638 0.036 Uiso 1 1 calc R . . C13 C 0.8947(3) 0.4244(3) 0.23494(14) 0.0388(10) Uani 1 1 d . . . H13A H 0.9189 0.3737 0.2131 0.047 Uiso 1 1 calc R . . C14 C 0.9418(3) 0.5159(3) 0.23652(14) 0.0424(10) Uani 1 1 d . . . H14A H 0.9983 0.5283 0.2158 0.051 Uiso 1 1 calc R . . C15 C 0.9069(3) 0.5898(3) 0.26823(15) 0.0424(10) Uani 1 1 d . . . H15A H 0.9397 0.6529 0.2696 0.051 Uiso 1 1 calc R . . C16 C 0.8252(3) 0.5718(3) 0.29772(13) 0.0328(9) Uani 1 1 d . . . H16A H 0.8011 0.6231 0.3193 0.039 Uiso 1 1 calc R . . C17 C 0.3201(2) 0.4531(2) 0.21452(11) 0.0202(7) Uani 1 1 d . . . N17 N 0.3982(2) 0.50804(19) 0.20445(9) 0.0200(6) Uani 1 1 d . A . S18 S 0.21801(7) 0.45650(7) 0.17484(3) 0.0318(2) Uani 1 1 d . . . C19 C 0.2783(3) 0.5551(3) 0.13906(13) 0.0327(9) Uani 1 1 d . A . H19A H 0.2732 0.5408 0.1027 0.039 Uiso 1 1 calc R . . H19B H 0.2454 0.6202 0.1458 0.039 Uiso 1 1 calc R . . C20 C 0.3886(3) 0.5592(3) 0.15504(12) 0.0269(8) Uani 1 1 d D . . H20A H 0.4312 0.5245 0.1295 0.032 Uiso 0.609(14) 1 calc PR A 1 H20B H 0.4228 0.5157 0.1320 0.032 Uiso 0.391(14) 1 d PR A 2 C21 C 0.4197(5) 0.6684(3) 0.1594(2) 0.0284(18) Uani 0.609(14) 1 d PGD A 1 C22 C 0.3839(5) 0.7326(3) 0.1964(2) 0.046(2) Uani 0.609(14) 1 d PGD A 1 H22A H 0.3391 0.7082 0.2213 0.056 Uiso 0.609(14) 1 calc PR A 1 C23 C 0.4135(6) 0.8324(3) 0.1969(3) 0.051(3) Uani 0.609(14) 1 d PG A 1 H23A H 0.3890 0.8763 0.2222 0.062 Uiso 0.609(14) 1 calc PR A 1 C24 C 0.4790(6) 0.8681(3) 0.1605(3) 0.055(4) Uani 0.609(14) 1 d PG A 1 H24A H 0.4992 0.9363 0.1609 0.066 Uiso 0.609(14) 1 calc PR A 1 C25 C 0.5148(5) 0.8040(5) 0.1235(3) 0.051(3) Uani 0.609(14) 1 d PG A 1 H25A H 0.5595 0.8283 0.0986 0.061 Uiso 0.609(14) 1 calc PR A 1 C26 C 0.4851(5) 0.7041(4) 0.1230(2) 0.036(2) Uani 0.609(14) 1 d PGD A 1 H26A H 0.5096 0.6603 0.0977 0.043 Uiso 0.609(14) 1 calc PR A 1 C21' C 0.4408(7) 0.6585(4) 0.1480(3) 0.019(3) Uiso 0.391(14) 1 d PGD A 2 C22' C 0.4099(6) 0.7361(5) 0.1791(3) 0.026(3) Uiso 0.391(14) 1 d PGD A 2 H22B H 0.3616 0.7239 0.2046 0.031 Uiso 0.391(14) 1 calc PR A 2 C23' C 0.4496(7) 0.8316(4) 0.1729(4) 0.027(3) Uiso 0.391(14) 1 d PG A 2 H23B H 0.4284 0.8847 0.1942 0.032 Uiso 0.391(14) 1 calc PR A 2 C24' C 0.5202(8) 0.8495(5) 0.1357(4) 0.034(3) Uiso 0.391(14) 1 d PG A 2 H24B H 0.5474 0.9147 0.1315 0.040 Uiso 0.391(14) 1 calc PR A 2 C25' C 0.5512(7) 0.7718(7) 0.1046(3) 0.040(3) Uiso 0.391(14) 1 d PG A 2 H25B H 0.5995 0.7840 0.0791 0.048 Uiso 0.391(14) 1 calc PR A 2 C26' C 0.5115(7) 0.6763(6) 0.1107(3) 0.030(3) Uiso 0.391(14) 1 d PGD A 2 H26B H 0.5326 0.6232 0.0895 0.036 Uiso 0.391(14) 1 calc PR A 2 Fe2 Fe 0.40070(4) 0.40070(4) 0.0000 0.03022(19) Uani 1 2 d S . . Cl1 Cl 0.35252(7) 0.32393(7) 0.07360(3) 0.0368(2) Uani 1 1 d . . . Cl2 Cl 0.36189(9) 0.56925(8) 0.01050(4) 0.0524(3) Uani 1 1 d . . . N30 N 0.6346(10) 0.7770(11) 0.0149(6) 0.141(5) Uani 0.50 1 d PU B -1 C31 C 0.6360(8) 0.6885(11) 0.0131(6) 0.087(4) Uani 0.50 1 d P B -1 C32 C 0.6363(9) 0.5919(10) 0.0186(4) 0.088(5) Uani 0.50 1 d P B -1 H32A H 0.6565 0.5750 0.0529 0.132 Uiso 0.50 1 calc PR B -1 H32B H 0.6837 0.5621 -0.0052 0.132 Uiso 0.50 1 calc PR B -1 H32C H 0.5690 0.5656 0.0121 0.132 Uiso 0.50 1 calc PR B -1 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 Fe1 0.0168(2) 0.0168(2) 0.0178(3) 0.00098(18) 0.00098(18) -0.0008(3) N1 0.0239(15) 0.0172(14) 0.0182(13) 0.0005(11) 0.0037(11) -0.0021(12) C2 0.030(2) 0.0191(18) 0.0225(17) -0.0019(15) 0.0064(15) 0.0008(15) C3 0.042(2) 0.026(2) 0.027(2) 0.0049(16) 0.0110(17) -0.0042(18) C4 0.038(2) 0.032(2) 0.041(2) -0.0015(18) 0.0133(18) -0.0134(19) C5 0.027(2) 0.029(2) 0.033(2) -0.0070(17) 0.0067(16) -0.0084(16) C6 0.0191(17) 0.0229(18) 0.0261(18) -0.0054(14) 0.0052(15) -0.0022(14) C7 0.029(2) 0.0210(18) 0.0177(17) 0.0009(14) 0.0014(15) 0.0060(16) N7 0.0215(15) 0.0181(15) 0.0163(13) -0.0012(11) 0.0004(11) 0.0005(12) S8 0.0440(6) 0.0494(6) 0.0268(5) 0.0179(5) -0.0050(5) 0.0010(5) C9 0.036(2) 0.045(2) 0.0215(19) 0.0007(17) -0.0093(16) 0.005(2) C10 0.028(2) 0.026(2) 0.0266(19) -0.0005(15) -0.0055(16) 0.0023(16) C11 0.0208(18) 0.0287(19) 0.0198(16) -0.0013(15) -0.0063(14) 0.0031(17) C12 0.027(2) 0.029(2) 0.033(2) -0.0044(16) -0.0030(16) -0.0004(17) C13 0.032(2) 0.043(2) 0.042(2) -0.0074(19) 0.0102(18) 0.004(2) C14 0.024(2) 0.057(3) 0.046(3) 0.002(2) 0.0091(18) -0.006(2) C15 0.030(2) 0.037(2) 0.060(3) -0.001(2) -0.001(2) -0.009(2) C16 0.031(2) 0.029(2) 0.039(2) -0.0095(17) -0.0034(18) -0.0001(18) C17 0.0188(17) 0.0192(18) 0.0228(17) -0.0107(14) 0.0009(14) 0.0021(15) N17 0.0230(15) 0.0172(15) 0.0199(14) -0.0009(11) -0.0005(12) 0.0007(13) S18 0.0236(5) 0.0386(6) 0.0331(5) -0.0056(4) -0.0067(4) -0.0032(4) C19 0.032(2) 0.034(2) 0.0318(19) 0.0027(17) -0.0121(17) 0.0032(18) C20 0.028(2) 0.0272(19) 0.0253(18) 0.0027(15) -0.0059(15) -0.0006(17) C21 0.028(4) 0.037(4) 0.020(4) 0.016(3) -0.010(3) 0.002(3) C22 0.068(6) 0.024(4) 0.047(5) -0.002(3) -0.008(5) -0.003(4) C23 0.072(6) 0.026(4) 0.055(6) 0.002(3) -0.024(5) 0.001(4) C24 0.057(6) 0.030(4) 0.078(8) 0.017(4) -0.032(6) -0.020(4) C25 0.043(5) 0.038(5) 0.072(6) 0.032(5) -0.020(5) -0.008(5) C26 0.030(4) 0.040(4) 0.039(4) 0.009(3) -0.014(3) 0.003(4) Fe2 0.0337(3) 0.0337(3) 0.0234(4) -0.0021(2) 0.0021(2) 0.0077(4) Cl1 0.0399(6) 0.0454(6) 0.0250(5) 0.0023(4) -0.0022(4) -0.0004(5) Cl2 0.0828(8) 0.0358(6) 0.0387(6) -0.0022(5) 0.0137(5) 0.0189(6) N30 0.120(8) 0.126(8) 0.177(9) 0.023(8) 0.023(7) -0.008(7) C31 0.045(7) 0.085(10) 0.130(13) 0.026(10) 0.028(7) 0.008(7) C32 0.085(10) 0.087(11) 0.091(10) -0.027(7) 0.042(7) -0.023(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 Fe1 N1 1.888(2) 8_665 ? Fe1 N1 1.888(2) . ? Fe1 N7 1.997(2) . ? Fe1 N7 1.997(2) 8_665 ? Fe1 N17 2.003(3) 8_665 ? Fe1 N17 2.003(3) . ? N1 C2 1.336(4) . ? N1 C6 1.350(4) . ? C2 C3 1.391(5) . ? C2 C7 1.458(5) . ? C3 C4 1.380(5) . ? C4 C5 1.384(5) . ? C5 C6 1.371(4) . ? C6 C17 1.455(4) . ? C7 N7 1.286(4) . ? C7 S8 1.731(3) . ? N7 C10 1.475(4) . ? S8 C9 1.814(4) . ? C9 C10 1.532(5) . ? C10 C11 1.512(5) . ? C11 C16 1.386(5) . ? C11 C12 1.389(4) . ? C12 C13 1.374(5) . ? C13 C14 1.374(5) . ? C14 C15 1.379(5) . ? C15 C16 1.366(5) . ? C17 N17 1.303(4) . ? C17 S18 1.725(3) . ? N17 C20 1.488(4) . ? S18 C19 1.813(4) . ? C19 C20 1.533(5) . ? C20 C21' 1.509(6) . ? C20 C21 1.520(4) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C25 C26 1.3900 . ? C21' C22' 1.3900 . ? C21' C26' 1.3900 . ? C22' C23' 1.3900 . ? C23' C24' 1.3900 . ? C24' C25' 1.3900 . ? C25' C26' 1.3900 . ? Fe2 Cl1 2.3043(10) . ? Fe2 Cl1 2.3043(10) 7 ? Fe2 Cl2 2.3252(11) . ? Fe2 Cl2 2.3252(11) 7 ? N30 C31 1.181(17) . ? C31 C32 1.298(15) . ? 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 Fe1 N1 179.97(17) 8_665 . ? N1 Fe1 N7 100.20(11) 8_665 . ? N1 Fe1 N7 79.78(11) . . ? N1 Fe1 N7 79.78(11) 8_665 8_665 ? N1 Fe1 N7 100.20(11) . 8_665 ? N7 Fe1 N7 96.13(14) . 8_665 ? N1 Fe1 N17 79.40(11) 8_665 8_665 ? N1 Fe1 N17 100.62(11) . 8_665 ? N7 Fe1 N17 87.11(10) . 8_665 ? N7 Fe1 N17 159.17(10) 8_665 8_665 ? N1 Fe1 N17 100.62(11) 8_665 . ? N1 Fe1 N17 79.40(11) . . ? N7 Fe1 N17 159.17(10) . . ? N7 Fe1 N17 87.11(10) 8_665 . ? N17 Fe1 N17 97.16(14) 8_665 . ? C2 N1 C6 119.8(3) . . ? C2 N1 Fe1 119.8(2) . . ? C6 N1 Fe1 120.4(2) . . ? N1 C2 C3 121.4(3) . . ? N1 C2 C7 109.5(3) . . ? C3 C2 C7 129.1(3) . . ? C4 C3 C2 118.1(3) . . ? C3 C4 C5 120.5(3) . . ? C6 C5 C4 118.2(3) . . ? N1 C6 C5 121.9(3) . . ? N1 C6 C17 109.5(3) . . ? C5 C6 C17 128.4(3) . . ? N7 C7 C2 117.0(3) . . ? N7 C7 S8 118.9(3) . . ? C2 C7 S8 123.4(3) . . ? C7 N7 C10 112.4(2) . . ? C7 N7 Fe1 113.7(2) . . ? C10 N7 Fe1 131.5(2) . . ? C7 S8 C9 89.17(16) . . ? C10 C9 S8 106.7(2) . . ? N7 C10 C11 114.9(3) . . ? N7 C10 C9 108.3(3) . . ? C11 C10 C9 111.2(3) . . ? C16 C11 C12 118.6(3) . . ? C16 C11 C10 120.1(3) . . ? C12 C11 C10 121.3(3) . . ? C13 C12 C11 120.2(3) . . ? C12 C13 C14 120.3(3) . . ? C13 C14 C15 120.0(3) . . ? C16 C15 C14 119.8(4) . . ? C15 C16 C11 121.1(3) . . ? N17 C17 C6 116.3(3) . . ? N17 C17 S18 119.4(2) . . ? C6 C17 S18 124.0(2) . . ? C17 N17 C20 111.8(3) . . ? C17 N17 Fe1 114.3(2) . . ? C20 N17 Fe1 132.4(2) . . ? C17 S18 C19 89.49(16) . . ? C20 C19 S18 107.8(2) . . ? N17 C20 C21' 118.2(4) . . ? N17 C20 C21 110.4(3) . . ? C21' C20 C21 16.5(3) . . ? N17 C20 C19 108.2(3) . . ? C21' C20 C19 116.1(5) . . ? C21 C20 C19 108.5(4) . . ? C22 C21 C26 120.0 . . ? C22 C21 C20 123.5(3) . . ? C26 C21 C20 116.5(3) . . ? C23 C22 C21 120.0 . . ? C22 C23 C24 120.0 . . ? C25 C24 C23 120.0 . . ? C24 C25 C26 120.0 . . ? C25 C26 C21 120.0 . . ? C22' C21' C26' 120.0 . . ? C22' C21' C20 116.3(4) . . ? C26' C21' C20 123.5(4) . . ? C21' C22' C23' 120.0 . . ? C24' C23' C22' 120.0 . . ? C25' C24' C23' 120.0 . . ? C26' C25' C24' 120.0 . . ? C25' C26' C21' 120.0 . . ? Cl1 Fe2 Cl1 118.45(6) . 7 ? Cl1 Fe2 Cl2 105.40(3) . . ? Cl1 Fe2 Cl2 105.86(4) 7 . ? Cl1 Fe2 Cl2 105.86(4) . 7 ? Cl1 Fe2 Cl2 105.40(3) 7 7 ? Cl2 Fe2 Cl2 116.45(7) . 7 ? N30 C31 C32 171.4(18) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.416 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.071 #===END data_[Fe(L2)Br2] _database_code_depnum_ccdc_archive 'CCDC 859234' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H27 Br2 Fe N3 S2, 0.33(C4 H8 O)' _chemical_formula_sum 'C20.33 H29.67 Br2 Fe N3 O0.33 S2' _chemical_formula_weight 601.26 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 15.5290(2) _cell_length_b 27.9269(4) _cell_length_c 17.3305(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7515.84(17) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21861 _cell_measurement_theta_min 3.7564 _cell_measurement_theta_max 32.3659 _exptl_crystal_description needles _exptl_crystal_colour 'Very dark blue' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 3.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.67079 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 51745 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0690 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 32.38 _reflns_number_total 12312 _reflns_number_gt 8468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0293 _refine_ls_wR_factor_obs+ 0.0529 _refine_ls_abs_structure_Flack+ 0.000(5) _refine_ls_R_factor_obs- 0.0572 _refine_ls_wR_factor_obs- 0.1326 _refine_ls_abs_structure_Flack- 1.012(5) ; _chemical_absolute_configuration ad _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^)+(0.0265P)^2^+0.6623P] 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, 5504 Friedel pairs' _refine_ls_abs_structure_Flack -0.012(5) _refine_ls_number_reflns 12312 _refine_ls_number_parameters 408 _refine_ls_number_restraints 79 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.138 _refine_ls_shift/su_max 0.002 _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 Fe Fe 0.31239(3) 0.649002(16) 0.47257(2) 0.02354(10) Uani 1 1 d . . . Br1 Br 0.24381(2) 0.711437(11) 0.398303(18) 0.03314(8) Uani 1 1 d . . . Br2 Br 0.28406(2) 0.600696(12) 0.587570(17) 0.03297(8) Uani 1 1 d . . . N1 N 0.42972(15) 0.62720(9) 0.42565(12) 0.0216(5) Uani 1 1 d . . . C2 C 0.43277(18) 0.58932(10) 0.37758(15) 0.0193(6) Uani 1 1 d . . . C3 C 0.5113(2) 0.57249(12) 0.35020(16) 0.0271(7) Uani 1 1 d . . . H3A H 0.5132 0.5461 0.3156 0.033 Uiso 1 1 calc R . . C4 C 0.5862(2) 0.59435(13) 0.37369(17) 0.0342(8) Uani 1 1 d . . . H4A H 0.6402 0.5831 0.3555 0.041 Uiso 1 1 calc R . . C5 C 0.5826(2) 0.63214(13) 0.42306(17) 0.0323(8) Uani 1 1 d . . . H5A H 0.6340 0.6470 0.4407 0.039 Uiso 1 1 calc R . . C6 C 0.50284(19) 0.64850(11) 0.44718(17) 0.0249(6) Uani 1 1 d . . . C7 C 0.3487(2) 0.56719(10) 0.36223(15) 0.0207(6) Uani 1 1 d . . . N7 N 0.27937(14) 0.58246(8) 0.39383(13) 0.0201(5) Uani 1 1 d . . . S8 S 0.34511(6) 0.51499(3) 0.30594(5) 0.03093(18) Uani 1 1 d . . . C9 C 0.2294(2) 0.51517(11) 0.31446(18) 0.0300(7) Uani 1 1 d . . . H9A H 0.2027 0.5275 0.2665 0.036 Uiso 1 1 calc R . . H9B H 0.2078 0.4824 0.3240 0.036 Uiso 1 1 calc R . . C10 C 0.20763(19) 0.54800(10) 0.38284(15) 0.0211(6) Uani 1 1 d . . . H10A H 0.2067 0.5272 0.4298 0.025 Uiso 1 1 calc R . . C11 C 0.11713(19) 0.57058(12) 0.37647(17) 0.0283(7) Uani 1 1 d . . . C12 C 0.1128(2) 0.60561(13) 0.30927(18) 0.0375(8) Uani 1 1 d . . . H12A H 0.1269 0.5889 0.2612 0.056 Uiso 1 1 calc R . . H12B H 0.1541 0.6316 0.3177 0.056 Uiso 1 1 calc R . . H12C H 0.0545 0.6189 0.3056 0.056 Uiso 1 1 calc R . . C13 C 0.0530(2) 0.52949(13) 0.3631(2) 0.0451(10) Uani 1 1 d . . . H13A H 0.0676 0.5128 0.3151 0.068 Uiso 1 1 calc R . . H13B H -0.0055 0.5425 0.3592 0.068 Uiso 1 1 calc R . . H13C H 0.0558 0.5070 0.4064 0.068 Uiso 1 1 calc R . . C14 C 0.0942(2) 0.59635(14) 0.45187(19) 0.0407(9) Uani 1 1 d . . . H14A H 0.0368 0.6106 0.4473 0.061 Uiso 1 1 calc R . . H14B H 0.1366 0.6216 0.4620 0.061 Uiso 1 1 calc R . . H14C H 0.0946 0.5733 0.4945 0.061 Uiso 1 1 calc R . . C17 C 0.4891(2) 0.69096(12) 0.49765(18) 0.0290(7) Uani 1 1 d . . . N17 N 0.41500(17) 0.70074(9) 0.52454(13) 0.0270(6) Uani 1 1 d . . . S18 S 0.57624(7) 0.72764(4) 0.51633(7) 0.0602(3) Uani 1 1 d . . . C19 C 0.5092(3) 0.76186(15) 0.5801(3) 0.0622(13) Uani 1 1 d . . . H19A H 0.5239 0.7547 0.6345 0.075 Uiso 1 1 calc R . . H19B H 0.5176 0.7965 0.5710 0.075 Uiso 1 1 calc R . . C20 C 0.4158(2) 0.74784(12) 0.56352(18) 0.0315(7) Uani 1 1 d . . . H20A H 0.3932 0.7716 0.5254 0.038 Uiso 1 1 calc R . . C21 C 0.3577(2) 0.75144(14) 0.63559(18) 0.0394(9) Uani 1 1 d . . . C22 C 0.3671(3) 0.80173(16) 0.6694(2) 0.0646(13) Uani 1 1 d . . . H22A H 0.4267 0.8067 0.6863 0.097 Uiso 1 1 calc R . . H22B H 0.3283 0.8052 0.7137 0.097 Uiso 1 1 calc R . . H22C H 0.3523 0.8255 0.6301 0.097 Uiso 1 1 calc R . . C23 C 0.3814(3) 0.71445(16) 0.6942(2) 0.0626(13) Uani 1 1 d . . . H23A H 0.3752 0.6825 0.6715 0.094 Uiso 1 1 calc R . . H23B H 0.3432 0.7173 0.7390 0.094 Uiso 1 1 calc R . . H23C H 0.4412 0.7193 0.7104 0.094 Uiso 1 1 calc R . . C24 C 0.2645(3) 0.74420(17) 0.6122(3) 0.0653(13) Uani 1 1 d . . . H24A H 0.2573 0.7121 0.5904 0.098 Uiso 1 1 calc R . . H24B H 0.2485 0.7682 0.5734 0.098 Uiso 1 1 calc R . . H24C H 0.2274 0.7477 0.6576 0.098 Uiso 1 1 calc R . . Fe' Fe 0.75010(4) 0.5000 0.5000 0.02426(13) Uani 1 2 d S . . Br1' Br 0.80507(2) 0.552506(12) 0.399792(17) 0.03013(7) Uani 1 1 d . . . N1' N 0.6164(2) 0.5000 0.5000 0.0235(8) Uani 1 2 d S . . C2' C 0.5726(2) 0.53015(12) 0.54511(18) 0.0320(8) Uani 1 1 d . . . C3' C 0.4838(2) 0.53128(14) 0.5452(2) 0.0413(9) Uani 1 1 d . . . H3'A H 0.4537 0.5537 0.5766 0.050 Uiso 1 1 calc R . . C4' C 0.4399(3) 0.5000 0.5000 0.0410(13) Uani 1 2 d S . . H4'A H 0.3787 0.5000 0.5000 0.049 Uiso 1 2 calc SR . . C7' C 0.6284(2) 0.55970(12) 0.59473(18) 0.0310(7) Uani 1 1 d . . . N7' N 0.71043(16) 0.55847(8) 0.58850(13) 0.0260(5) Uani 1 1 d . . . S8' S 0.58267(7) 0.59471(4) 0.66806(6) 0.0553(3) Uani 1 1 d . . . C9' C 0.6881(3) 0.61966(15) 0.6869(2) 0.0545(11) Uani 1 1 d . . . H9'A H 0.6939 0.6515 0.6622 0.065 Uiso 1 1 calc R . . H9'B H 0.6974 0.6233 0.7431 0.065 Uiso 1 1 calc R . . C10' C 0.7530(2) 0.58478(11) 0.65312(17) 0.0345(8) Uani 1 1 d . . . H10B H 0.7649 0.5605 0.6942 0.041 Uiso 1 1 calc R . . C11' C 0.8408(2) 0.60826(12) 0.63324(19) 0.0371(8) Uani 1 1 d . . . C12' C 0.8311(3) 0.64427(13) 0.5680(2) 0.0565(12) Uani 1 1 d . . . H12D H 0.8873 0.6586 0.5565 0.085 Uiso 1 1 calc R . . H12E H 0.7907 0.6694 0.5836 0.085 Uiso 1 1 calc R . . H12F H 0.8092 0.6280 0.5220 0.085 Uiso 1 1 calc R . . C13' C 0.8728(3) 0.63360(17) 0.7057(2) 0.0704(14) Uani 1 1 d . . . H13D H 0.9281 0.6491 0.6949 0.106 Uiso 1 1 calc R . . H13E H 0.8801 0.6102 0.7473 0.106 Uiso 1 1 calc R . . H13F H 0.8307 0.6578 0.7215 0.106 Uiso 1 1 calc R . . C14' C 0.9050(2) 0.57013(13) 0.6106(2) 0.0415(9) Uani 1 1 d . . . H14D H 0.9601 0.5852 0.5977 0.062 Uiso 1 1 calc R . . H14E H 0.8834 0.5525 0.5657 0.062 Uiso 1 1 calc R . . H14F H 0.9132 0.5479 0.6538 0.062 Uiso 1 1 calc R . . O30 O 0.5000(7) 0.67060(17) 0.2590(6) 0.0394(17) Uiso 0.429(5) 1 d PDU A -1 C31 C 0.5796(7) 0.6979(4) 0.2595(8) 0.052(3) Uiso 0.429(5) 1 d PDU A -1 H31A H 0.6233 0.6821 0.2266 0.062 Uiso 0.429(5) 1 calc PR A -1 H31B H 0.6025 0.7001 0.3127 0.062 Uiso 0.429(5) 1 calc PR A -1 C32 C 0.5597(7) 0.7467(4) 0.2292(9) 0.070(3) Uiso 0.429(5) 1 d PDU A -1 H32A H 0.5949 0.7537 0.1830 0.084 Uiso 0.429(5) 1 calc PR A -1 H32B H 0.5716 0.7713 0.2689 0.084 Uiso 0.429(5) 1 calc PR A -1 C33 C 0.4648(7) 0.7461(4) 0.2089(7) 0.068(3) Uiso 0.429(5) 1 d PDU A -1 H33A H 0.4559 0.7402 0.1531 0.082 Uiso 0.429(5) 1 calc PR A -1 H33B H 0.4365 0.7766 0.2233 0.082 Uiso 0.429(5) 1 calc PR A -1 C34 C 0.4314(7) 0.7045(4) 0.2575(8) 0.047(3) Uiso 0.429(5) 1 d PDU A -1 H34A H 0.4172 0.7154 0.3104 0.056 Uiso 0.429(5) 1 calc PR A -1 H34B H 0.3792 0.6904 0.2339 0.056 Uiso 0.429(5) 1 calc PR A -1 O30A O 0.489(3) 0.6851(12) 0.287(2) 0.051(6) Uiso 0.071(5) 1 d PDU A -2 C31A C 0.565(3) 0.6903(16) 0.240(4) 0.045(7) Uiso 0.071(5) 1 d PDU A -2 H31C H 0.5707 0.6629 0.2044 0.054 Uiso 0.071(5) 1 calc PR A -2 H31D H 0.6174 0.6914 0.2732 0.054 Uiso 0.071(5) 1 calc PR A -2 C32A C 0.556(3) 0.7362(18) 0.196(3) 0.039(6) Uiso 0.071(5) 1 d PDU A -2 H32C H 0.6106 0.7546 0.1967 0.047 Uiso 0.071(5) 1 calc PR A -2 H32D H 0.5403 0.7297 0.1415 0.047 Uiso 0.071(5) 1 calc PR A -2 C33A C 0.486(4) 0.7635(11) 0.236(3) 0.053(7) Uiso 0.071(5) 1 d PDU A -2 H33C H 0.4361 0.7680 0.2007 0.063 Uiso 0.071(5) 1 calc PR A -2 H33D H 0.5069 0.7953 0.2523 0.063 Uiso 0.071(5) 1 calc PR A -2 C34A C 0.461(4) 0.7337(16) 0.304(3) 0.053(7) Uiso 0.071(5) 1 d PDU A -2 H34C H 0.4893 0.7458 0.3514 0.064 Uiso 0.071(5) 1 calc PR A -2 H34D H 0.3977 0.7346 0.3119 0.064 Uiso 0.071(5) 1 calc PR A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0192(2) 0.0264(2) 0.0251(2) 0.00214(18) 0.00240(17) 0.00299(19) Br1 0.03511(18) 0.02865(16) 0.03565(15) 0.00127(14) -0.00466(15) 0.00786(14) Br2 0.03692(18) 0.03381(17) 0.02819(15) 0.00674(14) 0.00341(13) -0.00146(14) N1 0.0154(12) 0.0279(14) 0.0215(12) 0.0058(10) 0.0024(10) 0.0003(11) C2 0.0222(15) 0.0162(15) 0.0194(13) 0.0023(11) 0.0023(11) 0.0066(12) C3 0.0268(17) 0.0318(18) 0.0226(14) 0.0023(13) 0.0036(13) 0.0109(15) C4 0.0249(17) 0.047(2) 0.0306(16) 0.0054(16) 0.0039(13) 0.0076(16) C5 0.0228(17) 0.041(2) 0.0334(17) 0.0041(15) -0.0020(13) -0.0053(15) C6 0.0147(14) 0.0318(17) 0.0280(14) 0.0062(14) 0.0033(12) -0.0014(13) C7 0.0284(16) 0.0171(15) 0.0167(12) 0.0048(11) -0.0039(12) 0.0021(13) N7 0.0156(11) 0.0252(13) 0.0195(10) 0.0037(10) 0.0033(10) 0.0006(10) S8 0.0341(5) 0.0283(5) 0.0304(4) -0.0072(3) 0.0005(3) 0.0032(4) C9 0.0314(19) 0.0266(17) 0.0320(16) -0.0025(14) -0.0045(13) -0.0016(14) C10 0.0263(16) 0.0141(13) 0.0228(13) 0.0037(11) -0.0044(11) -0.0070(12) C11 0.0194(16) 0.0342(19) 0.0313(16) 0.0058(14) 0.0006(12) -0.0025(14) C12 0.035(2) 0.037(2) 0.0402(18) 0.0003(17) -0.0130(16) 0.0051(17) C13 0.030(2) 0.039(2) 0.066(3) -0.0002(19) -0.0036(18) -0.0132(17) C14 0.0274(18) 0.054(2) 0.0410(19) -0.0019(18) 0.0076(15) 0.0045(17) C17 0.0254(17) 0.0320(18) 0.0295(15) -0.0033(13) 0.0004(14) -0.0096(14) N17 0.0294(15) 0.0296(15) 0.0220(12) -0.0005(11) -0.0014(11) -0.0024(12) S18 0.0407(6) 0.0607(7) 0.0792(7) -0.0285(6) 0.0153(5) -0.0282(5) C19 0.053(3) 0.055(3) 0.079(3) -0.035(2) 0.021(2) -0.028(2) C20 0.040(2) 0.0254(18) 0.0293(16) 0.0023(14) 0.0009(15) -0.0023(15) C21 0.043(2) 0.046(2) 0.0293(17) -0.0096(16) 0.0002(16) -0.0126(18) C22 0.084(4) 0.058(3) 0.052(2) -0.031(2) 0.015(2) -0.019(3) C23 0.101(4) 0.056(3) 0.0311(19) 0.007(2) -0.006(2) -0.020(3) C24 0.039(2) 0.086(3) 0.071(3) -0.043(3) 0.016(2) 0.001(2) Fe' 0.0193(3) 0.0296(3) 0.0238(3) 0.0023(2) 0.000 0.000 Br1' 0.02720(16) 0.03558(17) 0.02759(14) 0.00553(14) 0.00319(14) 0.00013(13) N1' 0.0245(19) 0.0130(17) 0.0329(19) 0.0054(15) 0.000 0.000 C2' 0.0276(18) 0.036(2) 0.0327(17) 0.0160(15) 0.0096(14) 0.0036(15) C3' 0.030(2) 0.050(2) 0.043(2) 0.0241(18) 0.0112(16) 0.0106(18) C4' 0.013(2) 0.059(4) 0.051(3) 0.029(3) 0.000 0.000 C7' 0.0305(17) 0.0346(18) 0.0281(15) 0.0102(16) 0.0050(14) 0.0097(14) N7' 0.0300(14) 0.0227(13) 0.0254(12) -0.0010(11) 0.0026(11) 0.0036(11) S8' 0.0553(7) 0.0648(8) 0.0459(5) -0.0069(5) 0.0238(5) 0.0208(6) C9' 0.072(3) 0.047(2) 0.045(2) -0.0161(18) 0.008(2) 0.010(2) C10' 0.049(2) 0.0321(18) 0.0225(14) 0.0006(13) 0.0014(16) 0.0041(17) C11' 0.054(2) 0.0201(17) 0.0374(17) -0.0071(15) -0.0047(16) -0.0059(17) C12' 0.079(3) 0.030(2) 0.060(2) 0.0033(19) 0.012(2) -0.006(2) C13' 0.087(4) 0.063(3) 0.061(3) -0.025(2) -0.003(3) -0.016(3) C14' 0.036(2) 0.042(2) 0.046(2) 0.0011(18) -0.0045(17) -0.0084(17) _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 Fe N1 2.086(2) . ? Fe N17 2.332(3) . ? Fe N7 2.362(2) . ? Fe Br1 2.4147(5) . ? Fe Br2 2.4466(5) . ? N1 C6 1.335(4) . ? N1 C2 1.347(4) . ? C2 C3 1.390(4) . ? C2 C7 1.469(4) . ? C3 C4 1.375(5) . ? C4 C5 1.360(5) . ? C5 C6 1.385(4) . ? C6 C17 1.489(4) . ? C7 N7 1.281(4) . ? C7 S8 1.755(3) . ? N7 C10 1.484(4) . ? S8 C9 1.803(3) . ? C9 C10 1.536(4) . ? C10 C11 1.544(4) . ? C11 C12 1.523(4) . ? C11 C14 1.534(5) . ? C11 C13 1.537(4) . ? C17 N17 1.272(4) . ? C17 S18 1.727(3) . ? N17 C20 1.479(4) . ? S18 C19 1.794(4) . ? C19 C20 1.530(5) . ? C20 C21 1.543(5) . ? C21 C23 1.494(5) . ? C21 C24 1.517(5) . ? C21 C22 1.529(5) . ? Fe' N1' 2.076(4) . ? Fe' N7' 2.323(2) 4_566 ? Fe' N7' 2.323(2) . ? Fe' Br1' 2.4279(4) 4_566 ? Fe' Br1' 2.4279(4) . ? N1' C2' 1.335(4) 4_566 ? N1' C2' 1.335(4) . ? C2' C3' 1.380(5) . ? C2' C7' 1.474(5) . ? C3' C4' 1.357(5) . ? C4' C3' 1.357(5) 4_566 ? C7' N7' 1.279(4) . ? C7' S8' 1.754(3) . ? N7' C10' 1.494(4) . ? S8' C9' 1.809(5) . ? C9' C10' 1.519(5) . ? C10' C11' 1.551(5) . ? C11' C14' 1.511(5) . ? C11' C12' 1.520(5) . ? C11' C13' 1.525(5) . ? O30 C34 1.427(11) . ? O30 C31 1.452(10) . ? C31 C32 1.492(11) . ? C32 C33 1.515(11) . ? C33 C34 1.526(11) . ? O30A C31A 1.446(16) . ? O30A C34A 1.454(17) . ? C31A C32A 1.504(15) . ? C32A C33A 1.496(15) . ? C33A C34A 1.500(15) . ? 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 Fe N17 74.61(9) . . ? N1 Fe N7 74.62(9) . . ? N17 Fe N7 149.21(9) . . ? N1 Fe Br1 112.85(6) . . ? N17 Fe Br1 93.43(7) . . ? N7 Fe Br1 99.47(6) . . ? N1 Fe Br2 108.28(6) . . ? N17 Fe Br2 98.62(6) . . ? N7 Fe Br2 89.87(5) . . ? Br1 Fe Br2 138.85(2) . . ? C6 N1 C2 119.5(3) . . ? C6 N1 Fe 120.2(2) . . ? C2 N1 Fe 120.06(19) . . ? N1 C2 C3 120.5(3) . . ? N1 C2 C7 114.3(2) . . ? C3 C2 C7 125.1(3) . . ? C4 C3 C2 119.4(3) . . ? C5 C4 C3 119.8(3) . . ? C4 C5 C6 118.8(3) . . ? N1 C6 C5 122.0(3) . . ? N1 C6 C17 113.4(3) . . ? C5 C6 C17 124.6(3) . . ? N7 C7 C2 122.0(3) . . ? N7 C7 S8 119.2(2) . . ? C2 C7 S8 118.6(2) . . ? C7 N7 C10 111.1(2) . . ? C7 N7 Fe 109.04(18) . . ? C10 N7 Fe 138.35(17) . . ? C7 S8 C9 89.08(14) . . ? C10 C9 S8 106.5(2) . . ? N7 C10 C9 108.7(2) . . ? N7 C10 C11 115.3(2) . . ? C9 C10 C11 112.9(2) . . ? C12 C11 C14 109.9(3) . . ? C12 C11 C13 109.6(3) . . ? C14 C11 C13 109.2(3) . . ? C12 C11 C10 111.0(2) . . ? C14 C11 C10 110.0(2) . . ? C13 C11 C10 107.2(3) . . ? N17 C17 C6 121.0(3) . . ? N17 C17 S18 120.9(3) . . ? C6 C17 S18 118.1(2) . . ? C17 N17 C20 110.6(3) . . ? C17 N17 Fe 110.1(2) . . ? C20 N17 Fe 137.1(2) . . ? C17 S18 C19 88.68(17) . . ? C20 C19 S18 107.3(3) . . ? N17 C20 C19 108.7(3) . . ? N17 C20 C21 115.0(3) . . ? C19 C20 C21 112.6(3) . . ? C23 C21 C24 108.9(4) . . ? C23 C21 C22 110.6(3) . . ? C24 C21 C22 108.4(4) . . ? C23 C21 C20 111.2(3) . . ? C24 C21 C20 109.4(3) . . ? C22 C21 C20 108.4(3) . . ? N1' Fe' N7' 74.62(6) . 4_566 ? N1' Fe' N7' 74.62(6) . . ? N7' Fe' N7' 149.25(13) 4_566 . ? N1' Fe' Br1' 110.585(16) . 4_566 ? N7' Fe' Br1' 98.11(6) 4_566 4_566 ? N7' Fe' Br1' 92.60(6) . 4_566 ? N1' Fe' Br1' 110.585(16) . . ? N7' Fe' Br1' 92.60(6) 4_566 . ? N7' Fe' Br1' 98.11(6) . . ? Br1' Fe' Br1' 138.83(3) 4_566 . ? C2' N1' C2' 118.7(4) 4_566 . ? C2' N1' Fe' 120.6(2) 4_566 . ? C2' N1' Fe' 120.6(2) . . ? N1' C2' C3' 121.7(4) . . ? N1' C2' C7' 113.3(3) . . ? C3' C2' C7' 125.0(3) . . ? C4' C3' C2' 119.1(4) . . ? C3' C4' C3' 119.8(5) . 4_566 ? N7' C7' C2' 121.4(3) . . ? N7' C7' S8' 118.6(3) . . ? C2' C7' S8' 119.8(2) . . ? C7' N7' C10' 111.4(3) . . ? C7' N7' Fe' 109.8(2) . . ? C10' N7' Fe' 136.3(2) . . ? C7' S8' C9' 88.81(17) . . ? C10' C9' S8' 106.5(3) . . ? N7' C10' C9' 108.1(3) . . ? N7' C10' C11' 115.5(2) . . ? C9' C10' C11' 113.4(3) . . ? C14' C11' C12' 109.8(3) . . ? C14' C11' C13' 109.0(3) . . ? C12' C11' C13' 109.7(3) . . ? C14' C11' C10' 109.9(3) . . ? C12' C11' C10' 111.0(3) . . ? C13' C11' C10' 107.4(3) . . ? C34 O30 C31 106.7(6) . . ? O30 C31 C32 107.5(7) . . ? C31 C32 C33 105.9(7) . . ? C32 C33 C34 102.1(7) . . ? O30 C34 C33 105.1(8) . . ? C31A O30A C34A 105.4(18) . . ? O30A C31A C32A 107.2(13) . . ? C33A C32A C31A 105.5(9) . . ? C32A C33A C34A 105.8(10) . . ? O30A C34A C33A 106.3(15) . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.820 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.106 #===END data_[Fe(L4)Cl2] _database_code_depnum_ccdc_archive 'CCDC 859235' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H27 Cl2 Fe N3 S2' _chemical_formula_sum 'C35 H27 Cl2 Fe N3 S2' _chemical_formula_weight 680.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 '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 12.66754(8) _cell_length_b 15.12678(8) _cell_length_c 16.74135(10) _cell_angle_alpha 90 _cell_angle_beta 109.6105(7) _cell_angle_gamma 90 _cell_volume 3021.89(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 17335 _cell_measurement_theta_min 2.7984 _cell_measurement_theta_max 71.2145 _exptl_crystal_description blocks _exptl_crystal_colour Brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 7.162 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.64069 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41695 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 71.43 _reflns_number_total 5836 _reflns_number_gt 4542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0402P)^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 5836 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0371 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0608 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _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 Fe Fe 0.19466(2) 0.750238(19) 0.212716(17) 0.02680(8) Uani 1 1 d . . . Cl1 Cl 0.05977(4) 0.67629(3) 0.11481(3) 0.03513(11) Uani 1 1 d . . . Cl2 Cl 0.31999(4) 0.85754(3) 0.21209(3) 0.03292(11) Uani 1 1 d . . . N1 N 0.23535(11) 0.70002(9) 0.33592(8) 0.0231(3) Uani 1 1 d . . . C2 C 0.18115(14) 0.73519(11) 0.38491(11) 0.0257(4) Uani 1 1 d . . . C3 C 0.19384(16) 0.70222(13) 0.46515(11) 0.0334(4) Uani 1 1 d . . . H3A H 0.1554 0.7284 0.4991 0.040 Uiso 1 1 calc R . . C4 C 0.26380(17) 0.63039(14) 0.49427(12) 0.0387(5) Uani 1 1 d . . . H4A H 0.2723 0.6052 0.5481 0.046 Uiso 1 1 calc R . . C5 C 0.32115(17) 0.59560(13) 0.44444(12) 0.0356(4) Uani 1 1 d . . . H5A H 0.3705 0.5469 0.4639 0.043 Uiso 1 1 calc R . . C6 C 0.30573(14) 0.63274(11) 0.36545(10) 0.0261(4) Uani 1 1 d . . . C7 C 0.10657(14) 0.80988(11) 0.34603(10) 0.0246(4) Uani 1 1 d . . . N7 N 0.09313(11) 0.83422(9) 0.26983(9) 0.0244(3) Uani 1 1 d . . . S8 S 0.03308(4) 0.86439(3) 0.40265(3) 0.03151(11) Uani 1 1 d . . . C9 C -0.05135(15) 0.91719(14) 0.30511(11) 0.0346(4) Uani 1 1 d . . . H9A H -0.1232 0.8854 0.2800 0.042 Uiso 1 1 calc R . . H9B H -0.0676 0.9792 0.3159 0.042 Uiso 1 1 calc R . . C10 C 0.01850(14) 0.91369(12) 0.24455(11) 0.0270(4) Uani 1 1 d . . . C11 C -0.05339(15) 0.90347(11) 0.15079(11) 0.0284(4) Uani 1 1 d . . . C12 C -0.16869(16) 0.89320(13) 0.12273(13) 0.0385(5) Uani 1 1 d . . . H12A H -0.2073 0.8913 0.1625 0.046 Uiso 1 1 calc R . . C13 C -0.22846(18) 0.88554(15) 0.03611(14) 0.0484(6) Uani 1 1 d . . . H13A H -0.3075 0.8782 0.0176 0.058 Uiso 1 1 calc R . . C14 C -0.17470(19) 0.88844(13) -0.02235(13) 0.0440(5) Uani 1 1 d . . . H14A H -0.2161 0.8838 -0.0812 0.053 Uiso 1 1 calc R . . C15 C -0.05954(18) 0.89819(14) 0.00504(12) 0.0410(5) Uani 1 1 d . . . H15A H -0.0212 0.8996 -0.0350 0.049 Uiso 1 1 calc R . . C16 C 0.00000(17) 0.90589(13) 0.09088(12) 0.0364(4) Uani 1 1 d . . . H16A H 0.0791 0.9130 0.1090 0.044 Uiso 1 1 calc R . . C17 C 0.09145(14) 0.99771(12) 0.25883(11) 0.0273(4) Uani 1 1 d . . . C18 C 0.04760(16) 1.07368(12) 0.21308(12) 0.0351(4) Uani 1 1 d . . . H18A H -0.0251 1.0723 0.1716 0.042 Uiso 1 1 calc R . . C19 C 0.10914(17) 1.15177(13) 0.22744(14) 0.0426(5) Uani 1 1 d . . . H19A H 0.0793 1.2028 0.1945 0.051 Uiso 1 1 calc R . . C20 C 0.21338(17) 1.15541(14) 0.28939(14) 0.0425(5) Uani 1 1 d . . . H20A H 0.2550 1.2090 0.2999 0.051 Uiso 1 1 calc R . . C21 C 0.25680(16) 1.08039(13) 0.33612(13) 0.0396(5) Uani 1 1 d . . . H21A H 0.3281 1.0827 0.3794 0.048 Uiso 1 1 calc R . . C22 C 0.19734(15) 1.00243(13) 0.32028(12) 0.0337(4) Uani 1 1 d . . . H22A H 0.2291 0.9510 0.3518 0.040 Uiso 1 1 calc R . . C23 C 0.36680(14) 0.60101(11) 0.30929(11) 0.0262(4) Uani 1 1 d . . . N23 N 0.33999(11) 0.62442(9) 0.23169(8) 0.0231(3) Uani 1 1 d . . . S24 S 0.48185(4) 0.52880(3) 0.35174(3) 0.03478(12) Uani 1 1 d . . . C25 C 0.51883(14) 0.55034(12) 0.25793(11) 0.0295(4) Uani 1 1 d . . . H25A H 0.5722 0.6003 0.2678 0.035 Uiso 1 1 calc R . . H25B H 0.5535 0.4975 0.2421 0.035 Uiso 1 1 calc R . . C26 C 0.40722(14) 0.57342(11) 0.18763(11) 0.0254(4) Uani 1 1 d . . . C27 C 0.33744(14) 0.49230(11) 0.14707(11) 0.0255(4) Uani 1 1 d . . . C28 C 0.37267(15) 0.40618(12) 0.16812(12) 0.0331(4) Uani 1 1 d . . . H28A H 0.4410 0.3952 0.2129 0.040 Uiso 1 1 calc R . . C29 C 0.30899(17) 0.33543(13) 0.12428(13) 0.0384(5) Uani 1 1 d . . . H29A H 0.3334 0.2766 0.1399 0.046 Uiso 1 1 calc R . . C30 C 0.20996(16) 0.35045(13) 0.05788(13) 0.0365(4) Uani 1 1 d . . . H30A H 0.1678 0.3024 0.0264 0.044 Uiso 1 1 calc R . . C31 C 0.17340(14) 0.43652(13) 0.03812(11) 0.0309(4) Uani 1 1 d . . . H31A H 0.1052 0.4474 -0.0067 0.037 Uiso 1 1 calc R . . C32 C 0.23488(14) 0.50654(12) 0.08276(11) 0.0279(4) Uani 1 1 d . . . H32A H 0.2073 0.5651 0.0697 0.033 Uiso 1 1 calc R . . C33 C 0.43575(14) 0.62989(12) 0.12164(11) 0.0270(4) Uani 1 1 d . . . C34 C 0.42806(15) 0.59651(13) 0.04201(11) 0.0325(4) Uani 1 1 d . . . H34A H 0.3984 0.5390 0.0259 0.039 Uiso 1 1 calc R . . C35 C 0.46332(16) 0.64666(15) -0.01382(13) 0.0401(5) Uani 1 1 d . . . H35A H 0.4573 0.6235 -0.0679 0.048 Uiso 1 1 calc R . . C36 C 0.50715(17) 0.73023(14) 0.00912(14) 0.0430(5) Uani 1 1 d . . . H36A H 0.5320 0.7643 -0.0288 0.052 Uiso 1 1 calc R . . C37 C 0.51464(17) 0.76403(13) 0.08757(14) 0.0402(5) Uani 1 1 d . . . H37A H 0.5446 0.8215 0.1034 0.048 Uiso 1 1 calc R . . C38 C 0.47878(15) 0.71456(12) 0.14311(13) 0.0328(4) Uani 1 1 d . . . H38A H 0.4836 0.7387 0.1966 0.039 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 Fe 0.02736(14) 0.03183(16) 0.01898(13) -0.00054(12) 0.00484(11) -0.00837(12) Cl1 0.0274(2) 0.0408(3) 0.0312(2) -0.0113(2) 0.00190(17) -0.00268(18) Cl2 0.0322(2) 0.0295(2) 0.0401(2) -0.00413(19) 0.01623(19) -0.00749(18) N1 0.0260(7) 0.0213(7) 0.0203(7) -0.0016(6) 0.0056(6) -0.0030(6) C2 0.0269(8) 0.0259(9) 0.0226(8) -0.0025(7) 0.0060(7) -0.0053(7) C3 0.0405(10) 0.0377(11) 0.0224(9) -0.0007(8) 0.0111(8) -0.0006(9) C4 0.0493(12) 0.0422(12) 0.0246(9) 0.0081(9) 0.0125(9) 0.0033(10) C5 0.0431(11) 0.0315(11) 0.0290(10) 0.0060(8) 0.0080(9) 0.0058(9) C6 0.0288(9) 0.0230(9) 0.0230(8) -0.0008(7) 0.0042(7) -0.0019(7) C7 0.0256(8) 0.0246(9) 0.0239(9) -0.0030(7) 0.0087(7) -0.0042(7) N7 0.0222(7) 0.0257(8) 0.0241(7) -0.0004(6) 0.0062(6) -0.0012(6) S8 0.0325(2) 0.0375(3) 0.0265(2) -0.00134(19) 0.01262(18) 0.0036(2) C9 0.0289(9) 0.0439(12) 0.0323(10) 0.0049(9) 0.0117(8) 0.0054(8) C10 0.0244(8) 0.0283(10) 0.0275(9) 0.0009(8) 0.0078(7) 0.0029(7) C11 0.0294(9) 0.0229(9) 0.0289(9) 0.0009(7) 0.0047(8) 0.0005(7) C12 0.0289(9) 0.0419(12) 0.0389(11) -0.0001(9) 0.0040(8) -0.0036(8) C13 0.0356(11) 0.0489(14) 0.0461(13) -0.0036(11) -0.0058(10) -0.0070(10) C14 0.0537(13) 0.0314(11) 0.0314(10) -0.0010(9) -0.0061(10) 0.0002(9) C15 0.0522(13) 0.0383(12) 0.0277(10) 0.0037(9) 0.0070(9) 0.0043(10) C16 0.0339(10) 0.0403(11) 0.0315(10) 0.0010(9) 0.0063(8) 0.0007(9) C17 0.0279(9) 0.0290(10) 0.0267(9) -0.0033(7) 0.0114(7) 0.0020(7) C18 0.0313(10) 0.0292(10) 0.0401(11) -0.0011(8) 0.0058(8) 0.0030(8) C19 0.0410(11) 0.0275(11) 0.0550(13) 0.0011(9) 0.0106(10) 0.0059(9) C20 0.0380(11) 0.0306(11) 0.0585(14) -0.0087(10) 0.0154(10) -0.0054(9) C21 0.0295(10) 0.0414(12) 0.0440(12) -0.0045(9) 0.0071(9) -0.0026(9) C22 0.0292(9) 0.0344(11) 0.0345(10) 0.0014(8) 0.0070(8) 0.0014(8) C23 0.0252(8) 0.0221(9) 0.0267(9) 0.0005(7) 0.0026(7) 0.0012(7) N23 0.0225(7) 0.0215(7) 0.0239(7) -0.0031(6) 0.0060(6) -0.0008(6) S24 0.0340(2) 0.0348(3) 0.0292(2) 0.0043(2) 0.00227(19) 0.0110(2) C25 0.0238(8) 0.0281(10) 0.0320(9) -0.0004(8) 0.0033(8) 0.0037(7) C26 0.0226(8) 0.0237(9) 0.0280(9) -0.0013(7) 0.0059(7) 0.0042(7) C27 0.0267(8) 0.0260(9) 0.0248(8) -0.0027(7) 0.0100(7) -0.0004(7) C28 0.0312(10) 0.0291(10) 0.0361(10) 0.0004(8) 0.0074(8) 0.0029(8) C29 0.0395(11) 0.0247(10) 0.0511(12) -0.0031(9) 0.0152(9) 0.0016(8) C30 0.0351(10) 0.0328(11) 0.0434(11) -0.0104(9) 0.0154(9) -0.0083(8) C31 0.0257(9) 0.0365(11) 0.0297(9) -0.0022(8) 0.0081(8) -0.0033(8) C32 0.0261(8) 0.0274(9) 0.0300(9) 0.0001(8) 0.0092(7) 0.0010(7) C33 0.0201(8) 0.0288(9) 0.0318(9) 0.0014(8) 0.0083(7) 0.0034(7) C34 0.0286(9) 0.0343(10) 0.0356(10) -0.0026(8) 0.0119(8) -0.0009(8) C35 0.0380(10) 0.0479(13) 0.0378(11) 0.0015(10) 0.0170(9) 0.0024(9) C36 0.0397(11) 0.0439(12) 0.0514(13) 0.0126(10) 0.0231(10) 0.0037(9) C37 0.0372(10) 0.0275(10) 0.0593(13) 0.0047(10) 0.0206(10) 0.0003(8) C38 0.0282(9) 0.0293(10) 0.0417(11) -0.0019(8) 0.0127(8) 0.0028(8) _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 Fe N1 2.0937(14) . ? Fe Cl1 2.2310(5) . ? Fe N7 2.2378(14) . ? Fe Cl2 2.2730(5) . ? Fe N23 2.5923(14) . ? N1 C6 1.334(2) . ? N1 C2 1.343(2) . ? C2 C3 1.391(2) . ? C2 C7 1.476(2) . ? C3 C4 1.383(3) . ? C4 C5 1.381(3) . ? C5 C6 1.389(2) . ? C6 C23 1.484(2) . ? C7 N7 1.283(2) . ? C7 S8 1.7428(17) . ? N7 C10 1.500(2) . ? S8 C9 1.8100(18) . ? C9 C10 1.554(2) . ? C10 C11 1.535(2) . ? C10 C17 1.542(2) . ? C11 C12 1.385(3) . ? C11 C16 1.386(3) . ? C12 C13 1.397(3) . ? C13 C14 1.368(3) . ? C14 C15 1.382(3) . ? C15 C16 1.386(3) . ? C17 C18 1.389(3) . ? C17 C22 1.392(2) . ? C18 C19 1.391(3) . ? C19 C20 1.380(3) . ? C20 C21 1.383(3) . ? C21 C22 1.376(3) . ? C23 N23 1.278(2) . ? C23 S24 1.7683(17) . ? N23 C26 1.512(2) . ? S24 C25 1.8126(19) . ? C25 C26 1.546(2) . ? C26 C27 1.531(2) . ? C26 C33 1.533(2) . ? C27 C28 1.384(2) . ? C27 C32 1.398(2) . ? C28 C29 1.392(3) . ? C29 C30 1.387(3) . ? C30 C31 1.384(3) . ? C31 C32 1.377(2) . ? C33 C38 1.391(2) . ? C33 C34 1.398(2) . ? C34 C35 1.389(3) . ? C35 C36 1.382(3) . ? C36 C37 1.383(3) . ? C37 C38 1.384(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 Fe Cl1 114.62(4) . . ? N1 Fe N7 76.81(5) . . ? Cl1 Fe N7 100.97(4) . . ? N1 Fe Cl2 108.80(4) . . ? Cl1 Fe Cl2 135.93(2) . . ? N7 Fe Cl2 95.69(4) . . ? N1 Fe N23 71.52(5) . . ? Cl1 Fe N23 93.39(3) . . ? N7 Fe N23 148.30(5) . . ? Cl2 Fe N23 93.23(3) . . ? C6 N1 C2 119.40(15) . . ? C6 N1 Fe 123.70(11) . . ? C2 N1 Fe 116.77(11) . . ? N1 C2 C3 122.04(17) . . ? N1 C2 C7 114.61(15) . . ? C3 C2 C7 123.34(17) . . ? C4 C3 C2 118.34(18) . . ? C5 C4 C3 119.41(17) . . ? C4 C5 C6 119.12(18) . . ? N1 C6 C5 121.62(17) . . ? N1 C6 C23 115.97(15) . . ? C5 C6 C23 122.41(16) . . ? N7 C7 C2 120.64(16) . . ? N7 C7 S8 119.22(13) . . ? C2 C7 S8 120.12(13) . . ? C7 N7 C10 111.80(14) . . ? C7 N7 Fe 111.00(11) . . ? C10 N7 Fe 137.12(11) . . ? C7 S8 C9 88.84(8) . . ? C10 C9 S8 106.27(12) . . ? N7 C10 C11 108.01(14) . . ? N7 C10 C17 109.18(13) . . ? C11 C10 C17 111.12(14) . . ? N7 C10 C9 106.63(14) . . ? C11 C10 C9 113.46(14) . . ? C17 C10 C9 108.28(15) . . ? C12 C11 C16 118.21(17) . . ? C12 C11 C10 123.66(17) . . ? C16 C11 C10 118.12(16) . . ? C11 C12 C13 120.3(2) . . ? C14 C13 C12 120.9(2) . . ? C13 C14 C15 119.30(19) . . ? C14 C15 C16 120.0(2) . . ? C11 C16 C15 121.37(19) . . ? C18 C17 C22 118.23(17) . . ? C18 C17 C10 119.23(16) . . ? C22 C17 C10 122.38(17) . . ? C17 C18 C19 120.66(18) . . ? C20 C19 C18 120.22(19) . . ? C19 C20 C21 119.41(19) . . ? C22 C21 C20 120.39(18) . . ? C21 C22 C17 121.05(18) . . ? N23 C23 C6 122.52(15) . . ? N23 C23 S24 118.80(14) . . ? C6 C23 S24 118.68(12) . . ? C23 N23 C26 110.71(14) . . ? C23 N23 Fe 105.28(11) . . ? C26 N23 Fe 143.90(10) . . ? C23 S24 C25 87.63(8) . . ? C26 C25 S24 105.30(12) . . ? N23 C26 C27 106.82(13) . . ? N23 C26 C33 112.02(14) . . ? C27 C26 C33 111.56(14) . . ? N23 C26 C25 105.36(13) . . ? C27 C26 C25 113.65(14) . . ? C33 C26 C25 107.34(14) . . ? C28 C27 C32 118.56(16) . . ? C28 C27 C26 123.54(15) . . ? C32 C27 C26 117.84(15) . . ? C27 C28 C29 120.61(17) . . ? C30 C29 C28 120.32(18) . . ? C31 C30 C29 119.04(18) . . ? C32 C31 C30 120.72(17) . . ? C31 C32 C27 120.64(17) . . ? C38 C33 C34 118.35(17) . . ? C38 C33 C26 119.58(16) . . ? C34 C33 C26 121.89(16) . . ? C35 C34 C33 120.62(19) . . ? C36 C35 C34 120.2(2) . . ? C35 C36 C37 119.69(19) . . ? C36 C37 C38 120.33(19) . . ? C37 C38 C33 120.85(19) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 71.43 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.239 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.044 #===END data_[Co(L2)Cl2] _database_code_depnum_ccdc_archive 'CCDC 859236' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H27 Cl2 Co N3 S2, 0.67(C H2 Cl2)' _chemical_formula_sum 'C19.67 H28.33 Cl3.33 Co N3 S2' _chemical_formula_weight 548.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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 12.12020(13) _cell_length_b 32.9663(4) _cell_length_c 9.29999(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3715.89(7) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15729 _cell_measurement_theta_min 2.6779 _cell_measurement_theta_max 71.2118 _exptl_crystal_description blocks _exptl_crystal_colour Green _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1698 _exptl_absorpt_coefficient_mu 10.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.56805 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23675 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 71.41 _reflns_number_total 7104 _reflns_number_gt 6696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0312 _refine_ls_wR_factor_obs+ 0.0811 _refine_ls_abs_structure_Flack+ 0.000(3) _refine_ls_R_factor_obs- 0.1380 _refine_ls_wR_factor_obs- 0.3629 _refine_ls_abs_structure_Flack- *** ; _chemical_absolute_configuration ad _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^)+(0.0540P)^2^+1.7709P] 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 SHELXL _refine_ls_extinction_coef 0.00085(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 3054 Friedel pairs' _refine_ls_abs_structure_Flack -0.039(2) _refine_ls_number_reflns 7104 _refine_ls_number_parameters 408 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0836 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.002 _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 Co Co 1.04149(3) 0.697649(13) 0.26402(4) 0.01876(11) Uani 1 1 d . . . Cl1 Cl 0.89570(6) 0.67204(2) 0.38780(8) 0.02776(16) Uani 1 1 d . . . Cl2 Cl 1.21430(6) 0.70992(2) 0.34156(9) 0.03061(17) Uani 1 1 d . . . N1 N 1.00426(18) 0.69918(6) 0.0509(2) 0.0175(4) Uani 1 1 d . . . C2 C 1.0361(2) 0.66919(7) -0.0392(3) 0.0174(5) Uani 1 1 d . . . C3 C 1.0060(2) 0.66930(8) -0.1830(3) 0.0246(6) Uani 1 1 d . . . H3A H 1.0306 0.6485 -0.2461 0.030 Uiso 1 1 calc R . . C4 C 0.9389(3) 0.70044(9) -0.2332(3) 0.0284(6) Uani 1 1 d . . . H4A H 0.9154 0.7007 -0.3306 0.034 Uiso 1 1 calc R . . C5 C 0.9066(3) 0.73094(9) -0.1404(3) 0.0268(6) Uani 1 1 d . . . H5A H 0.8608 0.7525 -0.1728 0.032 Uiso 1 1 calc R . . C6 C 0.9423(2) 0.72942(8) 0.0005(3) 0.0204(5) Uani 1 1 d . . . C7 C 1.1048(2) 0.63795(8) 0.0319(3) 0.0182(5) Uani 1 1 d . . . N7 N 1.11082(19) 0.63679(7) 0.1676(3) 0.0217(5) Uani 1 1 d . . . S8 S 1.18596(6) 0.605457(19) -0.07238(8) 0.02367(15) Uani 1 1 d . . . C9 C 1.2298(3) 0.58032(11) 0.0894(4) 0.0446(9) Uani 1 1 d . . . H9A H 1.1955 0.5531 0.0959 0.054 Uiso 1 1 calc R . . H9B H 1.3110 0.5770 0.0893 0.054 Uiso 1 1 calc R . . C10 C 1.1936(2) 0.60691(9) 0.2188(3) 0.0263(6) Uani 1 1 d . . . H10A H 1.2597 0.6224 0.2520 0.032 Uiso 1 1 calc R . . C11 C 1.1530(3) 0.58112(9) 0.3461(3) 0.0287(6) Uani 1 1 d . . . C12 C 1.0433(3) 0.56050(11) 0.3108(5) 0.0487(9) Uani 1 1 d . . . H12A H 1.0194 0.5441 0.3931 0.073 Uiso 1 1 calc R . . H12B H 1.0526 0.5430 0.2266 0.073 Uiso 1 1 calc R . . H12C H 0.9874 0.5812 0.2900 0.073 Uiso 1 1 calc R . . C13 C 1.2414(4) 0.54916(13) 0.3817(4) 0.0534(11) Uani 1 1 d . . . H13A H 1.2160 0.5324 0.4622 0.080 Uiso 1 1 calc R . . H13B H 1.3102 0.5628 0.4083 0.080 Uiso 1 1 calc R . . H13C H 1.2541 0.5320 0.2974 0.080 Uiso 1 1 calc R . . C14 C 1.1362(3) 0.60782(11) 0.4790(4) 0.0395(8) Uani 1 1 d . . . H14A H 1.1102 0.5911 0.5592 0.059 Uiso 1 1 calc R . . H14B H 1.0814 0.6288 0.4578 0.059 Uiso 1 1 calc R . . H14C H 1.2064 0.6206 0.5052 0.059 Uiso 1 1 calc R . . C17 C 0.9181(2) 0.76092(8) 0.1104(3) 0.0224(6) Uani 1 1 d . . . N17 N 0.96161(19) 0.75893(6) 0.2355(2) 0.0201(5) Uani 1 1 d . . . S18 S 0.83032(7) 0.80125(2) 0.06824(10) 0.0399(2) Uani 1 1 d . . . C19 C 0.8688(4) 0.82518(11) 0.2357(4) 0.0512(11) Uani 1 1 d . . . H19A H 0.9219 0.8474 0.2178 0.061 Uiso 1 1 calc R . . H19B H 0.8029 0.8366 0.2837 0.061 Uiso 1 1 calc R . . C20 C 0.9221(2) 0.79217(8) 0.3310(3) 0.0253(6) Uani 1 1 d . . . H20A H 0.8635 0.7808 0.3952 0.030 Uiso 1 1 calc R . . C21 C 1.0141(2) 0.80978(8) 0.4269(3) 0.0229(5) Uani 1 1 d . . . C22 C 0.9706(3) 0.84828(9) 0.5018(4) 0.0337(7) Uani 1 1 d . . . H22A H 1.0285 0.8596 0.5633 0.051 Uiso 1 1 calc R . . H22B H 0.9062 0.8414 0.5607 0.051 Uiso 1 1 calc R . . H22C H 0.9493 0.8683 0.4291 0.051 Uiso 1 1 calc R . . C23 C 1.1172(3) 0.81984(10) 0.3401(4) 0.0424(9) Uani 1 1 d . . . H23A H 1.1446 0.7952 0.2932 0.064 Uiso 1 1 calc R . . H23B H 1.1741 0.8306 0.4043 0.064 Uiso 1 1 calc R . . H23C H 1.0991 0.8402 0.2669 0.064 Uiso 1 1 calc R . . C24 C 1.0421(3) 0.77891(10) 0.5438(4) 0.0394(8) Uani 1 1 d . . . H24A H 1.0704 0.7541 0.4992 0.059 Uiso 1 1 calc R . . H24B H 0.9756 0.7726 0.5993 0.059 Uiso 1 1 calc R . . H24C H 1.0984 0.7903 0.6080 0.059 Uiso 1 1 calc R . . Co' Co 0.5000 0.5000 0.69720(6) 0.01776(14) Uani 1 2 d S . . Cl1' Cl 0.57159(6) 0.44525(2) 0.80755(8) 0.02959(16) Uani 1 1 d . . . N1' N 0.5000 0.5000 0.4785(3) 0.0156(6) Uani 1 2 d S . . C2' C 0.5703(2) 0.52383(8) 0.4054(3) 0.0201(5) Uani 1 1 d . . . C3' C 0.5701(2) 0.52557(11) 0.2568(3) 0.0310(7) Uani 1 1 d . . . H3'A H 0.6169 0.5439 0.2070 0.037 Uiso 1 1 calc R . . C4' C 0.5000 0.5000 0.1823(5) 0.0379(11) Uani 1 2 d S . . H4'A H 0.5000 0.5000 0.0802 0.045 Uiso 1 2 calc SR . . C7' C 0.6489(2) 0.54590(8) 0.4984(3) 0.0176(5) Uani 1 1 d . . . N7' N 0.65312(17) 0.53844(6) 0.6323(2) 0.0167(4) Uani 1 1 d . . . S8' S 0.73549(6) 0.58272(2) 0.42366(8) 0.02825(16) Uani 1 1 d . . . C9' C 0.8082(2) 0.58541(9) 0.5935(3) 0.0279(6) Uani 1 1 d . . . H9'A H 0.8797 0.5710 0.5868 0.033 Uiso 1 1 calc R . . H9'B H 0.8225 0.6140 0.6197 0.033 Uiso 1 1 calc R . . C10' C 0.7339(2) 0.56517(8) 0.7069(3) 0.0193(5) Uani 1 1 d . . . H10B H 0.6911 0.5872 0.7557 0.023 Uiso 1 1 calc R . . C11' C 0.7998(2) 0.54235(8) 0.8241(3) 0.0205(5) Uani 1 1 d . . . C12' C 0.8483(2) 0.50327(9) 0.7641(3) 0.0274(6) Uani 1 1 d . . . H12D H 0.8896 0.4892 0.8398 0.041 Uiso 1 1 calc R . . H12E H 0.8979 0.5097 0.6841 0.041 Uiso 1 1 calc R . . H12F H 0.7885 0.4857 0.7297 0.041 Uiso 1 1 calc R . . C13' C 0.8923(3) 0.57004(11) 0.8785(4) 0.0373(8) Uani 1 1 d . . . H13D H 0.9348 0.5559 0.9528 0.056 Uiso 1 1 calc R . . H13E H 0.8602 0.5948 0.9193 0.056 Uiso 1 1 calc R . . H13F H 0.9410 0.5772 0.7984 0.056 Uiso 1 1 calc R . . C14' C 0.7241(3) 0.53268(9) 0.9502(3) 0.0279(6) Uani 1 1 d . . . H14D H 0.7657 0.5181 1.0243 0.042 Uiso 1 1 calc R . . H14E H 0.6627 0.5157 0.9170 0.042 Uiso 1 1 calc R . . H14F H 0.6950 0.5580 0.9905 0.042 Uiso 1 1 calc R . . C30 C 0.6826(7) 0.66055(16) 0.1377(7) 0.072(2) Uani 0.767(5) 1 d PD A 1 H30A H 0.6832 0.6616 0.2441 0.086 Uiso 0.767(5) 1 calc PR A 1 H30B H 0.7540 0.6492 0.1054 0.086 Uiso 0.767(5) 1 calc PR A 1 Cl3 Cl 0.66706(11) 0.70903(5) 0.06969(19) 0.0623(6) Uani 0.767(5) 1 d PD A 1 Cl4 Cl 0.5688(2) 0.62754(7) 0.0761(3) 0.0815(7) Uani 0.767(5) 1 d PD A 1 C30' C 0.6009(12) 0.6639(4) 0.1465(15) 0.037(3) Uiso 0.233(5) 1 d PD A 2 H30C H 0.5474 0.6849 0.1772 0.045 Uiso 0.233(5) 1 calc PR A 2 H30D H 0.6404 0.6535 0.2320 0.045 Uiso 0.233(5) 1 calc PR A 2 Cl3' Cl 0.6950(8) 0.6835(3) 0.0163(10) 0.116(3) Uiso 0.233(5) 1 d PD A 2 Cl4' Cl 0.5328(8) 0.6233(3) 0.0510(11) 0.084(3) Uiso 0.233(5) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0180(2) 0.0232(2) 0.0151(2) 0.00209(16) 0.00040(16) -0.00200(16) Cl1 0.0264(3) 0.0287(3) 0.0282(3) 0.0027(3) 0.0092(3) -0.0043(3) Cl2 0.0190(3) 0.0295(3) 0.0433(4) 0.0024(3) -0.0045(3) -0.0018(3) N1 0.0189(10) 0.0137(9) 0.0201(11) 0.0018(8) 0.0013(9) -0.0003(8) C2 0.0211(13) 0.0159(11) 0.0153(12) -0.0025(9) 0.0042(10) -0.0046(10) C3 0.0322(15) 0.0211(12) 0.0206(13) -0.0021(10) 0.0006(12) -0.0044(11) C4 0.0385(16) 0.0278(14) 0.0189(13) 0.0014(11) -0.0082(12) -0.0032(12) C5 0.0330(16) 0.0232(14) 0.0243(15) 0.0016(11) -0.0071(12) 0.0027(12) C6 0.0235(14) 0.0172(12) 0.0205(13) 0.0020(10) -0.0024(11) -0.0003(10) C7 0.0192(12) 0.0148(11) 0.0205(14) -0.0045(10) 0.0056(10) -0.0027(10) N7 0.0237(11) 0.0183(10) 0.0232(12) 0.0044(9) 0.0035(9) 0.0066(9) S8 0.0267(3) 0.0198(3) 0.0246(3) -0.0057(3) 0.0074(3) 0.0012(2) C9 0.060(2) 0.0445(19) 0.0298(18) 0.0063(15) 0.0150(17) 0.0308(18) C10 0.0251(14) 0.0254(13) 0.0286(15) 0.0034(12) 0.0040(12) 0.0128(11) C11 0.0329(16) 0.0237(14) 0.0295(16) 0.0068(12) 0.0057(13) 0.0100(12) C12 0.056(2) 0.0358(18) 0.055(2) 0.0078(17) 0.0095(19) -0.0091(17) C13 0.067(3) 0.051(2) 0.042(2) 0.0221(18) 0.0113(19) 0.037(2) C14 0.054(2) 0.0398(18) 0.0250(16) 0.0049(14) 0.0056(14) 0.0140(16) C17 0.0220(13) 0.0208(12) 0.0243(14) -0.0001(11) -0.0029(11) 0.0026(11) N17 0.0225(11) 0.0157(10) 0.0221(12) -0.0012(9) 0.0020(9) 0.0024(9) S18 0.0483(5) 0.0316(4) 0.0398(4) -0.0084(3) -0.0194(4) 0.0220(3) C19 0.073(3) 0.0359(19) 0.044(2) -0.0184(16) -0.0243(19) 0.0324(19) C20 0.0262(14) 0.0244(13) 0.0253(14) -0.0074(11) 0.0010(12) 0.0062(11) C21 0.0257(14) 0.0207(12) 0.0223(13) -0.0038(11) 0.0018(11) -0.0003(10) C22 0.0416(19) 0.0258(15) 0.0336(17) -0.0102(12) -0.0020(15) 0.0016(13) C23 0.0377(19) 0.0312(16) 0.058(2) -0.0082(16) 0.0138(17) -0.0114(14) C24 0.058(2) 0.0340(16) 0.0261(16) -0.0048(13) -0.0067(15) 0.0102(15) Co' 0.0221(3) 0.0194(3) 0.0118(3) 0.000 0.000 0.0072(2) Cl1' 0.0250(3) 0.0222(3) 0.0416(4) 0.0109(3) -0.0125(3) 0.0001(2) N1' 0.0113(14) 0.0173(14) 0.0181(15) 0.000 0.000 0.0056(11) C2' 0.0145(12) 0.0283(14) 0.0176(13) 0.0037(10) 0.0049(10) 0.0096(10) C3' 0.0248(15) 0.0514(19) 0.0169(14) 0.0073(13) 0.0045(11) 0.0018(14) C4' 0.029(2) 0.070(3) 0.015(2) 0.000 0.000 -0.001(2) C7' 0.0127(12) 0.0198(12) 0.0203(13) 0.0057(10) 0.0052(10) 0.0032(10) N7' 0.0107(10) 0.0189(10) 0.0204(11) 0.0002(9) 0.0041(8) 0.0004(8) S8' 0.0251(3) 0.0329(4) 0.0267(4) 0.0128(3) 0.0042(3) -0.0050(3) C9' 0.0238(14) 0.0290(14) 0.0308(16) 0.0099(12) 0.0005(12) -0.0086(11) C10' 0.0176(12) 0.0176(11) 0.0228(13) 0.0011(10) 0.0017(11) -0.0047(9) C11' 0.0185(12) 0.0214(12) 0.0215(13) 0.0022(10) -0.0002(11) -0.0039(10) C12' 0.0190(13) 0.0274(14) 0.0357(16) 0.0048(13) -0.0020(12) 0.0030(11) C13' 0.0317(17) 0.0405(17) 0.0396(19) 0.0028(14) -0.0107(14) -0.0182(14) C14' 0.0273(15) 0.0350(15) 0.0213(14) 0.0035(12) 0.0021(12) -0.0052(12) C30 0.115(7) 0.047(3) 0.053(3) 0.006(3) -0.019(4) 0.024(3) Cl3 0.0470(8) 0.0669(10) 0.0729(11) 0.0260(8) 0.0021(7) -0.0022(6) Cl4 0.0905(16) 0.0576(10) 0.0965(16) 0.0003(9) -0.0383(13) 0.0111(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 Co N1 2.034(2) . ? Co Cl2 2.2518(8) . ? Co N17 2.256(2) . ? Co Cl1 2.2717(8) . ? Co N7 2.353(2) . ? N1 C6 1.333(3) . ? N1 C2 1.352(3) . ? C2 C3 1.387(4) . ? C2 C7 1.480(4) . ? C3 C4 1.390(4) . ? C4 C5 1.382(4) . ? C5 C6 1.380(4) . ? C6 C17 1.486(4) . ? C7 N7 1.265(4) . ? C7 S8 1.748(3) . ? N7 C10 1.484(3) . ? S8 C9 1.798(3) . ? C9 C10 1.553(4) . ? C10 C11 1.538(4) . ? C11 C12 1.529(5) . ? C11 C14 1.531(4) . ? C11 C13 1.539(4) . ? C17 N17 1.279(4) . ? C17 S18 1.747(3) . ? N17 C20 1.490(3) . ? S18 C19 1.807(4) . ? C19 C20 1.545(4) . ? C20 C21 1.542(4) . ? C21 C23 1.524(4) . ? C21 C24 1.527(4) . ? C21 C22 1.541(4) . ? Co' N1' 2.034(3) . ? Co' Cl1' 2.2502(7) 2_665 ? Co' Cl1' 2.2502(7) . ? Co' N7' 2.327(2) . ? Co' N7' 2.327(2) 2_665 ? N1' C2' 1.344(3) 2_665 ? N1' C2' 1.344(3) . ? C2' C3' 1.383(4) . ? C2' C7' 1.478(4) . ? C3' C4' 1.382(4) . ? C4' C3' 1.382(4) 2_665 ? C7' N7' 1.270(4) . ? C7' S8' 1.749(3) . ? N7' C10' 1.489(3) . ? S8' C9' 1.811(3) . ? C9' C10' 1.539(4) . ? C10' C11' 1.547(4) . ? C11' C12' 1.522(4) . ? C11' C14' 1.523(4) . ? C11' C13' 1.532(4) . ? C30 Cl3 1.729(5) . ? C30 Cl4 1.849(7) . ? C30' Cl3' 1.785(12) . ? C30' Cl4' 1.806(12) . ? 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 Co Cl2 120.94(7) . . ? N1 Co N17 76.59(8) . . ? Cl2 Co N17 106.02(6) . . ? N1 Co Cl1 109.30(7) . . ? Cl2 Co Cl1 128.90(3) . . ? N17 Co Cl1 93.35(6) . . ? N1 Co N7 74.27(8) . . ? Cl2 Co N7 86.73(6) . . ? N17 Co N7 150.71(8) . . ? Cl1 Co N7 98.86(6) . . ? C6 N1 C2 119.3(2) . . ? C6 N1 Co 119.08(18) . . ? C2 N1 Co 121.49(17) . . ? N1 C2 C3 121.3(2) . . ? N1 C2 C7 113.1(2) . . ? C3 C2 C7 125.5(2) . . ? C2 C3 C4 118.7(3) . . ? C5 C4 C3 119.6(3) . . ? C6 C5 C4 118.5(3) . . ? N1 C6 C5 122.5(3) . . ? N1 C6 C17 113.1(2) . . ? C5 C6 C17 124.4(2) . . ? N7 C7 C2 120.0(2) . . ? N7 C7 S8 120.2(2) . . ? C2 C7 S8 119.66(19) . . ? C7 N7 C10 112.3(2) . . ? C7 N7 Co 109.51(18) . . ? C10 N7 Co 133.22(19) . . ? C7 S8 C9 89.12(14) . . ? C10 C9 S8 107.7(2) . . ? N7 C10 C11 113.4(2) . . ? N7 C10 C9 108.5(2) . . ? C11 C10 C9 112.0(2) . . ? C12 C11 C14 108.3(3) . . ? C12 C11 C10 111.0(3) . . ? C14 C11 C10 110.2(2) . . ? C12 C11 C13 110.3(3) . . ? C14 C11 C13 108.2(3) . . ? C10 C11 C13 108.8(3) . . ? N17 C17 C6 120.6(2) . . ? N17 C17 S18 119.6(2) . . ? C6 C17 S18 119.8(2) . . ? C17 N17 C20 111.8(2) . . ? C17 N17 Co 109.26(18) . . ? C20 N17 Co 136.62(18) . . ? C17 S18 C19 88.94(14) . . ? C20 C19 S18 107.1(2) . . ? N17 C20 C21 112.9(2) . . ? N17 C20 C19 108.1(2) . . ? C21 C20 C19 111.6(3) . . ? C23 C21 C24 109.9(3) . . ? C23 C21 C22 109.9(2) . . ? C24 C21 C22 107.7(2) . . ? C23 C21 C20 111.6(3) . . ? C24 C21 C20 108.8(2) . . ? C22 C21 C20 108.9(2) . . ? N1' Co' Cl1' 117.14(2) . 2_665 ? N1' Co' Cl1' 117.14(2) . . ? Cl1' Co' Cl1' 125.73(5) 2_665 . ? N1' Co' N7' 74.96(6) . . ? Cl1' Co' N7' 89.37(5) 2_665 . ? Cl1' Co' N7' 104.34(6) . . ? N1' Co' N7' 74.96(6) . 2_665 ? Cl1' Co' N7' 104.34(6) 2_665 2_665 ? Cl1' Co' N7' 89.37(5) . 2_665 ? N7' Co' N7' 149.93(11) . 2_665 ? C2' N1' C2' 119.2(3) 2_665 . ? C2' N1' Co' 120.39(16) 2_665 . ? C2' N1' Co' 120.39(16) . . ? N1' C2' C3' 121.9(3) . . ? N1' C2' C7' 113.6(2) . . ? C3' C2' C7' 124.5(3) . . ? C4' C3' C2' 118.5(3) . . ? C3' C4' C3' 119.9(4) . 2_665 ? N7' C7' C2' 120.3(2) . . ? N7' C7' S8' 120.0(2) . . ? C2' C7' S8' 119.7(2) . . ? C7' N7' C10' 111.6(2) . . ? C7' N7' Co' 109.14(18) . . ? C10' N7' Co' 136.53(17) . . ? C7' S8' C9' 88.80(13) . . ? C10' C9' S8' 106.98(19) . . ? N7' C10' C9' 108.8(2) . . ? N7' C10' C11' 112.4(2) . . ? C9' C10' C11' 113.0(2) . . ? C12' C11' C14' 109.8(2) . . ? C12' C11' C13' 110.1(2) . . ? C14' C11' C13' 108.1(2) . . ? C12' C11' C10' 110.7(2) . . ? C14' C11' C10' 109.4(2) . . ? C13' C11' C10' 108.7(2) . . ? Cl3 C30 Cl4 110.4(3) . . ? Cl3' C30' Cl4' 103.2(8) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 71.41 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.607 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.062 #===END data_[Co(L3)Cl2] _database_code_depnum_ccdc_archive 'CCDC 859237' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H23 Cl2 Co N3 S2, 2/3(CH2Cl2)' _chemical_formula_sum 'C17.67 H24.33 Cl3.33 Co N3 S2' _chemical_formula_weight 519.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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 12.29660(6) _cell_length_b 32.40514(16) _cell_length_c 8.69965(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3466.58(3) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31196 _cell_measurement_theta_min 2.7213 _cell_measurement_theta_max 71.2738 _exptl_crystal_description 'blocky needles' _exptl_crystal_colour Green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1602 _exptl_absorpt_coefficient_mu 11.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.55133 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49848 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 71.42 _reflns_number_total 6703 _reflns_number_gt 6356 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0216 _refine_ls_wR_factor_obs+ 0.0545 _refine_ls_abs_structure_Flack+ 0.0000(19) _refine_ls_R_factor_obs- 0.1300 _refine_ls_wR_factor_obs- 0.3450 _refine_ls_abs_structure_Flack- **** ; _chemical_absolute_configuration ad _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^)+(0.0341P)^2^+0.5031P] 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 SHELXL _refine_ls_extinction_coef 0.00051(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, 2885 Friedel pairs' _refine_ls_abs_structure_Flack -0.0390(18) _refine_ls_number_reflns 6703 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0235 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0557 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 Co Co 0.46153(2) 0.198033(9) 0.25030(3) 0.02086(7) Uani 1 1 d . . . Cl1 Cl 0.60245(4) 0.164284(15) 0.13538(5) 0.03110(11) Uani 1 1 d . . . Cl2 Cl 0.31395(4) 0.208541(17) 0.10137(7) 0.03878(13) Uani 1 1 d . . . N1 N 0.50862(12) 0.20490(5) 0.47711(17) 0.0219(3) Uani 1 1 d . . . C2 C 0.48172(15) 0.17644(6) 0.5826(2) 0.0252(4) Uani 1 1 d . . . C3 C 0.51819(17) 0.17922(7) 0.7333(2) 0.0321(4) Uani 1 1 d . . . H3A H 0.4974 0.1593 0.8079 0.039 Uiso 1 1 calc R . . C4 C 0.58585(18) 0.21189(7) 0.7717(2) 0.0353(5) Uani 1 1 d . . . H4A H 0.6133 0.2141 0.8734 0.042 Uiso 1 1 calc R . . C5 C 0.61358(17) 0.24113(7) 0.6633(2) 0.0299(4) Uani 1 1 d . . . H5A H 0.6599 0.2636 0.6889 0.036 Uiso 1 1 calc R . . C6 C 0.57169(15) 0.23684(6) 0.5152(2) 0.0236(4) Uani 1 1 d . . . C7 C 0.41023(16) 0.14413(6) 0.5178(2) 0.0260(4) Uani 1 1 d . . . N7 N 0.38852(14) 0.14467(5) 0.3749(2) 0.0284(4) Uani 1 1 d . . . S8 S 0.34749(5) 0.107084(15) 0.63372(7) 0.03637(13) Uani 1 1 d . . . C9 C 0.2940(3) 0.08275(9) 0.4632(3) 0.0671(10) Uani 1 1 d . . . H9A H 0.3355 0.0574 0.4393 0.081 Uiso 1 1 calc R . . H9B H 0.2167 0.0752 0.4785 0.081 Uiso 1 1 calc R . . C10 C 0.30491(18) 0.11419(7) 0.3309(3) 0.0369(5) Uani 1 1 d . . . H10A H 0.2341 0.1291 0.3217 0.044 Uiso 1 1 calc R . . C11 C 0.3286(2) 0.09431(8) 0.1776(3) 0.0477(6) Uani 1 1 d . . . H11A H 0.3374 0.1171 0.1012 0.057 Uiso 1 1 calc R . . C12 C 0.4303(3) 0.06909(10) 0.1726(5) 0.0859(13) Uani 1 1 d . . . H12A H 0.4920 0.0860 0.2060 0.129 Uiso 1 1 calc R . . H12B H 0.4429 0.0594 0.0673 0.129 Uiso 1 1 calc R . . H12C H 0.4228 0.0453 0.2413 0.129 Uiso 1 1 calc R . . C13 C 0.2287(3) 0.06890(10) 0.1274(4) 0.0712(9) Uani 1 1 d . . . H13A H 0.1636 0.0863 0.1312 0.107 Uiso 1 1 calc R . . H13B H 0.2195 0.0454 0.1969 0.107 Uiso 1 1 calc R . . H13C H 0.2395 0.0589 0.0223 0.107 Uiso 1 1 calc R . . C17 C 0.58822(14) 0.26582(5) 0.3865(2) 0.0227(4) Uani 1 1 d . . . N17 N 0.54098(12) 0.25923(4) 0.25810(18) 0.0218(3) Uani 1 1 d . . . S18 S 0.67261(4) 0.308687(15) 0.40452(6) 0.03255(11) Uani 1 1 d . . . C19 C 0.62647(18) 0.32686(6) 0.2180(3) 0.0329(5) Uani 1 1 d . . . H19A H 0.5739 0.3497 0.2304 0.039 Uiso 1 1 calc R . . H19B H 0.6887 0.3368 0.1561 0.039 Uiso 1 1 calc R . . C20 C 0.57165(15) 0.28952(6) 0.1388(2) 0.0254(4) Uani 1 1 d . . . H20A H 0.6271 0.2762 0.0709 0.030 Uiso 1 1 calc R . . C21 C 0.47545(17) 0.30193(6) 0.0380(2) 0.0309(4) Uani 1 1 d . . . H21A H 0.4513 0.2768 -0.0191 0.037 Uiso 1 1 calc R . . C22 C 0.5115(2) 0.33399(8) -0.0819(3) 0.0470(6) Uani 1 1 d . . . H22A H 0.4490 0.3419 -0.1453 0.071 Uiso 1 1 calc R . . H22B H 0.5682 0.3221 -0.1474 0.071 Uiso 1 1 calc R . . H22C H 0.5402 0.3584 -0.0293 0.071 Uiso 1 1 calc R . . C23 C 0.37818(18) 0.31773(7) 0.1294(3) 0.0395(5) Uani 1 1 d . . . H23A H 0.3567 0.2970 0.2055 0.059 Uiso 1 1 calc R . . H23B H 0.3173 0.3230 0.0594 0.059 Uiso 1 1 calc R . . H23C H 0.3980 0.3434 0.1822 0.059 Uiso 1 1 calc R . . Co' Co 0.5000 0.5000 0.16649(5) 0.02106(10) Uani 1 2 d S . . Cl1' Cl 0.42396(4) 0.554756(16) 0.28728(6) 0.03723(12) Uani 1 1 d . . . N1' N 0.5000 0.5000 -0.0682(2) 0.0239(5) Uani 1 2 d S . . C2' C 0.42604(18) 0.47768(6) -0.1432(2) 0.0303(4) Uani 1 1 d . . . C3' C 0.4246(2) 0.47629(8) -0.3028(3) 0.0471(6) Uani 1 1 d . . . H3'A H 0.3735 0.4596 -0.3563 0.056 Uiso 1 1 calc R . . C4' C 0.5000 0.5000 -0.3811(4) 0.0613(12) Uani 1 2 d S . . H4'A H 0.5000 0.5000 -0.4903 0.074 Uiso 1 2 calc SR . . C7' C 0.34962(16) 0.45634(6) -0.0397(2) 0.0279(4) Uani 1 1 d . . . N7' N 0.35574(13) 0.46315(5) 0.10451(19) 0.0255(3) Uani 1 1 d . . . S8' S 0.25462(5) 0.420718(19) -0.10711(7) 0.04480(15) Uani 1 1 d . . . C9' C 0.20363(19) 0.41386(7) 0.0874(3) 0.0410(5) Uani 1 1 d . . . H9'A H 0.1283 0.4245 0.0955 0.049 Uiso 1 1 calc R . . H9'B H 0.2035 0.3842 0.1152 0.049 Uiso 1 1 calc R . . C10' C 0.27970(16) 0.43813(6) 0.1959(3) 0.0296(4) Uani 1 1 d . . . H10B H 0.3237 0.4175 0.2547 0.036 Uiso 1 1 calc R . . C11' C 0.22001(17) 0.46495(7) 0.3126(3) 0.0354(5) Uani 1 1 d . . . H11B H 0.2767 0.4787 0.3771 0.042 Uiso 1 1 calc R . . C12' C 0.1541(2) 0.49882(8) 0.2369(4) 0.0525(7) Uani 1 1 d . . . H12D H 0.1189 0.5156 0.3162 0.079 Uiso 1 1 calc R . . H12E H 0.0985 0.4865 0.1706 0.079 Uiso 1 1 calc R . . H12F H 0.2023 0.5163 0.1750 0.079 Uiso 1 1 calc R . . C13' C 0.1499(2) 0.43875(10) 0.4212(3) 0.0562(7) Uani 1 1 d . . . H13D H 0.1131 0.4568 0.4952 0.084 Uiso 1 1 calc R . . H13E H 0.1964 0.4192 0.4765 0.084 Uiso 1 1 calc R . . H13F H 0.0956 0.4236 0.3613 0.084 Uiso 1 1 calc R . . C30 C 0.2982(2) 0.33724(8) 0.5637(3) 0.0484(6) Uani 1 1 d . . . H30A H 0.2581 0.3478 0.6543 0.058 Uiso 1 1 calc R . . H30B H 0.2477 0.3374 0.4751 0.058 Uiso 1 1 calc R . . Cl4 Cl 0.40831(5) 0.37040(2) 0.52407(7) 0.04784(15) Uani 1 1 d . . . Cl5 Cl 0.33983(5) 0.286511(19) 0.59984(10) 0.05729(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 Co 0.01968(14) 0.02215(14) 0.02074(14) -0.00271(12) 0.00030(11) -0.00016(11) Cl1 0.0304(2) 0.0322(2) 0.0307(2) -0.00117(19) 0.00661(18) 0.00891(19) Cl2 0.0280(2) 0.0368(3) 0.0515(3) -0.0020(2) -0.0156(2) 0.0008(2) N1 0.0215(7) 0.0207(7) 0.0236(7) -0.0012(6) -0.0014(6) 0.0021(6) C2 0.0259(10) 0.0245(9) 0.0253(9) 0.0027(7) 0.0039(7) 0.0057(7) C3 0.0366(11) 0.0331(10) 0.0268(10) 0.0062(8) 0.0018(8) 0.0060(8) C4 0.0400(11) 0.0422(12) 0.0237(10) -0.0018(9) -0.0071(9) 0.0064(10) C5 0.0309(10) 0.0315(10) 0.0273(10) -0.0031(8) -0.0059(8) 0.0003(8) C6 0.0224(9) 0.0240(9) 0.0243(9) -0.0030(7) -0.0027(7) 0.0018(7) C7 0.0266(10) 0.0205(9) 0.0310(10) 0.0014(8) 0.0089(8) 0.0036(7) N7 0.0300(9) 0.0236(8) 0.0317(9) -0.0037(7) 0.0077(7) -0.0073(7) S8 0.0424(3) 0.0247(2) 0.0419(3) 0.0079(2) 0.0146(2) -0.0010(2) C9 0.099(2) 0.0534(16) 0.0487(16) -0.0114(13) 0.0277(16) -0.0463(17) C10 0.0303(11) 0.0308(11) 0.0495(14) -0.0107(10) 0.0085(10) -0.0116(9) C11 0.0669(17) 0.0367(12) 0.0395(13) -0.0080(10) 0.0099(12) -0.0213(12) C12 0.064(2) 0.0569(18) 0.137(4) -0.041(2) 0.044(2) -0.0164(15) C13 0.083(2) 0.0551(18) 0.076(2) -0.0247(16) -0.0182(18) -0.0194(16) C17 0.0206(9) 0.0206(9) 0.0268(9) -0.0022(7) -0.0007(7) -0.0004(7) N17 0.0229(7) 0.0185(7) 0.0239(7) -0.0007(6) 0.0013(6) 0.0008(6) S18 0.0349(3) 0.0260(2) 0.0368(3) 0.0001(2) -0.0093(2) -0.0101(2) C19 0.0367(11) 0.0261(10) 0.0358(11) 0.0046(8) -0.0056(9) -0.0081(8) C20 0.0277(10) 0.0236(9) 0.0249(9) 0.0028(7) 0.0034(7) -0.0008(7) C21 0.0374(11) 0.0269(10) 0.0284(10) -0.0003(8) -0.0049(8) 0.0003(9) C22 0.0607(16) 0.0447(13) 0.0356(12) 0.0142(10) -0.0050(11) -0.0005(12) C23 0.0338(11) 0.0368(11) 0.0480(14) 0.0036(10) -0.0032(10) 0.0072(9) Co' 0.0225(2) 0.0236(2) 0.0171(2) 0.000 0.000 0.00049(16) Cl1' 0.0357(3) 0.0315(2) 0.0445(3) -0.0124(2) 0.0089(2) 0.0003(2) N1' 0.0315(12) 0.0216(11) 0.0188(11) 0.000 0.000 0.0025(9) C2' 0.0407(12) 0.0245(9) 0.0256(10) -0.0023(8) -0.0048(8) 0.0062(8) C3' 0.0757(18) 0.0424(13) 0.0231(10) -0.0068(9) -0.0124(11) -0.0031(13) C4' 0.106(4) 0.059(2) 0.0192(15) 0.000 0.000 -0.007(2) C7' 0.0292(10) 0.0233(9) 0.0312(10) -0.0045(8) -0.0069(8) 0.0007(8) N7' 0.0225(8) 0.0250(8) 0.0289(8) -0.0022(7) -0.0022(7) 0.0006(6) S8' 0.0500(3) 0.0420(3) 0.0424(3) -0.0116(3) -0.0132(3) -0.0150(3) C9' 0.0340(11) 0.0370(12) 0.0519(14) -0.0157(11) -0.0006(10) -0.0085(9) C10' 0.0253(10) 0.0237(10) 0.0398(11) 0.0026(8) -0.0027(8) -0.0029(8) C11' 0.0287(10) 0.0406(12) 0.0369(11) -0.0081(10) 0.0035(9) -0.0112(9) C12' 0.0406(12) 0.0356(12) 0.081(2) -0.0055(14) 0.0167(14) 0.0047(10) C13' 0.0451(14) 0.0675(18) 0.0561(17) 0.0057(14) 0.0134(13) -0.0131(13) C30 0.0413(13) 0.0413(13) 0.0627(17) 0.0040(12) 0.0064(11) 0.0018(11) Cl4 0.0508(3) 0.0510(3) 0.0417(3) 0.0042(3) 0.0019(3) -0.0096(3) Cl5 0.0439(3) 0.0369(3) 0.0911(5) -0.0017(3) -0.0032(3) 0.0019(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 Co N1 2.0683(15) . ? Co N17 2.2116(15) . ? Co N7 2.2297(16) . ? Co Cl2 2.2557(6) . ? Co Cl1 2.2799(5) . ? N1 C6 1.335(2) . ? N1 C2 1.343(2) . ? C2 C3 1.388(3) . ? C2 C7 1.479(3) . ? C3 C4 1.387(3) . ? C4 C5 1.379(3) . ? C5 C6 1.395(3) . ? C6 C17 1.476(3) . ? C7 N7 1.272(3) . ? C7 S8 1.7471(19) . ? N7 C10 1.476(3) . ? S8 C9 1.804(3) . ? C9 C10 1.543(4) . ? C10 C11 1.509(3) . ? C11 C12 1.495(4) . ? C11 C13 1.542(4) . ? C17 N17 1.277(2) . ? C17 S18 1.7409(18) . ? N17 C20 1.478(2) . ? S18 C19 1.817(2) . ? C19 C20 1.547(3) . ? C20 C21 1.526(3) . ? C21 C23 1.525(3) . ? C21 C22 1.537(3) . ? Co' N1' 2.042(2) . ? Co' N7' 2.2053(16) . ? Co' N7' 2.2053(16) 2_665 ? Co' Cl1' 2.2642(5) . ? Co' Cl1' 2.2642(5) 2_665 ? N1' C2' 1.332(2) . ? N1' C2' 1.332(2) 2_665 ? C2' C3' 1.389(3) . ? C2' C7' 1.473(3) . ? C3' C4' 1.383(3) . ? C4' C3' 1.383(3) 2_665 ? C7' N7' 1.276(3) . ? C7' S8' 1.744(2) . ? N7' C10' 1.471(3) . ? S8' C9' 1.819(3) . ? C9' C10' 1.544(3) . ? C10' C11' 1.525(3) . ? C11' C12' 1.515(3) . ? C11' C13' 1.535(3) . ? C30 Cl5 1.750(3) . ? C30 Cl4 1.763(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 Co N17 75.56(6) . . ? N1 Co N7 74.47(6) . . ? N17 Co N7 149.12(6) . . ? N1 Co Cl2 139.19(5) . . ? N17 Co Cl2 103.75(4) . . ? N7 Co Cl2 94.15(5) . . ? N1 Co Cl1 104.90(4) . . ? N17 Co Cl1 96.19(4) . . ? N7 Co Cl1 98.47(5) . . ? Cl2 Co Cl1 115.60(2) . . ? C6 N1 C2 120.38(17) . . ? C6 N1 Co 118.88(12) . . ? C2 N1 Co 120.62(13) . . ? N1 C2 C3 121.43(18) . . ? N1 C2 C7 111.85(17) . . ? C3 C2 C7 126.71(18) . . ? C4 C3 C2 118.08(19) . . ? C5 C4 C3 120.53(19) . . ? C4 C5 C6 118.13(19) . . ? N1 C6 C5 121.42(18) . . ? N1 C6 C17 112.64(16) . . ? C5 C6 C17 125.93(18) . . ? N7 C7 C2 119.18(17) . . ? N7 C7 S8 118.75(16) . . ? C2 C7 S8 121.95(15) . . ? C7 N7 C10 112.99(17) . . ? C7 N7 Co 113.68(13) . . ? C10 N7 Co 132.30(15) . . ? C7 S8 C9 89.25(11) . . ? C10 C9 S8 107.04(17) . . ? N7 C10 C11 112.38(18) . . ? N7 C10 C9 108.0(2) . . ? C11 C10 C9 113.2(2) . . ? C12 C11 C10 114.8(3) . . ? C12 C11 C13 111.5(2) . . ? C10 C11 C13 108.9(2) . . ? N17 C17 C6 119.64(16) . . ? N17 C17 S18 118.91(14) . . ? C6 C17 S18 121.45(14) . . ? C17 N17 C20 112.78(15) . . ? C17 N17 Co 112.20(12) . . ? C20 N17 Co 133.38(12) . . ? C17 S18 C19 89.55(9) . . ? C20 C19 S18 106.29(13) . . ? N17 C20 C21 112.38(15) . . ? N17 C20 C19 108.53(15) . . ? C21 C20 C19 112.81(16) . . ? C23 C21 C20 113.36(17) . . ? C23 C21 C22 110.66(19) . . ? C20 C21 C22 110.14(18) . . ? N1' Co' N7' 75.85(5) . . ? N1' Co' N7' 75.85(5) . 2_665 ? N7' Co' N7' 151.70(9) . 2_665 ? N1' Co' Cl1' 117.651(17) . . ? N7' Co' Cl1' 101.86(4) . . ? N7' Co' Cl1' 91.22(4) 2_665 . ? N1' Co' Cl1' 117.651(17) . 2_665 ? N7' Co' Cl1' 91.22(4) . 2_665 ? N7' Co' Cl1' 101.86(4) 2_665 2_665 ? Cl1' Co' Cl1' 124.70(3) . 2_665 ? C2' N1' C2' 121.4(2) . 2_665 ? C2' N1' Co' 119.30(12) . . ? C2' N1' Co' 119.30(12) 2_665 . ? N1' C2' C3' 121.0(2) . . ? N1' C2' C7' 113.02(18) . . ? C3' C2' C7' 126.0(2) . . ? C4' C3' C2' 117.7(2) . . ? C3' C4' C3' 121.0(3) 2_665 . ? N7' C7' C2' 118.81(18) . . ? N7' C7' S8' 118.97(16) . . ? C2' C7' S8' 122.18(15) . . ? C7' N7' C10' 113.50(17) . . ? C7' N7' Co' 112.42(14) . . ? C10' N7' Co' 132.64(13) . . ? C7' S8' C9' 89.95(10) . . ? C10' C9' S8' 107.32(15) . . ? N7' C10' C11' 110.58(16) . . ? N7' C10' C9' 109.58(18) . . ? C11' C10' C9' 113.93(17) . . ? C12' C11' C10' 112.4(2) . . ? C12' C11' C13' 111.6(2) . . ? C10' C11' C13' 111.4(2) . . ? Cl5 C30 Cl4 112.51(14) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 71.42 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.227 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.042 #===END data_[Co(L5)Cl2] _database_code_depnum_ccdc_archive 'CCDC 859238' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 Cl2 Co N3 S2' _chemical_formula_sum 'C25 H19 Cl2 Co N3 S2' _chemical_formula_weight 555.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 '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 15.10734(17) _cell_length_b 10.71590(11) _cell_length_c 15.64386(17) _cell_angle_alpha 90 _cell_angle_beta 109.7307(12) _cell_angle_gamma 90 _cell_volume 2383.88(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9274 _cell_measurement_theta_min 2.9958 _cell_measurement_theta_max 71.1833 _exptl_crystal_description blocks _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.2397 _exptl_crystal_size_mid 0.1307 _exptl_crystal_size_min 0.1033 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.547 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1132 _exptl_absorpt_coefficient_mu 9.497 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.272 _exptl_absorpt_correction_T_max 0.474 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19167 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0298 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 71.45 _reflns_number_total 4579 _reflns_number_gt 3679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0389P)^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 SHELXL _refine_ls_extinction_coef 0.00065(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4579 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0615 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _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 Co Co 0.274323(19) 0.34109(3) 0.49440(2) 0.02151(8) Uani 1 1 d . . . Cl1 Cl 0.25497(3) 0.53167(4) 0.55113(3) 0.03006(11) Uani 1 1 d . . . Cl2 Cl 0.16829(3) 0.20936(5) 0.40427(3) 0.03095(11) Uani 1 1 d . . . N1 N 0.41538(10) 0.30929(14) 0.54310(10) 0.0219(3) Uani 1 1 d . . . C2 C 0.46957(12) 0.33846(17) 0.49312(12) 0.0223(4) Uani 1 1 d . . . C3 C 0.56693(13) 0.32750(17) 0.52837(13) 0.0263(4) Uani 1 1 d . . . H3A H 0.6046 0.3486 0.4926 0.032 Uiso 1 1 calc R . . C4 C 0.60769(12) 0.28539(18) 0.61636(13) 0.0273(4) Uani 1 1 d . . . H4A H 0.6740 0.2762 0.6413 0.033 Uiso 1 1 calc R . . C5 C 0.55219(13) 0.25646(18) 0.66855(13) 0.0267(4) Uani 1 1 d . . . H5A H 0.5796 0.2280 0.7293 0.032 Uiso 1 1 calc R . . C6 C 0.45560(12) 0.27037(17) 0.62938(12) 0.0232(4) Uani 1 1 d . . . C7 C 0.41569(12) 0.38447(17) 0.40250(12) 0.0223(4) Uani 1 1 d . . . N7 N 0.32557(10) 0.41149(14) 0.38001(10) 0.0224(3) Uani 1 1 d . . . S8 S 0.46260(3) 0.40789(5) 0.31794(3) 0.02993(12) Uani 1 1 d . . . C9 C 0.35565(13) 0.45890(19) 0.24861(13) 0.0294(4) Uani 1 1 d . . . H9A H 0.3429 0.4855 0.1877 0.035 Uiso 1 1 calc R . . C10 C 0.29034(13) 0.45667(17) 0.29181(12) 0.0245(4) Uani 1 1 d . . . C11 C 0.19264(13) 0.50149(18) 0.25232(13) 0.0260(4) Uani 1 1 d . . . C12 C 0.15218(14) 0.52098(19) 0.15896(13) 0.0314(4) Uani 1 1 d . . . H12A H 0.1888 0.5088 0.1208 0.038 Uiso 1 1 calc R . . C13 C 0.05898(14) 0.55803(19) 0.12142(14) 0.0351(5) Uani 1 1 d . . . H13A H 0.0328 0.5710 0.0577 0.042 Uiso 1 1 calc R . . C14 C 0.00312(14) 0.5766(2) 0.17490(15) 0.0357(5) Uani 1 1 d . . . C15 C 0.04555(14) 0.5643(2) 0.26835(15) 0.0364(5) Uani 1 1 d . . . H15A H 0.0099 0.5815 0.3067 0.044 Uiso 1 1 calc R . . C16 C 0.13839(13) 0.5276(2) 0.30681(13) 0.0313(4) Uani 1 1 d . . . H16A H 0.1655 0.5201 0.3709 0.038 Uiso 1 1 calc R . . C17 C -0.10001(14) 0.6082(2) 0.13393(17) 0.0484(6) Uani 1 1 d . . . H17A H -0.1181 0.6102 0.0676 0.073 Uiso 1 1 calc R . . H17B H -0.1116 0.6901 0.1560 0.073 Uiso 1 1 calc R . . H17C H -0.1373 0.5448 0.1516 0.073 Uiso 1 1 calc R . . C18 C 0.38618(13) 0.24197(18) 0.67369(12) 0.0253(4) Uani 1 1 d . . . N18 N 0.29575(10) 0.24671(15) 0.62637(10) 0.0235(3) Uani 1 1 d . . . S19 S 0.41226(4) 0.19479(6) 0.78363(3) 0.03554(13) Uani 1 1 d . . . C20 C 0.29465(14) 0.1757(2) 0.76434(14) 0.0365(5) Uani 1 1 d . . . H20A H 0.2691 0.1470 0.8085 0.044 Uiso 1 1 calc R . . C21 C 0.24223(14) 0.20714(19) 0.67722(13) 0.0286(4) Uani 1 1 d . . . C22 C 0.13936(13) 0.1930(2) 0.63621(13) 0.0286(4) Uani 1 1 d . . . C23 C 0.09680(14) 0.0826(2) 0.64987(14) 0.0336(5) Uani 1 1 d . . . H23A H 0.1337 0.0195 0.6883 0.040 Uiso 1 1 calc R . . C24 C 0.00140(14) 0.0646(2) 0.60791(15) 0.0360(5) Uani 1 1 d . . . H24A H -0.0261 -0.0120 0.6164 0.043 Uiso 1 1 calc R . . C25 C -0.05527(14) 0.1566(2) 0.55341(14) 0.0328(5) Uani 1 1 d . . . C26 C -0.01281(14) 0.2675(2) 0.54126(13) 0.0328(5) Uani 1 1 d . . . H26A H -0.0503 0.3318 0.5049 0.039 Uiso 1 1 calc R . . C27 C 0.08333(13) 0.2855(2) 0.58125(13) 0.0311(4) Uani 1 1 d . . . H27A H 0.1111 0.3611 0.5712 0.037 Uiso 1 1 calc R . . C28 C -0.15962(14) 0.1367(2) 0.50740(16) 0.0424(5) Uani 1 1 d . . . H28A H -0.1944 0.1912 0.5352 0.064 Uiso 1 1 calc R . . H28B H -0.1752 0.0494 0.5144 0.064 Uiso 1 1 calc R . . H28C H -0.1769 0.1566 0.4427 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.01887(15) 0.02354(16) 0.02099(15) -0.00229(13) 0.00526(11) -0.00202(12) Cl1 0.0385(3) 0.0267(2) 0.0294(2) -0.00524(19) 0.0173(2) -0.00128(19) Cl2 0.0316(2) 0.0327(3) 0.0263(2) -0.00675(19) 0.00688(19) -0.01087(19) N1 0.0205(7) 0.0233(8) 0.0218(8) -0.0001(6) 0.0071(6) -0.0016(6) C2 0.0250(9) 0.0190(9) 0.0248(9) -0.0021(8) 0.0109(8) -0.0020(7) C3 0.0239(9) 0.0233(10) 0.0334(10) -0.0008(8) 0.0121(8) -0.0014(7) C4 0.0191(9) 0.0250(10) 0.0359(11) -0.0014(8) 0.0067(8) -0.0004(7) C5 0.0259(9) 0.0245(10) 0.0252(10) 0.0011(8) 0.0029(8) 0.0001(7) C6 0.0240(9) 0.0236(10) 0.0216(9) -0.0005(8) 0.0071(7) -0.0006(7) C7 0.0249(9) 0.0206(9) 0.0240(9) -0.0007(7) 0.0115(8) -0.0035(7) N7 0.0238(8) 0.0216(8) 0.0227(8) -0.0009(6) 0.0090(6) -0.0038(6) S8 0.0320(3) 0.0336(3) 0.0301(3) 0.0063(2) 0.0183(2) 0.0036(2) C9 0.0353(11) 0.0306(11) 0.0239(10) 0.0035(8) 0.0123(8) 0.0006(8) C10 0.0290(10) 0.0218(10) 0.0224(9) -0.0009(8) 0.0085(8) -0.0032(7) C11 0.0280(10) 0.0236(10) 0.0252(10) -0.0004(8) 0.0074(8) -0.0046(7) C12 0.0365(11) 0.0293(11) 0.0268(10) 0.0009(9) 0.0086(9) -0.0040(8) C13 0.0417(12) 0.0294(12) 0.0257(10) 0.0041(9) 0.0001(9) -0.0040(9) C14 0.0317(11) 0.0286(11) 0.0399(12) 0.0058(10) 0.0030(9) -0.0021(9) C15 0.0335(11) 0.0391(13) 0.0359(12) 0.0043(10) 0.0109(9) 0.0026(9) C16 0.0285(10) 0.0363(12) 0.0265(10) 0.0011(9) 0.0059(8) -0.0001(8) C17 0.0313(12) 0.0483(15) 0.0552(15) 0.0140(12) 0.0011(11) 0.0032(10) C18 0.0275(10) 0.0269(10) 0.0206(9) 0.0016(8) 0.0070(8) 0.0005(8) N18 0.0240(8) 0.0281(9) 0.0197(7) 0.0034(7) 0.0089(6) -0.0004(6) S19 0.0311(3) 0.0530(3) 0.0214(2) 0.0091(2) 0.00737(19) 0.0035(2) C20 0.0342(11) 0.0526(14) 0.0260(10) 0.0083(10) 0.0145(9) -0.0002(10) C21 0.0307(10) 0.0320(11) 0.0262(10) 0.0032(8) 0.0139(8) -0.0005(8) C22 0.0293(10) 0.0354(11) 0.0262(10) 0.0011(8) 0.0161(8) -0.0012(8) C23 0.0320(11) 0.0376(12) 0.0354(11) 0.0077(9) 0.0168(9) 0.0019(9) C24 0.0335(11) 0.0368(12) 0.0443(12) 0.0044(10) 0.0218(10) -0.0035(9) C25 0.0297(11) 0.0401(12) 0.0329(11) -0.0014(9) 0.0163(9) -0.0017(9) C26 0.0328(11) 0.0369(12) 0.0307(11) 0.0034(9) 0.0134(9) 0.0027(9) C27 0.0306(10) 0.0334(11) 0.0334(11) 0.0014(9) 0.0164(9) -0.0032(8) C28 0.0310(11) 0.0475(15) 0.0482(14) 0.0056(11) 0.0129(10) -0.0031(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 Co N1 2.0351(14) . ? Co N18 2.2224(15) . ? Co Cl2 2.2409(5) . ? Co Cl1 2.2844(5) . ? Co N7 2.3036(14) . ? N1 C2 1.346(2) . ? N1 C6 1.346(2) . ? C2 C3 1.391(2) . ? C2 C7 1.462(3) . ? C3 C4 1.380(3) . ? C4 C5 1.389(3) . ? C5 C6 1.387(2) . ? C6 C18 1.471(2) . ? C7 N7 1.318(2) . ? C7 S8 1.7170(17) . ? N7 C10 1.388(2) . ? S8 C9 1.704(2) . ? C9 C10 1.372(2) . ? C10 C11 1.475(3) . ? C11 C12 1.396(3) . ? C11 C16 1.396(3) . ? C12 C13 1.388(3) . ? C13 C14 1.389(3) . ? C14 C15 1.390(3) . ? C14 C17 1.510(3) . ? C15 C16 1.383(3) . ? C18 N18 1.317(2) . ? C18 S19 1.7061(18) . ? N18 C21 1.378(2) . ? S19 C20 1.711(2) . ? C20 C21 1.367(3) . ? C21 C22 1.475(3) . ? C22 C27 1.395(3) . ? C22 C23 1.397(3) . ? C23 C24 1.381(3) . ? C24 C25 1.392(3) . ? C25 C26 1.393(3) . ? C25 C28 1.511(3) . ? C26 C27 1.387(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 Co N18 76.72(6) . . ? N1 Co Cl2 124.46(5) . . ? N18 Co Cl2 98.44(4) . . ? N1 Co Cl1 105.04(5) . . ? N18 Co Cl1 92.50(4) . . ? Cl2 Co Cl1 130.51(2) . . ? N1 Co N7 76.20(5) . . ? N18 Co N7 152.75(5) . . ? Cl2 Co N7 94.23(4) . . ? Cl1 Co N7 97.45(4) . . ? C2 N1 C6 119.83(15) . . ? C2 N1 Co 120.60(12) . . ? C6 N1 Co 119.24(11) . . ? N1 C2 C3 121.29(17) . . ? N1 C2 C7 113.15(15) . . ? C3 C2 C7 125.54(16) . . ? C4 C3 C2 118.63(17) . . ? C3 C4 C5 120.31(17) . . ? C6 C5 C4 118.06(17) . . ? N1 C6 C5 121.86(16) . . ? N1 C6 C18 112.61(16) . . ? C5 C6 C18 125.51(17) . . ? N7 C7 C2 121.32(15) . . ? N7 C7 S8 114.83(14) . . ? C2 C7 S8 123.85(13) . . ? C7 N7 C10 110.92(14) . . ? C7 N7 Co 107.96(11) . . ? C10 N7 Co 140.35(12) . . ? C9 S8 C7 89.31(9) . . ? C10 C9 S8 111.48(14) . . ? C9 C10 N7 113.44(17) . . ? C9 C10 C11 124.93(17) . . ? N7 C10 C11 121.59(16) . . ? C12 C11 C16 117.98(18) . . ? C12 C11 C10 120.66(17) . . ? C16 C11 C10 121.35(17) . . ? C13 C12 C11 120.59(19) . . ? C12 C13 C14 121.46(19) . . ? C13 C14 C15 117.51(19) . . ? C13 C14 C17 121.8(2) . . ? C15 C14 C17 120.7(2) . . ? C16 C15 C14 121.6(2) . . ? C15 C16 C11 120.63(19) . . ? N18 C18 C6 119.77(16) . . ? N18 C18 S19 114.89(13) . . ? C6 C18 S19 125.27(14) . . ? C18 N18 C21 111.28(16) . . ? C18 N18 Co 109.75(11) . . ? C21 N18 Co 138.26(13) . . ? C18 S19 C20 89.14(9) . . ? C21 C20 S19 111.33(14) . . ? C20 C21 N18 113.32(17) . . ? C20 C21 C22 125.36(17) . . ? N18 C21 C22 121.17(17) . . ? C27 C22 C23 118.74(18) . . ? C27 C22 C21 121.72(18) . . ? C23 C22 C21 119.50(19) . . ? C24 C23 C22 120.4(2) . . ? C23 C24 C25 121.3(2) . . ? C24 C25 C26 118.09(19) . . ? C24 C25 C28 121.25(19) . . ? C26 C25 C28 120.7(2) . . ? C27 C26 C25 121.2(2) . . ? C26 C27 C22 120.27(19) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 71.45 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.217 _refine_diff_density_min -0.210 _refine_diff_density_rms 0.047 #===END data_[Ni(L8)Br] _database_code_depnum_ccdc_archive 'CCDC 859239' #TrackingRef 'Dalton 12-11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H19 Br N2 Ni S2, C H2 Cl2' _chemical_formula_sum 'C25 H21 Br Cl2 N2 Ni S2' _chemical_formula_weight 623.08 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' S S 0.1246 0.1234 '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' Ni Ni 0.3393 1.1124 '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(1) 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' _cell_length_a 7.66033(7) _cell_length_b 12.99066(11) _cell_length_c 24.7438(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2462.33(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 45860 _cell_measurement_theta_min 3.9429 _cell_measurement_theta_max 32.2793 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.681 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 2.815 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.79841 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81747 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 3.95 _diffrn_reflns_theta_max 32.38 _reflns_number_total 8437 _reflns_number_gt 7117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0310 _refine_ls_wR_factor_obs+ 0.0729 _refine_ls_abs_structure_Flack+ 0.000(6) _refine_ls_R_factor_obs- 0.0647 _refine_ls_wR_factor_obs- 0.1653 _refine_ls_abs_structure_Flack- **** ; _chemical_absolute_configuration ad _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^)+(0.0402P)^2^+1.5513P] 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, 3667 Friedel pairs' _refine_ls_abs_structure_Flack -0.013(6) _refine_ls_number_reflns 8437 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0797 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _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 Ni Ni 0.77581(3) 0.50163(2) 0.589102(9) 0.01529(5) Uani 1 1 d . . . Br Br 0.77716(3) 0.504366(17) 0.684256(8) 0.02353(5) Uani 1 1 d . . . C1 C 0.7745(3) 0.49920(15) 0.51487(8) 0.0171(3) Uani 1 1 d . . . C2 C 0.7399(3) 0.58900(15) 0.48655(9) 0.0174(4) Uani 1 1 d . . . C3 C 0.7387(3) 0.58870(18) 0.42994(9) 0.0209(4) Uani 1 1 d . . . H3A H 0.7131 0.6495 0.4101 0.025 Uiso 1 1 calc R . . C4 C 0.7763(3) 0.49612(17) 0.40352(8) 0.0234(4) Uani 1 1 d . . . H4A H 0.7781 0.4952 0.3651 0.028 Uiso 1 1 calc R . . C5 C 0.8112(3) 0.40542(17) 0.43138(9) 0.0206(4) Uani 1 1 d . . . H5A H 0.8353 0.3434 0.4125 0.025 Uiso 1 1 calc R . . C6 C 0.8100(3) 0.40782(15) 0.48806(9) 0.0178(4) Uani 1 1 d . . . C7 C 0.7124(3) 0.67121(15) 0.52555(8) 0.0176(4) Uani 1 1 d . . . N7 N 0.7253(2) 0.64444(13) 0.57622(7) 0.0175(3) Uani 1 1 d . . . S8 S 0.66432(8) 0.79929(4) 0.51208(2) 0.02352(11) Uani 1 1 d . . . C9 C 0.7100(3) 0.82954(17) 0.58264(10) 0.0245(4) Uani 1 1 d . . . H9A H 0.8315 0.8542 0.5869 0.029 Uiso 1 1 calc R . . H9B H 0.6295 0.8835 0.5960 0.029 Uiso 1 1 calc R . . C10 C 0.6823(3) 0.72819(16) 0.61395(9) 0.0188(4) Uani 1 1 d . . . H10A H 0.7665 0.7260 0.6448 0.023 Uiso 1 1 calc R . . C11 C 0.4984(3) 0.71830(15) 0.63615(9) 0.0164(3) Uani 1 1 d . . . C12 C 0.3754(3) 0.65014(16) 0.61520(9) 0.0200(4) Uani 1 1 d . . . H12A H 0.4069 0.6054 0.5864 0.024 Uiso 1 1 calc R . . C13 C 0.2078(3) 0.64697(16) 0.63593(11) 0.0237(4) Uani 1 1 d . . . H13A H 0.1252 0.5999 0.6214 0.028 Uiso 1 1 calc R . . C14 C 0.1595(3) 0.71210(18) 0.67780(10) 0.0251(4) Uani 1 1 d . . . H14A H 0.0440 0.7102 0.6918 0.030 Uiso 1 1 calc R . . C15 C 0.2819(3) 0.78019(18) 0.69910(9) 0.0239(5) Uani 1 1 d . . . H15A H 0.2503 0.8246 0.7280 0.029 Uiso 1 1 calc R . . C16 C 0.4494(3) 0.78335(17) 0.67825(9) 0.0211(4) Uani 1 1 d . . . H16A H 0.5319 0.8304 0.6928 0.025 Uiso 1 1 calc R . . C17 C 0.8363(3) 0.32768(15) 0.52841(8) 0.0178(4) Uani 1 1 d . . . N17 N 0.8241(2) 0.35803(13) 0.57861(7) 0.0176(3) Uani 1 1 d . . . S18 S 0.87908(8) 0.19835(4) 0.51691(2) 0.02593(12) Uani 1 1 d . . . C19 C 0.8379(3) 0.17302(17) 0.58814(10) 0.0256(5) Uani 1 1 d . . . H19A H 0.7165 0.1491 0.5936 0.031 Uiso 1 1 calc R . . H19B H 0.9187 0.1196 0.6019 0.031 Uiso 1 1 calc R . . C20 C 0.8684(3) 0.27611(16) 0.61761(9) 0.0189(4) Uani 1 1 d . . . H20A H 0.7858 0.2805 0.6488 0.023 Uiso 1 1 calc R . . C21 C 1.0535(3) 0.28701(14) 0.63880(9) 0.0168(3) Uani 1 1 d . . . C22 C 1.1770(3) 0.35165(16) 0.61558(9) 0.0187(4) Uani 1 1 d . . . H22A H 1.1462 0.3931 0.5854 0.022 Uiso 1 1 calc R . . C23 C 1.3461(3) 0.35593(17) 0.63638(11) 0.0240(4) Uani 1 1 d . . . H23A H 1.4295 0.4010 0.6207 0.029 Uiso 1 1 calc R . . C24 C 1.3931(3) 0.29455(18) 0.67998(10) 0.0253(4) Uani 1 1 d . . . H24A H 1.5088 0.2969 0.6938 0.030 Uiso 1 1 calc R . . C25 C 1.2695(3) 0.22945(18) 0.70342(9) 0.0243(5) Uani 1 1 d . . . H25A H 1.3005 0.1874 0.7333 0.029 Uiso 1 1 calc R . . C26 C 1.1021(3) 0.22653(17) 0.68296(9) 0.0217(4) Uani 1 1 d . . . H26A H 1.0182 0.1825 0.6992 0.026 Uiso 1 1 calc R . . C30 C 0.7935(4) -0.0026(2) 0.74062(10) 0.0351(5) Uani 1 1 d . A 1 H30A H 0.8666 0.0445 0.7625 0.042 Uiso 1 1 calc R A 1 H30B H 0.7425 -0.0547 0.7652 0.042 Uiso 1 1 calc R A 1 Cl1 Cl 0.92338(11) -0.06380(7) 0.69222(4) 0.0497(2) Uani 1 1 d . A 1 Cl2 Cl 0.62543(11) 0.06751(7) 0.70953(4) 0.0539(2) Uani 1 1 d . A 1 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 Ni 0.01589(11) 0.01564(11) 0.01433(10) 0.00049(11) -0.00049(8) 0.00235(11) Br 0.02980(11) 0.02539(10) 0.01539(8) 0.00072(9) -0.00126(7) 0.00154(10) C1 0.0182(8) 0.0158(7) 0.0172(8) -0.0016(8) 0.0001(6) 0.0017(8) C2 0.0185(10) 0.0163(8) 0.0175(9) -0.0003(7) 0.0016(8) -0.0006(7) C3 0.0245(11) 0.0223(10) 0.0159(9) 0.0015(7) -0.0001(8) -0.0021(8) C4 0.0298(10) 0.0242(9) 0.0163(8) 0.0004(9) -0.0001(7) -0.0032(10) C5 0.0247(11) 0.0184(9) 0.0187(10) -0.0038(7) -0.0016(8) -0.0011(8) C6 0.0184(10) 0.0177(8) 0.0174(9) 0.0002(7) -0.0023(8) 0.0007(7) C7 0.0176(9) 0.0163(8) 0.0188(9) 0.0019(7) 0.0005(8) 0.0028(7) N7 0.0182(8) 0.0179(7) 0.0162(8) -0.0021(6) 0.0004(7) 0.0028(7) S8 0.0306(3) 0.0165(2) 0.0234(2) 0.0032(2) 0.0028(2) 0.0026(2) C9 0.0283(12) 0.0192(9) 0.0260(11) -0.0028(8) 0.0042(9) -0.0029(8) C10 0.0196(10) 0.0167(8) 0.0200(9) -0.0028(7) -0.0003(7) 0.0013(7) C11 0.0180(9) 0.0165(8) 0.0145(8) 0.0005(8) -0.0015(7) 0.0025(7) C12 0.0231(11) 0.0147(8) 0.0222(10) -0.0003(8) -0.0009(8) -0.0001(8) C13 0.0234(11) 0.0203(9) 0.0274(11) 0.0021(9) -0.0015(10) -0.0021(8) C14 0.0231(11) 0.0278(10) 0.0245(11) 0.0068(9) 0.0032(8) 0.0050(9) C15 0.0255(12) 0.0271(10) 0.0193(10) 0.0006(8) 0.0019(9) 0.0075(9) C16 0.0239(11) 0.0220(9) 0.0174(9) -0.0023(8) -0.0022(8) 0.0026(8) C17 0.0183(9) 0.0159(8) 0.0191(9) -0.0010(7) -0.0018(7) 0.0005(7) N17 0.0188(8) 0.0166(7) 0.0175(8) 0.0022(6) -0.0024(7) 0.0022(6) S18 0.0343(3) 0.0165(2) 0.0269(3) -0.0024(2) -0.0056(2) 0.0031(2) C19 0.0281(12) 0.0180(9) 0.0306(12) 0.0027(8) -0.0070(10) -0.0037(8) C20 0.0184(10) 0.0174(9) 0.0209(9) 0.0042(7) -0.0023(8) 0.0010(7) C21 0.0180(9) 0.0152(8) 0.0171(8) -0.0002(8) -0.0018(8) 0.0014(7) C22 0.0195(10) 0.0163(8) 0.0203(10) 0.0018(7) 0.0005(8) 0.0013(7) C23 0.0210(11) 0.0257(10) 0.0254(10) -0.0036(9) 0.0006(10) -0.0024(8) C24 0.0187(10) 0.0312(11) 0.0260(11) -0.0059(9) -0.0047(8) 0.0038(9) C25 0.0251(12) 0.0284(10) 0.0193(10) 0.0039(8) -0.0036(9) 0.0051(9) C26 0.0228(11) 0.0221(9) 0.0201(10) 0.0027(8) -0.0011(8) 0.0012(8) C30 0.0499(15) 0.0298(11) 0.0256(10) 0.0017(10) 0.0013(10) -0.0001(14) Cl1 0.0424(4) 0.0537(4) 0.0530(5) -0.0261(4) -0.0103(3) 0.0193(3) Cl2 0.0358(4) 0.0500(4) 0.0760(6) -0.0127(4) -0.0022(4) 0.0137(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 Ni C1 1.8371(19) . ? Ni N17 1.9193(17) . ? Ni N7 1.9217(18) . ? Ni Br 2.3548(3) . ? C1 C2 1.387(3) . ? C1 C6 1.387(3) . ? C2 C3 1.401(3) . ? C2 C7 1.455(3) . ? C3 C4 1.399(3) . ? C4 C5 1.391(3) . ? C5 C6 1.403(3) . ? C6 C17 1.456(3) . ? C7 N7 1.305(3) . ? C7 S8 1.736(2) . ? N7 C10 1.471(3) . ? S8 C9 1.823(2) . ? C9 C10 1.542(3) . ? C10 C11 1.518(3) . ? C11 C12 1.393(3) . ? C11 C16 1.393(3) . ? C12 C13 1.383(3) . ? C13 C14 1.388(3) . ? C14 C15 1.393(4) . ? C15 C16 1.384(3) . ? C17 N17 1.307(3) . ? C17 S18 1.735(2) . ? N17 C20 1.476(3) . ? S18 C19 1.821(3) . ? C19 C20 1.543(3) . ? C20 C21 1.519(3) . ? C21 C22 1.389(3) . ? C21 C26 1.396(3) . ? C22 C23 1.395(3) . ? C23 C24 1.389(3) . ? C24 C25 1.396(4) . ? C25 C26 1.379(3) . ? C30 Cl1 1.748(3) . ? C30 Cl2 1.755(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 C1 Ni N17 81.32(8) . . ? C1 Ni N7 81.35(8) . . ? N17 Ni N7 162.67(8) . . ? C1 Ni Br 179.87(7) . . ? N17 Ni Br 98.57(5) . . ? N7 Ni Br 98.75(5) . . ? C2 C1 C6 121.06(19) . . ? C2 C1 Ni 119.46(15) . . ? C6 C1 Ni 119.47(15) . . ? C1 C2 C3 120.28(19) . . ? C1 C2 C7 108.07(18) . . ? C3 C2 C7 131.64(19) . . ? C4 C3 C2 117.9(2) . . ? C5 C4 C3 122.4(2) . . ? C4 C5 C6 118.38(19) . . ? C1 C6 C5 119.91(19) . . ? C1 C6 C17 108.12(18) . . ? C5 C6 C17 131.95(19) . . ? N7 C7 C2 115.52(18) . . ? N7 C7 S8 117.12(16) . . ? C2 C7 S8 127.36(16) . . ? C7 N7 C10 113.31(17) . . ? C7 N7 Ni 115.59(14) . . ? C10 N7 Ni 130.83(14) . . ? C7 S8 C9 88.97(10) . . ? C10 C9 S8 105.70(15) . . ? N7 C10 C11 112.01(17) . . ? N7 C10 C9 106.38(17) . . ? C11 C10 C9 112.44(18) . . ? C12 C11 C16 118.8(2) . . ? C12 C11 C10 123.16(19) . . ? C16 C11 C10 118.01(19) . . ? C13 C12 C11 120.6(2) . . ? C12 C13 C14 120.4(2) . . ? C13 C14 C15 119.3(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C11 120.7(2) . . ? N17 C17 C6 115.22(18) . . ? N17 C17 S18 117.49(16) . . ? C6 C17 S18 127.29(16) . . ? C17 N17 C20 112.79(17) . . ? C17 N17 Ni 115.82(14) . . ? C20 N17 Ni 131.04(14) . . ? C17 S18 C19 89.05(10) . . ? C20 C19 S18 105.93(15) . . ? N17 C20 C21 111.91(17) . . ? N17 C20 C19 106.39(17) . . ? C21 C20 C19 112.68(18) . . ? C22 C21 C26 118.8(2) . . ? C22 C21 C20 123.33(19) . . ? C26 C21 C20 117.83(19) . . ? C21 C22 C23 120.3(2) . . ? C24 C23 C22 120.3(2) . . ? C23 C24 C25 119.6(2) . . ? C26 C25 C24 119.7(2) . . ? C25 C26 C21 121.3(2) . . ? Cl1 C30 Cl2 110.68(15) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.006 _refine_diff_density_min -0.781 _refine_diff_density_rms 0.093 #===END