# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Nicholas Long' _publ_contact_author_email n.long@imperial.ac.uk _publ_section_title ; Hemilabile and reversible carbon monoxide binding properties of iron(II), cobalt(II) and nickel(II) complexes containing a new tridentate PSN ligand ; loop_ _publ_author_name C.Tate A.deMello A.Gee S.Kealey R.Vilar-Compte A.White N.Long # Attachment '- Dalton Trans 300611 cif file.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 813887' #TrackingRef '- Dalton Trans 300611 cif file.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Fe N2 P2 S2, 2(B F4)' _chemical_formula_sum 'C40 H40 B2 F8 Fe N2 P2 S2' _chemical_formula_weight 904.27 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _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 11.8126(7) _cell_length_b 13.2594(6) _cell_length_c 12.5685(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.625(4) _cell_angle_gamma 90.00 _cell_volume 1955.43(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3734 _cell_measurement_theta_min 3.0599 _cell_measurement_theta_max 29.1962 _exptl_crystal_description blocks _exptl_crystal_colour Pink _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.536 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.911 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET) (compiled May 6 2009,17:20:42) 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 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7634 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 29.26 _reflns_number_total 4304 _reflns_number_gt 2868 _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^)+(0.0856P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4304 _refine_ls_number_parameters 267 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1458 _refine_ls_wR_factor_gt 0.1259 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Fe Fe 0.5000 0.5000 0.5000 0.01912(18) Uani 1 2 d S . . N1 N 0.5805(2) 0.6281(2) 0.5566(2) 0.0221(6) Uani 1 1 d D . . H1A H 0.549(3) 0.6845(15) 0.526(2) 0.033(10) Uiso 1 1 d D . . H1B H 0.590(4) 0.634(3) 0.6284(4) 0.060(13) Uiso 1 1 d D . . C1 C 0.6996(3) 0.6363(2) 0.5384(2) 0.0265(7) Uani 1 1 d . . . C2 C 0.7663(3) 0.7161(3) 0.5792(3) 0.0366(9) Uani 1 1 d . . . H2A H 0.7355 0.7653 0.6227 0.044 Uiso 1 1 calc R . . C3 C 0.8774(4) 0.7244(3) 0.5568(3) 0.0467(11) Uani 1 1 d . . . H3A H 0.9236 0.7786 0.5858 0.056 Uiso 1 1 calc R . . C4 C 0.9213(3) 0.6543(3) 0.4927(3) 0.0406(9) Uani 1 1 d . . . H4A H 0.9976 0.6614 0.4769 0.049 Uiso 1 1 calc R . . C5 C 0.8580(3) 0.5745(3) 0.4511(3) 0.0324(8) Uani 1 1 d . . . H5A H 0.8894 0.5265 0.4066 0.039 Uiso 1 1 calc R . . C6 C 0.7454(3) 0.5649(2) 0.4756(2) 0.0240(7) Uani 1 1 d . . . S7 S 0.65671(7) 0.46473(6) 0.42162(6) 0.0235(2) Uani 1 1 d . . . C8 C 0.7248(3) 0.3574(2) 0.4954(3) 0.0276(7) Uani 1 1 d . . . H8A H 0.6825 0.2947 0.4739 0.033 Uiso 1 1 calc R . . H8B H 0.8038 0.3497 0.4777 0.033 Uiso 1 1 calc R . . C9 C 0.7260(3) 0.3737(3) 0.6150(3) 0.0299(8) Uani 1 1 d . . . H9A H 0.7844 0.4247 0.6395 0.036 Uiso 1 1 calc R . . H9B H 0.7466 0.3098 0.6532 0.036 Uiso 1 1 calc R . . P10 P 0.58601(8) 0.41646(6) 0.64754(6) 0.0221(2) Uani 1 1 d . . . C11 C 0.5086(3) 0.3032(2) 0.6799(2) 0.0269(7) Uani 1 1 d . . . C12 C 0.5434(4) 0.2073(3) 0.6519(3) 0.0339(8) Uani 1 1 d . . . H12A H 0.6128 0.1993 0.6214 0.041 Uiso 1 1 calc R . . C13 C 0.4772(4) 0.1235(3) 0.6682(3) 0.0433(10) Uani 1 1 d . . . H13A H 0.5020 0.0584 0.6496 0.052 Uiso 1 1 calc R . . C14 C 0.3757(4) 0.1341(3) 0.7111(3) 0.0430(10) Uani 1 1 d . . . H14A H 0.3300 0.0766 0.7210 0.052 Uiso 1 1 calc R . . C15 C 0.3409(4) 0.2288(3) 0.7397(3) 0.0373(9) Uani 1 1 d . . . H15A H 0.2715 0.2361 0.7704 0.045 Uiso 1 1 calc R . . C16 C 0.4061(3) 0.3128(3) 0.7241(2) 0.0318(8) Uani 1 1 d . . . H16A H 0.3810 0.3776 0.7436 0.038 Uiso 1 1 calc R . . C17 C 0.6195(3) 0.4824(2) 0.7755(2) 0.0281(8) Uani 1 1 d . . . C18 C 0.7253(3) 0.4745(3) 0.8354(3) 0.0335(8) Uani 1 1 d . . . H18A H 0.7837 0.4360 0.8089 0.040 Uiso 1 1 calc R . . C19 C 0.7464(4) 0.5225(3) 0.9340(3) 0.0413(10) Uani 1 1 d . . . H19A H 0.8187 0.5149 0.9751 0.050 Uiso 1 1 calc R . . C20 C 0.6646(4) 0.5804(3) 0.9725(3) 0.0473(11) Uani 1 1 d . . . H20A H 0.6806 0.6142 1.0392 0.057 Uiso 1 1 calc R . . C21 C 0.5582(4) 0.5896(3) 0.9141(3) 0.0494(11) Uani 1 1 d . . . H21A H 0.5007 0.6291 0.9409 0.059 Uiso 1 1 calc R . . C22 C 0.5358(4) 0.5405(3) 0.8155(3) 0.0370(9) Uani 1 1 d . . . H22A H 0.4629 0.5469 0.7755 0.044 Uiso 1 1 calc R . . B B 0.4586(4) 0.8390(3) 0.6877(3) 0.0325(9) Uani 1 1 d . . . F1 F 0.3546(2) 0.88569(18) 0.6807(2) 0.0527(6) Uani 1 1 d . . . F2 F 0.5290(2) 0.8818(2) 0.77045(19) 0.0574(7) Uani 1 1 d . . . F3 F 0.4458(2) 0.73640(16) 0.7061(2) 0.0552(7) Uani 1 1 d . . . F4 F 0.5063(3) 0.8504(2) 0.5928(2) 0.0705(9) 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 Fe 0.0178(4) 0.0182(3) 0.0213(3) -0.0006(2) 0.0019(2) 0.0004(3) N1 0.0166(16) 0.0260(14) 0.0241(12) 0.0007(12) 0.0041(11) 0.0008(11) C1 0.028(2) 0.0279(16) 0.0230(14) 0.0018(13) 0.0000(13) -0.0037(14) C2 0.034(2) 0.044(2) 0.0327(17) -0.0058(16) 0.0071(15) -0.0141(18) C3 0.042(3) 0.058(3) 0.0394(19) -0.0067(19) 0.0014(18) -0.025(2) C4 0.019(2) 0.061(3) 0.0425(19) 0.0026(19) 0.0060(16) -0.0120(18) C5 0.024(2) 0.0399(19) 0.0333(16) 0.0031(16) 0.0054(14) 0.0007(16) C6 0.0169(19) 0.0294(16) 0.0250(14) 0.0058(13) 0.0000(12) -0.0035(13) S7 0.0226(5) 0.0240(4) 0.0242(4) -0.0010(3) 0.0034(3) 0.0012(3) C8 0.019(2) 0.0283(16) 0.0365(17) 0.0021(14) 0.0092(14) 0.0055(14) C9 0.030(2) 0.0254(16) 0.0325(16) 0.0035(14) -0.0036(14) 0.0049(14) P10 0.0212(5) 0.0220(4) 0.0229(4) 0.0008(3) 0.0011(3) 0.0022(3) C11 0.034(2) 0.0244(16) 0.0213(14) 0.0046(13) -0.0009(13) 0.0017(14) C12 0.043(3) 0.0255(17) 0.0350(18) 0.0027(15) 0.0121(16) 0.0046(16) C13 0.059(3) 0.0241(17) 0.050(2) -0.0027(17) 0.017(2) -0.0030(18) C14 0.052(3) 0.0305(19) 0.048(2) 0.0064(18) 0.0119(19) -0.0115(18) C15 0.032(2) 0.041(2) 0.0407(19) 0.0101(17) 0.0122(16) 0.0003(17) C16 0.039(2) 0.0274(17) 0.0285(16) 0.0048(14) 0.0025(15) 0.0048(15) C17 0.039(2) 0.0242(17) 0.0207(14) 0.0024(13) 0.0003(13) -0.0020(14) C18 0.035(2) 0.0315(18) 0.0321(16) 0.0008(15) -0.0020(15) -0.0032(15) C19 0.042(3) 0.046(2) 0.0324(18) 0.0022(17) -0.0078(17) -0.0114(18) C20 0.068(3) 0.044(2) 0.0282(17) -0.0076(18) -0.0025(18) -0.010(2) C21 0.060(3) 0.052(3) 0.037(2) -0.0131(19) 0.0076(19) 0.007(2) C22 0.039(3) 0.041(2) 0.0299(17) -0.0059(16) -0.0017(15) 0.0065(18) B 0.035(3) 0.031(2) 0.0321(18) -0.0017(17) 0.0061(17) -0.0006(18) F1 0.0349(16) 0.0467(13) 0.0740(16) 0.0094(12) -0.0044(12) 0.0051(11) F2 0.0395(17) 0.0771(18) 0.0529(13) -0.0082(13) -0.0064(11) -0.0153(13) F3 0.070(2) 0.0309(11) 0.0689(16) 0.0034(11) 0.0266(14) 0.0034(11) F4 0.110(3) 0.0609(16) 0.0476(14) 0.0043(13) 0.0381(15) -0.0005(16) _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 2.034(3) . ? Fe N1 2.034(3) 3_666 ? Fe S7 2.2443(9) . ? Fe S7 2.2443(9) 3_666 ? Fe P10 2.2941(8) 3_666 ? Fe P10 2.2941(8) . ? N1 C1 1.455(4) . ? C1 C6 1.383(5) . ? C1 C2 1.383(5) . ? C2 C3 1.378(6) . ? C3 C4 1.370(6) . ? C4 C5 1.365(5) . ? C5 C6 1.405(5) . ? C6 S7 1.777(3) . ? S7 C8 1.833(3) . ? C8 C9 1.517(4) . ? C9 P10 1.838(4) . ? P10 C11 1.829(3) . ? P10 C17 1.834(3) . ? C11 C12 1.393(5) . ? C11 C16 1.395(5) . ? C12 C13 1.388(5) . ? C13 C14 1.377(6) . ? C14 C15 1.382(5) . ? C15 C16 1.382(5) . ? C17 C18 1.386(5) . ? C17 C22 1.392(5) . ? C18 C19 1.389(5) . ? C19 C20 1.367(6) . ? C20 C21 1.386(6) . ? C21 C22 1.397(5) . ? B F1 1.369(5) . ? B F2 1.377(5) . ? B F4 1.385(5) . ? B F3 1.392(5) . ? 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 N1 180.0 . 3_666 ? N1 Fe S7 87.21(8) . . ? N1 Fe S7 92.79(8) 3_666 . ? N1 Fe S7 92.79(8) . 3_666 ? N1 Fe S7 87.21(8) 3_666 3_666 ? S7 Fe S7 180.0 . 3_666 ? N1 Fe P10 91.43(7) . 3_666 ? N1 Fe P10 88.57(7) 3_666 3_666 ? S7 Fe P10 93.25(3) . 3_666 ? S7 Fe P10 86.75(3) 3_666 3_666 ? N1 Fe P10 88.57(7) . . ? N1 Fe P10 91.43(7) 3_666 . ? S7 Fe P10 86.75(3) . . ? S7 Fe P10 93.25(3) 3_666 . ? P10 Fe P10 180.0 3_666 . ? C1 N1 Fe 115.4(2) . . ? C6 C1 C2 119.5(3) . . ? C6 C1 N1 119.2(3) . . ? C2 C1 N1 121.2(3) . . ? C3 C2 C1 120.0(4) . . ? C4 C3 C2 120.0(4) . . ? C5 C4 C3 121.5(4) . . ? C4 C5 C6 118.5(3) . . ? C1 C6 C5 120.4(3) . . ? C1 C6 S7 118.5(3) . . ? C5 C6 S7 121.0(3) . . ? C6 S7 C8 100.51(15) . . ? C6 S7 Fe 99.02(11) . . ? C8 S7 Fe 106.00(11) . . ? C9 C8 S7 110.1(2) . . ? C8 C9 P10 111.0(2) . . ? C11 P10 C17 105.04(14) . . ? C11 P10 C9 106.38(16) . . ? C17 P10 C9 103.53(17) . . ? C11 P10 Fe 112.95(10) . . ? C17 P10 Fe 120.65(11) . . ? C9 P10 Fe 107.14(11) . . ? C12 C11 C16 118.6(3) . . ? C12 C11 P10 121.6(3) . . ? C16 C11 P10 119.5(3) . . ? C13 C12 C11 120.4(4) . . ? C14 C13 C12 120.5(4) . . ? C13 C14 C15 119.6(4) . . ? C14 C15 C16 120.5(4) . . ? C15 C16 C11 120.5(3) . . ? C18 C17 C22 118.6(3) . . ? C18 C17 P10 122.0(3) . . ? C22 C17 P10 119.4(3) . . ? C17 C18 C19 120.6(4) . . ? C20 C19 C18 120.7(4) . . ? C19 C20 C21 119.8(4) . . ? C20 C21 C22 119.8(4) . . ? C17 C22 C21 120.5(4) . . ? F1 B F2 108.8(3) . . ? F1 B F4 110.2(3) . . ? F2 B F4 109.6(4) . . ? F1 B F3 109.8(3) . . ? F2 B F3 110.2(3) . . ? F4 B F3 108.2(3) . . ? _diffrn_measured_fraction_theta_max 0.808 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.825 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.116 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 813888' #TrackingRef '- Dalton Trans 300611 cif file.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 Co N2 P2 S2, 2(C2 H3 N), 2(B F4)' _chemical_formula_sum 'C44 H46 B2 Co F8 N4 P2 S2' _chemical_formula_weight 989.46 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' B B 0.0090 0.0039 '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' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3729(4) _cell_length_b 12.5243(4) _cell_length_c 17.5572(6) _cell_angle_alpha 87.578(3) _cell_angle_beta 79.920(3) _cell_angle_gamma 68.689(3) _cell_volume 2293.22(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 11961 _cell_measurement_theta_min 2.5547 _cell_measurement_theta_max 72.3828 _exptl_crystal_description tablets _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 5.045 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_T_max 0.743 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) 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 _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 18577 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 72.53 _reflns_number_total 8863 _reflns_number_gt 8224 _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^)+(0.0585P)^2^+1.2552P] 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 8863 _refine_ls_number_parameters 673 _refine_ls_number_restraints 798 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1120 _refine_ls_wR_factor_gt 0.1099 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.232 _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 Co1A Co 0.5000 0.5000 0.0000 0.02944(14) Uani 1 2 d S . . N1A N 0.6012(2) 0.3766(2) 0.06106(13) 0.0366(5) Uani 1 1 d . . . H1A H 0.6843 0.3574 0.0398 0.044 Uiso 1 1 calc R . . H1B H 0.5915 0.4051 0.1089 0.044 Uiso 1 1 calc R . . C1A C 0.5736(3) 0.2756(2) 0.06854(15) 0.0360(5) Uani 1 1 d . . . C2A C 0.6455(3) 0.1806(3) 0.10648(17) 0.0464(7) Uani 1 1 d . . . H2AA H 0.7160 0.1824 0.1278 0.056 Uiso 1 1 calc R . . C3A C 0.6136(4) 0.0837(3) 0.1129(2) 0.0584(9) Uani 1 1 d . . . H3AA H 0.6624 0.0194 0.1391 0.070 Uiso 1 1 calc R . . C4A C 0.5116(4) 0.0788(3) 0.0818(2) 0.0591(9) Uani 1 1 d . . . H4AA H 0.4909 0.0116 0.0869 0.071 Uiso 1 1 calc R . . C5A C 0.4405(4) 0.1715(3) 0.04342(19) 0.0508(7) Uani 1 1 d . . . H5AA H 0.3709 0.1688 0.0216 0.061 Uiso 1 1 calc R . . C6A C 0.4724(3) 0.2693(2) 0.03711(15) 0.0380(6) Uani 1 1 d . . . S7A S 0.39076(7) 0.38869(6) -0.01627(4) 0.03764(16) Uani 1 1 d . . . C8A C 0.2359(3) 0.4517(3) 0.0458(2) 0.0527(8) Uani 1 1 d . . . H8AA H 0.1802 0.5171 0.0195 0.063 Uiso 1 1 calc R . . H8AB H 0.1945 0.3940 0.0551 0.063 Uiso 1 1 calc R . . C9A C 0.2493(3) 0.4930(3) 0.1229(2) 0.0501(7) Uani 1 1 d . . . H9AA H 0.2836 0.4260 0.1554 0.060 Uiso 1 1 calc R . . H9AB H 0.1638 0.5419 0.1502 0.060 Uiso 1 1 calc R . . P10A P 0.35668(6) 0.57487(6) 0.10989(4) 0.03497(16) Uani 1 1 d . . . C11A C 0.2591(3) 0.7257(3) 0.10508(16) 0.0432(6) Uani 1 1 d . . . C12A C 0.1440(3) 0.7600(3) 0.0778(2) 0.0583(9) Uani 1 1 d . . . H12A H 0.1118 0.7044 0.0646 0.070 Uiso 1 1 calc R . . C13A C 0.0761(4) 0.8755(4) 0.0697(2) 0.0745(12) Uani 1 1 d . . . H13A H -0.0030 0.8988 0.0512 0.089 Uiso 1 1 calc R . . C14A C 0.1221(5) 0.9563(4) 0.0882(2) 0.0753(13) Uani 1 1 d . . . H14A H 0.0754 1.0353 0.0820 0.090 Uiso 1 1 calc R . . C15A C 0.2363(5) 0.9231(3) 0.1159(2) 0.0662(10) Uani 1 1 d . . . H15A H 0.2673 0.9795 0.1294 0.079 Uiso 1 1 calc R . . C16A C 0.3063(3) 0.8072(3) 0.12426(18) 0.0499(7) Uani 1 1 d . . . H16A H 0.3853 0.7842 0.1428 0.060 Uiso 1 1 calc R . . C17A C 0.4069(3) 0.5634(2) 0.20363(15) 0.0371(6) Uani 1 1 d . . . C18A C 0.3128(3) 0.5760(4) 0.26833(19) 0.0568(8) Uani 1 1 d . . . H18A H 0.2268 0.5919 0.2622 0.068 Uiso 1 1 calc R . . C19A C 0.3439(4) 0.5656(4) 0.34153(19) 0.0614(9) Uani 1 1 d . . . H19A H 0.2790 0.5739 0.3855 0.074 Uiso 1 1 calc R . . C20A C 0.4672(3) 0.5433(2) 0.35143(17) 0.0460(7) Uani 1 1 d . . . H20A H 0.4880 0.5351 0.4020 0.055 Uiso 1 1 calc R . . C21A C 0.5612(3) 0.5328(3) 0.28791(17) 0.0447(6) Uani 1 1 d . . . H21A H 0.6466 0.5185 0.2948 0.054 Uiso 1 1 calc R . . C22A C 0.5318(3) 0.5429(3) 0.21371(17) 0.0432(6) Uani 1 1 d . . . H22A H 0.5968 0.5359 0.1700 0.052 Uiso 1 1 calc R . . Co1B Co 0.5000 0.0000 0.5000 0.03003(14) Uani 1 2 d S . . N1B N 0.6852(2) -0.0552(2) 0.49929(14) 0.0415(5) Uani 1 1 d . . . H1C H 0.7122 -0.1311 0.5075 0.050 Uiso 1 1 calc R . . H1D H 0.7237 -0.0455 0.4516 0.050 Uiso 1 1 calc R . . C1B C 0.7283(3) -0.0043(3) 0.55275(16) 0.0417(6) Uani 1 1 d . . . C2B C 0.8580(3) -0.0306(4) 0.5539(2) 0.0621(9) Uani 1 1 d . . . H2BA H 0.9208 -0.0835 0.5169 0.074 Uiso 1 1 calc R . . C3B C 0.8953(4) 0.0204(5) 0.6088(3) 0.0772(13) Uani 1 1 d . . . H3BA H 0.9840 0.0020 0.6089 0.093 Uiso 1 1 calc R . . C4B C 0.8060(4) 0.0978(4) 0.6638(2) 0.0683(11) Uani 1 1 d . . . H4BA H 0.8335 0.1319 0.7012 0.082 Uiso 1 1 calc R . . C5B C 0.6770(3) 0.1249(3) 0.66377(18) 0.0505(7) Uani 1 1 d . . . H5BA H 0.6147 0.1773 0.7013 0.061 Uiso 1 1 calc R . . C6B C 0.6398(3) 0.0743(2) 0.60783(15) 0.0369(6) Uani 1 1 d . . . S7B S 0.47562(6) 0.10688(5) 0.60428(4) 0.03432(15) Uani 1 1 d . . . C8B C 0.4289(3) 0.2527(2) 0.56926(17) 0.0415(6) Uani 1 1 d . . . H8BA H 0.3375 0.2806 0.5638 0.050 Uiso 1 1 calc R . . H8BB H 0.4390 0.3033 0.6075 0.050 Uiso 1 1 calc R . . C9B C 0.5093(3) 0.2584(2) 0.49226(17) 0.0408(6) Uani 1 1 d . . . H9BA H 0.5972 0.2473 0.4999 0.049 Uiso 1 1 calc R . . H9BB H 0.4724 0.3352 0.4704 0.049 Uiso 1 1 calc R . . P10B P 0.51622(6) 0.14830(5) 0.42393(4) 0.03367(15) Uani 1 1 d . . . C11B C 0.3853(3) 0.2131(3) 0.37068(18) 0.0455(7) Uani 1 1 d . . . C12B C 0.2789(4) 0.3086(3) 0.3999(3) 0.0707(11) Uani 1 1 d . . . H12B H 0.2749 0.3431 0.4479 0.085 Uiso 1 1 calc R . . C13B C 0.1787(5) 0.3531(4) 0.3586(4) 0.0956(17) Uani 1 1 d . . . H13B H 0.1065 0.4187 0.3784 0.115 Uiso 1 1 calc R . . C14B C 0.1831(5) 0.3032(4) 0.2897(3) 0.0860(15) Uani 1 1 d . . . H14B H 0.1143 0.3346 0.2618 0.103 Uiso 1 1 calc R . . C15B C 0.2868(5) 0.2076(4) 0.2608(2) 0.0738(12) Uani 1 1 d . . . H15B H 0.2885 0.1725 0.2135 0.089 Uiso 1 1 calc R . . C16B C 0.3894(4) 0.1621(3) 0.30068(19) 0.0565(8) Uani 1 1 d . . . H16B H 0.4614 0.0968 0.2803 0.068 Uiso 1 1 calc R . . C17B C 0.6598(3) 0.1318(2) 0.35336(16) 0.0392(6) Uani 1 1 d . . . C18B C 0.6873(4) 0.2300(3) 0.3323(2) 0.0599(9) Uani 1 1 d . . . H18B H 0.6305 0.3027 0.3535 0.072 Uiso 1 1 calc R . . C19B C 0.7975(4) 0.2216(3) 0.2804(2) 0.0651(10) Uani 1 1 d . . . H19B H 0.8158 0.2888 0.2664 0.078 Uiso 1 1 calc R . . C20B C 0.8801(3) 0.1175(3) 0.24905(19) 0.0550(8) Uani 1 1 d . . . H20B H 0.9563 0.1124 0.2144 0.066 Uiso 1 1 calc R . . C21B C 0.8527(3) 0.0204(3) 0.26784(19) 0.0507(7) Uani 1 1 d . . . H21B H 0.9093 -0.0517 0.2455 0.061 Uiso 1 1 calc R . . C22B C 0.7420(3) 0.0275(3) 0.31966(17) 0.0432(6) Uani 1 1 d . . . H22B H 0.7229 -0.0397 0.3319 0.052 Uiso 1 1 calc R . . B10 B 0.0213(9) 0.6681(8) 0.9021(5) 0.051(2) Uani 0.455(4) 1 d PDU A 1 F11 F -0.0367(9) 0.6769(9) 0.9787(4) 0.076(2) Uani 0.455(4) 1 d PDU A 1 F12 F 0.1462(6) 0.6599(9) 0.8932(4) 0.092(2) Uani 0.455(4) 1 d PDU A 1 F13 F 0.0014(7) 0.5857(7) 0.8621(4) 0.0893(19) Uani 0.455(4) 1 d PDU A 1 F14 F -0.0495(7) 0.7664(6) 0.8696(5) 0.101(2) Uani 0.455(4) 1 d PDU A 1 B10' B 0.0548(13) 0.6656(11) 0.9068(8) 0.053(4) Uiso 0.326(7) 1 d PDU B 2 F11' F -0.0109(10) 0.6449(11) 0.9757(6) 0.043(2) Uiso 0.326(7) 1 d PDU B 2 F12' F 0.1705(9) 0.5710(8) 0.8929(6) 0.085(3) Uiso 0.326(7) 1 d PDU B 2 F13' F -0.0118(9) 0.6815(11) 0.8481(5) 0.089(3) Uiso 0.326(7) 1 d PDU B 2 F14' F 0.0950(8) 0.7554(6) 0.9112(4) 0.068(2) Uiso 0.326(7) 1 d PDU B 2 B10" B 0.0502(17) 0.6563(14) 0.8986(10) 0.069(5) Uiso 0.218(7) 1 d PDU C 3 F11" F 0.0059(11) 0.6086(12) 0.9634(7) 0.062(3) Uiso 0.218(7) 1 d PDU C 3 F12" F 0.1815(11) 0.6039(13) 0.8873(8) 0.061(4) Uiso 0.218(7) 1 d PDU C 3 F13" F 0.0131(14) 0.6223(14) 0.8371(7) 0.074(4) Uiso 0.218(7) 1 d PDU C 3 F14" F 0.0135(16) 0.7724(9) 0.9020(8) 0.088(4) Uiso 0.218(7) 1 d PDU C 3 B20 B 0.0577(9) 0.2991(9) 0.6329(7) 0.073(3) Uani 0.408(4) 1 d PDU D 1 F21 F 0.1782(5) 0.2320(5) 0.6454(6) 0.081(2) Uani 0.408(4) 1 d PDU D 1 F22 F -0.0075(7) 0.3696(8) 0.6951(6) 0.119(3) Uani 0.408(4) 1 d PDU D 1 F23 F 0.0796(11) 0.3644(10) 0.5715(6) 0.153(4) Uani 0.408(4) 1 d PDU D 1 F24 F -0.0013(11) 0.2279(11) 0.6163(7) 0.144(4) Uani 0.408(4) 1 d PDU D 1 B20' B 0.0553(15) 0.3149(14) 0.6474(9) 0.082(4) Uiso 0.320(6) 1 d PDU E 2 F21' F 0.1159(13) 0.3879(12) 0.6562(8) 0.149(5) Uiso 0.320(6) 1 d PDU E 2 F22' F -0.0022(10) 0.2927(12) 0.7172(5) 0.086(3) Uiso 0.320(6) 1 d PDU E 2 F23' F 0.1328(12) 0.2222(9) 0.6053(6) 0.106(3) Uiso 0.320(6) 1 d PDU E 2 F24' F -0.0404(9) 0.3695(8) 0.6036(6) 0.093(3) Uiso 0.320(6) 1 d PDU E 2 B20" B 0.0577(16) 0.2774(13) 0.6525(9) 0.084(5) Uiso 0.271(7) 1 d PDU F 3 F21" F 0.1760(11) 0.2650(12) 0.6687(8) 0.089(4) Uiso 0.271(7) 1 d PDU F 3 F22" F -0.0110(10) 0.2590(10) 0.7217(5) 0.074(3) Uiso 0.271(7) 1 d PDU F 3 F23" F 0.0640(11) 0.1909(8) 0.6039(5) 0.073(3) Uiso 0.271(7) 1 d PDU F 3 F24" F -0.0049(14) 0.3839(10) 0.6280(9) 0.107(4) Uiso 0.271(7) 1 d PDU F 3 N30 N 0.2947(9) 0.5253(6) 0.5453(5) 0.0682(19) Uani 0.702(13) 1 d PDU G 1 C31 C 0.2145(7) 0.6092(9) 0.5440(5) 0.055(2) Uani 0.702(13) 1 d PDU G 1 C32 C 0.1107(7) 0.7187(7) 0.5391(5) 0.100(3) Uani 0.702(13) 1 d PDU G 1 H32A H 0.0497 0.7079 0.5100 0.151 Uiso 0.702(13) 1 calc PR G 1 H32B H 0.1460 0.7738 0.5127 0.151 Uiso 0.702(13) 1 calc PR G 1 H32C H 0.0669 0.7479 0.5914 0.151 Uiso 0.702(13) 1 calc PR G 1 N30' N 0.3215(14) 0.5440(16) 0.5350(12) 0.053(4) Uiso 0.298(13) 1 d PDU G 2 C31' C 0.2145(18) 0.581(2) 0.5520(17) 0.056(6) Uiso 0.298(13) 1 d PDU G 2 C32' C 0.0785(18) 0.638(2) 0.5782(16) 0.122(7) Uiso 0.298(13) 1 d PDU G 2 H32D H 0.0572 0.7216 0.5778 0.184 Uiso 0.298(13) 1 calc PR G 2 H32E H 0.0552 0.6150 0.6309 0.184 Uiso 0.298(13) 1 calc PR G 2 H32F H 0.0310 0.6174 0.5436 0.184 Uiso 0.298(13) 1 calc PR G 2 N40 N 0.4087(4) 0.1819(4) 0.8164(3) 0.0871(11) Uani 1 1 d . . . C41 C 0.3044(4) 0.2416(4) 0.8265(2) 0.0635(9) Uani 1 1 d . . . C42 C 0.1734(6) 0.3189(6) 0.8408(4) 0.113(2) Uani 1 1 d . . . H42A H 0.1706 0.3981 0.8399 0.169 Uiso 1 1 calc R . . H42B H 0.1314 0.3039 0.8916 0.169 Uiso 1 1 calc R . . H42C H 0.1289 0.3073 0.8007 0.169 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 Co1A 0.0327(3) 0.0322(3) 0.0278(3) -0.0011(2) -0.0074(2) -0.0157(2) N1A 0.0444(12) 0.0391(12) 0.0319(11) -0.0010(9) -0.0081(9) -0.0209(10) C1A 0.0438(14) 0.0375(13) 0.0286(12) -0.0037(10) -0.0030(10) -0.0178(11) C2A 0.0568(18) 0.0419(15) 0.0406(15) 0.0011(12) -0.0127(13) -0.0159(13) C3A 0.088(3) 0.0397(16) 0.0492(18) 0.0054(13) -0.0175(17) -0.0229(17) C4A 0.093(3) 0.0427(17) 0.0521(18) 0.0025(14) -0.0118(18) -0.0373(18) C5A 0.069(2) 0.0509(17) 0.0458(16) -0.0022(13) -0.0097(15) -0.0374(16) C6A 0.0493(15) 0.0375(14) 0.0324(13) -0.0031(10) -0.0051(11) -0.0224(12) S7A 0.0425(3) 0.0419(3) 0.0366(3) -0.0023(3) -0.0130(3) -0.0217(3) C8A 0.0358(15) 0.063(2) 0.067(2) -0.0121(16) -0.0097(14) -0.0258(14) C9A 0.0377(15) 0.0623(19) 0.0556(18) -0.0128(15) 0.0027(13) -0.0278(14) P10A 0.0299(3) 0.0421(4) 0.0338(3) -0.0067(3) -0.0045(2) -0.0137(3) C11A 0.0404(14) 0.0474(16) 0.0339(13) -0.0071(11) -0.0040(11) -0.0066(12) C12A 0.0460(17) 0.064(2) 0.0550(19) -0.0073(16) -0.0158(15) -0.0035(15) C13A 0.061(2) 0.080(3) 0.057(2) -0.0005(19) -0.0157(18) 0.008(2) C14A 0.090(3) 0.055(2) 0.0459(19) 0.0022(16) -0.0028(19) 0.011(2) C15A 0.094(3) 0.0438(18) 0.0500(19) -0.0066(14) 0.0002(19) -0.0169(19) C16A 0.0568(18) 0.0456(16) 0.0412(16) -0.0062(12) -0.0026(13) -0.0135(14) C17A 0.0394(14) 0.0382(13) 0.0329(13) -0.0027(10) -0.0045(11) -0.0136(11) C18A 0.0420(16) 0.083(2) 0.0371(15) 0.0016(15) -0.0013(13) -0.0149(16) C19A 0.058(2) 0.085(3) 0.0346(16) 0.0043(15) -0.0006(14) -0.0213(18) C20A 0.067(2) 0.0371(14) 0.0331(14) 0.0034(11) -0.0130(13) -0.0163(14) C21A 0.0490(16) 0.0452(15) 0.0424(15) -0.0052(12) -0.0146(13) -0.0163(13) C22A 0.0441(15) 0.0534(17) 0.0353(14) -0.0090(12) -0.0045(12) -0.0215(13) Co1B 0.0318(3) 0.0291(3) 0.0281(3) -0.0029(2) -0.0042(2) -0.0098(2) N1B 0.0475(13) 0.0418(12) 0.0349(12) -0.0030(9) -0.0044(10) -0.0167(11) C1B 0.0417(15) 0.0411(15) 0.0364(14) 0.0009(11) -0.0072(11) -0.0080(12) C2B 0.0378(16) 0.076(2) 0.057(2) -0.0114(17) -0.0126(14) 0.0003(16) C3B 0.0409(18) 0.116(4) 0.067(2) -0.016(2) -0.0194(17) -0.013(2) C4B 0.053(2) 0.104(3) 0.054(2) -0.015(2) -0.0204(16) -0.028(2) C5B 0.0479(17) 0.0629(19) 0.0418(16) -0.0101(14) -0.0115(13) -0.0184(15) C6B 0.0357(13) 0.0410(14) 0.0341(13) -0.0002(11) -0.0076(10) -0.0130(11) S7B 0.0339(3) 0.0376(3) 0.0308(3) -0.0058(2) -0.0023(2) -0.0128(2) C8B 0.0415(14) 0.0330(13) 0.0435(15) -0.0100(11) -0.0024(12) -0.0069(11) C9B 0.0485(15) 0.0268(12) 0.0440(15) -0.0037(10) -0.0057(12) -0.0103(11) P10B 0.0375(3) 0.0264(3) 0.0325(3) -0.0001(2) -0.0046(3) -0.0066(2) C11B 0.0524(17) 0.0378(14) 0.0452(16) 0.0106(12) -0.0160(13) -0.0127(13) C12B 0.069(2) 0.0472(19) 0.085(3) -0.0001(18) -0.035(2) 0.0024(17) C13B 0.088(3) 0.061(3) 0.126(4) 0.009(3) -0.063(3) 0.006(2) C14B 0.087(3) 0.085(3) 0.096(3) 0.041(3) -0.056(3) -0.029(3) C15B 0.087(3) 0.100(3) 0.051(2) 0.025(2) -0.033(2) -0.046(3) C16B 0.064(2) 0.066(2) 0.0415(16) 0.0106(15) -0.0157(15) -0.0243(17) C17B 0.0448(15) 0.0370(14) 0.0335(13) 0.0031(10) -0.0037(11) -0.0138(12) C18B 0.077(2) 0.0431(17) 0.0545(19) -0.0001(14) 0.0096(17) -0.0244(17) C19B 0.084(3) 0.060(2) 0.056(2) 0.0046(16) 0.0076(18) -0.041(2) C20B 0.0533(18) 0.073(2) 0.0406(16) 0.0058(15) 0.0004(14) -0.0292(17) C21B 0.0459(16) 0.0536(18) 0.0443(16) -0.0016(13) 0.0015(13) -0.0122(14) C22B 0.0426(15) 0.0431(15) 0.0402(15) 0.0000(12) 0.0006(12) -0.0146(12) B10 0.060(4) 0.076(5) 0.043(4) 0.029(3) -0.031(3) -0.047(4) F11 0.074(5) 0.105(7) 0.063(3) -0.007(4) 0.000(3) -0.055(5) F12 0.048(3) 0.153(7) 0.086(4) 0.035(4) -0.019(3) -0.052(4) F13 0.098(4) 0.109(5) 0.079(4) -0.015(3) 0.003(3) -0.066(4) F14 0.102(5) 0.083(4) 0.125(5) 0.041(4) -0.040(4) -0.036(4) B20 0.025(4) 0.056(5) 0.109(6) 0.001(5) -0.002(4) 0.016(4) F21 0.027(2) 0.047(3) 0.145(6) -0.018(4) 0.006(3) 0.007(2) F22 0.062(4) 0.112(6) 0.137(6) -0.031(5) 0.005(4) 0.017(4) F23 0.147(7) 0.168(8) 0.141(7) 0.072(6) -0.030(6) -0.059(6) F24 0.104(6) 0.181(8) 0.172(8) -0.010(7) -0.031(6) -0.075(6) N30 0.082(5) 0.047(3) 0.067(4) 0.001(3) -0.026(4) -0.008(3) C31 0.054(3) 0.055(5) 0.048(4) 0.000(3) -0.007(2) -0.012(3) C32 0.060(4) 0.097(6) 0.109(6) -0.010(4) -0.019(4) 0.016(4) N40 0.079(3) 0.078(3) 0.109(3) 0.003(2) -0.016(2) -0.033(2) C41 0.074(3) 0.069(2) 0.059(2) -0.0008(17) -0.0102(18) -0.040(2) C42 0.080(3) 0.137(5) 0.106(4) -0.034(4) -0.012(3) -0.017(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 Co1A N1A 1.965(2) . ? Co1A N1A 1.965(2) 2_665 ? Co1A S7A 2.2328(6) . ? Co1A S7A 2.2328(6) 2_665 ? Co1A P10A 2.2802(7) 2_665 ? Co1A P10A 2.2802(7) . ? N1A C1A 1.406(3) . ? C1A C6A 1.388(4) . ? C1A C2A 1.395(4) . ? C2A C3A 1.382(5) . ? C3A C4A 1.387(6) . ? C4A C5A 1.378(5) . ? C5A C6A 1.393(4) . ? C6A S7A 1.776(3) . ? S7A C8A 1.818(3) . ? C8A C9A 1.519(5) . ? C9A P10A 1.841(3) . ? P10A C11A 1.817(3) . ? P10A C17A 1.818(3) . ? C11A C12A 1.386(5) . ? C11A C16A 1.391(5) . ? C12A C13A 1.385(6) . ? C13A C14A 1.370(7) . ? C14A C15A 1.381(7) . ? C15A C16A 1.395(5) . ? C17A C18A 1.388(4) . ? C17A C22A 1.390(4) . ? C18A C19A 1.380(5) . ? C19A C20A 1.368(5) . ? C20A C21A 1.377(5) . ? C21A C22A 1.390(4) . ? Co1B N1B 1.962(3) 2_656 ? Co1B N1B 1.962(3) . ? Co1B S7B 2.2318(6) 2_656 ? Co1B S7B 2.2318(6) . ? Co1B P10B 2.2849(6) 2_656 ? Co1B P10B 2.2849(6) . ? N1B C1B 1.402(4) . ? C1B C6B 1.392(4) . ? C1B C2B 1.393(5) . ? C2B C3B 1.382(6) . ? C3B C4B 1.386(6) . ? C4B C5B 1.380(5) . ? C5B C6B 1.393(4) . ? C6B S7B 1.772(3) . ? S7B C8B 1.819(3) . ? C8B C9B 1.509(4) . ? C9B P10B 1.837(3) . ? P10B C11B 1.815(3) . ? P10B C17B 1.820(3) . ? C11B C12B 1.393(5) . ? C11B C16B 1.395(5) . ? C12B C13B 1.388(6) . ? C13B C14B 1.370(8) . ? C14B C15B 1.377(8) . ? C15B C16B 1.394(5) . ? C17B C22B 1.384(4) . ? C17B C18B 1.396(4) . ? C18B C19B 1.387(5) . ? C19B C20B 1.369(6) . ? C20B C21B 1.375(5) . ? C21B C22B 1.395(4) . ? B10 F12 1.367(10) . ? B10 F14 1.368(10) . ? B10 F13 1.378(10) . ? B10 F11 1.380(10) . ? B10' F13' 1.350(13) . ? B10' F14' 1.369(13) . ? B10' F11' 1.374(13) . ? B10' F12' 1.405(13) . ? B10" F14" 1.360(15) . ? B10" F13" 1.361(15) . ? B10" F11" 1.365(15) . ? B10" F12" 1.376(15) . ? B20 F22 1.357(12) . ? B20 F24 1.362(12) . ? B20 F23 1.369(13) . ? B20 F21 1.373(10) . ? B20' F23' 1.331(14) . ? B20' F22' 1.354(14) . ? B20' F21' 1.357(14) . ? B20' F24' 1.396(15) . ? B20" F24" 1.356(14) . ? B20" F21" 1.375(14) . ? B20" F23" 1.382(14) . ? B20" F22" 1.384(15) . ? N30 C31 1.117(8) . ? C31 C32 1.459(10) . ? N30' C31' 1.122(17) . ? C31' C32' 1.446(19) . ? N40 C41 1.136(6) . ? C41 C42 1.435(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Co1A N1A 180.00(10) . 2_665 ? N1A Co1A S7A 87.42(7) . . ? N1A Co1A S7A 92.58(7) 2_665 . ? N1A Co1A S7A 92.58(7) . 2_665 ? N1A Co1A S7A 87.42(7) 2_665 2_665 ? S7A Co1A S7A 180.00(3) . 2_665 ? N1A Co1A P10A 90.64(7) . 2_665 ? N1A Co1A P10A 89.36(7) 2_665 2_665 ? S7A Co1A P10A 91.19(2) . 2_665 ? S7A Co1A P10A 88.81(2) 2_665 2_665 ? N1A Co1A P10A 89.36(7) . . ? N1A Co1A P10A 90.64(7) 2_665 . ? S7A Co1A P10A 88.81(2) . . ? S7A Co1A P10A 91.19(2) 2_665 . ? P10A Co1A P10A 180.0 2_665 . ? C1A N1A Co1A 117.67(18) . . ? C6A C1A C2A 118.7(3) . . ? C6A C1A N1A 119.4(2) . . ? C2A C1A N1A 121.9(3) . . ? C3A C2A C1A 119.6(3) . . ? C2A C3A C4A 121.3(3) . . ? C5A C4A C3A 119.8(3) . . ? C4A C5A C6A 119.0(3) . . ? C1A C6A C5A 121.7(3) . . ? C1A C6A S7A 116.9(2) . . ? C5A C6A S7A 121.3(2) . . ? C6A S7A C8A 102.87(16) . . ? C6A S7A Co1A 98.42(9) . . ? C8A S7A Co1A 105.57(10) . . ? C9A C8A S7A 111.4(2) . . ? C8A C9A P10A 111.6(2) . . ? C11A P10A C17A 103.83(13) . . ? C11A P10A C9A 107.95(15) . . ? C17A P10A C9A 102.54(15) . . ? C11A P10A Co1A 114.53(10) . . ? C17A P10A Co1A 121.50(9) . . ? C9A P10A Co1A 105.30(10) . . ? C12A C11A C16A 120.0(3) . . ? C12A C11A P10A 121.2(3) . . ? C16A C11A P10A 118.6(2) . . ? C13A C12A C11A 119.9(4) . . ? C14A C13A C12A 120.4(4) . . ? C13A C14A C15A 120.1(4) . . ? C14A C15A C16A 120.3(4) . . ? C11A C16A C15A 119.2(4) . . ? C18A C17A C22A 119.1(3) . . ? C18A C17A P10A 116.7(2) . . ? C22A C17A P10A 124.2(2) . . ? C19A C18A C17A 120.2(3) . . ? C20A C19A C18A 120.7(3) . . ? C19A C20A C21A 119.8(3) . . ? C20A C21A C22A 120.3(3) . . ? C17A C22A C21A 119.8(3) . . ? N1B Co1B N1B 180.00(14) 2_656 . ? N1B Co1B S7B 87.60(7) 2_656 2_656 ? N1B Co1B S7B 92.40(7) . 2_656 ? N1B Co1B S7B 92.40(7) 2_656 . ? N1B Co1B S7B 87.60(7) . . ? S7B Co1B S7B 180.000(18) 2_656 . ? N1B Co1B P10B 89.47(7) 2_656 2_656 ? N1B Co1B P10B 90.53(7) . 2_656 ? S7B Co1B P10B 89.05(2) 2_656 2_656 ? S7B Co1B P10B 90.95(2) . 2_656 ? N1B Co1B P10B 90.53(7) 2_656 . ? N1B Co1B P10B 89.47(7) . . ? S7B Co1B P10B 90.95(2) 2_656 . ? S7B Co1B P10B 89.05(2) . . ? P10B Co1B P10B 180.0 2_656 . ? C1B N1B Co1B 117.31(19) . . ? C6B C1B C2B 117.9(3) . . ? C6B C1B N1B 119.7(3) . . ? C2B C1B N1B 122.4(3) . . ? C3B C2B C1B 120.1(3) . . ? C2B C3B C4B 121.4(3) . . ? C5B C4B C3B 119.5(3) . . ? C4B C5B C6B 118.9(3) . . ? C1B C6B C5B 122.2(3) . . ? C1B C6B S7B 116.8(2) . . ? C5B C6B S7B 121.0(2) . . ? C6B S7B C8B 101.63(14) . . ? C6B S7B Co1B 98.23(9) . . ? C8B S7B Co1B 104.10(10) . . ? C9B C8B S7B 111.17(19) . . ? C8B C9B P10B 111.2(2) . . ? C11B P10B C17B 104.47(14) . . ? C11B P10B C9B 106.87(14) . . ? C17B P10B C9B 103.82(14) . . ? C11B P10B Co1B 114.64(10) . . ? C17B P10B Co1B 121.19(9) . . ? C9B P10B Co1B 104.60(9) . . ? C12B C11B C16B 119.6(3) . . ? C12B C11B P10B 121.6(3) . . ? C16B C11B P10B 118.7(3) . . ? C13B C12B C11B 119.8(4) . . ? C14B C13B C12B 120.4(5) . . ? C13B C14B C15B 120.3(4) . . ? C14B C15B C16B 120.3(4) . . ? C15B C16B C11B 119.5(4) . . ? C22B C17B C18B 118.7(3) . . ? C22B C17B P10B 123.4(2) . . ? C18B C17B P10B 117.9(2) . . ? C19B C18B C17B 120.1(3) . . ? C20B C19B C18B 120.6(3) . . ? C19B C20B C21B 119.9(3) . . ? C20B C21B C22B 120.1(3) . . ? C17B C22B C21B 120.4(3) . . ? F12 B10 F14 110.0(7) . . ? F12 B10 F13 114.8(9) . . ? F14 B10 F13 101.5(7) . . ? F12 B10 F11 112.8(7) . . ? F14 B10 F11 104.8(9) . . ? F13 B10 F11 111.8(7) . . ? F13' B10' F14' 109.6(10) . . ? F13' B10' F11' 112.8(11) . . ? F14' B10' F11' 113.3(11) . . ? F13' B10' F12' 112.2(11) . . ? F14' B10' F12' 102.8(10) . . ? F11' B10' F12' 105.7(10) . . ? F14" B10" F13" 110.8(13) . . ? F14" B10" F11" 115.0(13) . . ? F13" B10" F11" 108.0(13) . . ? F14" B10" F12" 111.4(13) . . ? F13" B10" F12" 105.6(13) . . ? F11" B10" F12" 105.5(12) . . ? F22 B20 F24 113.1(10) . . ? F22 B20 F23 108.7(10) . . ? F24 B20 F23 112.6(11) . . ? F22 B20 F21 110.4(10) . . ? F24 B20 F21 107.6(9) . . ? F23 B20 F21 103.9(9) . . ? F23' B20' F22' 114.6(13) . . ? F23' B20' F21' 111.7(13) . . ? F22' B20' F21' 109.9(12) . . ? F23' B20' F24' 104.6(11) . . ? F22' B20' F24' 107.7(12) . . ? F21' B20' F24' 107.9(12) . . ? F24" B20" F21" 112.5(13) . . ? F24" B20" F23" 113.2(12) . . ? F21" B20" F23" 112.1(12) . . ? F24" B20" F22" 109.1(12) . . ? F21" B20" F22" 105.4(11) . . ? F23" B20" F22" 103.8(11) . . ? N30 C31 C32 177.9(10) . . ? N30' C31' C32' 174(3) . . ? N40 C41 C42 178.4(5) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 71.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.753 _refine_diff_density_min -0.397 _refine_diff_density_rms 0.051 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 813889' #TrackingRef '- Dalton Trans 300611 cif file.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H40 N2 Ni P2 S2, 2(Cl O4)' _chemical_formula_sum 'C40 H40 Cl2 N2 Ni O8 P2 S2' _chemical_formula_weight 932.41 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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' Ni Ni -3.0029 0.5091 '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 12.00508(9) _cell_length_b 13.45669(11) _cell_length_c 12.62737(9) _cell_angle_alpha 90.00 _cell_angle_beta 94.8331(7) _cell_angle_gamma 90.00 _cell_volume 2032.68(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 14171 _cell_measurement_theta_min 3.2815 _cell_measurement_theta_max 72.3703 _exptl_crystal_description blocks _exptl_crystal_colour 'Pale brown' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964 _exptl_absorpt_coefficient_mu 4.068 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 0.719 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) 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 _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 21446 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 72.52 _reflns_number_total 4025 _reflns_number_gt 3682 _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^)+(0.0400P)^2^+1.1816P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00077(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4025 _refine_ls_number_parameters 268 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.5000 0.5000 0.5000 0.02189(12) Uani 1 2 d S . . N1 N 0.58135(12) 0.63242(11) 0.54886(12) 0.0274(3) Uani 1 1 d D . . H1A H 0.5471(18) 0.6845(11) 0.5153(17) 0.037(6) Uiso 1 1 d D . . H1B H 0.572(2) 0.6418(19) 0.6180(5) 0.045(7) Uiso 1 1 d D . . C1 C 0.69991(14) 0.63661(14) 0.53263(13) 0.0273(4) Uani 1 1 d . . . C2 C 0.76439(18) 0.71529(16) 0.57435(16) 0.0385(5) Uani 1 1 d . . . H2A H 0.7318 0.7646 0.6159 0.046 Uiso 1 1 calc R . . C3 C 0.87592(19) 0.72212(19) 0.55562(17) 0.0462(5) Uani 1 1 d . . . H3A H 0.9199 0.7756 0.5851 0.055 Uiso 1 1 calc R . . C4 C 0.92357(17) 0.65144(19) 0.49427(17) 0.0433(5) Uani 1 1 d . . . H4A H 1.0000 0.6570 0.4809 0.052 Uiso 1 1 calc R . . C5 C 0.86050(15) 0.57255(16) 0.45224(15) 0.0341(4) Uani 1 1 d . . . H5A H 0.8933 0.5242 0.4097 0.041 Uiso 1 1 calc R . . C6 C 0.74840(14) 0.56452(14) 0.47268(13) 0.0271(4) Uani 1 1 d . . . S7 S 0.66789(3) 0.46302(3) 0.41730(3) 0.02502(11) Uani 1 1 d . . . C8 C 0.72719(15) 0.35922(14) 0.49707(15) 0.0297(4) Uani 1 1 d . . . H8A H 0.6822 0.2988 0.4798 0.036 Uiso 1 1 calc R . . H8B H 0.8042 0.3464 0.4779 0.036 Uiso 1 1 calc R . . C9 C 0.73029(14) 0.37856(14) 0.61613(14) 0.0294(4) Uani 1 1 d . . . H9A H 0.7855 0.4315 0.6357 0.035 Uiso 1 1 calc R . . H9B H 0.7548 0.3175 0.6551 0.035 Uiso 1 1 calc R . . P10 P 0.59288(3) 0.41638(3) 0.65622(3) 0.02438(12) Uani 1 1 d . . . C11 C 0.51961(15) 0.30267(13) 0.68731(14) 0.0271(4) Uani 1 1 d . . . C12 C 0.55856(17) 0.20883(15) 0.66338(16) 0.0351(4) Uani 1 1 d . . . H12A H 0.6297 0.2018 0.6365 0.042 Uiso 1 1 calc R . . C13 C 0.4939(2) 0.12499(15) 0.67857(18) 0.0434(5) Uani 1 1 d . . . H13A H 0.5212 0.0610 0.6624 0.052 Uiso 1 1 calc R . . C14 C 0.3897(2) 0.13455(16) 0.71719(18) 0.0427(5) Uani 1 1 d . . . H14A H 0.3455 0.0773 0.7268 0.051 Uiso 1 1 calc R . . C15 C 0.35025(17) 0.22773(16) 0.74182(17) 0.0382(4) Uani 1 1 d . . . H15A H 0.2792 0.2343 0.7690 0.046 Uiso 1 1 calc R . . C16 C 0.41446(16) 0.31150(15) 0.72673(15) 0.0320(4) Uani 1 1 d . . . H16A H 0.3869 0.3753 0.7433 0.038 Uiso 1 1 calc R . . C17 C 0.62421(16) 0.48091(14) 0.78241(14) 0.0288(4) Uani 1 1 d . . . C18 C 0.72770(17) 0.47259(15) 0.84184(15) 0.0342(4) Uani 1 1 d . . . H18A H 0.7851 0.4328 0.8163 0.041 Uiso 1 1 calc R . . C19 C 0.74656(19) 0.52228(17) 0.93769(17) 0.0414(5) Uani 1 1 d . . . H19A H 0.8166 0.5157 0.9781 0.050 Uiso 1 1 calc R . . C20 C 0.6641(2) 0.58136(18) 0.97492(17) 0.0465(5) Uani 1 1 d . . . H20A H 0.6772 0.6151 1.0409 0.056 Uiso 1 1 calc R . . C21 C 0.5624(2) 0.59117(19) 0.91580(19) 0.0506(6) Uani 1 1 d . . . H21A H 0.5059 0.6323 0.9409 0.061 Uiso 1 1 calc R . . C22 C 0.54231(18) 0.54128(17) 0.82002(16) 0.0396(5) Uani 1 1 d . . . H22A H 0.4722 0.5484 0.7799 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.45404(4) 0.83654(3) 0.68553(3) 0.03055(12) Uani 1 1 d . . . O1 O 0.34898(13) 0.88634(12) 0.68870(14) 0.0493(4) Uani 1 1 d . . . O2 O 0.53182(13) 0.87787(14) 0.76486(13) 0.0529(4) Uani 1 1 d . . . O3 O 0.49533(19) 0.84892(14) 0.58297(13) 0.0621(5) Uani 1 1 d . . . O4 O 0.43927(14) 0.73206(11) 0.70483(14) 0.0484(4) 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 Ni 0.0181(2) 0.0225(2) 0.0250(2) -0.00111(15) 0.00134(15) -0.00042(15) N1 0.0241(7) 0.0260(7) 0.0321(8) -0.0031(6) 0.0028(6) -0.0011(6) C1 0.0250(8) 0.0324(9) 0.0243(8) 0.0015(7) 0.0012(6) -0.0064(7) C2 0.0404(11) 0.0431(11) 0.0321(9) -0.0075(8) 0.0045(8) -0.0146(9) C3 0.0398(11) 0.0595(14) 0.0391(11) -0.0082(10) 0.0023(9) -0.0253(10) C4 0.0265(9) 0.0619(14) 0.0415(11) 0.0008(10) 0.0029(8) -0.0158(9) C5 0.0261(9) 0.0434(11) 0.0329(9) 0.0024(8) 0.0045(7) -0.0037(8) C6 0.0232(8) 0.0326(9) 0.0252(8) 0.0033(7) 0.0003(6) -0.0033(7) S7 0.0206(2) 0.0284(2) 0.0261(2) -0.00167(15) 0.00232(15) 0.00028(15) C8 0.0238(8) 0.0304(9) 0.0354(9) 0.0001(7) 0.0043(7) 0.0053(7) C9 0.0231(8) 0.0324(9) 0.0322(9) 0.0033(7) -0.0003(7) 0.0035(7) P10 0.0226(2) 0.0242(2) 0.0261(2) 0.00085(16) 0.00047(15) 0.00215(16) C11 0.0290(8) 0.0267(9) 0.0253(8) 0.0027(7) 0.0013(6) 0.0014(7) C12 0.0389(10) 0.0296(9) 0.0382(10) 0.0011(8) 0.0119(8) 0.0022(8) C13 0.0564(13) 0.0266(10) 0.0492(12) -0.0009(9) 0.0173(10) -0.0016(9) C14 0.0494(12) 0.0340(10) 0.0461(11) 0.0051(9) 0.0119(9) -0.0092(9) C15 0.0340(10) 0.0407(11) 0.0407(10) 0.0077(9) 0.0083(8) -0.0007(8) C16 0.0324(9) 0.0311(9) 0.0328(9) 0.0035(7) 0.0047(7) 0.0048(7) C17 0.0322(9) 0.0262(8) 0.0276(8) 0.0012(7) 0.0003(7) -0.0004(7) C18 0.0336(10) 0.0354(10) 0.0330(9) 0.0020(8) -0.0017(7) -0.0023(8) C19 0.0416(11) 0.0470(12) 0.0341(10) 0.0008(9) -0.0059(8) -0.0101(9) C20 0.0590(14) 0.0469(13) 0.0329(10) -0.0097(9) 0.0001(9) -0.0090(10) C21 0.0574(14) 0.0520(14) 0.0420(12) -0.0153(10) 0.0020(10) 0.0115(11) C22 0.0403(11) 0.0417(11) 0.0358(10) -0.0060(8) -0.0029(8) 0.0083(9) Cl1 0.0317(2) 0.0288(2) 0.0309(2) -0.00023(16) 0.00092(16) -0.00017(16) O1 0.0344(8) 0.0447(9) 0.0675(10) 0.0025(8) -0.0037(7) 0.0089(7) O2 0.0366(8) 0.0700(12) 0.0499(9) -0.0046(8) -0.0087(7) -0.0160(8) O3 0.0942(14) 0.0568(11) 0.0388(9) 0.0074(8) 0.0255(9) 0.0089(10) O4 0.0580(10) 0.0274(7) 0.0613(10) 0.0021(7) 0.0146(8) 0.0017(7) _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 N1 2.0995(15) 3_666 ? Ni N1 2.0995(15) . ? Ni S7 2.3990(4) 3_666 ? Ni S7 2.3990(4) . ? Ni P10 2.4557(4) . ? Ni P10 2.4557(4) 3_666 ? N1 C1 1.456(2) . ? C1 C6 1.388(3) . ? C1 C2 1.389(3) . ? C2 C3 1.382(3) . ? C3 C4 1.381(4) . ? C4 C5 1.384(3) . ? C5 C6 1.396(2) . ? C6 S7 1.7818(18) . ? S7 C8 1.8308(19) . ? C8 C9 1.523(3) . ? C9 P10 1.8377(18) . ? P10 C11 1.8241(18) . ? P10 C17 1.8258(19) . ? C11 C12 1.389(3) . ? C11 C16 1.400(3) . ? C12 C13 1.392(3) . ? C13 C14 1.385(3) . ? C14 C15 1.385(3) . ? C15 C16 1.388(3) . ? C17 C22 1.390(3) . ? C17 C18 1.401(3) . ? C18 C19 1.385(3) . ? C19 C20 1.383(3) . ? C20 C21 1.383(3) . ? C21 C22 1.386(3) . ? Cl1 O2 1.4237(16) . ? Cl1 O1 1.4318(16) . ? Cl1 O3 1.4348(17) . ? Cl1 O4 1.4405(16) . ? 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 Ni N1 180.0 3_666 . ? N1 Ni S7 85.23(4) 3_666 3_666 ? N1 Ni S7 94.77(4) . 3_666 ? N1 Ni S7 94.77(4) 3_666 . ? N1 Ni S7 85.23(4) . . ? S7 Ni S7 180.0 3_666 . ? N1 Ni P10 90.89(4) 3_666 . ? N1 Ni P10 89.11(4) . . ? S7 Ni P10 94.971(14) 3_666 . ? S7 Ni P10 85.029(14) . . ? N1 Ni P10 89.11(4) 3_666 3_666 ? N1 Ni P10 90.89(4) . 3_666 ? S7 Ni P10 85.029(14) 3_666 3_666 ? S7 Ni P10 94.971(14) . 3_666 ? P10 Ni P10 180.0 . 3_666 ? C1 N1 Ni 115.31(11) . . ? C6 C1 C2 119.58(17) . . ? C6 C1 N1 120.62(15) . . ? C2 C1 N1 119.76(17) . . ? C3 C2 C1 120.2(2) . . ? C4 C3 C2 120.22(19) . . ? C3 C4 C5 120.30(19) . . ? C4 C5 C6 119.58(19) . . ? C1 C6 C5 120.12(17) . . ? C1 C6 S7 120.74(13) . . ? C5 C6 S7 119.11(15) . . ? C6 S7 C8 101.30(8) . . ? C6 S7 Ni 96.78(6) . . ? C8 S7 Ni 102.75(6) . . ? C9 C8 S7 112.88(13) . . ? C8 C9 P10 111.80(12) . . ? C11 P10 C17 106.19(8) . . ? C11 P10 C9 106.70(9) . . ? C17 P10 C9 104.38(9) . . ? C11 P10 Ni 111.27(6) . . ? C17 P10 Ni 121.96(6) . . ? C9 P10 Ni 105.25(6) . . ? C12 C11 C16 118.98(17) . . ? C12 C11 P10 122.60(14) . . ? C16 C11 P10 118.08(14) . . ? C11 C12 C13 120.33(18) . . ? C14 C13 C12 120.24(19) . . ? C15 C14 C13 119.95(19) . . ? C14 C15 C16 119.99(19) . . ? C15 C16 C11 120.51(18) . . ? C22 C17 C18 119.00(18) . . ? C22 C17 P10 118.47(14) . . ? C18 C17 P10 122.53(15) . . ? C19 C18 C17 120.13(19) . . ? C20 C19 C18 120.4(2) . . ? C19 C20 C21 119.8(2) . . ? C20 C21 C22 120.3(2) . . ? C21 C22 C17 120.4(2) . . ? O2 Cl1 O1 108.94(11) . . ? O2 Cl1 O3 109.50(12) . . ? O1 Cl1 O3 110.06(11) . . ? O2 Cl1 O4 110.19(11) . . ? O1 Cl1 O4 109.32(10) . . ? O3 Cl1 O4 108.83(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 72.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.310 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.050 #===END