# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'McAuley, A.' _publ_contact_author_email amcauley@uvic.ca _publ_section_title ; Structure and Electrochemistry of Isomeric Nickel(II) Complexes of a Macrotricyclic [9]-ane fused Cyclam. Evidence for a Stable trans-IV Conformation and a Redox Induced Rearrangement in a trans-I Structure. ; _publ_author_name A.McAuley # Attachment 'cNi9N4S2.cif' data_1_database_code_depnum_ccdc_archive _database_code_depnum_ccdc_archive 'CCDC 772067' #TrackingRef '- CIF for cis-Ni9N4S2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic cis-(C18H36N4S2)Ni(II)dichloridetetrahydrate _chemical_name_common cis-(C18H36N4S2)Ni(ii)dichloridetetrahydrate _chemical_melting_point ? _chemical_formula_moiety cis-[Ni(C18H36N4S2)]Cl24H2O _chemical_formula_sum 'C18 H44 Cl2 N4 Ni O4 S2' _chemical_formula_weight 574.30 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.450(3) _cell_length_b 12.188(2) _cell_length_c 11.897(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2530.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 488 _cell_measurement_theta_min 4 _cell_measurement_theta_max 50 _exptl_crystal_description na _exptl_crystal_colour Pink _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method na _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.175 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Smart1000 _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12895 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0355 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4440 _reflns_number_gt 3770 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0476P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.496(15) _refine_ls_number_reflns 4440 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Ni1 Ni 0.88010(2) 0.23631(3) 0.64508(4) 0.02229(11) Uani 1 1 d . . . Cl1 Cl 1.12366(6) -0.03303(9) 0.62836(11) 0.0631(3) Uani 1 1 d . . . Cl2 Cl 1.08952(6) 0.58294(9) 0.63232(11) 0.0593(3) Uani 1 1 d . . . S1 S 0.92181(6) 0.08800(8) 0.52009(9) 0.0401(3) Uani 1 1 d . . . S2 S 1.00939(5) 0.23965(9) 0.72009(9) 0.0437(3) Uani 1 1 d . . . N1 N 0.76905(17) 0.2053(3) 0.5705(3) 0.0390(8) Uani 1 1 d . . . N2 N 0.89792(19) 0.3345(3) 0.5023(3) 0.0401(8) Uani 1 1 d . . . N3 N 0.86321(16) 0.3764(2) 0.7561(3) 0.0329(7) Uani 1 1 d . . . N4 N 0.85745(17) 0.1427(2) 0.7895(3) 0.0350(8) Uani 1 1 d . . . C1 C 0.7581(2) 0.2985(4) 0.4914(4) 0.0542(12) Uani 1 1 d . . . H1A H 0.7433 0.3635 0.5332 0.065 Uiso 1 1 calc R . . H1B H 0.7172 0.2811 0.4392 0.065 Uiso 1 1 calc R . . C2 C 0.8303(3) 0.3214(4) 0.4272(3) 0.0518(13) Uani 1 1 d . . . H2A H 0.8398 0.2616 0.3753 0.062 Uiso 1 1 calc R . . H2B H 0.8237 0.3879 0.3835 0.062 Uiso 1 1 calc R . . C3 C 0.9116(3) 0.4520(3) 0.5320(4) 0.0557(13) Uani 1 1 d . . . H3A H 0.9213 0.4917 0.4628 0.067 Uiso 1 1 calc R . . H3B H 0.9582 0.4555 0.5763 0.067 Uiso 1 1 calc R . . C4 C 0.8497(3) 0.5128(3) 0.5958(4) 0.0583(12) Uani 1 1 d . . . H4A H 0.8072 0.5233 0.5443 0.070 Uiso 1 1 calc R . . H4B H 0.8697 0.5851 0.6131 0.070 Uiso 1 1 calc R . . C5 C 0.8166(2) 0.4659(3) 0.7045(3) 0.0454(10) Uani 1 1 d . . . H5A H 0.8115 0.5250 0.7586 0.055 Uiso 1 1 calc R . . H5B H 0.7657 0.4378 0.6892 0.055 Uiso 1 1 calc R . . C6 C 0.8187(2) 0.3295(3) 0.8524(3) 0.0341(9) Uani 1 1 d . . . H6A H 0.7653 0.3228 0.8310 0.041 Uiso 1 1 calc R . . H6B H 0.8217 0.3793 0.9159 0.041 Uiso 1 1 calc R . . C7 C 0.8487(2) 0.2187(3) 0.8871(3) 0.0409(9) Uani 1 1 d . . . H7A H 0.8980 0.2278 0.9236 0.049 Uiso 1 1 calc R . . H7B H 0.8138 0.1863 0.9412 0.049 Uiso 1 1 calc R . . C8 C 0.7892(3) 0.0713(4) 0.7760(4) 0.0559(13) Uani 1 1 d . . . H8A H 0.7840 0.0276 0.8437 0.067 Uiso 1 1 calc R . . H8B H 0.7992 0.0210 0.7145 0.067 Uiso 1 1 calc R . . C9 C 0.7133(2) 0.1259(4) 0.7538(4) 0.0609(14) Uani 1 1 d . . . H9A H 0.6990 0.1650 0.8216 0.073 Uiso 1 1 calc R . . H9B H 0.6757 0.0682 0.7432 0.073 Uiso 1 1 calc R . . C10 C 0.7048(2) 0.2068(4) 0.6545(4) 0.0530(11) Uani 1 1 d . . . H10A H 0.6573 0.1904 0.6154 0.064 Uiso 1 1 calc R . . H10B H 0.7004 0.2805 0.6846 0.064 Uiso 1 1 calc R . . C11 C 0.7622(2) 0.0986(4) 0.5082(4) 0.0502(12) Uani 1 1 d . . . H11A H 0.7207 0.1056 0.4545 0.060 Uiso 1 1 calc R . . H11B H 0.7475 0.0423 0.5617 0.060 Uiso 1 1 calc R . . C12 C 0.8325(2) 0.0590(4) 0.4458(3) 0.0487(11) Uani 1 1 d . . . H12A H 0.8342 0.0939 0.3725 0.058 Uiso 1 1 calc R . . H12B H 0.8284 -0.0195 0.4340 0.058 Uiso 1 1 calc R . . C13 C 0.9723(3) 0.1749(4) 0.4198(4) 0.0552(12) Uani 1 1 d . . . H13A H 1.0257 0.1530 0.4185 0.066 Uiso 1 1 calc R . . H13B H 0.9514 0.1612 0.3455 0.066 Uiso 1 1 calc R . . C14 C 0.9685(3) 0.2964(3) 0.4424(3) 0.0488(11) Uani 1 1 d . . . H14A H 1.0129 0.3171 0.4868 0.059 Uiso 1 1 calc R . . H14B H 0.9720 0.3349 0.3712 0.059 Uiso 1 1 calc R . . C21 C 0.9356(2) 0.4286(3) 0.7986(3) 0.0431(10) Uani 1 1 d . . . H21A H 0.9510 0.4845 0.7453 0.052 Uiso 1 1 calc R . . H21B H 0.9240 0.4653 0.8689 0.052 Uiso 1 1 calc R . . C22 C 1.0023(2) 0.3546(4) 0.8179(4) 0.0549(12) Uani 1 1 d . . . H22A H 0.9991 0.3257 0.8937 0.066 Uiso 1 1 calc R . . H22B H 1.0489 0.3976 0.8129 0.066 Uiso 1 1 calc R . . C23 C 1.0004(2) 0.1223(4) 0.8127(4) 0.0543(12) Uani 1 1 d . . . H23A H 1.0390 0.0686 0.7923 0.065 Uiso 1 1 calc R . . H23B H 1.0109 0.1458 0.8891 0.065 Uiso 1 1 calc R . . C24 C 0.9229(3) 0.0676(4) 0.8100(4) 0.0519(12) Uani 1 1 d . . . H24A H 0.9233 0.0120 0.7516 0.062 Uiso 1 1 calc R . . H24B H 0.9148 0.0306 0.8812 0.062 Uiso 1 1 calc R . . O1 O 0.98752(15) 0.7933(3) 0.6146(3) 0.0609(9) Uani 1 1 d . . . HO1A H 1.0107 0.7356 0.6370 0.091 Uiso 1 1 d R . . HO1B H 1.0196 0.8363 0.6544 0.091 Uiso 1 1 d R . . O2 O 0.8445(2) -0.2097(3) 0.4936(3) 0.0813(12) Uani 1 1 d . . . HO2A H 0.8012 -0.2177 0.5474 0.122 Uiso 1 1 d R . . HO2B H 0.8940 -0.1941 0.5421 0.122 Uiso 1 1 d R . . O3 O 1.1318(2) 0.2424(3) 0.2828(3) 0.0872(15) Uani 1 1 d . . . HO3A H 1.0928 0.2204 0.2392 0.131 Uiso 1 1 d R . . HO3B H 1.1857 0.2469 0.2435 0.131 Uiso 1 1 d R . . O4 O 1.22541(16) -0.2450(3) 0.6600(3) 0.0647(9) Uani 1 1 d . . . HO4A H 1.1930 -0.1913 0.6590 0.097 Uiso 1 1 d R . . HO4B H 1.1965 -0.3015 0.6499 0.097 Uiso 1 1 d 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 Ni1 0.0220(2) 0.0245(2) 0.02037(18) -0.0002(3) 0.0008(2) -0.00132(16) Cl1 0.0514(6) 0.0697(7) 0.0683(9) -0.0259(7) 0.0039(6) -0.0052(5) Cl2 0.0531(6) 0.0573(6) 0.0674(7) 0.0125(7) 0.0017(7) -0.0018(5) S1 0.0415(6) 0.0390(6) 0.0397(5) -0.0078(5) 0.0041(5) 0.0023(5) S2 0.0268(5) 0.0576(7) 0.0466(6) -0.0119(5) -0.0010(4) 0.0018(5) N1 0.0317(17) 0.048(2) 0.0377(19) -0.0116(15) -0.0056(14) 0.0013(15) N2 0.053(2) 0.0366(19) 0.0312(18) 0.0057(15) 0.0037(16) -0.0051(16) N3 0.0322(18) 0.0308(17) 0.0358(18) -0.0039(15) -0.0013(13) -0.0012(14) N4 0.0365(18) 0.0345(17) 0.0339(18) 0.0042(14) 0.0048(14) -0.0003(14) C1 0.055(3) 0.067(3) 0.040(2) -0.003(2) -0.019(2) 0.018(2) C2 0.074(3) 0.057(3) 0.025(2) 0.010(2) -0.014(2) 0.013(3) C3 0.096(4) 0.032(2) 0.039(2) 0.007(2) 0.012(2) -0.014(2) C4 0.093(4) 0.030(2) 0.053(3) 0.002(2) 0.001(3) 0.008(2) C5 0.055(3) 0.037(2) 0.044(2) -0.006(2) -0.001(2) 0.014(2) C6 0.034(2) 0.039(2) 0.029(2) -0.0064(17) 0.0049(17) 0.0036(18) C7 0.048(2) 0.046(2) 0.029(2) 0.0019(18) 0.0061(18) 0.004(2) C8 0.067(3) 0.044(3) 0.057(3) 0.004(2) 0.020(3) -0.023(2) C9 0.045(3) 0.072(3) 0.066(3) -0.020(3) 0.022(2) -0.026(2) C10 0.0225(18) 0.074(3) 0.063(3) -0.020(3) 0.003(2) -0.0034(17) C11 0.040(2) 0.060(3) 0.050(3) -0.021(2) -0.001(2) -0.019(2) C12 0.051(3) 0.046(3) 0.049(3) -0.017(2) -0.004(2) -0.004(2) C13 0.055(3) 0.063(3) 0.047(3) -0.013(2) 0.021(2) -0.004(2) C14 0.058(3) 0.052(3) 0.036(2) 0.001(2) 0.015(2) -0.007(2) C21 0.043(2) 0.042(2) 0.044(2) -0.017(2) -0.0008(19) -0.0139(19) C22 0.040(2) 0.064(3) 0.060(3) -0.024(3) -0.005(2) -0.005(2) C23 0.056(3) 0.066(3) 0.041(2) 0.001(2) -0.014(2) 0.030(2) C24 0.071(3) 0.037(2) 0.047(3) 0.007(2) 0.004(2) 0.019(2) O1 0.0387(15) 0.073(2) 0.071(2) 0.0048(17) -0.0063(15) -0.0004(14) O2 0.065(2) 0.111(3) 0.067(2) 0.027(2) -0.016(2) -0.014(2) O3 0.060(3) 0.149(4) 0.053(2) 0.014(2) -0.0014(17) -0.014(2) O4 0.0409(14) 0.092(2) 0.062(2) 0.0111(19) -0.0056(17) -0.0064(14) _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 Ni1 N4 2.100(3) . ? Ni1 N2 2.101(3) . ? Ni1 N1 2.164(3) . ? Ni1 N3 2.179(3) . ? Ni1 S2 2.4265(11) . ? Ni1 S1 2.4512(11) . ? S1 C13 1.822(4) . ? S1 C12 1.826(4) . ? S2 C23 1.813(4) . ? S2 C22 1.825(4) . ? N1 C1 1.487(5) . ? N1 C11 1.501(5) . ? N1 C10 1.502(5) . ? N2 C2 1.488(5) . ? N2 C3 1.495(5) . ? N2 C14 1.497(5) . ? N3 C5 1.492(5) . ? N3 C6 1.497(5) . ? N3 C21 1.501(4) . ? N4 C8 1.484(5) . ? N4 C24 1.484(5) . ? N4 C7 1.493(5) . ? C1 C2 1.499(7) . ? C3 C4 1.514(6) . ? C4 C5 1.528(5) . ? C6 C7 1.506(5) . ? C8 C9 1.506(6) . ? C9 C10 1.546(6) . ? C11 C12 1.514(5) . ? C13 C14 1.507(6) . ? C21 C22 1.490(6) . ? C23 C24 1.508(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ni1 N2 177.20(13) . . ? N4 Ni1 N1 94.12(12) . . ? N2 Ni1 N1 84.30(13) . . ? N4 Ni1 N3 84.50(13) . . ? N2 Ni1 N3 93.68(13) . . ? N1 Ni1 N3 105.32(11) . . ? N4 Ni1 S2 83.29(9) . . ? N2 Ni1 S2 98.64(9) . . ? N1 Ni1 S2 170.43(9) . . ? N3 Ni1 S2 83.66(8) . . ? N4 Ni1 S1 98.73(9) . . ? N2 Ni1 S1 83.42(10) . . ? N1 Ni1 S1 83.60(9) . . ? N3 Ni1 S1 170.35(8) . . ? S2 Ni1 S1 87.67(4) . . ? C13 S1 C12 102.0(2) . . ? C13 S1 Ni1 96.46(14) . . ? C12 S1 Ni1 100.55(14) . . ? C23 S2 C22 102.2(2) . . ? C23 S2 Ni1 97.47(15) . . ? C22 S2 Ni1 100.62(14) . . ? C1 N1 C11 109.8(3) . . ? C1 N1 C10 108.4(3) . . ? C11 N1 C10 106.2(3) . . ? C1 N1 Ni1 103.9(2) . . ? C11 N1 Ni1 115.1(2) . . ? C10 N1 Ni1 113.2(2) . . ? C2 N2 C3 111.8(3) . . ? C2 N2 C14 109.5(3) . . ? C3 N2 C14 106.1(3) . . ? C2 N2 Ni1 107.9(2) . . ? C3 N2 Ni1 112.2(2) . . ? C14 N2 Ni1 109.3(2) . . ? C5 N3 C6 108.1(3) . . ? C5 N3 C21 106.7(3) . . ? C6 N3 C21 109.9(3) . . ? C5 N3 Ni1 113.4(2) . . ? C6 N3 Ni1 103.6(2) . . ? C21 N3 Ni1 115.0(2) . . ? C8 N4 C24 105.9(3) . . ? C8 N4 C7 111.5(3) . . ? C24 N4 C7 109.5(3) . . ? C8 N4 Ni1 112.4(3) . . ? C24 N4 Ni1 108.9(2) . . ? C7 N4 Ni1 108.6(2) . . ? N1 C1 C2 110.9(3) . . ? N2 C2 C1 112.3(3) . . ? N2 C3 C4 118.2(4) . . ? C3 C4 C5 120.7(3) . . ? N3 C5 C4 114.6(3) . . ? N3 C6 C7 111.8(3) . . ? N4 C7 C6 112.3(3) . . ? N4 C8 C9 117.8(4) . . ? C8 C9 C10 120.0(4) . . ? N1 C10 C9 115.4(3) . . ? N1 C11 C12 117.0(3) . . ? C11 C12 S1 113.1(3) . . ? C14 C13 S1 115.7(3) . . ? N2 C14 C13 115.2(3) . . ? C22 C21 N3 116.9(3) . . ? C21 C22 S2 114.8(3) . . ? C24 C23 S2 114.4(3) . . ? N4 C24 C23 114.9(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.354 _refine_diff_density_min -0.235 _refine_diff_density_rms 0.052 # Attachment 'tNi9N4S2.cif' data_tNi9N4S2 _database_code_depnum_ccdc_archive 'CCDC 772068' #TrackingRef '- CIF for trans-Ni9N4S2.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic trans-[Ni([9]N4S2)]diperchlorate _chemical_name_common trans-(Ni((9)N4S2))diperchlorate _chemical_melting_point ? _chemical_formula_moiety trans-[Ni(C18H36N4S2)](ClO4)2 _chemical_formula_sum 'C18 H36 Cl2 N4 Ni O8 S2' _chemical_formula_weight 630.24 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' 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.384(9) _cell_length_b 10.118(2) _cell_length_c 14.300(3) _cell_angle_alpha 90.00 _cell_angle_beta 129.657(3) _cell_angle_gamma 90.00 _cell_volume 2493.3(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4 _cell_measurement_theta_max 50 _exptl_crystal_description ? _exptl_crystal_colour lightpink _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_method na _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type smart1000 _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6350 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2193 _reflns_number_gt 1713 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0785P)^2^+9.5812P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 2193 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1525 _refine_ls_wR_factor_gt 0.1419 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Ni1 Ni 0.0000 0.5000 0.0000 0.0259(3) Uani 1 2 d S . . Cl1 Cl 0.16774(8) -0.00676(12) 0.45508(13) 0.0508(4) Uani 1 1 d . . . S1 S 0.05476(7) 0.37447(14) 0.19294(11) 0.0449(4) Uani 1 1 d . . . O1 O 0.1058(5) -0.0575(8) 0.3458(6) 0.170(4) Uani 1 1 d . . . O2 O 0.2340(4) -0.0813(7) 0.5107(8) 0.148(3) Uani 1 1 d . . . O3 O 0.1501(5) -0.0168(5) 0.5359(7) 0.111(2) Uani 1 1 d . . . O4 O 0.1802(3) 0.1271(5) 0.4478(5) 0.0912(16) Uani 1 1 d . . . N1 N 0.1083(2) 0.4431(4) 0.0494(4) 0.0390(9) Uani 1 1 d . . . N2 N 0.0342(2) 0.6936(4) 0.0741(3) 0.0383(9) Uani 1 1 d . . . C1 C 0.0068(4) 0.2200(6) 0.1249(5) 0.0605(15) Uani 1 1 d . . . H1A H 0.0393 0.1494 0.1813 0.073 Uiso 1 1 calc R . . H1B H -0.0413 0.2191 0.1123 0.073 Uiso 1 1 calc R . . C2 C 0.1498(3) 0.3400(9) 0.2421(6) 0.082(2) Uani 1 1 d . . . H2A H 0.1873 0.3853 0.3188 0.098 Uiso 1 1 calc R . . H2B H 0.1592 0.2460 0.2582 0.098 Uiso 1 1 calc R . . C3 C 0.1651(4) 0.3743(9) 0.1645(7) 0.100(3) Uani 1 1 d . . . H3A H 0.1784 0.2931 0.1454 0.120 Uiso 1 1 calc R . . H3B H 0.2115 0.4284 0.2114 0.120 Uiso 1 1 calc R . . C4 C 0.1442(3) 0.5620(5) 0.0434(5) 0.0495(13) Uani 1 1 d . . . H4A H 0.1079 0.6009 -0.0369 0.059 Uiso 1 1 calc R . . H4B H 0.1899 0.5354 0.0540 0.059 Uiso 1 1 calc R . . C5 C 0.1677(3) 0.6665(6) 0.1377(7) 0.0725(19) Uani 1 1 d . . . H5A H 0.2195 0.6444 0.2107 0.087 Uiso 1 1 calc R . . H5B H 0.1716 0.7497 0.1083 0.087 Uiso 1 1 calc R . . C6 C 0.1188(3) 0.6916(6) 0.1752(5) 0.0533(13) Uani 1 1 d . . . H6A H 0.1301 0.6235 0.2324 0.064 Uiso 1 1 calc R . . H6B H 0.1340 0.7757 0.2173 0.064 Uiso 1 1 calc R . . C7 C 0.0114(4) 0.8084(5) -0.0074(5) 0.0608(15) Uani 1 1 d . . . H7A H -0.0338 0.8494 -0.0243 0.073 Uiso 1 1 calc R . . H7B H 0.0531 0.8727 0.0361 0.073 Uiso 1 1 calc R . . C8 C -0.0064(4) 0.7048(6) 0.1245(6) 0.0629(16) Uani 1 1 d . . . H8A H 0.0256 0.6634 0.2040 0.076 Uiso 1 1 calc R . . H8B H -0.0107 0.7977 0.1361 0.076 Uiso 1 1 calc R . . C9 C 0.0838(4) 0.3537(8) -0.0518(8) 0.095(3) Uani 1 1 d . . . H9A H 0.0875 0.4026 -0.1063 0.114 Uiso 1 1 calc R . . H9B H 0.1211 0.2821 -0.0180 0.114 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 Ni1 0.0277(4) 0.0274(4) 0.0264(4) 0.0001(3) 0.0191(3) 0.0010(3) Cl1 0.0507(8) 0.0420(7) 0.0625(8) -0.0018(6) 0.0375(7) -0.0026(6) S1 0.0429(7) 0.0587(8) 0.0383(7) 0.0028(6) 0.0284(6) 0.0004(6) O1 0.176(7) 0.121(5) 0.086(4) -0.020(4) 0.025(5) -0.059(5) O2 0.130(5) 0.127(6) 0.227(8) 0.068(6) 0.133(6) 0.065(5) O3 0.168(6) 0.093(4) 0.153(6) 0.002(3) 0.140(6) -0.007(4) O4 0.115(4) 0.061(3) 0.101(4) 0.006(3) 0.071(3) -0.021(3) N1 0.036(2) 0.042(2) 0.052(2) 0.0088(19) 0.0337(19) 0.0074(18) N2 0.044(2) 0.035(2) 0.036(2) -0.0047(17) 0.0257(19) -0.0041(17) C1 0.078(4) 0.049(3) 0.057(3) 0.012(3) 0.044(3) -0.001(3) C2 0.040(3) 0.145(7) 0.052(3) 0.036(4) 0.026(3) 0.024(4) C3 0.065(4) 0.141(7) 0.124(6) 0.096(6) 0.074(5) 0.069(4) C4 0.035(2) 0.057(3) 0.064(3) 0.006(3) 0.035(3) 0.002(2) C5 0.046(3) 0.066(4) 0.101(5) -0.030(4) 0.044(4) -0.023(3) C6 0.045(3) 0.048(3) 0.046(3) -0.012(2) 0.019(3) -0.009(2) C7 0.079(4) 0.031(3) 0.064(4) 0.000(2) 0.042(3) -0.002(3) C8 0.074(4) 0.067(4) 0.075(4) -0.018(3) 0.060(4) -0.001(3) C9 0.100(5) 0.099(5) 0.148(7) -0.069(5) 0.108(6) -0.037(4) _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 Ni1 N2 2.124(4) 5_565 ? Ni1 N2 2.124(4) . ? Ni1 N1 2.127(4) . ? Ni1 N1 2.127(4) 5_565 ? Ni1 S1 2.5321(13) 5_565 ? Ni1 S1 2.5321(13) . ? Cl1 O1 1.365(6) . ? Cl1 O2 1.377(6) . ? Cl1 O4 1.400(5) . ? Cl1 O3 1.445(6) . ? S1 C1 1.792(6) . ? S1 C2 1.798(6) . ? N1 C3 1.462(7) . ? N1 C4 1.480(7) . ? N1 C9 1.483(7) . ? N2 C6 1.477(6) . ? N2 C8 1.482(6) . ? N2 C7 1.486(6) . ? C1 C7 1.483(8) 5_565 ? C2 C3 1.398(9) . ? C4 C5 1.519(8) . ? C5 C6 1.517(8) . ? C7 C1 1.483(8) 5_565 ? C8 C9 1.461(9) 5_565 ? C9 C8 1.460(9) 5_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ni1 N2 180.0(3) 5_565 . ? N2 Ni1 N1 83.54(15) 5_565 . ? N2 Ni1 N1 96.46(15) . . ? N2 Ni1 N1 96.46(15) 5_565 5_565 ? N2 Ni1 N1 83.54(15) . 5_565 ? N1 Ni1 N1 180.0(2) . 5_565 ? N2 Ni1 S1 98.60(11) 5_565 5_565 ? N2 Ni1 S1 81.40(11) . 5_565 ? N1 Ni1 S1 98.88(11) . 5_565 ? N1 Ni1 S1 81.12(11) 5_565 5_565 ? N2 Ni1 S1 81.40(11) 5_565 . ? N2 Ni1 S1 98.60(11) . . ? N1 Ni1 S1 81.12(11) . . ? N1 Ni1 S1 98.88(11) 5_565 . ? S1 Ni1 S1 180.00(5) 5_565 . ? O1 Cl1 O2 112.8(6) . . ? O1 Cl1 O4 112.6(4) . . ? O2 Cl1 O4 112.4(4) . . ? O1 Cl1 O3 107.0(5) . . ? O2 Cl1 O3 104.1(5) . . ? O4 Cl1 O3 107.3(3) . . ? C1 S1 C2 101.1(4) . . ? C1 S1 Ni1 98.05(18) . . ? C2 S1 Ni1 98.8(2) . . ? C3 N1 C4 109.8(5) . . ? C3 N1 C9 108.8(6) . . ? C4 N1 C9 108.4(4) . . ? C3 N1 Ni1 119.3(3) . . ? C4 N1 Ni1 107.9(3) . . ? C9 N1 Ni1 102.0(3) . . ? C6 N2 C8 109.0(4) . . ? C6 N2 C7 111.3(4) . . ? C8 N2 C7 108.2(4) . . ? C6 N2 Ni1 107.7(3) . . ? C8 N2 Ni1 100.1(3) . . ? C7 N2 Ni1 119.7(3) . . ? C7 C1 S1 114.8(4) 5_565 . ? C3 C2 S1 118.0(4) . . ? C2 C3 N1 122.3(5) . . ? N1 C4 C5 114.0(5) . . ? C6 C5 C4 120.8(4) . . ? N2 C6 C5 114.8(5) . . ? C1 C7 N2 116.5(5) 5_565 . ? C9 C8 N2 116.1(5) 5_565 . ? C8 C9 N1 118.3(4) 5_565 . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.864 _refine_diff_density_min -0.389 _refine_diff_density_rms 0.093