Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 #====================================================== #============================================================ data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Vujovic, Dejana' 'Nassimbeni, Luigi R.' 'Raubenheimer, Helgard G.' _publ_contact_author_name 'Dr Dejana Vujovic' _publ_contact_author_address ; Department of Chemistry University of Stellenbosch Private Bag X1 Rondebosch 7700 SOUTH AFRICA ; _publ_contact_author_email DEJANA@SCIENCE.UCT.AC.ZA _publ_requested_journal 'Dalton Transactions' _publ_section_title ; New self-assembled one-dimensional nickel coordination polymers and hydrogen-bonded networks ; data_COMPOUND_1 _database_code_CSD 189528 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(4-aminobenzonitrile-N)-bis(?2-thiocyanato-N,S)) nickel(II) ; _chemical_name_common none _chemical_melting_point 'DSC onset temperature = 257.2oC' _chemical_formula_moiety Ni(NCS)2(C6H7N2)2 _chemical_formula_sum 'C16 H12 N6 Ni S2' _chemical_formula_weight 411.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 5.5903(2) _cell_length_b 24.6665(11) _cell_length_c 12.7539(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.465(2) _cell_angle_gamma 90.00 _cell_volume 1729.42(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3885 _cell_measurement_theta_min 3.30 _cell_measurement_theta_max 27.55 _exptl_crystal_description 'Rectangular plates' _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.375 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8204 _exptl_absorpt_correction_T_max 0.8748 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 6633 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 27.55 _reflns_number_total 3885 _reflns_number_gt 2372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0289P)^2^+1.9774P] 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 none _refine_ls_number_reflns 3885 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.116 _refine_ls_shift/su_mean 0.004 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 0.57188(8) -0.062043(19) 0.21944(3) 0.02410(14) Uani 1 1 d . . . S1C S 0.40413(15) -0.06283(5) 0.39062(7) 0.0338(2) Uani 1 1 d . . . S1D S 0.73454(15) -0.05944(4) 0.05032(7) 0.0304(2) Uani 1 1 d . . . N7A N 0.5498(6) 0.02499(13) 0.2202(3) 0.0312(7) Uani 1 1 d . . . N9A N 1.5241(7) 0.18880(16) 0.3680(3) 0.0573(10) Uani 1 1 d . . . N7B N 0.5428(6) -0.14863(13) 0.2100(3) 0.0303(8) Uani 1 1 d . . . N9B N 1.4308(8) -0.30871(16) 0.4795(3) 0.0659(12) Uani 1 1 d . . . N1C N 0.9012(5) -0.06379(12) 0.3121(2) 0.0242(6) Uani 1 1 d . . . N1D N 0.2368(5) -0.06122(13) 0.1278(2) 0.0270(7) Uani 1 1 d . . . C1A C 0.7596(6) 0.05820(15) 0.2504(3) 0.0280(8) Uani 1 1 d . . . C2A C 0.8562(7) 0.06545(16) 0.3572(3) 0.0357(9) Uani 1 1 d . . . H2A H 0.7854 0.0482 0.4088 0.043 Uiso 1 1 calc R . . C3A C 1.0568(7) 0.09806(16) 0.3875(3) 0.0376(10) Uani 1 1 d . . . H3A H 1.1208 0.1028 0.4594 0.045 Uiso 1 1 calc R . . C4A C 1.1639(7) 0.12388(15) 0.3111(3) 0.0327(9) Uani 1 1 d . . . C5A C 1.0699(7) 0.11529(15) 0.2038(3) 0.0355(9) Uani 1 1 d . . . H5A H 1.1424 0.1317 0.1519 0.043 Uiso 1 1 calc R . . C6A C 0.8681(7) 0.08227(15) 0.1739(3) 0.0323(9) Uani 1 1 d . . . H6A H 0.8063 0.0764 0.1020 0.039 Uiso 1 1 calc R . . C8A C 1.3662(8) 0.15965(17) 0.3425(3) 0.0401(10) Uani 1 1 d . . . C1B C 0.7316(7) -0.18208(14) 0.2657(3) 0.0290(8) Uani 1 1 d . . . C2B C 0.9100(7) -0.20241(14) 0.2140(3) 0.0305(9) Uani 1 1 d . . . H2B H 0.9066 -0.1940 0.1427 0.037 Uiso 1 1 calc R . . C3B C 1.0927(7) -0.23501(15) 0.2678(3) 0.0357(9) Uani 1 1 d . . . H3B H 1.2093 -0.2496 0.2323 0.043 Uiso 1 1 calc R . . C4B C 1.1013(7) -0.24594(15) 0.3754(3) 0.0382(10) Uani 1 1 d . . . C5B C 0.9251(8) -0.22449(17) 0.4276(3) 0.0420(10) Uani 1 1 d . . . H5B H 0.9320 -0.2314 0.4997 0.050 Uiso 1 1 calc R . . C6B C 0.7415(8) -0.19320(16) 0.3730(3) 0.0378(10) Uani 1 1 d . . . H6B H 0.6228 -0.1793 0.4081 0.045 Uiso 1 1 calc R . . C8B C 1.2884(9) -0.28104(17) 0.4324(4) 0.0484(11) Uani 1 1 d . . . C1C C 1.1081(6) -0.06366(14) 0.3447(3) 0.0229(7) Uani 1 1 d . . . C1D C 0.0301(6) -0.05994(14) 0.0954(3) 0.0232(7) Uani 1 1 d . . . H7A1 H 0.477(7) 0.0341(16) 0.154(3) 0.040(12) Uiso 1 1 d . . . H7A2 H 0.457(8) 0.0289(18) 0.266(3) 0.053(14) Uiso 1 1 d . . . H7B1 H 0.411(8) -0.1535(16) 0.232(3) 0.045(13) Uiso 1 1 d . . . H7B2 H 0.531(7) -0.1560(16) 0.140(3) 0.044(12) Uiso 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 Ni1 0.0125(2) 0.0348(3) 0.0245(2) 0.0006(2) 0.00187(17) 0.0007(2) S1C 0.0130(4) 0.0661(7) 0.0213(5) -0.0001(5) 0.0004(4) 0.0008(5) S1D 0.0143(4) 0.0536(6) 0.0224(5) 0.0012(5) 0.0013(4) -0.0016(4) N7A 0.0219(17) 0.0376(19) 0.0333(19) 0.0033(17) 0.0029(16) 0.0047(15) N9A 0.046(2) 0.053(2) 0.071(3) -0.007(2) 0.008(2) -0.009(2) N7B 0.0220(18) 0.0355(19) 0.0324(19) 0.0050(16) 0.0023(16) -0.0021(14) N9B 0.071(3) 0.047(2) 0.065(3) 0.008(2) -0.026(2) 0.009(2) N1C 0.0161(15) 0.0334(16) 0.0236(15) -0.0004(14) 0.0050(12) -0.0009(13) N1D 0.0138(15) 0.0439(18) 0.0230(15) 0.0021(14) 0.0025(12) 0.0012(14) C1A 0.0237(18) 0.027(2) 0.032(2) -0.0033(17) 0.0027(16) 0.0061(17) C2A 0.036(2) 0.045(2) 0.028(2) -0.0033(19) 0.0093(18) -0.005(2) C3A 0.039(2) 0.046(3) 0.026(2) -0.0041(18) -0.0007(18) 0.001(2) C4A 0.031(2) 0.026(2) 0.042(2) -0.0007(18) 0.0090(19) 0.0040(16) C5A 0.043(2) 0.031(2) 0.036(2) 0.0033(18) 0.014(2) 0.0050(19) C6A 0.040(2) 0.034(2) 0.0219(19) 0.0017(17) 0.0028(18) 0.0010(18) C8A 0.040(3) 0.036(2) 0.043(2) -0.003(2) 0.004(2) 0.000(2) C1B 0.030(2) 0.025(2) 0.0291(19) 0.0018(16) -0.0028(16) -0.0055(16) C2B 0.032(2) 0.030(2) 0.028(2) 0.0023(16) 0.0028(18) -0.0022(17) C3B 0.029(2) 0.032(2) 0.044(2) -0.0024(19) 0.0004(19) -0.0013(17) C4B 0.036(2) 0.028(2) 0.045(2) 0.0049(19) -0.008(2) -0.0022(17) C5B 0.054(3) 0.041(3) 0.029(2) 0.0112(19) 0.002(2) 0.002(2) C6B 0.040(2) 0.039(2) 0.036(2) 0.0057(19) 0.010(2) 0.0015(19) C8B 0.056(3) 0.034(2) 0.048(3) -0.001(2) -0.012(2) -0.003(2) C1C 0.0178(17) 0.0318(19) 0.0207(17) 0.0018(16) 0.0080(14) 0.0006(16) C1D 0.0231(18) 0.0262(19) 0.0214(17) 0.0025(16) 0.0072(15) 0.0018(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 Ni1 N1C 1.999(3) . ? Ni1 N1D 2.020(3) . ? Ni1 N7B 2.144(3) . ? Ni1 N7A 2.151(3) . ? Ni1 S1D 2.4891(10) . ? Ni1 S1C 2.5278(10) . ? S1C C1C 1.652(3) 1_455 ? S1D C1D 1.648(3) 1_655 ? N7A C1A 1.425(5) . ? N9A C8A 1.139(5) . ? N7B C1B 1.423(5) . ? N9B C8B 1.135(5) . ? N1C C1C 1.155(4) . ? N1D C1D 1.155(4) . ? C1A C6A 1.374(5) . ? C1A C2A 1.383(5) . ? C2A C3A 1.377(5) . ? C3A C4A 1.388(5) . ? C4A C5A 1.389(5) . ? C4A C8A 1.433(6) . ? C5A C6A 1.387(5) . ? C1B C2B 1.386(5) . ? C1B C6B 1.387(5) . ? C2B C3B 1.380(5) . ? C3B C4B 1.392(5) . ? C4B C5B 1.389(6) . ? C4B C8B 1.448(6) . ? C5B C6B 1.369(5) . ? C1C S1C 1.652(3) 1_655 ? C1D S1D 1.648(3) 1_455 ? 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 N1C Ni1 N1D 178.93(12) . . ? N1C Ni1 N7B 93.67(12) . . ? N1D Ni1 N7B 85.68(12) . . ? N1C Ni1 N7A 93.80(12) . . ? N1D Ni1 N7A 86.82(13) . . ? N7B Ni1 N7A 172.32(12) . . ? N1C Ni1 S1D 94.04(8) . . ? N1D Ni1 S1D 86.81(8) . . ? N7B Ni1 S1D 90.76(11) . . ? N7A Ni1 S1D 90.50(11) . . ? N1C Ni1 S1C 86.31(8) . . ? N1D Ni1 S1C 92.84(8) . . ? N7B Ni1 S1C 90.25(11) . . ? N7A Ni1 S1C 88.45(11) . . ? S1D Ni1 S1C 178.91(4) . . ? C1C S1C Ni1 101.47(11) 1_455 . ? C1D S1D Ni1 101.46(11) 1_655 . ? C1A N7A Ni1 122.0(2) . . ? C1B N7B Ni1 120.5(2) . . ? C1C N1C Ni1 165.1(3) . . ? C1D N1D Ni1 165.9(3) . . ? C6A C1A C2A 120.0(4) . . ? C6A C1A N7A 120.3(3) . . ? C2A C1A N7A 119.7(3) . . ? C3A C2A C1A 120.2(4) . . ? C2A C3A C4A 120.3(4) . . ? C3A C4A C5A 119.1(4) . . ? C3A C4A C8A 120.4(4) . . ? C5A C4A C8A 120.5(4) . . ? C6A C5A C4A 120.3(4) . . ? C1A C6A C5A 120.0(4) . . ? N9A C8A C4A 178.7(5) . . ? C2B C1B C6B 119.6(4) . . ? C2B C1B N7B 120.3(3) . . ? C6B C1B N7B 120.0(4) . . ? C3B C2B C1B 120.4(3) . . ? C2B C3B C4B 119.5(4) . . ? C5B C4B C3B 119.9(4) . . ? C5B C4B C8B 119.9(4) . . ? C3B C4B C8B 120.2(4) . . ? C6B C5B C4B 120.2(4) . . ? C5B C6B C1B 120.3(4) . . ? N9B C8B C4B 177.8(5) . . ? N1C C1C S1C 179.4(4) . 1_655 ? N1D C1D S1D 178.7(4) . 1_455 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7A H7A1 S1D 0.90(4) 2.73(4) 3.628(4) 178.12 . _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.711 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.079 #===END data_COMPOUND_2 _database_code_CSD 189529 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(3-aminobenzonitrile-N)-bis(?2-thiocyanato-N,S)) nickel(II) ; _chemical_name_common none _chemical_melting_point 'DSC onset temperature = 249.2oC' _chemical_formula_moiety Ni(NCS)2(C7H6N2)2 _chemical_formula_sum 'C16 H12 N6 Ni S2' _chemical_formula_weight 411.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 16.9554(3) _cell_length_b 5.55420(10) _cell_length_c 18.2897(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.4910(10) _cell_angle_gamma 90.00 _cell_volume 1720.78(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2120 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 28.26 _exptl_crystal_description 'rectangular plates' _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.381 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7993 _exptl_absorpt_correction_T_max 0.8196 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 5462 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 28.26 _reflns_number_total 2120 _reflns_number_gt 1948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0255P)^2^+1.4061P] 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 none _refine_ls_number_reflns 2120 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0226 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0587 _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 Ni1 Ni 0.0000 0.0000 0.5000 0.01570(8) Uani 1 2 d S . . S1 S 0.10761(2) -0.23737(6) 0.56922(2) 0.02509(10) Uani 1 1 d . . . N1 N -0.06428(7) -0.2974(2) 0.47625(6) 0.0190(2) Uani 1 1 d . . . N7A N -0.05711(7) 0.0693(2) 0.59972(7) 0.0207(2) Uani 1 1 d . . . N9A N -0.08133(8) -0.7764(3) 0.79103(7) 0.0304(3) Uani 1 1 d . . . C1 C -0.08246(8) -0.4886(2) 0.45720(7) 0.0161(3) Uani 1 1 d . . . C1A C -0.11045(8) -0.1062(2) 0.62594(7) 0.0196(3) Uani 1 1 d . . . C2A C -0.08286(8) -0.2824(3) 0.67429(7) 0.0207(3) Uani 1 1 d . . . H2A H -0.0300 -0.2853 0.6900 0.025 Uiso 1 1 calc R . . C3A C -0.13505(8) -0.4555(3) 0.69916(7) 0.0207(3) Uani 1 1 d . . . C4A C -0.21417(9) -0.4571(3) 0.67495(9) 0.0278(3) Uani 1 1 d . . . H4A H -0.2486 -0.5733 0.6915 0.033 Uiso 1 1 calc R . . C5A C -0.24028(9) -0.2824(3) 0.62590(9) 0.0317(3) Uani 1 1 d . . . H5A H -0.2928 -0.2824 0.6089 0.038 Uiso 1 1 calc R . . C6A C -0.18929(9) -0.1066(3) 0.60159(8) 0.0267(3) Uani 1 1 d . . . H6A H -0.2079 0.0110 0.5690 0.032 Uiso 1 1 calc R . . C8A C -0.10599(8) -0.6344(3) 0.75083(7) 0.0225(3) Uani 1 1 d . . . H71A H -0.0208(12) 0.094(4) 0.6301(11) 0.032(5) Uiso 1 1 d . . . H72A H -0.0819(10) 0.206(4) 0.5891(9) 0.028(4) Uiso 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 Ni1 0.01815(13) 0.00947(13) 0.01908(13) -0.00114(8) -0.00365(9) -0.00178(8) S1 0.02724(19) 0.01141(16) 0.0354(2) -0.00248(13) -0.01301(15) -0.00260(12) N1 0.0191(5) 0.0135(5) 0.0239(5) 0.0007(4) -0.0056(4) 0.0003(4) N7A 0.0231(6) 0.0170(6) 0.0218(6) -0.0019(5) -0.0019(5) -0.0020(5) N9A 0.0297(7) 0.0346(7) 0.0269(6) 0.0062(6) 0.0015(5) 0.0035(6) C1 0.0154(6) 0.0143(6) 0.0181(6) 0.0019(5) -0.0048(5) 0.0004(4) C1A 0.0208(6) 0.0190(6) 0.0189(6) -0.0032(5) 0.0013(5) -0.0004(5) C2A 0.0179(6) 0.0246(7) 0.0194(6) -0.0016(5) -0.0025(5) -0.0003(5) C3A 0.0208(6) 0.0231(7) 0.0182(6) -0.0007(5) -0.0001(5) 0.0023(5) C4A 0.0195(7) 0.0300(8) 0.0340(8) 0.0051(6) 0.0013(6) -0.0035(6) C5A 0.0169(7) 0.0379(9) 0.0396(8) 0.0082(7) -0.0051(6) -0.0004(6) C6A 0.0230(7) 0.0277(8) 0.0290(7) 0.0057(6) -0.0033(6) 0.0036(6) C8A 0.0214(6) 0.0255(7) 0.0206(6) 0.0004(6) 0.0025(5) -0.0001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.0159(11) . ? Ni1 N1 2.0159(11) 5_556 ? Ni1 N7A 2.1367(12) . ? Ni1 N7A 2.1367(12) 5_556 ? Ni1 S1 2.5435(3) 5_556 ? Ni1 S1 2.5435(3) . ? S1 C1 1.6475(13) 5_546 ? N1 C1 1.1553(17) . ? N7A C1A 1.4266(18) . ? N9A C8A 1.1449(19) . ? C1 S1 1.6475(13) 5_546 ? C1A C2A 1.387(2) . ? C1A C6A 1.390(2) . ? C2A C3A 1.3963(19) . ? C3A C4A 1.394(2) . ? C3A C8A 1.443(2) . ? C4A C5A 1.381(2) . ? C5A C6A 1.390(2) . ? 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 Ni1 N1 180.00(6) . 5_556 ? N1 Ni1 N7A 94.05(5) . . ? N1 Ni1 N7A 85.95(5) 5_556 . ? N1 Ni1 N7A 85.95(5) . 5_556 ? N1 Ni1 N7A 94.05(5) 5_556 5_556 ? N7A Ni1 N7A 180.0 . 5_556 ? N1 Ni1 S1 87.02(3) . 5_556 ? N1 Ni1 S1 92.98(3) 5_556 5_556 ? N7A Ni1 S1 89.41(4) . 5_556 ? N7A Ni1 S1 90.59(4) 5_556 5_556 ? N1 Ni1 S1 92.98(3) . . ? N1 Ni1 S1 87.02(3) 5_556 . ? N7A Ni1 S1 90.59(4) . . ? N7A Ni1 S1 89.41(4) 5_556 . ? S1 Ni1 S1 180.000(15) 5_556 . ? C1 S1 Ni1 99.32(5) 5_546 . ? C1 N1 Ni1 162.33(11) . . ? C1A N7A Ni1 118.77(9) . . ? N1 C1 S1 179.30(13) . 5_546 ? C2A C1A C6A 119.75(13) . . ? C2A C1A N7A 119.69(12) . . ? C6A C1A N7A 120.53(13) . . ? C1A C2A C3A 119.52(12) . . ? C4A C3A C2A 121.03(13) . . ? C4A C3A C8A 120.01(13) . . ? C2A C3A C8A 118.96(12) . . ? C5A C4A C3A 118.60(14) . . ? C4A C5A C6A 120.99(14) . . ? C5A C6A C1A 120.08(14) . . ? N9A C8A C3A 178.44(15) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 28.26 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.284 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.054 #===END data_COMPOUND_3 _database_code_CSD 189530 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(?2-2-aminobenzonitrile-N,N)-bis(thiocyanato-N)) nickel(II) ; _chemical_name_common none _chemical_melting_point 'DSC onset temperature = 180.1oC' _chemical_formula_moiety Ni(NCS)2(C7H6N2)2 _chemical_formula_sum 'C16 H12 N6 Ni S2' _chemical_formula_weight 411.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 22.1014(7) _cell_length_b 7.5459(3) _cell_length_c 11.1386(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.440(2) _cell_angle_gamma 90.00 _cell_volume 1704.34(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1958 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 27.51 _exptl_crystal_description 'rectangular plates' _exptl_crystal_colour blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 1.395 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9335 _exptl_absorpt_correction_T_max 0.9335 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 3494 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0605 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.51 _reflns_number_total 1958 _reflns_number_gt 1516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0252P)^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 none _refine_ls_number_reflns 1958 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0708 _refine_ls_wR_factor_gt 0.0652 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.121 _refine_ls_shift/su_mean 0.006 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 0.0000 0.0000 0.02045(14) Uani 1 2 d S . . S1 S 0.09497(3) 0.44522(8) 0.33287(5) 0.03349(18) Uani 1 1 d . . . N1 N 0.04675(8) 0.1827(3) 0.14016(16) 0.0256(4) Uani 1 1 d . . . N7A N -0.06785(8) 0.2102(3) -0.10021(19) 0.0235(4) Uani 1 1 d . . . N9A N -0.06259(8) 0.0697(2) -0.40668(15) 0.0268(4) Uani 1 1 d . . . C1 C 0.06642(9) 0.2922(3) 0.21922(19) 0.0233(5) Uani 1 1 d . . . C1A C -0.13462(9) 0.1731(3) -0.18484(18) 0.0219(5) Uani 1 1 d . . . C2A C -0.15129(9) 0.1185(3) -0.31376(18) 0.0222(5) Uani 1 1 d . . . C3A C -0.21692(9) 0.0867(3) -0.3966(2) 0.0279(5) Uani 1 1 d . . . H3A H -0.2276 0.0518 -0.4827 0.033 Uiso 1 1 calc R . . C4A C -0.26592(10) 0.1073(3) -0.3505(2) 0.0304(5) Uani 1 1 d . . . H4A H -0.3098 0.0884 -0.4058 0.036 Uiso 1 1 calc R . . C5A C -0.24948(10) 0.1560(3) -0.2222(2) 0.0320(5) Uani 1 1 d . . . H5A H -0.2824 0.1673 -0.1907 0.038 Uiso 1 1 calc R . . C6A C -0.18444(9) 0.1885(3) -0.1395(2) 0.0268(5) Uani 1 1 d . . . H6A H -0.1741 0.2208 -0.0531 0.032 Uiso 1 1 calc R . . C8A C -0.10107(10) 0.0935(3) -0.36405(19) 0.0229(5) Uani 1 1 d . . . H7A H -0.0489(10) 0.273(3) -0.141(2) 0.028(6) Uiso 1 1 d . . . H7B H -0.0674(9) 0.269(3) -0.039(2) 0.022(6) Uiso 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 Ni1 0.0227(2) 0.0242(3) 0.0148(2) -0.00114(15) 0.00782(15) 0.00050(15) S1 0.0413(4) 0.0323(4) 0.0241(3) -0.0062(2) 0.0101(3) -0.0112(3) N1 0.0273(9) 0.0294(12) 0.0193(9) -0.0002(8) 0.0083(7) 0.0021(8) N7A 0.0272(10) 0.0258(12) 0.0173(9) -0.0028(9) 0.0086(8) -0.0010(8) N9A 0.0286(9) 0.0319(13) 0.0199(10) 0.0005(8) 0.0094(8) 0.0004(8) C1 0.0235(11) 0.0271(14) 0.0200(10) 0.0037(9) 0.0093(8) -0.0001(9) C1A 0.0238(11) 0.0197(13) 0.0198(10) 0.0031(8) 0.0061(8) 0.0042(8) C2A 0.0260(11) 0.0221(13) 0.0200(10) 0.0028(9) 0.0108(8) 0.0032(9) C3A 0.0325(12) 0.0274(15) 0.0200(11) -0.0013(9) 0.0065(9) 0.0008(10) C4A 0.0228(11) 0.0299(15) 0.0338(12) 0.0002(10) 0.0062(9) -0.0018(10) C5A 0.0312(12) 0.0358(16) 0.0346(12) 0.0033(10) 0.0189(10) 0.0036(10) C6A 0.0324(12) 0.0290(15) 0.0213(10) 0.0008(9) 0.0129(9) 0.0059(9) C8A 0.0279(11) 0.0212(14) 0.0157(10) -0.0002(9) 0.0044(8) -0.0006(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 Ni1 N1 2.0304(18) 5 ? Ni1 N1 2.0304(18) . ? Ni1 N9A 2.1011(17) 6_556 ? Ni1 N9A 2.1012(17) 2_554 ? Ni1 N7A 2.1631(18) . ? Ni1 N7A 2.1631(18) 5 ? S1 C1 1.643(2) . ? N1 C1 1.159(3) . ? N7A C1A 1.428(2) . ? N9A C8A 1.141(2) . ? N9A Ni1 2.1012(17) 2_554 ? C1A C6A 1.386(3) . ? C1A C2A 1.395(3) . ? C2A C3A 1.396(3) . ? C2A C8A 1.441(3) . ? C3A C4A 1.379(3) . ? C4A C5A 1.377(3) . ? C5A C6A 1.386(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 Ni1 N1 180.00(12) 5 . ? N1 Ni1 N9A 88.65(6) 5 6_556 ? N1 Ni1 N9A 91.35(6) . 6_556 ? N1 Ni1 N9A 91.35(6) 5 2_554 ? N1 Ni1 N9A 88.65(6) . 2_554 ? N9A Ni1 N9A 180.00(6) 6_556 2_554 ? N1 Ni1 N7A 93.72(7) 5 . ? N1 Ni1 N7A 86.28(7) . . ? N9A Ni1 N7A 88.93(7) 6_556 . ? N9A Ni1 N7A 91.07(7) 2_554 . ? N1 Ni1 N7A 86.28(7) 5 5 ? N1 Ni1 N7A 93.72(7) . 5 ? N9A Ni1 N7A 91.07(7) 6_556 5 ? N9A Ni1 N7A 88.93(7) 2_554 5 ? N7A Ni1 N7A 180.00(11) . 5 ? C1 N1 Ni1 172.27(16) . . ? C1A N7A Ni1 121.28(14) . . ? C8A N9A Ni1 172.51(17) . 2_554 ? N1 C1 S1 179.1(2) . . ? C6A C1A C2A 118.45(17) . . ? C6A C1A N7A 120.35(18) . . ? C2A C1A N7A 121.19(17) . . ? C1A C2A C3A 120.71(17) . . ? C1A C2A C8A 120.65(17) . . ? C3A C2A C8A 118.63(17) . . ? C4A C3A C2A 119.86(19) . . ? C5A C4A C3A 119.61(19) . . ? C4A C5A C6A 120.84(19) . . ? C5A C6A C1A 120.47(19) . . ? N9A C8A C2A 177.8(2) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.363 _refine_diff_density_min -0.419 _refine_diff_density_rms 0.072 #===END data_COMPOUND_4 _database_code_CSD 189531 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(?2-4-aminobenzonitrile-N,N)-bis(thiocyanato-N)) nickel(II) 4-aminobenzonitrile clathrate ; _chemical_name_common none _chemical_melting_point 'DSC onset temperature = 230.7oC' _chemical_formula_moiety Ni(NCS)2(C7H6N2)2.(C7H6N2) _chemical_formula_sum 'C23 H18 N8 Ni S2' _chemical_formula_weight 529.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 9.37110(10) _cell_length_b 13.2066(2) _cell_length_c 19.5217(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.9030(10) _cell_angle_gamma 90.00 _cell_volume 2403.20(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5476 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.45 _exptl_crystal_description 'rectangular plates' _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8236 _exptl_absorpt_correction_T_max 0.9058 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'combination of phi and omega' _diffrn_reflns_number 5476 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5476 _reflns_number_gt 4387 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED a graphical interface to SHELXL (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0283P)^2^+1.0889P] 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 none _refine_ls_number_reflns 5476 _refine_ls_number_parameters 331 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.305 _refine_ls_shift/su_mean 0.009 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 0.65129(2) 0.455589(15) 0.177213(11) 0.01906(7) Uani 1 1 d . . . S3C S 0.36097(5) 0.29407(4) -0.00072(2) 0.03602(13) Uani 1 1 d . . . S3D S 0.93890(5) 0.61613(3) 0.35694(2) 0.03134(12) Uani 1 1 d . . . N7G N 1.1727(2) 0.52709(16) 0.50643(10) 0.0394(4) Uani 1 1 d . . . N7A N 0.76181(14) 0.31590(11) 0.20944(9) 0.0219(3) Uani 1 1 d . . . N9A N 0.47332(14) 0.39353(11) 0.21765(7) 0.0240(3) Uani 1 1 d . . . N7B N 0.54084(14) 0.59647(11) 0.14684(9) 0.0219(3) Uani 1 1 d . . . N9B N 0.82930(15) 0.51484(11) 0.13608(8) 0.0268(3) Uani 1 1 d . . . N1C N 0.57470(16) 0.38853(11) 0.08761(8) 0.0266(3) Uani 1 1 d . . . N1D N 0.72544(16) 0.52342(11) 0.26739(8) 0.0284(3) Uani 1 1 d . . . N9G N 1.67531(19) 0.27500(13) 0.35123(8) 0.0392(4) Uani 1 1 d . . . C1A C -0.08612(16) 0.31688(12) 0.21501(9) 0.0195(3) Uani 1 1 d . . . C2A C -0.01346(17) 0.29068(13) 0.15882(9) 0.0231(4) Uani 1 1 d . . . H2A H -0.0637 0.2638 0.1194 0.028 Uiso 1 1 calc R . . C3A C 0.13337(17) 0.30458(13) 0.16147(9) 0.0236(4) Uani 1 1 d . . . H3A H 0.1820 0.2878 0.1238 0.028 Uiso 1 1 calc R . . C4A C 0.20784(16) 0.34405(12) 0.22112(9) 0.0206(3) Uani 1 1 d . . . C5A C 0.13663(17) 0.36613(12) 0.27875(9) 0.0220(4) Uani 1 1 d . . . H5A H 0.1875 0.3901 0.3189 0.026 Uiso 1 1 calc R . . C6A C -0.00993(17) 0.35201(12) 0.27561(9) 0.0209(3) Uani 1 1 d . . . H6A H -0.0580 0.3659 0.3139 0.025 Uiso 1 1 calc R . . C8A C 0.35706(17) 0.36907(12) 0.22082(9) 0.0221(4) Uani 1 1 d . . . C1B C 1.38846(16) 0.59267(12) 0.14094(9) 0.0196(3) Uani 1 1 d . . . C2B C 1.31374(17) 0.55950(12) 0.07964(9) 0.0226(4) Uani 1 1 d . . . H2B H 1.3621 0.5479 0.0411 0.027 Uiso 1 1 calc R . . C3B C 1.16751(17) 0.54399(13) 0.07648(9) 0.0241(4) Uani 1 1 d . . . H3B H 1.1175 0.5199 0.0361 0.029 Uiso 1 1 calc R . . C4B C 1.09475(17) 0.56445(12) 0.13364(9) 0.0225(4) Uani 1 1 d . . . C5B C 1.16836(18) 0.60140(13) 0.19414(9) 0.0244(4) Uani 1 1 d . . . H5B H 1.1192 0.6170 0.2318 0.029 Uiso 1 1 calc R . . C6B C 1.31542(18) 0.61457(12) 0.19764(9) 0.0232(4) Uani 1 1 d . . . H6B H 1.3656 0.6382 0.2381 0.028 Uiso 1 1 calc R . . C8B C 0.94520(18) 0.53939(12) 0.13341(9) 0.0239(4) Uani 1 1 d . . . C2C C 0.48617(19) 0.34748(13) 0.05164(9) 0.0248(4) Uani 1 1 d . . . C2D C 0.81390(19) 0.56192(12) 0.30461(9) 0.0239(4) Uani 1 1 d . . . C1G C 1.27024(19) 0.47612(14) 0.47315(9) 0.0288(4) Uani 1 1 d . . . C2G C 1.3558(2) 0.52622(14) 0.42909(10) 0.0326(4) Uani 1 1 d . . . H2G H 1.3426 0.5952 0.4210 0.039 Uiso 1 1 calc R . . C3G C 1.4589(2) 0.47530(15) 0.39760(10) 0.0321(4) Uani 1 1 d . . . H3G H 1.5157 0.5101 0.3691 0.038 Uiso 1 1 calc R . . C4G C 1.4787(2) 0.37098(14) 0.40820(9) 0.0300(4) Uani 1 1 d . . . C5G C 1.3909(2) 0.32042(14) 0.45050(10) 0.0354(5) Uani 1 1 d . . . H5G H 1.4023 0.2511 0.4574 0.042 Uiso 1 1 calc R . . C6G C 1.2881(2) 0.37099(14) 0.48212(10) 0.0351(4) Uani 1 1 d . . . H6G H 1.2299 0.3357 0.5096 0.042 Uiso 1 1 calc R . . C8G C 1.5882(2) 0.31805(15) 0.37651(10) 0.0319(4) Uani 1 1 d . . . H7A1 H 0.725(2) 0.2711(15) 0.1788(10) 0.028(5) Uiso 1 1 d . . . H7A2 H 0.7320(19) 0.3034(14) 0.2483(10) 0.022(5) Uiso 1 1 d . . . H7B1 H 0.575(2) 0.6389(15) 0.1784(10) 0.027(5) Uiso 1 1 d . . . H7B2 H 0.572(2) 0.6145(15) 0.1082(11) 0.031(6) Uiso 1 1 d . . . H7G1 H 1.162(3) 0.588(2) 0.4990(12) 0.054(8) Uiso 1 1 d . . . H7G2 H 1.130(3) 0.497(2) 0.5368(14) 0.055(8) Uiso 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 Ni1 0.01139(10) 0.02329(12) 0.02226(12) 0.00007(9) 0.00052(8) -0.00254(8) S3C 0.0404(3) 0.0368(3) 0.0289(3) 0.0002(2) -0.0059(2) -0.0157(2) S3D 0.0314(2) 0.0313(2) 0.0288(3) -0.00268(19) -0.0089(2) -0.00351(19) N7G 0.0383(10) 0.0377(11) 0.0429(11) 0.0060(9) 0.0081(9) 0.0050(9) N7A 0.0139(7) 0.0249(8) 0.0264(8) -0.0003(7) 0.0001(6) -0.0034(6) N9A 0.0170(7) 0.0270(8) 0.0280(8) 0.0038(6) 0.0016(6) -0.0004(6) N7B 0.0135(7) 0.0243(8) 0.0280(9) -0.0003(7) 0.0015(6) -0.0032(6) N9B 0.0175(7) 0.0267(8) 0.0363(9) 0.0048(7) 0.0038(6) -0.0012(6) N1C 0.0263(8) 0.0293(8) 0.0238(8) 0.0011(6) 0.0003(6) -0.0019(6) N1D 0.0239(8) 0.0298(8) 0.0301(8) -0.0018(7) -0.0034(7) -0.0014(6) N9G 0.0428(10) 0.0437(10) 0.0313(9) 0.0071(8) 0.0046(8) 0.0050(8) C1A 0.0139(7) 0.0176(8) 0.0264(9) 0.0030(7) -0.0002(7) -0.0004(6) C2A 0.0201(8) 0.0253(9) 0.0232(9) -0.0028(7) -0.0013(7) -0.0016(7) C3A 0.0218(8) 0.0244(8) 0.0255(9) 0.0017(7) 0.0067(7) 0.0011(7) C4A 0.0132(7) 0.0202(8) 0.0285(9) 0.0058(7) 0.0022(7) 0.0000(6) C5A 0.0171(8) 0.0232(8) 0.0250(9) 0.0011(7) -0.0016(7) -0.0017(7) C6A 0.0167(8) 0.0231(8) 0.0232(9) 0.0017(7) 0.0030(7) 0.0010(7) C8A 0.0190(8) 0.0208(8) 0.0261(9) 0.0051(7) 0.0011(7) 0.0015(7) C1B 0.0146(7) 0.0168(8) 0.0271(9) 0.0027(7) 0.0008(7) 0.0000(6) C2B 0.0177(8) 0.0278(9) 0.0227(9) 0.0042(7) 0.0043(7) 0.0009(7) C3B 0.0182(8) 0.0273(9) 0.0257(9) 0.0028(7) -0.0029(7) -0.0006(7) C4B 0.0143(7) 0.0208(8) 0.0325(10) 0.0075(7) 0.0033(7) 0.0007(6) C5B 0.0223(8) 0.0218(8) 0.0303(10) 0.0008(7) 0.0084(7) 0.0022(7) C6B 0.0212(8) 0.0203(8) 0.0279(9) -0.0022(7) 0.0013(7) -0.0010(7) C8B 0.0189(8) 0.0211(8) 0.0319(10) 0.0058(7) 0.0033(7) 0.0009(7) C2C 0.0281(9) 0.0248(9) 0.0216(9) 0.0037(7) 0.0026(8) -0.0004(7) C2D 0.0256(9) 0.0226(9) 0.0233(9) 0.0016(7) 0.0013(7) 0.0039(7) C1G 0.0243(9) 0.0339(10) 0.0268(9) -0.0015(8) -0.0044(8) -0.0008(8) C2G 0.0342(10) 0.0276(10) 0.0348(11) 0.0052(8) -0.0017(9) -0.0007(8) C3G 0.0306(10) 0.0360(10) 0.0290(10) 0.0048(8) 0.0004(8) -0.0056(8) C4G 0.0304(10) 0.0332(10) 0.0256(10) -0.0023(8) -0.0009(8) -0.0025(8) C5G 0.0459(12) 0.0249(9) 0.0359(11) 0.0012(8) 0.0063(9) -0.0031(9) C6G 0.0405(11) 0.0313(10) 0.0343(11) 0.0018(8) 0.0079(9) -0.0070(9) C8G 0.0337(10) 0.0351(10) 0.0258(10) 0.0040(8) -0.0021(8) -0.0018(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 Ni1 N1C 2.0252(15) . ? Ni1 N1D 2.0329(15) . ? Ni1 N9B 2.0773(14) . ? Ni1 N9A 2.0849(14) . ? Ni1 N7A 2.1766(14) . ? Ni1 N7B 2.1814(14) . ? S3C C2C 1.6347(18) . ? S3D C2D 1.6377(18) . ? N7G C1G 1.354(3) . ? N7A C1A 1.418(2) 1_655 ? N9A C8A 1.144(2) . ? N7B C1B 1.422(2) 1_455 ? N9B C8B 1.140(2) . ? N1C C2C 1.164(2) . ? N1D C2D 1.162(2) . ? N9G C8G 1.148(2) . ? C1A C2A 1.393(2) . ? C1A C6A 1.397(2) . ? C1A N7A 1.418(2) 1_455 ? C2A C3A 1.384(2) . ? C3A C4A 1.396(2) . ? C4A C5A 1.397(2) . ? C4A C8A 1.437(2) . ? C5A C6A 1.381(2) . ? C1B C6B 1.390(2) . ? C1B C2B 1.394(2) . ? C1B N7B 1.422(2) 1_655 ? C2B C3B 1.381(2) . ? C3B C4B 1.393(3) . ? C4B C5B 1.393(2) . ? C4B C8B 1.440(2) . ? C5B C6B 1.384(2) . ? C1G C2G 1.401(3) . ? C1G C6G 1.407(3) . ? C2G C3G 1.373(3) . ? C3G C4G 1.403(3) . ? C4G C5G 1.395(3) . ? C4G C8G 1.433(3) . ? C5G C6G 1.370(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 N1C Ni1 N1D 179.23(6) . . ? N1C Ni1 N9B 93.34(6) . . ? N1D Ni1 N9B 87.26(6) . . ? N1C Ni1 N9A 85.92(6) . . ? N1D Ni1 N9A 93.49(6) . . ? N9B Ni1 N9A 178.93(6) . . ? N1C Ni1 N7A 89.70(6) . . ? N1D Ni1 N7A 90.75(6) . . ? N9B Ni1 N7A 93.09(6) . . ? N9A Ni1 N7A 86.15(5) . . ? N1C Ni1 N7B 91.26(6) . . ? N1D Ni1 N7B 88.28(6) . . ? N9B Ni1 N7B 87.20(6) . . ? N9A Ni1 N7B 93.58(5) . . ? N7A Ni1 N7B 178.97(7) . . ? C1A N7A Ni1 117.32(10) 1_655 . ? C8A N9A Ni1 159.18(14) . . ? C1B N7B Ni1 115.88(10) 1_455 . ? C8B N9B Ni1 158.70(15) . . ? C2C N1C Ni1 153.11(14) . . ? C2D N1D Ni1 153.22(15) . . ? C2A C1A C6A 120.06(14) . . ? C2A C1A N7A 120.41(15) . 1_455 ? C6A C1A N7A 119.35(15) . 1_455 ? C3A C2A C1A 120.16(15) . . ? C2A C3A C4A 119.39(16) . . ? C3A C4A C5A 120.72(15) . . ? C3A C4A C8A 119.06(15) . . ? C5A C4A C8A 120.06(15) . . ? C6A C5A C4A 119.44(15) . . ? C5A C6A C1A 120.12(16) . . ? N9A C8A C4A 175.77(18) . . ? C6B C1B C2B 120.27(15) . . ? C6B C1B N7B 120.06(15) . 1_655 ? C2B C1B N7B 119.50(15) . 1_655 ? C3B C2B C1B 119.58(16) . . ? C2B C3B C4B 120.06(16) . . ? C3B C4B C5B 120.44(15) . . ? C3B C4B C8B 120.64(16) . . ? C5B C4B C8B 118.69(16) . . ? C6B C5B C4B 119.31(16) . . ? C5B C6B C1B 120.26(16) . . ? N9B C8B C4B 175.72(18) . . ? N1C C2C S3C 177.66(16) . . ? N1D C2D S3D 179.9(2) . . ? N7G C1G C2G 121.15(18) . . ? N7G C1G C6G 120.56(19) . . ? C2G C1G C6G 118.29(18) . . ? C3G C2G C1G 121.13(17) . . ? C2G C3G C4G 120.26(18) . . ? C5G C4G C3G 118.69(18) . . ? C5G C4G C8G 120.94(17) . . ? C3G C4G C8G 120.36(18) . . ? C6G C5G C4G 121.23(18) . . ? C5G C6G C1G 120.33(18) . . ? N9G C8G C4G 179.5(2) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N7A H7A2 N9G 0.85(2) 2.16(2) 3.012(2) 174.8(16) 1_455 N7B H7B2 S3C 0.87(2) 2.56(2) 3.4078(17) 167.1(18) 3_665 N7G H7G1 S3C 0.83(3) 2.73(3) 3.541(2) 169(2) 2_655 N7G H7G2 S3D 0.85(3) 2.69(3) 3.516(2) 166(2) 3_766 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.317 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.055 #===END data_COMPOUND_5 _database_code_CSD 189532 _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-(bis(?2-3-aminobenzonitrile-N,N)-bis(thiocyanato-N) nickel(II) benzene clathrate ; _chemical_name_common none _chemical_melting_point 'DSC onset temperature = 227.3oC' _chemical_formula_moiety Ni(NCS)2(C7H6N2)2.(C6H6) _chemical_formula_sum 'C11 H9 N3 Ni0.50 S' _chemical_formula_weight 244.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P21/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 8.6743(5) _cell_length_b 7.2741(5) _cell_length_c 17.4386(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.754(2) _cell_angle_gamma 90.00 _cell_volume 1084.43(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2352 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.10 _exptl_crystal_description 'rectangular plates' _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 504 _exptl_absorpt_coefficient_mu 1.109 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9067 _exptl_absorpt_correction_T_max 0.9466 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Combination of phi and omega' _diffrn_reflns_number 4183 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0595 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.10 _reflns_number_total 2352 _reflns_number_gt 1624 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius, 2000)' _computing_cell_refinement 'Collect (Nonius, 2000)' _computing_data_reduction 'Collect (Nonius, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED, a graphical interface to SHELX (1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0346P)^2^+0.8760P] 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 none _refine_ls_number_reflns 2352 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0767 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0876 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.005 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 0.0000 0.0000 0.02442(16) Uani 1 2 d S . . S1 S 0.02105(10) 0.48607(13) 0.18387(5) 0.0415(2) Uani 1 1 d . . . N9A N 0.8215(3) -0.0485(3) 0.06488(14) 0.0275(6) Uani 1 1 d . . . N1 N 0.0490(3) 0.2301(3) 0.06696(15) 0.0310(6) Uani 1 1 d . . . N7A N 0.1602(3) -0.1691(3) 0.07770(15) 0.0272(5) Uani 1 1 d . . . C3A C 0.5761(3) -0.0295(3) 0.12997(15) 0.0218(6) Uani 1 1 d . . . C2A C 0.4386(3) -0.1060(3) 0.08949(15) 0.0204(6) Uani 1 1 d . . . H2A H 0.4391 -0.1652 0.0423 0.024 Uiso 1 1 calc R . . C1A C 0.3017(3) -0.0936(4) 0.11978(16) 0.0218(6) Uani 1 1 d . . . C2G C 0.6593(3) 0.5356(4) 0.01163(18) 0.0287(7) Uani 1 1 d . . . H2G H 0.7661 0.5596 0.0193 0.034 Uiso 1 1 calc R . . C1 C 0.0380(3) 0.3360(4) 0.11577(17) 0.0276(6) Uani 1 1 d . . . C3G C 0.5937(4) 0.4516(4) 0.06926(18) 0.0301(7) Uani 1 1 d . . . H3G H 0.6566 0.4189 0.1159 0.036 Uiso 1 1 calc R . . C8A C 0.7158(3) -0.0411(3) 0.09562(17) 0.0239(6) Uani 1 1 d . . . C6A C 0.3027(3) -0.0031(4) 0.19035(16) 0.0291(6) Uani 1 1 d . . . H6A H 0.2109 0.0064 0.2110 0.035 Uiso 1 1 calc R . . C4A C 0.5781(3) 0.0602(4) 0.20062(17) 0.0285(7) Uani 1 1 d . . . H4A H 0.6701 0.1104 0.2275 0.034 Uiso 1 1 calc R . . C1G C 0.5651(4) 0.5843(4) -0.05808(18) 0.0295(6) Uani 1 1 d . . . H1G H 0.6089 0.6410 -0.0971 0.035 Uiso 1 1 calc R . . C5A C 0.4400(4) 0.0728(4) 0.22982(17) 0.0330(7) Uani 1 1 d . . . H5A H 0.4392 0.1333 0.2767 0.040 Uiso 1 1 calc R . . H7A H 0.1849 -0.2583 0.0460 0.040(9) Uiso 1 1 d R . . H8A H 0.0992 -0.2156 0.1128 0.052(11) 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 0.0140(2) 0.0250(3) 0.0349(3) -0.0014(2) 0.00583(19) -0.0021(2) S1 0.0389(5) 0.0482(5) 0.0391(5) -0.0126(4) 0.0119(4) -0.0078(4) N9A 0.0157(12) 0.0299(14) 0.0371(15) 0.0008(10) 0.0048(11) -0.0018(9) N1 0.0214(13) 0.0304(13) 0.0407(15) -0.0036(12) 0.0042(11) -0.0008(10) N7A 0.0145(11) 0.0268(12) 0.0404(15) 0.0008(11) 0.0050(10) -0.0005(10) C3A 0.0164(12) 0.0226(15) 0.0258(14) 0.0044(11) 0.0020(11) 0.0001(10) C2A 0.0184(13) 0.0212(14) 0.0217(14) 0.0015(10) 0.0041(11) 0.0000(10) C1A 0.0158(13) 0.0202(13) 0.0289(15) 0.0047(11) 0.0020(11) 0.0002(11) C2G 0.0257(14) 0.0230(15) 0.0374(17) -0.0051(12) 0.0053(12) -0.0024(11) C1 0.0158(14) 0.0315(16) 0.0352(17) 0.0037(13) 0.0038(12) -0.0025(12) C3G 0.0327(16) 0.0261(15) 0.0299(16) -0.0031(11) 0.0010(13) 0.0007(12) C8A 0.0177(14) 0.0222(15) 0.0297(16) 0.0009(10) -0.0018(12) -0.0016(10) C6A 0.0283(15) 0.0312(15) 0.0309(15) 0.0047(14) 0.0141(12) 0.0065(14) C4A 0.0284(16) 0.0287(15) 0.0258(16) 0.0020(11) -0.0026(12) -0.0008(12) C1G 0.0348(17) 0.0240(14) 0.0318(17) -0.0012(12) 0.0121(13) -0.0001(13) C5A 0.0435(19) 0.0332(15) 0.0224(16) -0.0019(12) 0.0060(14) 0.0050(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 N1 2.044(2) 3 ? Ni1 N1 2.044(2) . ? Ni1 N9A 2.096(2) 3_655 ? Ni1 N9A 2.096(2) 1_455 ? Ni1 N7A 2.155(2) 3 ? Ni1 N7A 2.155(2) . ? S1 C1 1.638(3) . ? N9A C8A 1.139(4) . ? N9A Ni1 2.096(2) 1_655 ? N1 C1 1.164(4) . ? N7A C1A 1.429(3) . ? C3A C4A 1.392(4) . ? C3A C2A 1.395(4) . ? C3A C8A 1.442(4) . ? C2A C1A 1.382(4) . ? C1A C6A 1.394(4) . ? C2G C3G 1.378(4) . ? C2G C1G 1.391(4) . ? C3G C1G 1.384(4) 3_665 ? C6A C5A 1.385(4) . ? C4A C5A 1.382(4) . ? C1G C3G 1.384(4) 3_665 ? 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 Ni1 N1 180.00(13) 3 . ? N1 Ni1 N9A 86.02(9) 3 3_655 ? N1 Ni1 N9A 93.98(9) . 3_655 ? N1 Ni1 N9A 93.98(9) 3 1_455 ? N1 Ni1 N9A 86.02(9) . 1_455 ? N9A Ni1 N9A 180.00(10) 3_655 1_455 ? N1 Ni1 N7A 93.37(9) 3 3 ? N1 Ni1 N7A 86.63(9) . 3 ? N9A Ni1 N7A 91.21(9) 3_655 3 ? N9A Ni1 N7A 88.79(9) 1_455 3 ? N1 Ni1 N7A 86.63(9) 3 . ? N1 Ni1 N7A 93.37(9) . . ? N9A Ni1 N7A 88.79(9) 3_655 . ? N9A Ni1 N7A 91.21(9) 1_455 . ? N7A Ni1 N7A 180.00(15) 3 . ? C8A N9A Ni1 166.7(2) . 1_655 ? C1 N1 Ni1 157.7(2) . . ? C1A N7A Ni1 120.65(17) . . ? C4A C3A C2A 121.1(2) . . ? C4A C3A C8A 120.7(2) . . ? C2A C3A C8A 118.2(2) . . ? C1A C2A C3A 119.8(2) . . ? C2A C1A C6A 119.4(2) . . ? C2A C1A N7A 119.8(2) . . ? C6A C1A N7A 120.7(2) . . ? C3G C2G C1G 119.8(3) . . ? N1 C1 S1 179.4(3) . . ? C2G C3G C1G 120.3(3) . 3_665 ? N9A C8A C3A 176.5(3) . . ? C5A C6A C1A 120.2(2) . . ? C5A C4A C3A 118.4(3) . . ? C3G C1G C2G 119.9(3) 3_665 . ? C4A C5A C6A 121.1(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.383 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.070 #===END