Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Kilkenny, Mairi' 'Nassimbeni, Luigi R.' _publ_contact_author_name 'Prof Luigi R Nassimbeni' _publ_contact_author_address ; Department of Chemistry University of Cape Town Rondebosch 7701 SOUTH AFRICA ; _publ_contact_author_email 'XRAYLUIG@SCIENCE.UCT.AC.ZA' _publ_section_title ; Tetrakis(3-cyanopyridine)diisothiocyanatonickel(II) and its clathrates with EtOH and CH2Cl2: Structures, thermal stabilities and enthalpies of guest release ; #CRYSTALLOGRAPHIC DATA FOR HOST COMPOUND 1 data_c:\mairi\mk17-3\NiHost1: #COMPOUND 1 _database_code_CSD 168905 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H16 N10 Ni S2' _chemical_formula_weight 591.32 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' _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+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 20.439(4) _cell_length_b 10.413(2) _cell_length_c 12.946(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2755.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6794 _exptl_absorpt_correction_T_max 0.7575 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7207 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6333 _reflns_number_gt 4580 _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^)+(0.0449P)^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 SHELXL _refine_ls_extinction_coef 0.0057(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(11) _refine_ls_number_reflns 6333 _refine_ls_number_parameters 353 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0890 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 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 0.882966(15) 0.57172(3) 0.58658(3) 0.03963(10) Uani 1 1 d . . . N1 N 0.88973(13) 0.5762(2) 0.7415(2) 0.0487(7) Uani 1 1 d . . . N3 N 0.83001(10) 0.7495(2) 0.5893(2) 0.0454(5) Uani 1 1 d . . . N5 N 0.92711(10) 0.3800(2) 0.5847(2) 0.0454(5) Uani 1 1 d . . . N4 N 0.97404(10) 0.6772(2) 0.57344(18) 0.0409(5) Uani 1 1 d . . . N6 N 0.78980(11) 0.4740(2) 0.5955(2) 0.0498(6) Uani 1 1 d . . . S1 S 0.89706(5) 0.55431(10) 0.95528(6) 0.0584(2) Uani 1 1 d . . . S2 S 0.90210(7) 0.60414(10) 0.22239(7) 0.0730(3) Uani 1 1 d . . . C2 C 0.88710(15) 0.5828(3) 0.3440(3) 0.0392(8) Uani 1 1 d . . . C1 C 0.89299(16) 0.5675(3) 0.8312(3) 0.0414(8) Uani 1 1 d . . . C15 C 0.95348(14) 0.3311(3) 0.4994(2) 0.0467(7) Uani 1 1 d . . . H9 H 0.9573 0.3836 0.4416 0.056 Uiso 1 1 calc R . . C19 C 0.92317(18) 0.3028(3) 0.6668(3) 0.0582(8) Uani 1 1 d . . . H12 H 0.9053 0.3358 0.7273 0.070 Uiso 1 1 calc R . . C16 C 0.97540(15) 0.2058(3) 0.4929(3) 0.0512(8) Uani 1 1 d . . . C17 C 0.97036(16) 0.1268(3) 0.5793(3) 0.0628(8) Uani 1 1 d . . . H10 H 0.9846 0.0420 0.5772 0.075 Uiso 1 1 calc R . . C23 C 0.66890(17) 0.3540(4) 0.5971(4) 0.0731(10) Uani 1 1 d . . . H14 H 0.6281 0.3143 0.5976 0.088 Uiso 1 1 calc R . . C5 C 0.75151(16) 0.9661(3) 0.5961(3) 0.0667(9) Uani 1 1 d . . . H2 H 0.7252 1.0389 0.5982 0.080 Uiso 1 1 calc R . . C9 C 1.02088(14) 0.6697(3) 0.6453(2) 0.0439(6) Uani 1 1 d . . . H5 H 1.0135 0.6187 0.7031 0.053 Uiso 1 1 calc R . . C21 C 0.74975(14) 0.4864(3) 0.6757(3) 0.0546(7) Uani 1 1 d . . . H13 H 0.7629 0.5369 0.7312 0.066 Uiso 1 1 calc R . . C4 C 0.79736(16) 0.9433(3) 0.6723(3) 0.0536(7) Uani 1 1 d . . . C25 C 0.76947(18) 0.4012(3) 0.5167(3) 0.0615(9) Uani 1 1 d . . . H16 H 0.7973 0.3908 0.4604 0.074 Uiso 1 1 calc R . . C13 C 0.98636(16) 0.7530(3) 0.4915(2) 0.0509(7) Uani 1 1 d . . . H8 H 0.9540 0.7618 0.4416 0.061 Uiso 1 1 calc R . . C10 C 1.07961(15) 0.7344(3) 0.6376(2) 0.0461(7) Uani 1 1 d . . . C7 C 0.78525(15) 0.7735(3) 0.5159(2) 0.0542(7) Uani 1 1 d . . . H4 H 0.7810 0.7156 0.4617 0.065 Uiso 1 1 calc R . . C20 C 1.00506(18) 0.1591(3) 0.3995(3) 0.0606(9) Uani 1 1 d . . . C3 C 0.83558(14) 0.8349(3) 0.6661(2) 0.0492(7) Uani 1 1 d . . . H1 H 0.8666 0.8203 0.7173 0.059 Uiso 1 1 calc R . . C12 C 1.04384(17) 0.8177(3) 0.4777(2) 0.0569(8) Uani 1 1 d . . . H7 H 1.0505 0.8676 0.4190 0.068 Uiso 1 1 calc R . . C11 C 1.09173(17) 0.8080(3) 0.5518(2) 0.0534(8) Uani 1 1 d . . . H6 H 1.1315 0.8503 0.5439 0.064 Uiso 1 1 calc R . . C24 C 0.7098(2) 0.3411(4) 0.5145(3) 0.0756(11) Uani 1 1 d . . . H15 H 0.6975 0.2923 0.4576 0.091 Uiso 1 1 calc R . . C14 C 1.12773(16) 0.7252(3) 0.7194(3) 0.0557(8) Uani 1 1 d . . . N8 N 1.16630(16) 0.7242(3) 0.7829(3) 0.0782(9) Uani 1 1 d . . . C22 C 0.68931(17) 0.4273(3) 0.6800(3) 0.0621(9) Uani 1 1 d . . . N9 N 1.02922(18) 0.1208(3) 0.3269(3) 0.0827(10) Uani 1 1 d . . . C8 C 0.80410(18) 1.0292(4) 0.7586(3) 0.0676(9) Uani 1 1 d . . . C26 C 0.6489(2) 0.4418(4) 0.7713(4) 0.0777(11) Uani 1 1 d . . . N7 N 0.8096(2) 1.0959(4) 0.8280(3) 0.0956(12) Uani 1 1 d . . . C6 C 0.74572(17) 0.8790(4) 0.5174(3) 0.0686(10) Uani 1 1 d . . . H3 H 0.7151 0.8917 0.4653 0.082 Uiso 1 1 calc R . . C18 C 0.94393(19) 0.1774(3) 0.6671(3) 0.0661(9) Uani 1 1 d . . . H11 H 0.9400 0.1276 0.7264 0.079 Uiso 1 1 calc R . . N2 N 0.87750(13) 0.5683(2) 0.4301(2) 0.0486(7) Uani 1 1 d . . . N10 N 0.6183(2) 0.4518(4) 0.8447(4) 0.1094(16) 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 Ni1 0.04283(16) 0.04727(18) 0.02879(14) -0.00180(17) 0.00034(19) 0.00162(17) N1 0.0572(17) 0.0570(18) 0.0318(16) -0.0012(10) 0.0008(11) 0.0021(12) N3 0.0417(10) 0.0546(13) 0.0399(10) -0.0037(14) -0.0019(13) 0.0039(10) N5 0.0481(11) 0.0473(12) 0.0409(10) 0.0009(14) 0.0031(13) 0.0002(10) N4 0.0437(11) 0.0424(12) 0.0366(12) 0.0000(11) -0.0008(10) 0.0036(9) N6 0.0473(12) 0.0563(13) 0.0457(14) 0.0027(13) 0.0025(13) -0.0021(10) S1 0.0616(5) 0.0817(6) 0.0320(4) 0.0055(4) 0.0010(4) -0.0132(4) S2 0.1232(9) 0.0605(5) 0.0354(5) 0.0042(4) 0.0132(5) 0.0094(6) C2 0.0470(19) 0.0397(17) 0.0308(19) -0.0043(11) -0.0036(13) 0.0044(12) C1 0.0367(16) 0.0412(18) 0.046(2) -0.0023(13) 0.0019(13) -0.0014(13) C15 0.0443(15) 0.0508(16) 0.0449(15) 0.0086(13) 0.0065(13) -0.0014(14) C19 0.077(2) 0.0533(19) 0.0444(16) 0.0041(15) 0.0103(17) 0.0006(17) C16 0.0470(17) 0.0450(17) 0.0616(19) -0.0002(14) 0.0123(14) -0.0009(13) C17 0.074(2) 0.0440(15) 0.070(2) 0.0079(19) 0.017(2) 0.0020(15) C23 0.0641(19) 0.072(2) 0.083(3) 0.027(2) -0.008(2) -0.0223(18) C5 0.0604(18) 0.068(2) 0.072(2) -0.001(2) 0.008(2) 0.0239(15) C9 0.0498(16) 0.0439(15) 0.0381(15) 0.0030(12) -0.0014(12) 0.0023(13) C21 0.0487(17) 0.0566(19) 0.0586(19) 0.0054(17) 0.0044(15) 0.0008(16) C4 0.0482(17) 0.0574(18) 0.0552(17) -0.0066(16) 0.0081(14) 0.0022(15) C25 0.068(2) 0.065(2) 0.0515(18) -0.0030(17) 0.0041(16) -0.0169(17) C13 0.0633(18) 0.0472(16) 0.0421(15) 0.0050(13) -0.0084(13) 0.0002(15) C10 0.0488(17) 0.0415(15) 0.0479(16) -0.0009(13) -0.0035(13) 0.0016(13) C7 0.0497(16) 0.068(2) 0.0452(15) -0.0072(15) -0.0074(13) 0.0094(15) C20 0.068(2) 0.0467(18) 0.067(2) 0.0074(16) 0.0209(17) 0.0044(17) C3 0.0434(15) 0.0574(17) 0.0468(15) -0.0076(15) -0.0022(13) 0.0017(14) C12 0.077(2) 0.0470(17) 0.0469(17) 0.0103(14) -0.0031(15) -0.0076(16) C11 0.0579(18) 0.0462(17) 0.0562(18) 0.0009(14) 0.0033(14) -0.0090(15) C24 0.086(3) 0.072(2) 0.068(2) 0.004(2) -0.012(2) -0.030(2) C14 0.057(2) 0.0490(18) 0.0608(19) 0.0060(16) -0.0042(16) -0.0059(15) N8 0.076(2) 0.079(2) 0.079(2) 0.0009(18) -0.0333(18) -0.0067(17) C22 0.0521(18) 0.060(2) 0.074(2) 0.0210(19) 0.0097(17) -0.0003(17) N9 0.104(3) 0.0620(19) 0.082(2) 0.0024(17) 0.040(2) 0.0148(19) C8 0.061(2) 0.068(2) 0.074(2) -0.016(2) 0.0085(18) 0.0069(17) C26 0.066(2) 0.065(2) 0.102(3) 0.018(2) 0.025(2) -0.0039(19) N7 0.100(3) 0.097(3) 0.090(3) -0.044(2) 0.015(2) -0.003(2) C6 0.062(2) 0.082(2) 0.062(2) -0.008(2) -0.0175(17) 0.0273(19) C18 0.095(3) 0.053(2) 0.0506(18) 0.0122(16) 0.0071(19) -0.0018(19) N2 0.0561(17) 0.0540(17) 0.0357(17) -0.0056(11) -0.0025(11) 0.0010(12) N10 0.093(3) 0.098(3) 0.137(4) 0.016(3) 0.061(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic)treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.011(3) . ? Ni1 N2 2.030(3) . ? Ni1 N3 2.145(2) . ? Ni1 N6 2.162(2) . ? Ni1 N4 2.168(2) . ? Ni1 N5 2.191(2) . ? N1 C1 1.167(5) . ? N3 C3 1.339(4) . ? N3 C7 1.342(4) . ? N5 C15 1.330(4) . ? N5 C19 1.335(4) . ? N4 C9 1.337(3) . ? N4 C13 1.346(4) . ? N6 C21 1.328(4) . ? N6 C25 1.338(4) . ? S1 C1 1.615(4) . ? S2 C2 1.619(3) . ? C2 N2 1.142(5) . ? C15 C16 1.382(4) . ? C19 C18 1.372(5) . ? C16 C17 1.393(5) . ? C16 C20 1.437(5) . ? C17 C18 1.365(5) . ? C23 C24 1.364(6) . ? C23 C22 1.382(6) . ? C5 C6 1.369(5) . ? C5 C4 1.381(5) . ? C9 C10 1.380(4) . ? C21 C22 1.381(4) . ? C4 C3 1.375(4) . ? C4 C8 1.438(5) . ? C25 C24 1.370(5) . ? C13 C12 1.366(5) . ? C10 C11 1.372(4) . ? C10 C14 1.449(4) . ? C7 C6 1.364(4) . ? C20 N9 1.135(4) . ? C12 C11 1.374(4) . ? C14 N8 1.139(4) . ? C22 C26 1.449(6) . ? C8 N7 1.141(5) . ? C26 N10 1.143(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 N1 Ni1 N2 179.15(11) . . ? N1 Ni1 N3 89.93(11) . . ? N2 Ni1 N3 90.20(10) . . ? N1 Ni1 N6 91.02(11) . . ? N2 Ni1 N6 89.82(11) . . ? N3 Ni1 N6 87.75(9) . . ? N1 Ni1 N4 90.43(10) . . ? N2 Ni1 N4 88.73(10) . . ? N3 Ni1 N4 89.84(8) . . ? N6 Ni1 N4 177.18(9) . . ? N1 Ni1 N5 90.21(11) . . ? N2 Ni1 N5 89.75(11) . . ? N3 Ni1 N5 174.00(8) . . ? N6 Ni1 N5 86.26(9) . . ? N4 Ni1 N5 96.16(8) . . ? C1 N1 Ni1 174.2(3) . . ? C3 N3 C7 117.4(2) . . ? C3 N3 Ni1 122.8(2) . . ? C7 N3 Ni1 119.6(2) . . ? C15 N5 C19 117.0(2) . . ? C15 N5 Ni1 121.7(2) . . ? C19 N5 Ni1 121.0(2) . . ? C9 N4 C13 116.6(2) . . ? C9 N4 Ni1 122.04(19) . . ? C13 N4 Ni1 121.31(19) . . ? C21 N6 C25 117.4(3) . . ? C21 N6 Ni1 122.6(2) . . ? C25 N6 Ni1 120.0(2) . . ? N2 C2 S2 178.9(3) . . ? N1 C1 S1 179.4(3) . . ? N5 C15 C16 122.9(3) . . ? N5 C19 C18 123.8(3) . . ? C15 C16 C17 119.0(3) . . ? C15 C16 C20 120.5(3) . . ? C17 C16 C20 120.4(3) . . ? C18 C17 C16 118.0(3) . . ? C24 C23 C22 118.6(3) . . ? C6 C5 C4 118.4(3) . . ? N4 C9 C10 123.0(3) . . ? N6 C21 C22 122.6(3) . . ? C3 C4 C5 119.0(3) . . ? C3 C4 C8 120.1(3) . . ? C5 C4 C8 120.9(3) . . ? N6 C25 C24 123.4(3) . . ? N4 C13 C12 123.6(3) . . ? C11 C10 C9 119.2(3) . . ? C11 C10 C14 120.4(3) . . ? C9 C10 C14 120.4(3) . . ? N3 C7 C6 123.0(3) . . ? N9 C20 C16 178.7(4) . . ? N3 C3 C4 122.7(3) . . ? C13 C12 C11 119.0(3) . . ? C10 C11 C12 118.5(3) . . ? C23 C24 C25 119.0(4) . . ? N8 C14 C10 176.6(4) . . ? C21 C22 C23 119.0(3) . . ? C21 C22 C26 119.8(4) . . ? C23 C22 C26 121.2(3) . . ? N7 C8 C4 179.1(5) . . ? N10 C26 C22 178.2(5) . . ? C7 C6 C5 119.5(3) . . ? C17 C18 C19 119.2(3) . . ? C2 N2 Ni1 164.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 N1 C1 -118(7) . . . . ? N3 Ni1 N1 C1 143(3) . . . . ? N6 Ni1 N1 C1 55(3) . . . . ? N4 Ni1 N1 C1 -127(3) . . . . ? N5 Ni1 N1 C1 -31(3) . . . . ? N1 Ni1 N3 C3 25.0(2) . . . . ? N2 Ni1 N3 C3 -154.1(2) . . . . ? N6 Ni1 N3 C3 116.1(2) . . . . ? N4 Ni1 N3 C3 -65.4(2) . . . . ? N5 Ni1 N3 C3 116.3(11) . . . . ? N1 Ni1 N3 C7 -149.4(2) . . . . ? N2 Ni1 N3 C7 31.4(2) . . . . ? N6 Ni1 N3 C7 -58.4(2) . . . . ? N4 Ni1 N3 C7 120.2(2) . . . . ? N5 Ni1 N3 C7 -58.1(12) . . . . ? N1 Ni1 N5 C15 -161.5(2) . . . . ? N2 Ni1 N5 C15 17.7(2) . . . . ? N3 Ni1 N5 C15 107.2(11) . . . . ? N6 Ni1 N5 C15 107.5(2) . . . . ? N4 Ni1 N5 C15 -71.0(2) . . . . ? N1 Ni1 N5 C19 24.9(3) . . . . ? N2 Ni1 N5 C19 -156.0(2) . . . . ? N3 Ni1 N5 C19 -66.4(12) . . . . ? N6 Ni1 N5 C19 -66.2(2) . . . . ? N4 Ni1 N5 C19 115.3(2) . . . . ? N1 Ni1 N4 C9 28.4(2) . . . . ? N2 Ni1 N4 C9 -151.5(2) . . . . ? N3 Ni1 N4 C9 118.3(2) . . . . ? N6 Ni1 N4 C9 149(2) . . . . ? N5 Ni1 N4 C9 -61.9(2) . . . . ? N1 Ni1 N4 C13 -152.2(2) . . . . ? N2 Ni1 N4 C13 27.9(2) . . . . ? N3 Ni1 N4 C13 -62.3(2) . . . . ? N6 Ni1 N4 C13 -31(2) . . . . ? N5 Ni1 N4 C13 117.5(2) . . . . ? N1 Ni1 N6 C21 27.2(2) . . . . ? N2 Ni1 N6 C21 -152.9(3) . . . . ? N3 Ni1 N6 C21 -62.7(2) . . . . ? N4 Ni1 N6 C21 -94(2) . . . . ? N5 Ni1 N6 C21 117.3(3) . . . . ? N1 Ni1 N6 C25 -155.2(3) . . . . ? N2 Ni1 N6 C25 24.7(3) . . . . ? N3 Ni1 N6 C25 114.9(3) . . . . ? N4 Ni1 N6 C25 84(2) . . . . ? N5 Ni1 N6 C25 -65.1(3) . . . . ? Ni1 N1 C1 S1 -28(43) . . . . ? C19 N5 C15 C16 1.0(4) . . . . ? Ni1 N5 C15 C16 -173.0(2) . . . . ? C15 N5 C19 C18 -0.7(5) . . . . ? Ni1 N5 C19 C18 173.2(3) . . . . ? N5 C15 C16 C17 -0.5(5) . . . . ? N5 C15 C16 C20 -178.4(3) . . . . ? C15 C16 C17 C18 -0.2(5) . . . . ? C20 C16 C17 C18 177.7(3) . . . . ? C13 N4 C9 C10 -0.6(4) . . . . ? Ni1 N4 C9 C10 178.9(2) . . . . ? C25 N6 C21 C22 0.2(5) . . . . ? Ni1 N6 C21 C22 177.9(2) . . . . ? C6 C5 C4 C3 0.4(5) . . . . ? C6 C5 C4 C8 -177.9(4) . . . . ? C21 N6 C25 C24 0.8(5) . . . . ? Ni1 N6 C25 C24 -176.9(3) . . . . ? C9 N4 C13 C12 1.9(4) . . . . ? Ni1 N4 C13 C12 -177.5(2) . . . . ? N4 C9 C10 C11 -1.4(5) . . . . ? N4 C9 C10 C14 178.3(3) . . . . ? C3 N3 C7 C6 -0.6(5) . . . . ? Ni1 N3 C7 C6 174.2(3) . . . . ? C15 C16 C20 N9 148(20) . . . . ? C17 C16 C20 N9 -30(20) . . . . ? C7 N3 C3 C4 0.5(4) . . . . ? Ni1 N3 C3 C4 -174.1(2) . . . . ? C5 C4 C3 N3 -0.4(5) . . . . ? C8 C4 C3 N3 177.8(3) . . . . ? N4 C13 C12 C11 -1.3(5) . . . . ? C9 C10 C11 C12 2.0(5) . . . . ? C14 C10 C11 C12 -177.7(3) . . . . ? C13 C12 C11 C10 -0.7(5) . . . . ? C22 C23 C24 C25 0.0(6) . . . . ? N6 C25 C24 C23 -0.9(6) . . . . ? C11 C10 C14 N8 36(7) . . . . ? C9 C10 C14 N8 -143(7) . . . . ? N6 C21 C22 C23 -1.1(5) . . . . ? N6 C21 C22 C26 178.1(3) . . . . ? C24 C23 C22 C21 1.0(6) . . . . ? C24 C23 C22 C26 -178.2(4) . . . . ? C3 C4 C8 N7 -33(27) . . . . ? C5 C4 C8 N7 145(26) . . . . ? C21 C22 C26 N10 -57(16) . . . . ? C23 C22 C26 N10 122(16) . . . . ? N3 C7 C6 C5 0.5(6) . . . . ? C4 C5 C6 C7 -0.4(6) . . . . ? C16 C17 C18 C19 0.4(6) . . . . ? N5 C19 C18 C17 0.1(6) . . . . ? S2 C2 N2 Ni1 16(17) . . . . ? N1 Ni1 N2 C2 -12(7) . . . . ? N3 Ni1 N2 C2 86.8(9) . . . . ? N6 Ni1 N2 C2 174.6(9) . . . . ? N4 Ni1 N2 C2 -3.0(9) . . . . ? N5 Ni1 N2 C2 -99.2(9) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.349 _refine_diff_density_min -0.339 _refine_diff_density_rms 0.050 #===END #CRYSTALLOGRAPHIC DATA FOR CLATHRATE 2 data_c:\ethc2c\NidiEt: #COMPOUND 2 _database_code_CSD 168906 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 N10 Ni O2 S2' _chemical_formula_weight 683.45 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' 'Ni' 'Ni' 0.3393 1.1124 '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 17.737(4) _cell_length_b 11.527(2) _cell_length_c 17.120(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.65(3) _cell_angle_gamma 90.00 _cell_volume 3476.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8676 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3921 _reflns_number_gt 2476 _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^)+(0.0681P)^2^+7.1246P] 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 3921 _refine_ls_number_parameters 193 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.0573 _refine_ls_wR_factor_ref 0.1639 _refine_ls_wR_factor_gt 0.1450 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.507 _refine_ls_shift/su_mean 0.015 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 0.5000 0.25851(5) 0.2500 0.0185(2) Uani 1 2 d S . . S1 S 0.70182(6) 0.24167(9) 0.08414(6) 0.0338(3) Uani 1 1 d . . . N1 N 0.58048(17) 0.2591(2) 0.17439(16) 0.0231(7) Uani 1 1 d . . . C1 C 0.6303(2) 0.2526(3) 0.13650(19) 0.0206(7) Uani 1 1 d . . . N3 N 0.43725(16) 0.1276(2) 0.18228(16) 0.0227(7) Uani 1 1 d . . . N2 N 0.44013(16) 0.3880(2) 0.18016(15) 0.0213(7) Uani 1 1 d . . . C4 C 0.3712(2) 0.5652(3) 0.0863(2) 0.0368(10) Uani 1 1 d . . . H10 H 0.3485 0.6244 0.0550 0.044 Uiso 1 1 calc R . . C10 C 0.3554(3) -0.0423(4) 0.0935(2) 0.0423(11) Uani 1 1 d . . . H2 H 0.3282 -0.0990 0.0636 0.051 Uiso 1 1 calc R . . C2 C 0.43678(19) 0.3840(3) 0.10169(19) 0.0224(8) Uani 1 1 d . . . H3 H 0.4582 0.3208 0.0786 0.027 Uiso 1 1 calc R . . C3 C 0.4028(2) 0.4701(3) 0.0536(2) 0.0254(8) Uani 1 1 d . . . C7 C 0.4000(2) 0.4581(3) -0.0306(2) 0.0319(9) Uani 1 1 d . . . C8 C 0.4724(2) 0.0459(3) 0.14449(19) 0.0252(8) Uani 1 1 d . . . H6 H 0.5252 0.0463 0.1486 0.030 Uiso 1 1 calc R . . C9 C 0.4333(2) -0.0391(3) 0.0996(2) 0.0304(9) Uani 1 1 d . . . C6 C 0.4083(2) 0.4804(3) 0.2116(2) 0.0295(9) Uani 1 1 d . . . H8 H 0.4092 0.4839 0.2660 0.035 Uiso 1 1 calc R . . C12 C 0.3611(2) 0.1239(4) 0.1757(2) 0.0341(9) Uani 1 1 d . . . H9 H 0.3359 0.1804 0.2014 0.041 Uiso 1 1 calc R . . C5 C 0.3746(3) 0.5694(3) 0.1677(2) 0.0392(11) Uani 1 1 d . . . H12 H 0.3541 0.6321 0.1922 0.047 Uiso 1 1 calc R . . C13 C 0.4749(3) -0.1235(4) 0.0582(2) 0.0389(10) Uani 1 1 d . . . C11 C 0.3184(3) 0.0411(4) 0.1330(3) 0.0482(12) Uani 1 1 d . . . H15 H 0.2657 0.0412 0.1307 0.058 Uiso 1 1 calc R . . N4 N 0.3970(2) 0.4465(3) -0.0970(2) 0.0490(10) Uani 1 1 d . . . N5 N 0.5068(2) -0.1882(4) 0.0251(2) 0.0578(11) Uani 1 1 d . . . O1A O 0.2013(5) 0.3606(10) 0.0932(6) 0.169(5) Uiso 0.633(10) 1 d PD . . C14 C 0.1903(4) 0.3766(3) 0.1739(6) 0.208(4) Uiso 1 1 d D . . C15 C 0.1883(9) 0.2515(6) 0.2034(8) 0.208(4) Uiso 1 1 d D . . O1B O 0.1535(5) 0.4817(6) 0.1463(6) 0.073(4) Uiso 0.367(10) 1 d PD . . 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 0.0190(4) 0.0217(4) 0.0151(3) 0.000 0.0036(2) 0.000 S1 0.0245(5) 0.0469(7) 0.0325(5) 0.0023(4) 0.0133(4) 0.0042(5) N1 0.0228(16) 0.0265(17) 0.0200(14) 0.0014(12) 0.0027(12) 0.0011(13) C1 0.0245(19) 0.0178(18) 0.0190(16) 0.0007(13) -0.0001(14) -0.0015(15) N3 0.0232(17) 0.0246(16) 0.0204(15) -0.0005(12) 0.0022(12) 0.0011(13) N2 0.0243(17) 0.0231(15) 0.0165(14) -0.0019(11) 0.0028(12) 0.0022(13) C4 0.041(3) 0.037(2) 0.032(2) 0.0097(18) 0.0009(19) 0.013(2) C10 0.043(3) 0.043(3) 0.041(2) -0.018(2) 0.004(2) -0.018(2) C2 0.021(2) 0.0272(19) 0.0189(17) -0.0019(14) 0.0030(14) -0.0007(15) C3 0.023(2) 0.033(2) 0.0206(17) 0.0039(15) 0.0044(15) 0.0014(16) C7 0.033(2) 0.036(2) 0.026(2) 0.0079(17) 0.0034(17) 0.0024(18) C8 0.026(2) 0.028(2) 0.0219(17) -0.0009(15) 0.0039(15) 0.0029(16) C9 0.037(3) 0.027(2) 0.0279(19) -0.0047(16) 0.0065(17) -0.0049(18) C6 0.031(2) 0.034(2) 0.0230(18) -0.0036(16) 0.0032(16) 0.0078(17) C12 0.029(2) 0.041(2) 0.032(2) -0.0091(17) 0.0026(17) 0.0032(19) C5 0.052(3) 0.033(2) 0.033(2) -0.0028(17) 0.007(2) 0.021(2) C13 0.050(3) 0.032(2) 0.035(2) -0.0092(18) 0.004(2) -0.005(2) C11 0.025(2) 0.065(3) 0.054(3) -0.024(2) 0.004(2) -0.010(2) N4 0.063(3) 0.057(2) 0.028(2) 0.0089(17) 0.0102(18) 0.011(2) N5 0.070(3) 0.052(3) 0.051(2) -0.025(2) 0.007(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.035(3) . ? Ni1 N1 2.035(3) 2_655 ? Ni1 N2 2.119(3) 2_655 ? Ni1 N2 2.119(3) . ? Ni1 N3 2.136(3) . ? Ni1 N3 2.136(3) 2_655 ? S1 C1 1.641(3) . ? N1 C1 1.158(5) . ? N3 C8 1.337(4) . ? N3 C12 1.342(5) . ? N2 C2 1.339(4) . ? N2 C6 1.347(4) . ? C4 C3 1.380(5) . ? C4 C5 1.390(5) . ? C10 C9 1.375(6) . ? C10 C11 1.383(6) . ? C2 C3 1.382(5) . ? C3 C7 1.442(5) . ? C7 N4 1.139(5) . ? C8 C9 1.381(5) . ? C9 C13 1.454(5) . ? C6 C5 1.367(5) . ? C12 C11 1.375(6) . ? C13 N5 1.129(5) . ? O1A C14 1.4300(3) . ? C14 O1B 1.4299(3) . ? C14 C15 1.5300(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 179.64(16) . 2_655 ? N1 Ni1 N2 90.80(11) . 2_655 ? N1 Ni1 N2 88.94(11) 2_655 2_655 ? N1 Ni1 N2 88.94(11) . . ? N1 Ni1 N2 90.80(11) 2_655 . ? N2 Ni1 N2 90.45(15) 2_655 . ? N1 Ni1 N3 90.96(11) . . ? N1 Ni1 N3 89.29(11) 2_655 . ? N2 Ni1 N3 178.22(10) 2_655 . ? N2 Ni1 N3 89.76(11) . . ? N1 Ni1 N3 89.29(11) . 2_655 ? N1 Ni1 N3 90.96(11) 2_655 2_655 ? N2 Ni1 N3 89.76(11) 2_655 2_655 ? N2 Ni1 N3 178.22(10) . 2_655 ? N3 Ni1 N3 90.09(16) . 2_655 ? C1 N1 Ni1 173.5(3) . . ? N1 C1 S1 178.8(3) . . ? C8 N3 C12 117.2(3) . . ? C8 N3 Ni1 121.2(2) . . ? C12 N3 Ni1 121.6(2) . . ? C2 N2 C6 117.2(3) . . ? C2 N2 Ni1 120.2(2) . . ? C6 N2 Ni1 122.5(2) . . ? C3 C4 C5 117.5(3) . . ? C9 C10 C11 118.3(4) . . ? N2 C2 C3 122.6(3) . . ? C4 C3 C2 119.9(3) . . ? C4 C3 C7 120.8(3) . . ? C2 C3 C7 119.3(3) . . ? N4 C7 C3 178.5(5) . . ? N3 C8 C9 122.4(4) . . ? C10 C9 C8 119.8(3) . . ? C10 C9 C13 120.5(4) . . ? C8 C9 C13 119.7(4) . . ? N2 C6 C5 123.4(3) . . ? N3 C12 C11 123.7(4) . . ? C6 C5 C4 119.4(3) . . ? N5 C13 C9 179.0(5) . . ? C12 C11 C10 118.5(4) . . ? O1A C14 O1B 84.1(8) . . ? O1A C14 C15 102.0(8) . . ? O1B C14 C15 151.7(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N1 C1 126(2) 2_655 . . . ? N2 Ni1 N1 C1 81(2) 2_655 . . . ? N2 Ni1 N1 C1 171(2) . . . . ? N3 Ni1 N1 C1 -99(2) . . . . ? N3 Ni1 N1 C1 -9(2) 2_655 . . . ? Ni1 N1 C1 S1 2(19) . . . . ? N1 Ni1 N3 C8 33.3(3) . . . . ? N1 Ni1 N3 C8 -146.9(3) 2_655 . . . ? N2 Ni1 N3 C8 -141(3) 2_655 . . . ? N2 Ni1 N3 C8 122.3(3) . . . . ? N3 Ni1 N3 C8 -56.0(2) 2_655 . . . ? N1 Ni1 N3 C12 -146.6(3) . . . . ? N1 Ni1 N3 C12 33.2(3) 2_655 . . . ? N2 Ni1 N3 C12 39(4) 2_655 . . . ? N2 Ni1 N3 C12 -57.6(3) . . . . ? N3 Ni1 N3 C12 124.1(3) 2_655 . . . ? N1 Ni1 N2 C2 38.5(3) . . . . ? N1 Ni1 N2 C2 -141.7(3) 2_655 . . . ? N2 Ni1 N2 C2 129.3(3) 2_655 . . . ? N3 Ni1 N2 C2 -52.4(3) . . . . ? N3 Ni1 N2 C2 33(4) 2_655 . . . ? N1 Ni1 N2 C6 -137.3(3) . . . . ? N1 Ni1 N2 C6 42.5(3) 2_655 . . . ? N2 Ni1 N2 C6 -46.5(2) 2_655 . . . ? N3 Ni1 N2 C6 131.8(3) . . . . ? N3 Ni1 N2 C6 -143(3) 2_655 . . . ? C6 N2 C2 C3 0.3(5) . . . . ? Ni1 N2 C2 C3 -175.7(3) . . . . ? C5 C4 C3 C2 -0.6(6) . . . . ? C5 C4 C3 C7 178.6(4) . . . . ? N2 C2 C3 C4 0.5(6) . . . . ? N2 C2 C3 C7 -178.6(3) . . . . ? C4 C3 C7 N4 -120(19) . . . . ? C2 C3 C7 N4 59(19) . . . . ? C12 N3 C8 C9 0.6(5) . . . . ? Ni1 N3 C8 C9 -179.3(3) . . . . ? C11 C10 C9 C8 0.1(6) . . . . ? C11 C10 C9 C13 -178.9(4) . . . . ? N3 C8 C9 C10 -0.8(5) . . . . ? N3 C8 C9 C13 178.2(3) . . . . ? C2 N2 C6 C5 -1.2(6) . . . . ? Ni1 N2 C6 C5 174.7(3) . . . . ? C8 N3 C12 C11 0.3(6) . . . . ? Ni1 N3 C12 C11 -179.8(3) . . . . ? N2 C6 C5 C4 1.2(7) . . . . ? C3 C4 C5 C6 -0.2(6) . . . . ? C10 C9 C13 N5 75(30) . . . . ? C8 C9 C13 N5 -104(29) . . . . ? N3 C12 C11 C10 -1.0(7) . . . . ? C9 C10 C11 C12 0.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.177 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.086 #===END #CRYSTALLOGRAPHIC DATA FOR CLATHRATE 3 data_c:\dcmc2c\NidiEt #COMPOUND 3 _database_code_CSD 168907 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H20 Cl4 N10 Ni S2' _chemical_formula_weight 761.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 17.8126(7) _cell_length_b 11.5532(4) _cell_length_c 17.1122(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.668(2) _cell_angle_gamma 90.00 _cell_volume 3490.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.017 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6867 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.00 _reflns_number_total 3598 _reflns_number_gt 2789 _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^)+(0.0765P)^2^+12.2913P] 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 3598 _refine_ls_number_parameters 233 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1453 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 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 0.5000 0.25691(4) 0.2500 0.01908(18) Uani 1 2 d S . . S1 S 0.70124(5) 0.23820(9) 0.08746(6) 0.0408(3) Uani 1 1 d . . . N1 N 0.57960(16) 0.2562(2) 0.17472(15) 0.0233(6) Uani 1 1 d . . . N2 N 0.43974(15) 0.3854(2) 0.17924(14) 0.0233(6) Uani 1 1 d . . . N3 N 0.43624(15) 0.1256(2) 0.18165(15) 0.0238(6) Uani 1 1 d . . . C1 C 0.62971(18) 0.2497(3) 0.13813(18) 0.0234(7) Uani 1 1 d . . . C4 C 0.3691(2) 0.5613(4) 0.0847(2) 0.0432(10) Uani 1 1 d . . . H2 H 0.3459 0.6202 0.0532 0.052 Uiso 1 1 calc R . . C2 C 0.43680(17) 0.3819(3) 0.10076(17) 0.0244(7) Uani 1 1 d . . . H1 H 0.4592 0.3199 0.0780 0.029 Uiso 1 1 calc R . . C10 C 0.3531(2) -0.0435(4) 0.0925(2) 0.0452(10) Uani 1 1 d . . . H6 H 0.3254 -0.1004 0.0628 0.054 Uiso 1 1 calc R . . C3 C 0.40153(19) 0.4675(3) 0.05190(19) 0.0303(7) Uani 1 1 d . . . C7 C 0.3991(2) 0.4560(3) -0.0323(2) 0.0356(8) Uani 1 1 d . . . C9 C 0.4309(2) -0.0388(3) 0.0970(2) 0.0347(8) Uani 1 1 d . . . C6 C 0.4072(2) 0.4763(3) 0.21060(19) 0.0331(8) Uani 1 1 d . . . H4 H 0.4085 0.4794 0.2651 0.040 Uiso 1 1 calc R . . C8 C 0.47073(19) 0.0464(3) 0.14259(18) 0.0274(7) Uani 1 1 d . . . H5 H 0.5233 0.0481 0.1459 0.033 Uiso 1 1 calc R . . C12 C 0.3605(2) 0.1208(3) 0.1763(2) 0.0363(8) Uani 1 1 d . . . H8 H 0.3358 0.1758 0.2033 0.044 Uiso 1 1 calc R . . C13 C 0.4724(2) -0.1206(3) 0.0555(2) 0.0426(9) Uani 1 1 d . . . C5 C 0.3721(3) 0.5650(4) 0.1660(2) 0.0499(11) Uani 1 1 d . . . H3 H 0.3507 0.6266 0.1902 0.060 Uiso 1 1 calc R . . C11 C 0.3174(2) 0.0382(4) 0.1329(3) 0.0493(11) Uani 1 1 d . . . H7 H 0.2650 0.0377 0.1310 0.059 Uiso 1 1 calc R . . N4 N 0.3958(2) 0.4462(4) -0.09915(19) 0.0524(9) Uani 1 1 d . . . N5 N 0.5064(2) -0.1827(3) 0.0221(2) 0.0566(10) Uani 1 1 d . . . Cl2B Cl 0.23414(17) 0.3050(3) 0.0424(2) 0.0823(12) Uani 0.423(3) 1 d PD . 2 Cl1B Cl 0.2122(2) 0.3443(4) 0.2094(3) 0.0947(14) Uani 0.423(3) 1 d PD . 2 C14B C 0.1784(6) 0.3748(11) 0.1082(3) 0.134(10) Uani 0.423(3) 1 d PD . 2 H10B H 0.1794 0.4578 0.0998 0.161 Uiso 0.423(3) 1 calc PR . 2 H9B H 0.1262 0.3492 0.0965 0.161 Uiso 0.423(3) 1 calc PR . 2 Cl1A Cl 0.0827(2) 0.3159(5) 0.2306(3) 0.155(3) Uani 0.423(3) 1 d PD . 1 Cl2A Cl 0.1812(3) 0.4398(7) 0.1443(6) 0.172(3) Uani 0.423(3) 1 d PD . 1 C14A C 0.1679(6) 0.3008(10) 0.1866(10) 0.139(9) Uani 0.423(3) 1 d PD . 1 H10A H 0.2103 0.2813 0.2260 0.167 Uiso 0.423(3) 1 calc PR . 1 H9A H 0.1623 0.2412 0.1464 0.167 Uiso 0.423(3) 1 calc PR . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0197(3) 0.0212(3) 0.0164(3) 0.000 0.0030(2) 0.000 S1 0.0270(5) 0.0608(7) 0.0378(5) 0.0047(4) 0.0155(4) 0.0090(4) N1 0.0237(13) 0.0266(15) 0.0194(12) 0.0011(10) 0.0022(10) 0.0017(10) N2 0.0264(13) 0.0254(14) 0.0180(12) 0.0006(10) 0.0031(10) 0.0031(11) N3 0.0261(13) 0.0222(13) 0.0225(13) -0.0023(10) 0.0014(10) -0.0008(10) C1 0.0227(15) 0.0252(17) 0.0218(15) 0.0021(12) 0.0013(12) 0.0018(12) C4 0.049(2) 0.044(2) 0.0358(19) 0.0138(17) 0.0037(17) 0.0217(18) C2 0.0250(16) 0.0279(17) 0.0208(14) -0.0013(12) 0.0054(12) 0.0000(12) C10 0.043(2) 0.045(2) 0.047(2) -0.0178(18) 0.0020(17) -0.0153(18) C3 0.0270(17) 0.041(2) 0.0235(15) 0.0053(14) 0.0032(13) 0.0025(14) C7 0.0323(18) 0.046(2) 0.0284(18) 0.0112(15) 0.0038(14) 0.0038(16) C9 0.041(2) 0.0320(19) 0.0312(17) -0.0042(14) 0.0061(15) -0.0041(15) C6 0.0413(19) 0.0355(19) 0.0230(15) -0.0006(14) 0.0065(14) 0.0140(16) C8 0.0310(17) 0.0263(17) 0.0252(15) -0.0022(13) 0.0045(13) 0.0020(13) C12 0.0287(18) 0.041(2) 0.0388(19) -0.0098(16) 0.0030(15) 0.0006(15) C13 0.051(2) 0.038(2) 0.039(2) -0.0147(17) 0.0045(17) -0.0045(18) C5 0.067(3) 0.046(2) 0.039(2) 0.0038(18) 0.0145(19) 0.031(2) C11 0.0299(19) 0.061(3) 0.056(2) -0.021(2) 0.0014(17) -0.0112(19) N4 0.063(2) 0.068(3) 0.0258(16) 0.0100(16) 0.0059(15) 0.0078(19) N5 0.063(2) 0.056(2) 0.050(2) -0.0235(19) 0.0062(18) 0.0043(19) Cl2B 0.066(2) 0.087(3) 0.088(2) 0.036(2) -0.0098(17) -0.0267(18) Cl1B 0.062(2) 0.112(3) 0.110(3) -0.037(3) 0.011(2) 0.006(2) C14B 0.25(3) 0.049(9) 0.083(11) -0.020(8) -0.047(14) -0.059(12) Cl1A 0.220(7) 0.136(5) 0.092(3) -0.026(3) -0.034(4) 0.100(5) Cl2A 0.093(4) 0.160(6) 0.267(9) -0.059(7) 0.036(5) -0.047(4) C14A 0.083(13) 0.22(3) 0.103(15) -0.004(17) -0.042(12) 0.009(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes)are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 2.039(3) . ? Ni1 N1 2.039(3) 2_655 ? Ni1 N2 2.116(3) 2_655 ? Ni1 N2 2.116(3) . ? Ni1 N3 2.146(3) . ? Ni1 N3 2.146(3) 2_655 ? S1 C1 1.640(3) . ? N1 C1 1.159(4) . ? N2 C2 1.338(4) . ? N2 C6 1.345(4) . ? N3 C8 1.331(4) . ? N3 C12 1.341(4) . ? C4 C3 1.382(5) . ? C4 C5 1.386(5) . ? C2 C3 1.390(5) . ? C10 C11 1.374(6) . ? C10 C9 1.380(5) . ? C3 C7 1.442(5) . ? C7 N4 1.143(5) . ? C9 C8 1.390(5) . ? C9 C13 1.444(5) . ? C6 C5 1.376(5) . ? C12 C11 1.378(5) . ? C13 N5 1.140(5) . ? Cl2B C14B 1.78999(12) . ? Cl2B Cl2B 2.065(9) 7 ? Cl1B C14B 1.79000(13) . ? Cl1A C14A 1.79000(13) . ? Cl2A C14A 1.79000(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N1 179.55(14) . 2_655 ? N1 Ni1 N2 91.25(10) . 2_655 ? N1 Ni1 N2 89.06(10) 2_655 2_655 ? N1 Ni1 N2 89.06(10) . . ? N1 Ni1 N2 91.25(10) 2_655 . ? N2 Ni1 N2 90.86(14) 2_655 . ? N1 Ni1 N3 90.86(10) . . ? N1 Ni1 N3 88.83(10) 2_655 . ? N2 Ni1 N3 177.84(9) 2_655 . ? N2 Ni1 N3 89.60(11) . . ? N1 Ni1 N3 88.83(10) . 2_655 ? N1 Ni1 N3 90.86(10) 2_655 2_655 ? N2 Ni1 N3 89.60(11) 2_655 2_655 ? N2 Ni1 N3 177.84(9) . 2_655 ? N3 Ni1 N3 90.01(14) . 2_655 ? C1 N1 Ni1 172.8(2) . . ? C2 N2 C6 117.6(3) . . ? C2 N2 Ni1 120.1(2) . . ? C6 N2 Ni1 122.2(2) . . ? C8 N3 C12 117.7(3) . . ? C8 N3 Ni1 120.9(2) . . ? C12 N3 Ni1 121.4(2) . . ? N1 C1 S1 178.9(3) . . ? C3 C4 C5 118.0(3) . . ? N2 C2 C3 122.4(3) . . ? C11 C10 C9 118.2(3) . . ? C4 C3 C2 119.6(3) . . ? C4 C3 C7 121.3(3) . . ? C2 C3 C7 119.1(3) . . ? N4 C7 C3 178.7(4) . . ? C10 C9 C8 119.6(3) . . ? C10 C9 C13 121.5(3) . . ? C8 C9 C13 118.9(3) . . ? N2 C6 C5 123.2(3) . . ? N3 C8 C9 122.2(3) . . ? N3 C12 C11 123.2(3) . . ? N5 C13 C9 178.0(5) . . ? C6 C5 C4 119.1(3) . . ? C10 C11 C12 119.1(4) . . ? C14B Cl2B Cl2B 161.2(5) . 7 ? Cl1B C14B Cl2B 112.1(3) . . ? Cl2A C14A Cl1A 104.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 N1 C1 -61(2) 2_655 . . . ? N2 Ni1 N1 C1 74(2) 2_655 . . . ? N2 Ni1 N1 C1 165(2) . . . . ? N3 Ni1 N1 C1 -106(2) . . . . ? N3 Ni1 N1 C1 -16(2) 2_655 . . . ? N1 Ni1 N2 C2 37.2(2) . . . . ? N1 Ni1 N2 C2 -142.5(2) 2_655 . . . ? N2 Ni1 N2 C2 128.4(3) 2_655 . . . ? N3 Ni1 N2 C2 -53.7(2) . . . . ? N3 Ni1 N2 C2 26(3) 2_655 . . . ? N1 Ni1 N2 C6 -138.8(3) . . . . ? N1 Ni1 N2 C6 41.5(3) 2_655 . . . ? N2 Ni1 N2 C6 -47.5(2) 2_655 . . . ? N3 Ni1 N2 C6 130.4(3) . . . . ? N3 Ni1 N2 C6 -150(3) 2_655 . . . ? N1 Ni1 N3 C8 31.1(2) . . . . ? N1 Ni1 N3 C8 -148.6(2) 2_655 . . . ? N2 Ni1 N3 C8 -137(3) 2_655 . . . ? N2 Ni1 N3 C8 120.2(2) . . . . ? N3 Ni1 N3 C8 -57.7(2) 2_655 . . . ? N1 Ni1 N3 C12 -148.4(3) . . . . ? N1 Ni1 N3 C12 31.9(3) 2_655 . . . ? N2 Ni1 N3 C12 43(3) 2_655 . . . ? N2 Ni1 N3 C12 -59.4(3) . . . . ? N3 Ni1 N3 C12 122.8(3) 2_655 . . . ? Ni1 N1 C1 S1 23(18) . . . . ? C6 N2 C2 C3 -0.3(5) . . . . ? Ni1 N2 C2 C3 -176.4(2) . . . . ? C5 C4 C3 C2 -1.1(6) . . . . ? C5 C4 C3 C7 178.5(4) . . . . ? N2 C2 C3 C4 1.1(5) . . . . ? N2 C2 C3 C7 -178.5(3) . . . . ? C4 C3 C7 N4 -79(20) . . . . ? C2 C3 C7 N4 100(20) . . . . ? C11 C10 C9 C8 0.8(6) . . . . ? C11 C10 C9 C13 -179.3(4) . . . . ? C2 N2 C6 C5 -0.6(6) . . . . ? Ni1 N2 C6 C5 175.5(3) . . . . ? C12 N3 C8 C9 0.4(5) . . . . ? Ni1 N3 C8 C9 -179.1(2) . . . . ? C10 C9 C8 N3 -0.9(5) . . . . ? C13 C9 C8 N3 179.1(3) . . . . ? C8 N3 C12 C11 0.2(5) . . . . ? Ni1 N3 C12 C11 179.8(3) . . . . ? C10 C9 C13 N5 139(13) . . . . ? C8 C9 C13 N5 -41(14) . . . . ? N2 C6 C5 C4 0.5(7) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? C9 C10 C11 C12 -0.2(7) . . . . ? N3 C12 C11 C10 -0.3(7) . . . . ? Cl2B Cl2B C14B Cl1B 112.6(10) 7 . . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 1.220 _refine_diff_density_min -0.864 _refine_diff_density_rms 0.086 #===END