Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Nishikiori, Shin-ichi' 'Sekiya, Ryo' _publ_contact_author_name 'Dr Shin-ichi Nishikiori' _publ_contact_author_address ; Basic Science The University of Tokyo 3-8-1 Komaba Megro Tokyo 153-8902 JAPAN ; _publ_contact_author_email CNSKOR@MAIL.ECC.U-TOKYO.AC.JP _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Preparative Strategy for Supramolecular Inclusion Compounds by Combination of Dimmer Formation of Isonicotinic Acid and Coordination Bonding ; data_anthraceneinclude _database_code_CSD 171788 _audit_creation_date 2001-10-29T19:06:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; catena-bis(N-isonicotinic acid)nickel(II)-bis(\m-isothiocyanato-N,N',S,S') 1/2(anthracene) ; _chemical_formula_moiety 'C21 H15 N4 Ni O4 S2' _chemical_formula_sum 'C21 H15 N4 Ni O4 S2' _chemical_formula_weight 510.2 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2337(7) _cell_length_b 11.0126(13) _cell_length_c 16.7266(16) _cell_angle_alpha 104.590(3) _cell_angle_beta 54.736(5) _cell_angle_gamma 97.602(8) _cell_volume 1052.74(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.61 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 522 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.158 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8782 _exptl_absorpt_correction_T_max 1.0000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_number 4652 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4652 _reflns_number_observed 3772 _reflns_observed_criterion >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material SHELXL-97 #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0847P)^2^+0.3314P] 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_number_reflns 4652 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0571 _refine_ls_R_factor_obs 0.0393 _refine_ls_wR_factor_all 0.1408 _refine_ls_wR_factor_obs 0.1151 _refine_ls_goodness_of_fit_all 1.156 _refine_ls_restrained_S_all 1.156 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.513 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.137 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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_thermal_displace_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 0 0 0.02617(15) Uani 1 2 d S . . Ni2 Ni 0 0.5 0 0.02670(15) Uani 1 2 d S . . S1 S -0.36361(13) 0.39221(7) 0.10853(6) 0.0356(2) Uani 1 1 d . . . S2 S -0.34263(13) 0.86849(7) 0.04337(7) 0.0389(2) Uani 1 1 d . . . O11 O -0.2838(5) 0.1230(3) 0.49405(19) 0.0541(7) Uani 1 1 d . . . H211 H -0.2668 0.1406 0.54 0.081 Uiso 1 1 calc R . . O12 O 0.0861(5) 0.0791(3) 0.4021(2) 0.0588(8) Uani 1 1 d . . . O21 O -0.2306(5) 0.2372(3) 0.6383(2) 0.0612(8) Uani 1 1 d . . . O22 O 0.1337(5) 0.1844(3) 0.5466(2) 0.0607(8) Uani 1 1 d . . . H222 H 0.1082 0.1535 0.5039 0.091 Uiso 1 1 calc R . . N1 N -0.2070(4) 0.1517(2) 0.0622(2) 0.0326(6) Uani 1 1 d . . . N2 N -0.1930(4) 0.6404(2) 0.0272(2) 0.0331(6) Uani 1 1 d . . . N11 N -0.0601(4) 0.0044(2) 0.1409(2) 0.0327(6) Uani 1 1 d . . . N21 N -0.0061(4) 0.4090(2) 0.87386(19) 0.0314(5) Uani 1 1 d . . . C1 C -0.2723(5) 0.2503(3) 0.0812(2) 0.0268(6) Uani 1 1 d . . . C2 C -0.2546(5) 0.7345(3) 0.0339(2) 0.0277(6) Uani 1 1 d . . . C11 C 0.1121(6) -0.0196(3) 0.1432(3) 0.0392(7) Uani 1 1 d . . . H11 H 0.2459 -0.0522 0.083 0.047 Uiso 1 1 calc R . . C12 C 0.1020(6) 0.0014(4) 0.2299(3) 0.0425(8) Uani 1 1 d . . . H12 H 0.227 -0.0159 0.228 0.051 Uiso 1 1 calc R . . C13 C -0.0954(6) 0.0483(3) 0.3197(3) 0.0372(7) Uani 1 1 d . . . C14 C -0.2788(6) 0.0676(3) 0.3198(3) 0.0403(8) Uani 1 1 d . . . H14 H -0.4165 0.0959 0.3797 0.048 Uiso 1 1 calc R . . C15 C -0.2552(5) 0.0444(3) 0.2295(3) 0.0380(7) Uani 1 1 d . . . H15 H -0.3803 0.057 0.2299 0.046 Uiso 1 1 calc R . . C16 C -0.0957(6) 0.0845(4) 0.4115(3) 0.0425(8) Uani 1 1 d . . . C21 C -0.1919(5) 0.4175(3) 0.8765(3) 0.0377(7) Uani 1 1 d . . . H21 H -0.3155 0.4632 0.9345 0.045 Uiso 1 1 calc R . . C22 C -0.2099(6) 0.3627(3) 0.7986(3) 0.0384(7) Uani 1 1 d . . . H22 H -0.3436 0.3701 0.8041 0.046 Uiso 1 1 calc R . . C23 C -0.0277(5) 0.2964(3) 0.7118(2) 0.0360(7) Uani 1 1 d . . . C24 C 0.1680(6) 0.2879(3) 0.7071(3) 0.0387(7) Uani 1 1 d . . . H24 H 0.295 0.2445 0.6493 0.046 Uiso 1 1 calc R . . C25 C 0.1704(5) 0.3447(3) 0.7890(2) 0.0354(7) Uani 1 1 d . . . H25 H 0.3017 0.3383 0.7857 0.042 Uiso 1 1 calc R . . C26 C -0.0462(6) 0.2361(4) 0.6270(3) 0.0422(8) Uani 1 1 d . . . C101 C 0.0054(9) 0.6577(5) 0.7409(4) 0.0695(13) Uani 1 1 d . . . H101 H -0.0916 0.6922 0.8091 0.083 Uiso 1 1 calc R . . C102 C 1.0623(9) 0.3448(5) 0.3231(4) 0.0695(13) Uani 1 1 d . . . H102 H 1.2037 0.3125 0.2969 0.083 Uiso 1 1 calc R . . C103 C 0.9229(8) 0.3938(4) 0.4225(4) 0.0631(12) Uani 1 1 d . . . H103 H 0.9673 0.3925 0.4645 0.076 Uiso 1 1 calc R . . C104 C 0.7096(7) 0.4469(4) 0.4633(3) 0.0517(10) Uani 1 1 d . . . C105 C 0.3583(8) 0.5549(4) 0.6023(3) 0.0522(10) Uani 1 1 d . . . C106 C 0.2062(9) 0.6113(4) 0.7056(3) 0.0625(12) Uani 1 1 d . . . H106 H 0.2481 0.6159 0.7494 0.075 Uiso 1 1 calc R . . C107 C 0.5645(8) 0.5022(4) 0.5637(3) 0.0559(11) Uani 1 1 d . . . H107 H 0.6072 0.5039 0.6068 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0291(3) 0.0223(3) 0.0288(3) 0.0011(2) -0.0177(2) 0.00611(19) Ni2 0.0283(3) 0.0221(3) 0.0297(3) 0.0021(2) -0.0166(2) 0.00526(19) S1 0.0298(4) 0.0277(4) 0.0411(4) 0.0065(3) -0.0143(3) 0.0077(3) S2 0.0323(4) 0.0270(4) 0.0600(6) 0.0080(4) -0.0270(4) 0.0053(3) O11 0.0541(17) 0.0712(19) 0.0320(13) 0.0012(12) -0.0236(12) 0.0084(14) O12 0.0591(17) 0.078(2) 0.0447(15) -0.0063(14) -0.0359(14) 0.0204(15) O21 0.0490(16) 0.088(2) 0.0477(16) -0.0115(15) -0.0346(14) 0.0156(15) O22 0.0539(17) 0.088(2) 0.0359(14) -0.0137(14) -0.0290(13) 0.0197(15) N1 0.0321(13) 0.0247(13) 0.0373(14) 0.0024(10) -0.0184(11) 0.0039(10) N2 0.0314(13) 0.0286(13) 0.0399(15) 0.0063(11) -0.0201(12) 0.0039(10) N11 0.0335(14) 0.0337(14) 0.0330(13) 0.0033(11) -0.0202(11) 0.0059(10) N21 0.0306(13) 0.0340(14) 0.0302(13) 0.0029(10) -0.0182(11) 0.0041(10) C1 0.0266(14) 0.0278(15) 0.0252(13) 0.0032(11) -0.0146(11) 0.0029(11) C2 0.0236(13) 0.0262(14) 0.0287(14) 0.0009(11) -0.0137(11) 0.0022(11) C11 0.0375(17) 0.0459(19) 0.0327(16) -0.0018(14) -0.0198(14) 0.0150(14) C12 0.0414(19) 0.053(2) 0.0378(18) 0.0002(15) -0.0256(15) 0.0145(15) C13 0.0415(18) 0.0396(17) 0.0329(16) 0.0026(13) -0.0232(14) 0.0054(13) C14 0.0340(17) 0.051(2) 0.0307(16) 0.0040(14) -0.0160(14) 0.0048(14) C15 0.0323(16) 0.0445(19) 0.0382(17) 0.0055(14) -0.0206(14) 0.0062(13) C16 0.049(2) 0.046(2) 0.0327(17) 0.0023(15) -0.0237(16) 0.0071(15) C21 0.0299(16) 0.0451(19) 0.0331(16) -0.0009(14) -0.0167(13) 0.0089(13) C22 0.0331(17) 0.0435(18) 0.0384(17) 0.0018(14) -0.0218(14) 0.0045(13) C23 0.0354(17) 0.0379(17) 0.0332(16) 0.0028(13) -0.0200(14) 0.0016(13) C24 0.0359(17) 0.0421(18) 0.0334(16) -0.0016(14) -0.0185(14) 0.0098(13) C25 0.0300(16) 0.0366(17) 0.0384(17) 0.0004(13) -0.0202(13) 0.0071(12) C26 0.045(2) 0.046(2) 0.0355(17) -0.0002(15) -0.0246(16) 0.0058(15) C101 0.082(4) 0.054(3) 0.053(3) 0.017(2) -0.028(2) -0.013(2) C102 0.060(3) 0.064(3) 0.072(3) 0.023(2) -0.029(2) -0.013(2) C103 0.065(3) 0.062(3) 0.070(3) 0.027(2) -0.042(2) -0.021(2) C104 0.062(3) 0.049(2) 0.052(2) 0.0215(18) -0.036(2) -0.0180(18) C105 0.066(3) 0.048(2) 0.047(2) 0.0188(17) -0.034(2) -0.0179(19) C106 0.080(3) 0.060(3) 0.049(2) 0.020(2) -0.037(2) -0.019(2) C107 0.072(3) 0.064(3) 0.052(2) 0.028(2) -0.045(2) -0.023(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 2.026(3) 2 ? Ni1 N1 2.026(3) . ? Ni1 N11 2.124(3) 2 ? Ni1 N11 2.124(3) . ? Ni1 S2 2.5040(8) 2_565 ? Ni1 S2 2.5040(8) 1_545 ? Ni2 N2 2.008(3) 2_565 ? Ni2 N2 2.008(3) . ? Ni2 N21 2.119(3) 2_566 ? Ni2 N21 2.119(3) 1_554 ? Ni2 S1 2.5237(8) . ? Ni2 S1 2.5237(8) 2_565 ? S1 C1 1.629(3) . ? S2 C2 1.619(3) . ? S2 Ni1 2.5040(9) 1_565 ? O11 C16 1.275(4) . ? O12 C16 1.240(5) . ? O12 O22 2.569(4) . ? O21 C26 1.235(4) . ? O22 C26 1.272(4) . ? O21 O11 2.639(4) . ? N1 C1 1.137(4) . ? N2 C2 1.136(4) . ? N11 C11 1.330(4) . ? N11 C15 1.343(4) . ? N21 C21 1.334(4) . ? N21 C25 1.336(4) . ? N21 Ni2 2.119(3) 1_556 ? C11 C12 1.369(5) . ? C12 C13 1.374(5) . ? C13 C14 1.370(5) . ? C13 C16 1.486(5) . ? C14 C15 1.376(5) . ? C21 C22 1.364(5) . ? C22 C23 1.375(5) . ? C23 C24 1.387(5) . ? C23 C26 1.480(5) . ? C24 C25 1.365(5) . ? C101 C106 1.331(7) . ? C101 C102 1.404(8) 2_666 ? C102 C103 1.353(7) . ? C102 C101 1.404(8) 2_666 ? C103 C104 1.418(7) . ? C104 C107 1.383(6) . ? C104 C105 1.432(6) 2_666 ? C105 C107 1.381(6) . ? C105 C106 1.424(6) . ? C105 C104 1.432(6) 2_666 ? 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(17) 2 . ? N1 Ni1 N11 90.18(11) 2 2 ? N1 Ni1 N11 89.82(11) . 2 ? N1 Ni1 N11 89.82(11) 2 . ? N1 Ni1 N11 90.18(11) . . ? N11 Ni1 N11 180.00(14) 2 . ? N1 Ni1 S2 86.98(8) 2 2_565 ? N1 Ni1 S2 93.02(8) . 2_565 ? N11 Ni1 S2 90.59(7) 2 2_565 ? N11 Ni1 S2 89.41(7) . 2_565 ? N1 Ni1 S2 93.02(8) 2 1_545 ? N1 Ni1 S2 86.98(8) . 1_545 ? N11 Ni1 S2 89.41(7) 2 1_545 ? N11 Ni1 S2 90.59(7) . 1_545 ? S2 Ni1 S2 180 2_565 1_545 ? N2 Ni2 N2 180.00(18) 2_565 . ? N2 Ni2 N21 89.95(11) 2_565 2_566 ? N2 Ni2 N21 90.05(11) . 2_566 ? N2 Ni2 N21 90.05(11) 2_565 1_554 ? N2 Ni2 N21 89.95(11) . 1_554 ? N21 Ni2 N21 180.00(8) 2_566 1_554 ? N2 Ni2 S1 92.91(8) 2_565 . ? N2 Ni2 S1 87.09(8) . . ? N21 Ni2 S1 91.12(7) 2_566 . ? N21 Ni2 S1 88.88(7) 1_554 . ? N2 Ni2 S1 87.09(8) 2_565 2_565 ? N2 Ni2 S1 92.91(8) . 2_565 ? N21 Ni2 S1 88.88(7) 2_566 2_565 ? N21 Ni2 S1 91.12(7) 1_554 2_565 ? S1 Ni2 S1 180.00(3) . 2_565 ? C1 S1 Ni2 101.39(10) . . ? C2 S2 Ni1 101.19(10) . 1_565 ? C1 N1 Ni1 162.4(2) . . ? C2 N2 Ni2 163.6(2) . . ? C11 N11 C15 117.0(3) . . ? C11 N11 Ni1 118.7(2) . . ? C15 N11 Ni1 123.9(2) . . ? C21 N21 C25 117.1(3) . . ? C21 N21 Ni2 119.5(2) . 1_556 ? C25 N21 Ni2 123.4(2) . 1_556 ? N1 C1 S1 179.5(3) . . ? N2 C2 S2 179.8(3) . . ? N11 C11 C12 123.3(3) . . ? C11 C12 C13 119.1(3) . . ? C14 C13 C12 118.7(3) . . ? C14 C13 C16 122.6(3) . . ? C12 C13 C16 118.5(3) . . ? C13 C14 C15 118.6(3) . . ? N11 C15 C14 123.1(3) . . ? O12 C16 O11 125.0(3) . . ? O12 C16 C13 118.1(3) . . ? O11 C16 C13 116.8(3) . . ? N21 C21 C22 123.4(3) . . ? C21 C22 C23 119.1(3) . . ? C22 C23 C24 118.4(3) . . ? C22 C23 C26 119.4(3) . . ? C24 C23 C26 122.2(3) . . ? C25 C24 C23 118.6(3) . . ? N21 C25 C24 123.5(3) . . ? O21 C26 O22 124.5(3) . . ? O21 C26 C23 119.5(3) . . ? O22 C26 C23 116.0(3) . . ? C106 C101 C102 121.0(5) . 2_666 ? C103 C102 C101 120.4(5) . 2_666 ? C102 C103 C104 120.6(5) . . ? C107 C104 C103 122.9(4) . . ? C107 C104 C105 118.2(4) . 2_666 ? C103 C104 C105 118.9(4) . 2_666 ? C107 C105 C106 123.1(4) . . ? C107 C105 C104 119.5(4) . 2_666 ? C106 C105 C104 117.5(5) . 2_666 ? C101 C106 C105 121.6(5) . . ? C105 C107 C104 122.3(4) . . ? data_pyreneinclude _database_code_CSD 171789 _audit_creation_date 2001-10-29T18:49:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; catena-bis(N-3-(4-pyridyl)acrylic acid)-nicekl(II)-bis (\m-isothiocyanato-N,N',S,S')1/2(pyrene) ; _chemical_formula_moiety 'C26 H19 N4 Ni O4 S2' _chemical_formula_sum 'C26 H19 N4 Ni O4 S2' _chemical_formula_weight 574.28 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9991(8) _cell_length_b 11.0440(6) _cell_length_c 21.3223(13) _cell_angle_alpha 101.551(2) _cell_angle_beta 37.779(2) _cell_angle_gamma 99.3920(10) _cell_volume 1271.89(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 27.5 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.5 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 590 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.968 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8073 _exptl_absorpt_correction_T_max 1.0000 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_number 5772 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5772 _reflns_number_observed 4589 _reflns_observed_criterion >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material SHELXL-97 #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0594P)^2^+0.4490P] 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_number_reflns 5772 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_obs 0.04 _refine_ls_wR_factor_all 0.113 _refine_ls_wR_factor_obs 0.1052 _refine_ls_goodness_of_fit_all 1.108 _refine_ls_restrained_S_all 1.108 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 0.663 _refine_diff_density_min -0.562 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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_thermal_displace_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 1 0.5 1 0.02801(12) Uani 1 2 d S . . Ni2 Ni 1 0 1 0.02900(12) Uani 1 2 d S . . S1 S 1.39697(12) 0.11373(6) 0.85597(5) 0.04141(17) Uani 1 1 d . . . S2 S 1.36718(12) 0.63143(6) 0.91447(6) 0.04410(19) Uani 1 1 d . . . O11 O 1.2223(4) 0.3613(2) 0.49386(16) 0.0599(6) Uani 1 1 d . . . O12 O 0.8328(4) 0.3981(3) 0.60992(19) 0.0855(10) Uani 1 1 d . . . H212 H 0.8697 0.3724 0.5601 0.128 Uiso 1 1 calc R . . O21 O 0.7511(4) -0.2489(3) 0.63608(18) 0.0698(7) Uani 1 1 d . . . H221 H 0.7812 -0.2822 0.589 0.105 Uiso 1 1 calc R . . O22 O 1.1135(4) -0.3239(2) 0.53129(17) 0.0600(6) Uani 1 1 d . . . N1 N 1.2233(4) 0.35162(19) 0.91629(17) 0.0361(5) Uani 1 1 d . . . N2 N 1.2080(4) 0.86180(19) 0.95105(17) 0.0356(5) Uani 1 1 d . . . N11 N 1.0631(4) 0.5130(2) 0.88255(16) 0.0356(5) Uani 1 1 d . . . N21 N 1.0124(4) -0.08332(19) 0.89778(16) 0.0351(4) Uani 1 1 d . . . C1 C 1.2968(4) 0.2535(2) 0.89094(18) 0.0295(5) Uani 1 1 d . . . C2 C 1.2728(4) 0.7664(2) 0.93645(18) 0.0288(5) Uani 1 1 d . . . C11 C 1.2755(5) 0.4777(3) 0.7837(2) 0.0417(6) Uani 1 1 d . . . H11 H 1.4051 0.4652 0.7663 0.05 Uiso 1 1 calc R . . C12 C 1.3116(5) 0.4588(3) 0.7063(2) 0.0443(6) Uani 1 1 d . . . H12 H 1.4626 0.4345 0.6386 0.053 Uiso 1 1 calc R . . C13 C 1.1209(5) 0.4763(3) 0.7303(2) 0.0401(6) Uani 1 1 d . . . C14 C 0.9054(5) 0.5203(3) 0.8317(2) 0.0453(7) Uani 1 1 d . . . H14 H 0.7759 0.5384 0.8504 0.054 Uiso 1 1 calc R . . C15 C 0.8840(5) 0.5370(3) 0.9041(2) 0.0428(6) Uani 1 1 d . . . H15 H 0.738 0.5664 0.9715 0.051 Uiso 1 1 calc R . . C16 C 1.1500(5) 0.4423(3) 0.6509(2) 0.0461(7) Uani 1 1 d . . . H16 H 1.3044 0.4191 0.5842 0.055 Uiso 1 1 calc R . . C17 C 0.9800(6) 0.4414(3) 0.6647(2) 0.0541(8) Uani 1 1 d . . . H17 H 0.8271 0.4701 0.7296 0.065 Uiso 1 1 calc R . . C18 C 1.0186(6) 0.3973(3) 0.5832(2) 0.0515(7) Uani 1 1 d . . . C21 C 1.2110(5) -0.1389(2) 0.8042(2) 0.0396(6) Uani 1 1 d . . . H21 H 1.343 -0.1466 0.7862 0.048 Uiso 1 1 calc R . . C22 C 1.2308(5) -0.1855(3) 0.7328(2) 0.0405(6) Uani 1 1 d . . . H22 H 1.3738 -0.2229 0.6685 0.049 Uiso 1 1 calc R . . C23 C 1.0378(5) -0.1765(2) 0.7570(2) 0.0372(5) Uani 1 1 d . . . C24 C 0.8290(5) -0.1212(3) 0.8552(2) 0.0448(6) Uani 1 1 d . . . H24 H 0.6932 -0.1143 0.8757 0.054 Uiso 1 1 calc R . . C25 C 0.8231(5) -0.0770(3) 0.9219(2) 0.0424(6) Uani 1 1 d . . . H25 H 0.681 -0.0406 0.9873 0.051 Uiso 1 1 calc R . . C26 C 1.0590(5) -0.2234(3) 0.6810(2) 0.0409(6) Uani 1 1 d . . . H26 H 1.199 -0.2667 0.62 0.049 Uiso 1 1 calc R . . C27 C 0.8982(5) -0.2100(3) 0.6910(2) 0.0446(6) Uani 1 1 d . . . H27 H 0.7603 -0.1636 0.7498 0.054 Uiso 1 1 calc R . . C28 C 0.9273(5) -0.2651(3) 0.6133(2) 0.0450(6) Uani 1 1 d . . . C101 C 1.5194(9) 0.0515(4) 0.5816(4) 0.0776(12) Uani 1 1 d . . . C102 C 1.3725(12) 0.1169(5) 0.6800(5) 0.0971(16) Uani 1 1 d . . . H102 H 1.4288 0.1311 0.7031 0.117 Uiso 1 1 calc R . . C103 C 1.1480(13) 0.1600(5) 0.7424(5) 0.1088(19) Uani 1 1 d . . . H103 H 1.0543 0.2014 0.8074 0.131 Uiso 1 1 calc R . . C104 C 1.0600(10) 0.1429(4) 0.7106(4) 0.0956(15) Uani 1 1 d . . . H104 H 0.9081 0.1731 0.7536 0.115 Uiso 1 1 calc R . . C105 C 1.1956(8) 0.0813(4) 0.6153(4) 0.0759(11) Uani 1 1 d . . . C106 C 1.4293(7) 0.0332(3) 0.5488(3) 0.0642(10) Uani 1 1 d . . . C107 C 1.1170(9) 0.0595(5) 0.5764(5) 0.0908(15) Uani 1 1 d . . . H107 H 0.9674 0.0899 0.6168 0.109 Uiso 1 1 calc R . . C108 C 1.7501(10) 0.0024(5) 0.5153(5) 0.0917(16) Uani 1 1 d . . . H108 H 1.8096 0.014 0.537 0.11 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0281(2) 0.0243(2) 0.0337(2) 0.00095(16) -0.0246(2) 0.00400(16) Ni2 0.0306(2) 0.0239(2) 0.0340(2) -0.00231(16) -0.0257(2) 0.00701(16) S1 0.0325(3) 0.0311(3) 0.0417(3) 0.0001(3) -0.0241(3) 0.0095(2) S2 0.0346(3) 0.0286(3) 0.0678(5) 0.0099(3) -0.0391(4) 0.0011(2) O11 0.0457(12) 0.0920(17) 0.0427(11) -0.0133(11) -0.0354(11) 0.0222(12) O12 0.0493(13) 0.160(3) 0.0496(13) -0.0325(16) -0.0416(12) 0.0391(16) O21 0.0522(13) 0.112(2) 0.0545(13) -0.0273(13) -0.0457(12) 0.0326(13) O22 0.0491(12) 0.0865(17) 0.0479(12) -0.0186(11) -0.0399(11) 0.0250(11) N1 0.0314(10) 0.0319(10) 0.0400(11) 0.0028(9) -0.0265(10) 0.0038(8) N2 0.0336(11) 0.0299(10) 0.0408(11) 0.0003(9) -0.0285(10) 0.0053(8) N11 0.0336(11) 0.0398(11) 0.0375(11) 0.0021(9) -0.0285(10) 0.0058(9) N21 0.0333(10) 0.0353(11) 0.0373(11) -0.0034(9) -0.0282(10) 0.0068(9) C1 0.0257(11) 0.0317(12) 0.0288(11) 0.0033(9) -0.0208(10) 0.0004(9) C2 0.0267(11) 0.0295(11) 0.0331(11) 0.0022(9) -0.0242(10) 0.0015(9) C11 0.0310(13) 0.0555(16) 0.0405(14) 0.0064(12) -0.0280(12) 0.0036(11) C12 0.0319(13) 0.0598(17) 0.0334(13) 0.0023(12) -0.0234(12) 0.0073(12) C13 0.0400(14) 0.0443(14) 0.0387(13) 0.0033(11) -0.0311(12) 0.0053(11) C14 0.0411(14) 0.0580(17) 0.0459(15) -0.0029(13) -0.0357(14) 0.0158(13) C15 0.0364(13) 0.0541(16) 0.0377(13) -0.0041(12) -0.0286(12) 0.0155(12) C16 0.0430(15) 0.0576(17) 0.0384(14) -0.0014(12) -0.0317(13) 0.0121(13) C17 0.0471(16) 0.074(2) 0.0404(15) -0.0133(14) -0.0343(14) 0.0231(15) C18 0.0477(16) 0.069(2) 0.0428(15) -0.0067(14) -0.0368(14) 0.0160(15) C21 0.0373(13) 0.0427(14) 0.0436(14) -0.0047(11) -0.0330(13) 0.0110(11) C22 0.0356(13) 0.0436(14) 0.0383(13) -0.0078(11) -0.0286(12) 0.0115(11) C23 0.0360(13) 0.0362(13) 0.0399(13) 0.0003(11) -0.0304(12) 0.0020(10) C24 0.0361(14) 0.0552(16) 0.0450(15) -0.0069(13) -0.0332(13) 0.0090(12) C25 0.0314(13) 0.0507(15) 0.0392(13) -0.0093(12) -0.0271(12) 0.0117(11) C26 0.0381(13) 0.0432(14) 0.0384(13) -0.0043(11) -0.0299(12) 0.0059(11) C27 0.0362(14) 0.0558(17) 0.0362(13) -0.0019(12) -0.0275(12) 0.0054(12) C28 0.0390(14) 0.0569(17) 0.0401(14) 0.0007(13) -0.0316(13) 0.0040(13) C101 0.098(3) 0.075(3) 0.103(3) 0.046(2) -0.088(3) -0.033(2) C102 0.132(5) 0.084(3) 0.126(4) 0.052(3) -0.113(4) -0.045(3) C103 0.129(5) 0.068(3) 0.099(4) 0.032(3) -0.082(4) -0.026(3) C104 0.091(3) 0.069(3) 0.101(4) 0.029(3) -0.068(3) -0.015(2) C105 0.078(3) 0.064(2) 0.100(3) 0.043(2) -0.071(3) -0.026(2) C106 0.068(2) 0.063(2) 0.092(2) 0.046(2) -0.067(2) -0.0300(18) C107 0.072(3) 0.093(3) 0.128(4) 0.048(3) -0.080(3) -0.017(2) C108 0.094(3) 0.107(4) 0.138(4) 0.060(3) -0.103(4) -0.033(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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(2) . ? Ni1 N1 2.035(2) 2_767 ? Ni1 N11 2.118(2) 2_767 ? Ni1 N11 2.118(2) . ? Ni1 S2 2.5140(7) . ? Ni1 S2 2.5140(7) 2_767 ? Ni2 N2 2.032(2) 1_545 ? Ni2 N2 2.032(2) 2_767 ? Ni2 N21 2.111(2) 2_757 ? Ni2 N21 2.111(2) . ? Ni2 S1 2.5512(7) 2_757 ? Ni2 S1 2.5512(7) . ? S1 C1 1.637(2) . ? S2 C2 1.633(2) . ? O11 C18 1.250(4) . ? O12 C18 1.272(4) . ? O11 O21 2.636(4) 2_756 ? O21 C28 1.274(3) . ? O22 C28 1.247(3) . ? O22 O12 2.610(4) 2_756 ? N1 C1 1.157(3) . ? N2 C2 1.153(3) . ? N2 Ni2 2.032(2) 1_565 ? N11 C11 1.339(3) . ? N11 C15 1.342(3) . ? N21 C21 1.335(3) . ? N21 C25 1.345(3) . ? C11 C12 1.382(4) . ? C12 C13 1.388(4) . ? C13 C14 1.389(4) . ? C13 C16 1.467(4) . ? C14 C15 1.372(4) . ? C16 C17 1.307(4) . ? C17 C18 1.463(4) . ? C21 C22 1.379(4) . ? C22 C23 1.382(4) . ? C23 C24 1.390(4) . ? C23 C26 1.464(4) . ? C24 C25 1.369(4) . ? C26 C27 1.316(4) . ? C27 C28 1.464(4) . ? C101 C106 1.403(5) . ? C101 C102 1.411(7) . ? C101 C108 1.423(7) . ? C102 C103 1.374(8) . ? C103 C104 1.369(8) . ? C104 C105 1.370(7) . ? C105 C107 1.426(7) . ? C105 C106 1.437(6) . ? C106 C106 1.414(8) 2_856 ? C107 C108 1.325(7) 2_856 ? C108 C107 1.325(7) 2_856 ? 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 180.0(2) . 2_767 ? N1 Ni1 N11 89.08(9) . 2_767 ? N1 Ni1 N11 90.92(9) 2_767 2_767 ? N1 Ni1 N11 90.92(9) . . ? N1 Ni1 N11 89.08(9) 2_767 . ? N11 Ni1 N11 180.000(2) 2_767 . ? N1 Ni1 S2 86.79(6) . . ? N1 Ni1 S2 93.21(6) 2_767 . ? N11 Ni1 S2 88.51(6) 2_767 . ? N11 Ni1 S2 91.49(6) . . ? N1 Ni1 S2 93.21(6) . 2_767 ? N1 Ni1 S2 86.79(6) 2_767 2_767 ? N11 Ni1 S2 91.49(6) 2_767 2_767 ? N11 Ni1 S2 88.51(6) . 2_767 ? S2 Ni1 S2 180.00(6) . 2_767 ? N2 Ni2 N2 180.00(15) 1_545 2_767 ? N2 Ni2 N21 90.31(8) 1_545 2_757 ? N2 Ni2 N21 89.69(8) 2_767 2_757 ? N2 Ni2 N21 89.69(8) 1_545 . ? N2 Ni2 N21 90.31(8) 2_767 . ? N21 Ni2 N21 180 2_757 . ? N2 Ni2 S1 93.48(6) 1_545 2_757 ? N2 Ni2 S1 86.53(6) 2_767 2_757 ? N21 Ni2 S1 89.92(6) 2_757 2_757 ? N21 Ni2 S1 90.08(6) . 2_757 ? N2 Ni2 S1 86.53(6) 1_545 . ? N2 Ni2 S1 93.47(6) 2_767 . ? N21 Ni2 S1 90.08(6) 2_757 . ? N21 Ni2 S1 89.92(6) . . ? S1 Ni2 S1 180.00(3) 2_757 . ? C1 S1 Ni2 100.59(8) . . ? C2 S2 Ni1 100.61(8) . . ? C1 N1 Ni1 162.5(2) . . ? C2 N2 Ni2 162.6(2) . 1_565 ? C11 N11 C15 116.8(2) . . ? C11 N11 Ni1 120.37(17) . . ? C15 N11 Ni1 121.94(18) . . ? C21 N21 C25 116.5(2) . . ? C21 N21 Ni2 122.22(17) . . ? C25 N21 Ni2 121.19(17) . . ? N1 C1 S1 179.2(2) . . ? N2 C2 S2 179.4(3) . . ? N11 C11 C12 123.3(2) . . ? C11 C12 C13 119.5(2) . . ? C12 C13 C14 117.1(3) . . ? C12 C13 C16 119.6(2) . . ? C14 C13 C16 123.3(2) . . ? C15 C14 C13 119.8(2) . . ? N11 C15 C14 123.3(2) . . ? C17 C16 C13 126.3(3) . . ? C16 C17 C18 123.2(3) . . ? O11 C18 O12 123.3(3) . . ? O11 C18 C17 121.1(3) . . ? O12 C18 C17 115.6(3) . . ? N21 C21 C22 123.5(2) . . ? C21 C22 C23 119.9(2) . . ? C22 C23 C24 116.7(2) . . ? C22 C23 C26 120.3(2) . . ? C24 C23 C26 123.0(2) . . ? C25 C24 C23 120.0(2) . . ? N21 C25 C24 123.4(2) . . ? C27 C26 C23 126.0(3) . . ? C26 C27 C28 122.7(3) . . ? O22 C28 O21 123.6(3) . . ? O22 C28 C27 121.0(3) . . ? O21 C28 C27 115.4(3) . . ? C106 C101 C102 117.5(5) . . ? C106 C101 C108 118.8(5) . . ? C102 C101 C108 123.6(5) . . ? C103 C102 C101 121.6(5) . . ? C104 C103 C102 121.1(6) . . ? C103 C104 C105 120.0(5) . . ? C104 C105 C107 123.5(5) . . ? C104 C105 C106 120.3(5) . . ? C107 C105 C106 116.2(5) . . ? C101 C106 C106 119.0(5) . 2_856 ? C101 C106 C105 119.5(4) . . ? C106 C106 C105 121.5(4) 2_856 . ? C108 C107 C105 122.3(5) 2_856 . ? C107 C108 C101 122.2(4) 2_856 . ?