Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_z _database_code_CSD 165608 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Cao, Rong' 'Hong, Maochun' 'Sun, Daofeng' 'Zhao, Yingjun' _publ_contact_author_name 'Prof Maochun Hong' _publ_contact_author_address ; State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Scie Fuzhou Fujian 350002 P. R. China. ; _publ_contact_author_email 'HMC@MS.FJIRSM.AC.CN' _publ_section_title ; A novel coordination polymer containing puckered rhombus grids ; _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20 N2 Ni O4 S2' _chemical_formula_weight 547.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0854(3) _cell_length_b 11.1224(3) _cell_length_c 11.720 _cell_angle_alpha 63.3730(10) _cell_angle_beta 82.0080(10) _cell_angle_gamma 80.1420(10) _cell_volume 1269.56(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.06 _exptl_crystal_description sheet _exptl_crystal_colour green _exptl_crystal_size_max .24 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min .5348 _exptl_absorpt_correction_T_max 1.0000 _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 6634 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0846 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.06 _reflns_number_total 4446 _reflns_number_gt 2934 _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^)+(0.0923P)^2^+2.7906P] 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 4446 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0714 _refine_ls_wR_factor_ref 0.2118 _refine_ls_wR_factor_gt 0.1831 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.20148(8) 0.27513(8) 0.16857(8) 0.0414(3) Uani 1 1 d . . . S1 S 0.34950(18) 0.75163(19) 0.59983(17) 0.0537(5) Uani 1 1 d . . . O1 O 0.2969(4) 0.3488(4) 0.2595(4) 0.0442(11) Uani 1 1 d . . . O2 O 0.1053(4) 0.4328(5) 0.2202(5) 0.0522(12) Uani 1 1 d . . . N1 N 0.2506(5) 0.4138(5) 0.9870(5) 0.0418(13) Uani 1 1 d . . . C1 C 0.2029(6) 0.4291(7) 0.2653(6) 0.0409(15) Uani 1 1 d . . . C2 C 0.2101(6) 0.5193(6) 0.3276(6) 0.0408(15) Uani 1 1 d . . . C3 C 0.3226(6) 0.5359(7) 0.3554(6) 0.0480(17) Uani 1 1 d . . . H3A H 0.3944 0.4902 0.3353 0.058 Uiso 1 1 calc R . . C4 C 0.3286(6) 0.6191(7) 0.4124(7) 0.0497(17) Uani 1 1 d . . . H4A H 0.4047 0.6303 0.4287 0.060 Uiso 1 1 calc R . . C5 C 0.2237(6) 0.6862(6) 0.4457(6) 0.0432(16) Uani 1 1 d . . . C6 C 0.1130(7) 0.6655(8) 0.4230(8) 0.066(2) Uani 1 1 d . . . H6A H 0.0410 0.7061 0.4488 0.079 Uiso 1 1 calc R . . C7 C 0.1059(7) 0.5848(9) 0.3619(8) 0.065(2) Uani 1 1 d . . . H7A H 0.0297 0.5754 0.3444 0.078 Uiso 1 1 calc R . . C8 C 0.2274(7) 0.7868(7) 0.4990(7) 0.0514(18) Uani 1 1 d . . . H8A H 0.1500 0.7925 0.5474 0.062 Uiso 1 1 calc R . . H8B H 0.2332 0.8752 0.4276 0.062 Uiso 1 1 calc R . . C9 C 0.3060(6) 0.6171(7) 0.7456(6) 0.0442(16) Uani 1 1 d . . . C10 C 0.3922(6) 0.5557(7) 0.8364(6) 0.0488(17) Uani 1 1 d . . . H10A H 0.4706 0.5820 0.8177 0.059 Uiso 1 1 calc R . . C11 C 0.3611(6) 0.4557(7) 0.9541(6) 0.0482(17) Uani 1 1 d . . . H11A H 0.4202 0.4152 1.0138 0.058 Uiso 1 1 calc R . . C12 C 0.1682(6) 0.4706(7) 0.8984(6) 0.0478(17) Uani 1 1 d . . . H12A H 0.0913 0.4405 0.9193 0.057 Uiso 1 1 calc R . . C13 C 0.1917(6) 0.5722(7) 0.7770(6) 0.0486(17) Uani 1 1 d . . . H13A H 0.1319 0.6093 0.7181 0.058 Uiso 1 1 calc R . . S2 S 0.61545(17) -0.24969(19) 0.2276(2) 0.0565(5) Uani 1 1 d . . . N2 N 0.3361(5) 0.1171(6) 0.1815(5) 0.0459(13) Uani 1 1 d . . . O3 O 1.0724(4) 0.2024(5) 0.1138(4) 0.0500(12) Uani 1 1 d . . . O4 O 1.0890(4) 0.1320(5) 0.3189(4) 0.0533(12) Uani 1 1 d . . . C21 C 1.0429(6) 0.1265(7) 0.2295(6) 0.0434(15) Uani 1 1 d . . . C22 C 0.9553(6) 0.0257(7) 0.2602(6) 0.0475(17) Uani 1 1 d . . . C23 C 0.8978(6) -0.0339(6) 0.3796(6) 0.0400(15) Uani 1 1 d . . . H23A H 0.9119 -0.0110 0.4434 0.048 Uiso 1 1 calc R . . C24 C 0.8179(6) -0.1292(7) 0.4061(6) 0.0452(16) Uani 1 1 d . . . H24A H 0.7777 -0.1678 0.4870 0.054 Uiso 1 1 calc R . . C25 C 0.7981(6) -0.1665(7) 0.3134(7) 0.0477(17) Uani 1 1 d . . . C26 C 0.8578(8) -0.1096(9) 0.1952(8) 0.069(2) Uani 1 1 d . . . H26A H 0.8459 -0.1351 0.1325 0.083 Uiso 1 1 calc R . . C27 C 0.9359(8) -0.0141(9) 0.1680(8) 0.071(2) Uani 1 1 d . . . H27A H 0.9759 0.0240 0.0870 0.086 Uiso 1 1 calc R . . C28 C 0.7152(7) -0.2737(7) 0.3485(8) 0.0566(19) Uani 1 1 d . . . H28A H 0.6643 -0.2797 0.4247 0.068 Uiso 1 1 calc R . . H28B H 0.7661 -0.3601 0.3705 0.068 Uiso 1 1 calc R . . C29 C 0.5113(6) -0.1083(7) 0.2156(6) 0.0450(16) Uani 1 1 d . . . C30 C 0.4156(7) -0.0727(8) 0.1389(7) 0.0562(19) Uani 1 1 d . . . H30A H 0.4079 -0.1245 0.0969 0.067 Uiso 1 1 calc R . . C31 C 0.3318(7) 0.0376(8) 0.1236(7) 0.0552(19) Uani 1 1 d . . . H31A H 0.2686 0.0588 0.0706 0.066 Uiso 1 1 calc R . . C32 C 0.4260(6) 0.0812(7) 0.2586(7) 0.0509(18) Uani 1 1 d . . . H32A H 0.4303 0.1334 0.3013 0.061 Uiso 1 1 calc R . . C33 C 0.5133(6) -0.0293(7) 0.2789(7) 0.0498(17) Uani 1 1 d . . . H33A H 0.5735 -0.0509 0.3352 0.060 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 Ni 0.0448(5) 0.0391(5) 0.0443(5) -0.0197(4) -0.0057(4) -0.0090(4) S1 0.0692(12) 0.0435(10) 0.0523(11) -0.0206(9) 0.0005(9) -0.0210(9) O1 0.043(3) 0.041(3) 0.056(3) -0.028(2) -0.008(2) -0.002(2) O2 0.045(3) 0.051(3) 0.069(3) -0.032(3) -0.014(2) -0.001(2) N1 0.040(3) 0.040(3) 0.045(3) -0.017(3) -0.004(2) -0.008(2) C1 0.039(4) 0.039(4) 0.047(4) -0.021(3) 0.000(3) -0.009(3) C2 0.044(4) 0.031(3) 0.045(4) -0.015(3) -0.001(3) -0.004(3) C3 0.042(4) 0.049(4) 0.060(4) -0.032(4) 0.006(3) -0.006(3) C4 0.043(4) 0.051(4) 0.065(5) -0.035(4) 0.001(3) -0.007(3) C5 0.055(4) 0.026(3) 0.046(4) -0.014(3) -0.003(3) -0.003(3) C6 0.050(4) 0.056(5) 0.109(7) -0.056(5) -0.022(4) 0.018(4) C7 0.044(4) 0.075(6) 0.099(6) -0.059(5) -0.021(4) 0.005(4) C8 0.077(5) 0.029(3) 0.051(4) -0.020(3) -0.009(4) -0.004(3) C9 0.055(4) 0.039(4) 0.047(4) -0.026(3) 0.003(3) -0.014(3) C10 0.045(4) 0.055(5) 0.052(4) -0.027(4) -0.002(3) -0.014(3) C11 0.046(4) 0.055(4) 0.047(4) -0.022(4) -0.009(3) -0.010(3) C12 0.040(4) 0.050(4) 0.055(4) -0.022(4) -0.001(3) -0.012(3) C13 0.049(4) 0.045(4) 0.048(4) -0.014(3) -0.009(3) -0.009(3) S2 0.0507(11) 0.0432(10) 0.0886(14) -0.0386(10) -0.0076(10) -0.0076(8) N2 0.047(3) 0.043(3) 0.053(3) -0.025(3) -0.011(3) -0.002(3) O3 0.055(3) 0.054(3) 0.041(3) -0.016(2) -0.004(2) -0.020(2) O4 0.068(3) 0.054(3) 0.044(3) -0.021(2) -0.002(2) -0.026(3) C21 0.047(4) 0.045(4) 0.044(4) -0.023(3) -0.004(3) -0.010(3) C22 0.045(4) 0.053(4) 0.047(4) -0.022(3) 0.000(3) -0.013(3) C23 0.043(4) 0.039(4) 0.042(4) -0.021(3) -0.005(3) -0.003(3) C24 0.046(4) 0.037(4) 0.044(4) -0.012(3) 0.004(3) -0.007(3) C25 0.046(4) 0.045(4) 0.053(4) -0.021(3) -0.005(3) -0.007(3) C26 0.082(6) 0.088(6) 0.064(5) -0.046(5) 0.005(4) -0.049(5) C27 0.086(6) 0.100(7) 0.052(5) -0.048(5) 0.018(4) -0.051(5) C28 0.054(4) 0.041(4) 0.077(5) -0.025(4) -0.012(4) -0.005(3) C29 0.044(4) 0.042(4) 0.055(4) -0.024(3) -0.001(3) -0.011(3) C30 0.067(5) 0.053(5) 0.070(5) -0.042(4) -0.014(4) -0.006(4) C31 0.062(5) 0.058(5) 0.056(4) -0.031(4) -0.014(4) -0.009(4) C32 0.054(4) 0.049(4) 0.067(5) -0.038(4) -0.015(4) -0.004(3) C33 0.044(4) 0.051(4) 0.064(4) -0.032(4) -0.017(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni N1 2.056(5) 1_554 ? Ni O3 2.057(4) 1_455 ? Ni N2 2.065(5) . ? Ni O1 2.078(4) . ? Ni O2 2.170(5) . ? Ni O4 2.179(4) 1_455 ? Ni C21 2.433(7) 1_455 ? Ni C1 2.443(6) . ? S1 C9 1.766(7) . ? S1 C8 1.798(7) . ? O1 C1 1.266(7) . ? O2 C1 1.256(7) . ? N1 C11 1.331(8) . ? N1 C12 1.337(8) . ? N1 Ni 2.056(5) 1_556 ? C1 C2 1.499(9) . ? C2 C7 1.369(9) . ? C2 C3 1.394(9) . ? C3 C4 1.377(9) . ? C4 C5 1.378(9) . ? C5 C6 1.369(10) . ? C5 C8 1.514(9) . ? C6 C7 1.392(10) . ? C9 C13 1.383(9) . ? C9 C10 1.386(9) . ? C10 C11 1.372(9) . ? C12 C13 1.388(9) . ? S2 C29 1.746(7) . ? S2 C28 1.816(7) . ? N2 C32 1.326(8) . ? N2 C31 1.345(8) . ? O3 C21 1.266(8) . ? O3 Ni 2.057(4) 1_655 ? O4 C21 1.257(7) . ? O4 Ni 2.179(4) 1_655 ? C21 C22 1.499(9) . ? C21 Ni 2.433(7) 1_655 ? C22 C23 1.367(9) . ? C22 C27 1.392(9) . ? C23 C24 1.398(9) . ? C24 C25 1.380(9) . ? C25 C26 1.365(10) . ? C25 C28 1.505(10) . ? C26 C27 1.383(10) . ? C29 C30 1.377(9) . ? C29 C33 1.385(9) . ? C30 C31 1.363(10) . ? C32 C33 1.378(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni O3 95.57(19) 1_554 1_455 ? N1 Ni N2 98.7(2) 1_554 . ? O3 Ni N2 94.0(2) 1_455 . ? N1 Ni O1 94.71(19) 1_554 . ? O3 Ni O1 165.37(18) 1_455 . ? N2 Ni O1 94.66(19) . . ? N1 Ni O2 92.2(2) 1_554 . ? O3 Ni O2 107.10(18) 1_455 . ? N2 Ni O2 155.16(19) . . ? O1 Ni O2 62.08(16) . . ? N1 Ni O4 156.96(19) 1_554 1_455 ? O3 Ni O4 62.30(17) 1_455 1_455 ? N2 Ni O4 89.8(2) . 1_455 ? O1 Ni O4 105.98(17) . 1_455 ? O2 Ni O4 88.70(18) . 1_455 ? N1 Ni C21 126.8(2) 1_554 1_455 ? O3 Ni C21 31.35(18) 1_455 1_455 ? N2 Ni C21 90.8(2) . 1_455 ? O1 Ni C21 136.7(2) . 1_455 ? O2 Ni C21 100.5(2) . 1_455 ? O4 Ni C21 31.02(18) 1_455 1_455 ? N1 Ni C1 94.2(2) 1_554 . ? O3 Ni C1 137.2(2) 1_455 . ? N2 Ni C1 125.4(2) . . ? O1 Ni C1 31.21(18) . . ? O2 Ni C1 30.87(18) . . ? O4 Ni C1 98.29(19) 1_455 . ? C21 Ni C1 121.8(2) 1_455 . ? C9 S1 C8 104.4(3) . . ? C1 O1 Ni 90.5(4) . . ? C1 O2 Ni 86.7(4) . . ? C11 N1 C12 117.4(6) . . ? C11 N1 Ni 122.5(4) . 1_556 ? C12 N1 Ni 120.0(4) . 1_556 ? O2 C1 O1 120.7(6) . . ? O2 C1 C2 120.5(6) . . ? O1 C1 C2 118.8(6) . . ? O2 C1 Ni 62.5(3) . . ? O1 C1 Ni 58.3(3) . . ? C2 C1 Ni 177.0(5) . . ? C7 C2 C3 118.1(6) . . ? C7 C2 C1 120.9(6) . . ? C3 C2 C1 121.0(6) . . ? C4 C3 C2 120.8(6) . . ? C3 C4 C5 121.1(6) . . ? C6 C5 C4 118.1(6) . . ? C6 C5 C8 119.4(6) . . ? C4 C5 C8 122.4(6) . . ? C5 C6 C7 121.4(7) . . ? C2 C7 C6 120.6(7) . . ? C5 C8 S1 116.6(5) . . ? C13 C9 C10 118.0(6) . . ? C13 C9 S1 125.0(5) . . ? C10 C9 S1 117.0(5) . . ? C11 C10 C9 119.5(6) . . ? N1 C11 C10 123.2(6) . . ? N1 C12 C13 123.3(6) . . ? C9 C13 C12 118.5(6) . . ? C29 S2 C28 104.2(3) . . ? C32 N2 C31 116.4(6) . . ? C32 N2 Ni 120.6(4) . . ? C31 N2 Ni 122.7(5) . . ? C21 O3 Ni 90.9(4) . 1_655 ? C21 O4 Ni 85.7(4) . 1_655 ? O4 C21 O3 120.8(6) . . ? O4 C21 C22 119.5(6) . . ? O3 C21 C22 119.6(6) . . ? O4 C21 Ni 63.3(3) . 1_655 ? O3 C21 Ni 57.7(3) . 1_655 ? C22 C21 Ni 173.4(5) . 1_655 ? C23 C22 C27 118.7(6) . . ? C23 C22 C21 121.4(6) . . ? C27 C22 C21 119.8(6) . . ? C22 C23 C24 120.2(6) . . ? C25 C24 C23 120.6(6) . . ? C26 C25 C24 119.2(6) . . ? C26 C25 C28 122.2(7) . . ? C24 C25 C28 118.5(6) . . ? C25 C26 C27 120.4(7) . . ? C26 C27 C22 120.9(7) . . ? C25 C28 S2 116.6(5) . . ? C30 C29 C33 115.9(6) . . ? C30 C29 S2 117.7(5) . . ? C33 C29 S2 126.3(5) . . ? C31 C30 C29 120.9(6) . . ? N2 C31 C30 123.1(7) . . ? N2 C32 C33 123.4(6) . . ? C32 C33 C29 120.1(6) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.074 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.107