# Copyright The Royal Society of Chemistry, 1998 # MANUSCRIPT 8/03489C # CIF file of [(CH3CN)Co(4-mpyt)4Pt]CH3CN (1) data_PtCo #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jul 22 11:34:35 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 832.85 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H30 Co N6 Pt S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 21.381(4) _cell_length_b 18.292(4) _cell_length_c 16.692(5) _cell_angle_alpha 89 _cell_angle_beta 89 _cell_angle_gamma 90 _cell_volume 6527(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 11.7 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prizmatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3272.00 _exptl_absorpt_coefficient_mu 5.056 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.998 _exptl_absorpt_correction_T_min 0.791 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC5S' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.69 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 4 3 -2 1 3 4 2 _diffrn_reflns_number 10294 _reflns_number_total 10294 _reflns_number_observed 2876 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI 0.258 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 29.94 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04329 _diffrn_orient_matrix_UB_12 0.01720 _diffrn_orient_matrix_UB_13 0.01319 _diffrn_orient_matrix_UB_21 -0.01564 _diffrn_orient_matrix_UB_22 0.05150 _diffrn_orient_matrix_UB_23 0.00346 _diffrn_orient_matrix_UB_31 -0.00884 _diffrn_orient_matrix_UB_32 -0.00696 _diffrn_orient_matrix_UB_33 0.05851 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Co 0 8 0.349 0.972 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Pt 0 8 -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N 0 48 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 32 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 224 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 240 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Pt1 0.21670(3) 0.11845(3) 0.20516(4) 0.0331(1) Uani d . 1.00 . Co2 0.2331(1) 0.2160(1) 0.3142(1) 0.0331(6) Uani d . 1.00 . S1 0.2812(2) 0.0390(2) 0.2760(3) 0.043(1) Uani d . 1.00 . S2 0.1299(2) 0.0761(2) 0.2756(3) 0.040(1) Uani d . 1.00 . S3 0.1545(2) 0.1998(2) 0.1338(3) 0.042(1) Uani d . 1.00 . S4 0.3045(2) 0.1610(2) 0.1367(3) 0.040(1) Uani d . 1.00 . N1 0.3237(6) 0.1673(7) 0.3358(8) 0.037(4) Uani d . 1.00 . N2 0.1892(6) 0.1437(7) 0.3980(8) 0.036(4) Uani d . 1.00 . N3 0.1424(6) 0.2591(7) 0.2812(9) 0.040(4) Uani d . 1.00 . N4 0.2747(6) 0.2830(6) 0.2215(7) 0.040(4) Uani d . 1.00 . N5 0.2460(7) 0.3019(8) 0.4022(9) 0.051(5) Uani d . 1.00 . N6 0.481(2) 0.318(2) 0.510(2) 0.18(2) Uani d . 1.00 . C1 0.3386(9) 0.0969(9) 0.319(1) 0.047(6) Uani d . 1.00 . C2 0.3976(9) 0.0672(9) 0.339(1) 0.041(6) Uani d . 1.00 . C3 0.4437(8) 0.107(1) 0.370(1) 0.051(6) Uani d . 1.00 . C4 0.4300(8) 0.181(1) 0.387(1) 0.051(6) Uani d . 1.00 . C5 0.3704(8) 0.2093(9) 0.367(1) 0.044(6) Uani d . 1.00 . C6 0.5056(9) 0.076(1) 0.390(1) 0.076(8) Uani d . 1.00 . C7 0.1469(8) 0.0903(8) 0.3776(10) 0.033(5) Uani d . 1.00 . C8 0.1150(7) 0.0499(8) 0.436(1) 0.035(5) Uani d . 1.00 . C9 0.1284(9) 0.059(1) 0.516(1) 0.050(6) Uani d . 1.00 . C10 0.1714(9) 0.111(1) 0.538(1) 0.052(6) Uani d . 1.00 . C11 0.2011(8) 0.1527(10) 0.478(1) 0.048(6) Uani d . 1.00 . C12 0.093(1) 0.015(1) 0.579(1) 0.082(8) Uani d . 1.00 . C13 0.1179(7) 0.2548(8) 0.204(1) 0.037(5) Uani d . 1.00 . C14 0.0649(8) 0.2960(10) 0.184(1) 0.046(6) Uani d . 1.00 . C15 0.0337(10) 0.3380(9) 0.239(2) 0.060(7) Uani d . 1.00 . C16 0.0567(10) 0.340(1) 0.318(1) 0.063(8) Uani d . 1.00 . C17 0.1083(8) 0.298(1) 0.334(1) 0.052(6) Uani d . 1.00 . C18 -0.0248(9) 0.379(1) 0.213(2) 0.092(9) Uani d . 1.00 . C19 0.3060(7) 0.2558(9) 0.1579(9) 0.030(5) Uani d . 1.00 . C20 0.3409(8) 0.2989(8) 0.1051(9) 0.033(5) Uani d . 1.00 . C21 0.3416(8) 0.3738(9) 0.1158(9) 0.039(5) Uani d . 1.00 . C22 0.3090(9) 0.4027(8) 0.178(1) 0.051(6) Uani d . 1.00 . C23 0.2768(9) 0.3577(8) 0.2289(9) 0.042(5) Uani d . 1.00 . C24 0.377(1) 0.4237(10) 0.060(1) 0.077(8) Uani d . 1.00 . C25 0.240(1) 0.4281(10) 0.470(1) 0.083(8) Uani d . 1.00 . C26 0.2450(9) 0.3556(10) 0.432(1) 0.047(6) Uani d . 1.00 . C27 0.4773(10) 0.339(1) 0.659(2) 0.077(9) Uani d . 1.00 . C28 0.481(1) 0.329(1) 0.572(2) 0.10(1) Uani d . 1.00 . H1 0.4046 0.0145 0.3294 0.0497 Uiso calc . 1.00 . H2 0.4608 0.2137 0.4127 0.0613 Uiso calc . 1.00 . H3 0.3618 0.2623 0.3742 0.0511 Uiso calc . 1.00 . H4 0.5023 0.0374 0.4296 0.0864 Uiso calc . 1.00 . H5 0.5259 0.0554 0.3440 0.0864 Uiso calc . 1.00 . H6 0.5335 0.1122 0.4123 0.0864 Uiso calc . 1.00 . H7 0.0829 0.0136 0.4190 0.0449 Uiso calc . 1.00 . H8 0.1805 0.1201 0.5938 0.0602 Uiso calc . 1.00 . H9 0.2329 0.1880 0.4948 0.0559 Uiso calc . 1.00 . H10 0.0485 0.0238 0.5769 0.0874 Uiso calc . 1.00 . H11 0.0989 -0.0371 0.5722 0.0874 Uiso calc . 1.00 . H12 0.1066 0.0268 0.6325 0.0874 Uiso calc . 1.00 . H13 0.0493 0.2934 0.1274 0.0543 Uiso calc . 1.00 . H14 0.0352 0.3693 0.3593 0.0733 Uiso calc . 1.00 . H15 0.1219 0.2956 0.3915 0.0661 Uiso calc . 1.00 . H16 -0.0421 0.4068 0.2579 0.1006 Uiso calc . 1.00 . H17 -0.0172 0.4133 0.1709 0.1006 Uiso calc . 1.00 . H18 -0.0574 0.3464 0.1956 0.1006 Uiso calc . 1.00 . H19 0.3644 0.2759 0.0619 0.0385 Uiso calc . 1.00 . H20 0.3094 0.4552 0.1878 0.0595 Uiso calc . 1.00 . H21 0.2519 0.3794 0.2730 0.0477 Uiso calc . 1.00 . H22 0.4085 0.4522 0.0870 0.0857 Uiso calc . 1.00 . H23 0.3985 0.3966 0.0179 0.0857 Uiso calc . 1.00 . H24 0.3496 0.4578 0.0330 0.0857 Uiso calc . 1.00 . H25 0.2793 0.4400 0.4989 0.0899 Uiso calc . 1.00 . H26 0.2342 0.4662 0.4321 0.0899 Uiso calc . 1.00 . H27 0.2077 0.4303 0.5091 0.0899 Uiso calc . 1.00 . H28 0.5128 0.3635 0.6845 0.0882 Uiso calc . 1.00 . H29 0.4404 0.3659 0.6782 0.0882 Uiso calc . 1.00 . H30 0.4744 0.2917 0.6901 0.0882 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt(1) 0.0376(3) 0.0255(3) 0.0362(3) -0.0022(4) -0.0023(4) -0.0067(3) Co(2) 0.036(1) 0.028(1) 0.035(1) -0.0024(9) -0.001(1) -0.0058(9) S(1) 0.046(3) 0.029(2) 0.054(3) -0.001(2) -0.006(3) -0.003(2) S(2) 0.037(3) 0.038(2) 0.045(3) -0.008(2) -0.003(2) -0.008(2) S(3) 0.047(3) 0.041(3) 0.038(3) 0.001(2) -0.002(2) -0.005(2) S(4) 0.048(3) 0.029(2) 0.042(3) 0.002(2) 0.009(2) -0.010(2) N(1) 0.039(9) 0.035(8) 0.037(9) -0.004(7) 0.006(7) 0.010(7) N(2) 0.031(8) 0.035(8) 0.041(9) 0.015(7) -0.003(7) -0.008(7) N(3) 0.027(7) 0.038(8) 0.05(1) 0.002(6) 0.009(8) 0.002(7) N(4) 0.05(1) 0.031(7) 0.036(9) -0.006(7) -0.003(8) -0.001(6) N(5) 0.05(1) 0.047(10) 0.05(1) -0.008(9) 0.004(9) -0.007(9) N(6) 0.18(3) 0.20(3) 0.16(3) -0.09(2) 0.07(3) -0.10(3) C(1) 0.05(1) 0.04(1) 0.05(1) -0.013(9) 0.004(10) 0.011(8) C(2) 0.04(1) 0.05(1) 0.04(1) 0.019(9) 0.010(10) -0.005(9) C(3) 0.04(1) 0.07(1) 0.05(1) -0.01(1) -0.001(10) -0.01(1) C(4) 0.03(1) 0.08(2) 0.04(1) -0.02(1) -0.017(10) -0.01(1) C(5) 0.05(1) 0.05(1) 0.03(1) -0.034(10) 0.010(9) -0.004(9) C(6) 0.03(1) 0.12(2) 0.08(2) 0.01(1) 0.00(1) -0.01(2) C(7) 0.027(10) 0.032(9) 0.04(1) -0.004(8) -0.001(9) -0.011(8) C(8) 0.023(9) 0.023(8) 0.06(1) 0.001(7) 0.016(9) 0.014(8) C(9) 0.06(1) 0.05(1) 0.04(1) 0.00(1) -0.01(1) -0.003(10) C(10) 0.06(1) 0.06(1) 0.04(1) 0.02(1) -0.016(10) 0.01(1) C(11) 0.05(1) 0.05(1) 0.04(1) -0.001(10) -0.005(10) -0.014(10) C(12) 0.10(2) 0.08(2) 0.06(1) -0.02(1) 0.01(1) 0.03(1) C(13) 0.036(9) 0.045(9) 0.030(9) -0.002(8) -0.012(10) -0.018(9) C(14) 0.028(10) 0.06(1) 0.05(1) 0.005(9) 0.000(9) 0.017(9) C(15) 0.04(1) 0.033(10) 0.10(2) 0.00(1) 0.00(1) 0.00(1) C(16) 0.05(1) 0.05(1) 0.09(2) 0.00(1) 0.01(1) 0.00(1) C(17) 0.03(1) 0.05(1) 0.07(1) -0.002(10) 0.00(1) -0.01(1) C(18) 0.05(1) 0.11(2) 0.11(2) 0.04(1) 0.01(1) -0.01(2) C(19) 0.026(9) 0.041(9) 0.024(9) 0.003(8) -0.018(7) -0.001(8) C(20) 0.05(1) 0.029(9) 0.025(9) 0.001(8) 0.007(8) -0.013(7) C(21) 0.05(1) 0.034(10) 0.028(9) -0.004(9) 0.008(8) -0.005(8) C(22) 0.08(1) 0.022(8) 0.06(1) -0.004(9) 0.00(1) -0.006(8) C(23) 0.07(1) 0.026(7) 0.032(9) 0.008(9) -0.007(10) -0.013(6) C(24) 0.11(2) 0.04(1) 0.08(2) -0.02(1) 0.04(2) -0.02(1) C(25) 0.17(2) 0.028(10) 0.05(1) 0.01(1) 0.00(2) -0.003(9) C(26) 0.07(1) 0.04(1) 0.04(1) 0.00(1) 0.00(1) 0.007(9) C(27) 0.04(1) 0.09(2) 0.10(2) 0.03(1) -0.01(1) 0.00(1) C(28) 0.08(2) 0.05(1) 0.16(3) -0.03(1) 0.00(2) -0.04(2) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00063|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2876 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0514 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0574 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.175 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -1.55 _refine_diff_density_max 0.94 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt(1) Co(2) 2.573(2) 1_555 1_555 yes Pt(1) S(1) 2.328(4) 1_555 1_555 yes Pt(1) S(2) 2.329(4) 1_555 1_555 yes Pt(1) S(3) 2.323(5) 1_555 1_555 yes Pt(1) S(4) 2.331(4) 1_555 1_555 yes Co(2) N(1) 2.16(1) 1_555 1_555 yes Co(2) N(2) 2.14(1) 1_555 1_555 yes Co(2) N(3) 2.16(1) 1_555 1_555 yes Co(2) N(4) 2.16(1) 1_555 1_555 yes Co(2) N(5) 2.17(2) 1_555 1_555 yes S(1) C(1) 1.77(2) 1_555 1_555 yes S(2) C(7) 1.76(2) 1_555 1_555 yes S(3) C(13) 1.74(2) 1_555 1_555 yes S(4) C(19) 1.77(2) 1_555 1_555 yes N(1) C(1) 1.35(2) 1_555 1_555 yes N(1) C(5) 1.36(2) 1_555 1_555 yes N(2) C(7) 1.37(2) 1_555 1_555 yes N(2) C(11) 1.36(2) 1_555 1_555 yes N(3) C(13) 1.39(2) 1_555 1_555 yes N(3) C(17) 1.35(2) 1_555 1_555 yes N(4) C(19) 1.35(2) 1_555 1_555 yes N(4) C(23) 1.37(2) 1_555 1_555 yes N(5) C(26) 1.10(2) 1_555 1_555 yes N(6) C(28) 1.07(4) 1_555 1_555 yes C(1) C(2) 1.41(2) 1_555 1_555 yes C(2) C(3) 1.33(2) 1_555 1_555 yes C(3) C(4) 1.42(2) 1_555 1_555 yes C(3) C(6) 1.48(2) 1_555 1_555 yes C(4) C(5) 1.41(2) 1_555 1_555 yes C(7) C(8) 1.39(2) 1_555 1_555 yes C(8) C(9) 1.38(2) 1_555 1_555 yes C(9) C(10) 1.38(2) 1_555 1_555 yes C(9) C(12) 1.53(2) 1_555 1_555 yes C(10) C(11) 1.41(2) 1_555 1_555 yes C(13) C(14) 1.40(2) 1_555 1_555 yes C(14) C(15) 1.38(2) 1_555 1_555 yes C(15) C(16) 1.41(3) 1_555 1_555 yes C(15) C(18) 1.53(2) 1_555 1_555 yes C(16) C(17) 1.37(3) 1_555 1_555 yes C(19) C(20) 1.40(2) 1_555 1_555 yes C(20) C(21) 1.38(2) 1_555 1_555 yes C(21) C(22) 1.36(2) 1_555 1_555 yes C(21) C(24) 1.51(2) 1_555 1_555 yes C(22) C(23) 1.37(2) 1_555 1_555 yes C(25) C(26) 1.47(2) 1_555 1_555 yes C(27) C(28) 1.47(3) 1_555 1_555 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Co(2) Pt(1) S(1) 89.6(1) 1_555 1_555 1_555 yes Co(2) Pt(1) S(2) 89.0(1) 1_555 1_555 1_555 yes Co(2) Pt(1) S(3) 89.8(1) 1_555 1_555 1_555 yes Co(2) Pt(1) S(4) 90.3(1) 1_555 1_555 1_555 yes S(1) Pt(1) S(2) 90.4(2) 1_555 1_555 1_555 yes S(1) Pt(1) S(3) 178.5(2) 1_555 1_555 1_555 yes S(1) Pt(1) S(4) 88.9(2) 1_555 1_555 1_555 yes S(2) Pt(1) S(3) 90.9(2) 1_555 1_555 1_555 yes S(2) Pt(1) S(4) 179.0(2) 1_555 1_555 1_555 yes S(3) Pt(1) S(4) 89.7(2) 1_555 1_555 1_555 yes Pt(1) Co(2) N(1) 87.4(4) 1_555 1_555 1_555 yes Pt(1) Co(2) N(2) 88.5(4) 1_555 1_555 1_555 yes Pt(1) Co(2) N(3) 87.1(4) 1_555 1_555 1_555 yes Pt(1) Co(2) N(4) 86.7(3) 1_555 1_555 1_555 yes Pt(1) Co(2) N(5) 177.5(4) 1_555 1_555 1_555 yes N(1) Co(2) N(2) 91.6(5) 1_555 1_555 1_555 yes N(1) Co(2) N(3) 174.2(5) 1_555 1_555 1_555 yes N(1) Co(2) N(4) 89.1(5) 1_555 1_555 1_555 yes N(1) Co(2) N(5) 94.1(6) 1_555 1_555 1_555 yes N(2) Co(2) N(3) 89.9(5) 1_555 1_555 1_555 yes N(2) Co(2) N(4) 175.1(5) 1_555 1_555 1_555 yes N(2) Co(2) N(5) 93.5(5) 1_555 1_555 1_555 yes N(3) Co(2) N(4) 88.9(5) 1_555 1_555 1_555 yes N(3) Co(2) N(5) 91.3(6) 1_555 1_555 1_555 yes N(4) Co(2) N(5) 91.3(5) 1_555 1_555 1_555 yes Pt(1) S(1) C(1) 104.1(6) 1_555 1_555 1_555 yes Pt(1) S(2) C(7) 106.0(6) 1_555 1_555 1_555 yes Pt(1) S(3) C(13) 106.4(6) 1_555 1_555 1_555 yes Pt(1) S(4) C(19) 104.2(6) 1_555 1_555 1_555 yes Co(2) N(1) C(1) 124(1) 1_555 1_555 1_555 yes Co(2) N(1) C(5) 119(1) 1_555 1_555 1_555 yes C(1) N(1) C(5) 116(1) 1_555 1_555 1_555 yes Co(2) N(2) C(7) 124(1) 1_555 1_555 1_555 yes Co(2) N(2) C(11) 118(1) 1_555 1_555 1_555 yes C(7) N(2) C(11) 116(1) 1_555 1_555 1_555 yes Co(2) N(3) C(13) 123(1) 1_555 1_555 1_555 yes Co(2) N(3) C(17) 120(1) 1_555 1_555 1_555 yes C(13) N(3) C(17) 115(1) 1_555 1_555 1_555 yes Co(2) N(4) C(19) 123(1) 1_555 1_555 1_555 yes Co(2) N(4) C(23) 120(1) 1_555 1_555 1_555 yes C(19) N(4) C(23) 114(1) 1_555 1_555 1_555 yes Co(2) N(5) C(26) 162(1) 1_555 1_555 1_555 yes S(1) C(1) N(1) 119(1) 1_555 1_555 1_555 yes S(1) C(1) C(2) 118(1) 1_555 1_555 1_555 yes N(1) C(1) C(2) 121(1) 1_555 1_555 1_555 yes C(1) C(2) C(3) 122(1) 1_555 1_555 1_555 yes C(1) C(2) H(1) 118(1) 1_555 1_555 1_555 no C(3) C(2) H(1) 119(1) 1_555 1_555 1_555 no C(2) C(3) C(4) 117(1) 1_555 1_555 1_555 yes C(2) C(3) C(6) 122(1) 1_555 1_555 1_555 yes C(4) C(3) C(6) 120(1) 1_555 1_555 1_555 yes C(3) C(4) C(5) 118(1) 1_555 1_555 1_555 yes C(3) C(4) H(2) 121(1) 1_555 1_555 1_555 no C(5) C(4) H(2) 119(2) 1_555 1_555 1_555 no N(1) C(5) C(4) 123(1) 1_555 1_555 1_555 yes N(1) C(5) H(3) 117(1) 1_555 1_555 1_555 no C(4) C(5) H(3) 119(1) 1_555 1_555 1_555 no C(3) C(6) H(4) 111(1) 1_555 1_555 1_555 no C(3) C(6) H(5) 111(1) 1_555 1_555 1_555 no C(3) C(6) H(6) 112(1) 1_555 1_555 1_555 no H(4) C(6) H(5) 106(2) 1_555 1_555 1_555 no H(4) C(6) H(6) 107(2) 1_555 1_555 1_555 no H(5) C(6) H(6) 107(1) 1_555 1_555 1_555 no S(2) C(7) N(2) 118(1) 1_555 1_555 1_555 yes S(2) C(7) C(8) 119(1) 1_555 1_555 1_555 yes N(2) C(7) C(8) 121(1) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120(1) 1_555 1_555 1_555 yes C(7) C(8) H(7) 119(1) 1_555 1_555 1_555 no C(1) C(2) C(3) 120.4(6) 1_555 1_555 1_555 yes C(1) C(2) H(1) 118.0(6) 1_555 1_555 1_555 no C(3) C(2) H(1) 120.7(6) 1_555 1_555 1_555 no C(2) C(3) C(4) 118.2(6) 1_555 1_555 1_555 yes C(2) C(3) C(6) 120.9(7) 1_555 1_555 1_555 yes C(4) C(3) C(6) 120.8(7) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.0(6) 1_555 1_555 1_555 yes C(3) C(4) H(2) 120.9(7) 1_555 1_555 1_555 no C(5) C(4) H(2) 120.1(7) 1_555 1_555 1_555 no N(1) C(5) C(4) 123.3(6) 1_555 1_555 1_555 yes N(1) C(5) H(3) 118.9(6) 1_555 1_555 1_555 no C(4) C(5) H(3) 117.3(6) 1_555 1_555 1_555 no C(3) C(6) H(4) 105.7(8) 1_555 1_555 1_555 no C(3) C(6) H(5) 111.0(7) 1_555 1_555 1_555 no C(3) C(6) H(6) 111.7(8) 1_555 1_555 1_555 no H(4) C(6) H(5) 106.2(9) 1_555 1_555 1_555 no H(4) C(6) H(6) 106.0(8) 1_555 1_555 1_555 no H(5) C(6) H(6) 115.4(10) 1_555 1_555 1_555 no S(2) C(7) N(2) 119.9(4) 1_555 1_555 1_555 yes S(2) C(7) C(8) 118.2(4) 1_555 1_555 1_555 yes N(2) C(7) C(8) 121.9(5) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120.8(6) 1_555 1_555 1_555 yes C(7) C(8) H(7) 120.9(6) 1_555 1_555 1_555 no C(9) C(8) H(7) 116.5(6) 1_555 1_555 1_555 no C(8) C(9) C(10) 117.0(6) 1_555 1_555 1_555 yes C(8) C(9) C(12) 121.9(6) 1_555 1_555 1_555 yes C(10) C(9) C(12) 121.1(6) 1_555 1_555 1_555 yes C(9) C(10) C(11) 119.9(6) 1_555 1_555 1_555 yes C(9) C(10) H(8) 113.3(6) 1_555 1_555 1_555 no C(11) C(10) H(8) 126.5(7) 1_555 1_555 1_555 no N(2) C(11) C(10) 123.5(6) 1_555 1_555 1_555 yes N(2) C(11) H(9) 118.8(6) 1_555 1_555 1_555 no C(10) C(11) H(9) 117.7(6) 1_555 1_555 1_555 no C(9) C(12) H(10) 108.1(7) 1_555 1_555 1_555 no C(9) C(12) H(11) 108.4(7) 1_555 1_555 1_555 no C(9) C(12) H(12) 110.9(7) 1_555 1_555 1_555 no H(10) C(12) H(11) 107.8(8) 1_555 1_555 1_555 no H(10) C(12) H(12) 110.8(8) 1_555 1_555 1_555 no H(11) C(12) H(12) 110.7(8) 1_555 1_555 1_555 no S(3) C(13) N(3) 119.3(4) 1_555 1_555 1_555 yes S(3) C(13) C(14) 117.9(5) 1_555 1_555 1_555 yes N(3) C(13) C(14) 122.8(5) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120.9(6) 1_555 1_555 1_555 yes C(13) C(14) H(13) 122.8(6) 1_555 1_555 1_555 no C(15) C(14) H(13) 115.9(6) 1_555 1_555 1_555 no C(14) C(15) C(16) 117.0(6) 1_555 1_555 1_555 yes C(14) C(15) C(18) 121.7(7) 1_555 1_555 1_555 yes C(16) C(15) C(18) 121.3(6) 1_555 1_555 1_555 yes C(15) C(16) C(17) 119.5(6) 1_555 1_555 1_555 yes C(15) C(16) H(14) 131.5(7) 1_555 1_555 1_555 no C(17) C(16) H(14) 108.0(6) 1_555 1_555 1_555 no N(3) C(17) C(16) 123.5(6) 1_555 1_555 1_555 yes N(3) C(17) H(15) 120.5(6) 1_555 1_555 1_555 no C(16) C(17) H(15) 116.0(6) 1_555 1_555 1_555 no C(15) C(18) H(16) 110.5(7) 1_555 1_555 1_555 no C(15) C(18) H(17) 111.5(7) 1_555 1_555 1_555 no C(15) C(18) H(18) 111.7(8) 1_555 1_555 1_555 no H(16) C(18) H(17) 107.1(8) 1_555 1_555 1_555 no H(16) C(18) H(18) 106.9(8) 1_555 1_555 1_555 no H(17) C(18) H(18) 108.9(8) 1_555 1_555 1_555 no S(4) C(19) N(4) 119.4(4) 1_555 1_555 1_555 yes S(4) C(19) C(20) 118.4(4) 1_555 1_555 1_555 yes N(4) C(19) C(20) 122.1(5) 1_555 1_555 1_555 yes C(19) C(20) C(21) 120.4(5) 1_555 1_555 1_555 yes C(19) C(20) H(19) 112.5(5) 1_555 1_555 1_555 no C(21) C(20) H(19) 126.7(6) 1_555 1_555 1_555 no C(20) C(21) C(22) 117.9(5) 1_555 1_555 1_555 yes C(20) C(21) C(24) 121.6(6) 1_555 1_555 1_555 yes C(22) C(21) C(24) 120.6(5) 1_555 1_555 1_555 yes C(21) C(22) C(23) 119.8(5) 1_555 1_555 1_555 yes C(21) C(22) H(20) 128.3(6) 1_555 1_555 1_555 no C(23) C(22) H(20) 111.7(6) 1_555 1_555 1_555 no N(4) C(23) C(22) 123.8(5) 1_555 1_555 1_555 yes N(4) C(23) H(21) 108.3(5) 1_555 1_555 1_555 no C(22) C(23) H(21) 127.9(6) 1_555 1_555 1_555 no C(21) C(24) H(22) 113.1(6) 1_555 1_555 1_555 no C(21) C(24) H(23) 112.7(7) 1_555 1_555 1_555 no C(21) C(24) H(24) 104.4(7) 1_555 1_555 1_555 no H(22) C(24) H(23) 108.1(7) 1_555 1_555 1_555 no H(22) C(24) H(24) 125.4(9) 1_555 1_555 1_555 no H(23) C(24) H(24) 91.1(6) 1_555 1_555 1_555 no C(26) C(25) H(25) 110.0(7) 1_555 1_555 1_555 no C(26) C(25) H(26) 110.8(7) 1_555 1_555 1_555 no C(26) C(25) H(27) 109.4(8) 1_555 1_555 1_555 no H(25) C(25) H(26) 109.7(9) 1_555 1_555 1_555 no H(25) C(25) H(27) 107.9(8) 1_555 1_555 1_555 no H(26) C(25) H(27) 109.0(7) 1_555 1_555 1_555 no N(5) C(26) C(25) 174.6(7) 1_555 1_555 1_555 yes C(28) C(27) H(28) 110.0(9) 1_555 1_555 1_555 no C(28) C(27) H(29) 114.5(9) 1_555 1_555 1_555 no C(28) C(27) H(30) 110.1(8) 1_555 1_555 1_555 no H(28) C(27) H(29) 109.0(8) 1_555 1_555 1_555 no H(28) C(27) H(30) 103.8(9) 1_555 1_555 1_555 no H(29) C(27) H(30) 108.9(9) 1_555 1_555 1_555 no N(6) C(28) C(27) 176(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt Ni 2.5314(7) 1_555 1_555 ? S(3) C(22) 3.517(6) 1_555 6_545 ? S(4) C(25) 3.527(8) 1_555 7_554 ? N(6) C(16) 3.48(1) 1_555 2_456 ? C(15) C(24) 3.522(10) 1_555 7_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_contact_author ; Isamu Kinoshita Graduate School of Science, Osaka City University, Sumiyoshi-ku, Osaka 558-8 585, JAPAN ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+81-6-605-3146' _publ_contact_author_fax '+81-6-690-2753' _publ_contact_author_email 'isamu@sci.osaka-cu.ac.jp' loop_ _publ_author_name 'Ken'ichi Kitano' _publ_author_address ; 'Graduate School of Science, Osaka City University, Sumiyoshi-ku, Osaka 558- 8585, JAPAN' ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END # CIF file of [(CH3CN)Ni(4-mpyt)4Pt]CH3CN (3) data_[Pt(4-mpyt)4Ni(NCMe)]MeCN #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jun 27 16:58:58 1997' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 832.62 _chemical_formula_analytical ? _chemical_formula_sum 'C28 H30 N6 Ni Pt S4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 21.362(3) _cell_length_b 18.237(2) _cell_length_c 16.608(2) _cell_angle_alpha 89 _cell_angle_beta 89 _cell_angle_gamma 90 _cell_volume 6470(2) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.7 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_Int_Tables_number 61 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' '1/2-x, -y,1/2+z' ' -x, -y, -z' '1/2-x,1/2+y, +z' ' +x,1/2-y,1/2+z' '1/2+x, +y,1/2-z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_meas 'not measured' _exptl_crystal_F_000 3280.00 _exptl_absorpt_coefficient_mu 5.170 _exptl_absorpt_correction_type '\y scans(North,Phillips & Mathews,1968)' _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_correction_T_min 0.618 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 7.04 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -2 -2 -3 0 -4 -2 -2 -2 -1 _diffrn_reflns_number 10275 _reflns_number_total 10272 _reflns_number_observed 5375 _reflns_observed_criterion >3.0sigma(I) _diffrn_reflns_av_R_equivalents 50.97 _diffrn_reflns_av_sigmaI/netI 0.074 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04208 _diffrn_orient_matrix_UB_12 -0.02400 _diffrn_orient_matrix_UB_13 -0.00112 _diffrn_orient_matrix_UB_21 0.02043 _diffrn_orient_matrix_UB_22 -0.04927 _diffrn_orient_matrix_UB_23 0.00277 _diffrn_orient_matrix_UB_31 -0.00172 _diffrn_orient_matrix_UB_32 0.00182 _diffrn_orient_matrix_UB_33 0.06014 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pt 0 8 -1.703 8.390 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni 0 8 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; C 0 224 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H 0 240 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N 0 48 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S 0 32 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ loop_ _atom_site_label _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_calc_flag _atom_site_calc_attached_atom _atom_site_occupancy _atom_site_refinement_flags Pt 0.21823(1) 0.11854(1) 0.20351(1) 0.03340(5) Uani d . 1.00 . Ni 0.23347(3) 0.21515(4) 0.31119(4) 0.0329(2) Uani d . 1.00 . S1 0.15724(8) 0.20048(8) 0.13082(9) 0.0421(4) Uani d . 1.00 . S2 0.13062(7) 0.07685(8) 0.27246(10) 0.0428(4) Uani d . 1.00 . S3 0.28172(8) 0.03894(7) 0.27607(10) 0.0435(4) Uani d . 1.00 . S4 0.30667(7) 0.16072(7) 0.13686(9) 0.0396(4) Uani d . 1.00 . N1 0.1438(2) 0.2577(2) 0.2800(3) 0.040(1) Uani d . 1.00 . N2 0.1908(2) 0.1445(2) 0.3950(3) 0.037(1) Uani d . 1.00 . N3 0.3224(2) 0.1683(2) 0.3347(3) 0.038(1) Uani d . 1.00 . N4 0.2745(2) 0.2818(2) 0.2206(3) 0.034(1) Uani d . 1.00 . N5 0.2455(3) 0.2996(3) 0.3975(3) 0.045(1) Uani d . 1.00 . N6 -0.0160(6) 0.1781(6) 0.4878(6) 0.161(5) Uani d . 1.00 . C1 0.1211(3) 0.2552(3) 0.2037(4) 0.040(2) Uani d . 1.00 . C2 0.0680(3) 0.2955(3) 0.1814(4) 0.047(2) Uani d . 1.00 . C3 0.0358(3) 0.3360(4) 0.2378(5) 0.058(2) Uani d . 1.00 . C4 0.0572(3) 0.3351(4) 0.3170(4) 0.060(2) Uani d . 1.00 . C5 0.1108(3) 0.2959(4) 0.3353(4) 0.050(2) Uani d . 1.00 . C6 -0.0237(4) 0.3780(5) 0.2149(6) 0.090(3) Uani d . 1.00 . C7 0.1489(3) 0.0918(3) 0.3745(4) 0.037(1) Uani d . 1.00 . C8 0.1175(3) 0.0506(3) 0.4323(4) 0.044(2) Uani d . 1.00 . C9 0.1295(3) 0.0604(3) 0.5131(4) 0.048(2) Uani d . 1.00 . C10 0.1743(3) 0.1123(4) 0.5335(4) 0.054(2) Uani d . 1.00 . C11 0.2038(3) 0.1519(4) 0.4740(4) 0.047(2) Uani d . 1.00 . C12 0.0966(4) 0.0161(4) 0.5769(5) 0.078(3) Uani d . 1.00 . C13 0.3376(3) 0.0974(3) 0.3203(3) 0.038(1) Uani d . 1.00 . C14 0.3954(3) 0.0682(3) 0.3392(4) 0.046(2) Uani d . 1.00 . C15 0.4418(3) 0.1114(4) 0.3721(4) 0.050(2) Uani d . 1.00 . C16 0.4272(3) 0.1853(4) 0.3856(4) 0.051(2) Uani d . 1.00 . C17 0.3685(3) 0.2112(3) 0.3660(4) 0.045(2) Uani d . 1.00 . C18 0.5046(3) 0.0809(5) 0.3932(5) 0.078(3) Uani d . 1.00 . C19 0.3082(3) 0.2548(3) 0.1570(3) 0.032(1) Uani d . 1.00 . C20 0.3423(3) 0.2998(3) 0.1064(3) 0.041(2) Uani d . 1.00 . C21 0.3430(3) 0.3748(3) 0.1183(3) 0.042(2) Uani d . 1.00 . C22 0.3076(3) 0.4026(3) 0.1799(4) 0.047(2) Uani d . 1.00 . C23 0.2744(3) 0.3559(3) 0.2288(4) 0.042(2) Uani d . 1.00 . C24 0.3802(4) 0.4249(4) 0.0647(5) 0.074(3) Uani d . 1.00 . C25 0.2403(5) 0.4261(4) 0.4674(4) 0.088(3) Uani d . 1.00 . C26 0.2446(3) 0.3536(3) 0.4308(4) 0.049(2) Uani d . 1.00 . C27 -0.0222(4) 0.1590(5) 0.3364(6) 0.081(3) Uani d . 1.00 . C28 -0.0181(5) 0.1717(5) 0.4208(6) 0.085(3) Uani d . 1.00 . H1 0.0479 0.2858 0.1204 0.0569 Uiso calc . 1.00 . H2 0.0344 0.3610 0.3594 0.0703 Uiso calc . 1.00 . H3 0.1310 0.3033 0.3968 0.0569 Uiso calc . 1.00 . H4 -0.0188 0.4289 0.2398 0.1101 Uiso calc . 1.00 . H5 -0.0259 0.3850 0.1604 0.1101 Uiso calc . 1.00 . H6 -0.0586 0.3579 0.2382 0.1101 Uiso calc . 1.00 . H7 0.0949 0.0062 0.4174 0.0569 Uiso calc . 1.00 . H8 0.1785 0.1204 0.5948 0.0569 Uiso calc . 1.00 . H9 0.2383 0.1902 0.4918 0.0569 Uiso calc . 1.00 . H10 0.0526 0.0263 0.5734 0.0982 Uiso calc . 1.00 . H11 0.1026 -0.0350 0.5651 0.0982 Uiso calc . 1.00 . H12 0.1118 0.0274 0.6275 0.0982 Uiso calc . 1.00 . H13 0.4085 0.0157 0.3236 0.0569 Uiso calc . 1.00 . H14 0.4537 0.2275 0.3983 0.0569 Uiso calc . 1.00 . H15 0.3604 0.2661 0.3779 0.0569 Uiso calc . 1.00 . H16 0.5005 0.0419 0.4331 0.0923 Uiso calc . 1.00 . H17 0.5311 0.1174 0.4158 0.0923 Uiso calc . 1.00 . H18 0.5249 0.0599 0.3474 0.0923 Uiso calc . 1.00 . H19 0.3606 0.2722 0.0586 0.0569 Uiso calc . 1.00 . H20 0.2977 0.4619 0.1946 0.0569 Uiso calc . 1.00 . H21 0.2422 0.3703 0.2784 0.0569 Uiso calc . 1.00 . H22 0.4185 0.4033 0.0458 0.0569 Uiso calc . 1.00 . H23 0.3913 0.4760 0.0930 0.0569 Uiso calc . 1.00 . H24 0.3470 0.4501 0.0289 0.0569 Uiso calc . 1.00 . H25 0.2466 0.4631 0.4275 0.1148 Uiso calc . 1.00 . H26 0.2701 0.4314 0.5087 0.1148 Uiso calc . 1.00 . H27 0.1990 0.4327 0.4896 0.1148 Uiso calc . 1.00 . H28 0.0083 0.1899 0.3078 0.0942 Uiso calc . 1.00 . H29 -0.0164 0.1109 0.3214 0.0942 Uiso calc . 1.00 . H30 -0.0630 0.1759 0.3159 0.0942 Uiso calc . 1.00 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pt 0.0345(1) 0.02834(9) 0.0374(1) -0.00181(9) -0.0020(1) -0.00689(9) Ni 0.0334(4) 0.0298(3) 0.0355(4) -0.0024(3) 0.0010(3) -0.0058(3) S(1) 0.0424(8) 0.0441(8) 0.0397(8) 0.0037(7) -0.0067(7) -0.0028(6) S(2) 0.0369(8) 0.0449(8) 0.0465(8) -0.0091(6) -0.0010(7) -0.0069(6) S(3) 0.0431(8) 0.0297(6) 0.0578(9) 0.0000(6) -0.0059(8) -0.0014(6) S(4) 0.0424(8) 0.0321(7) 0.0442(8) -0.0005(6) 0.0081(7) -0.0090(6) N(1) 0.039(3) 0.038(2) 0.042(3) -0.001(2) 0.003(2) -0.002(2) N(2) 0.034(3) 0.035(2) 0.041(3) 0.001(2) -0.003(2) -0.005(2) N(3) 0.036(3) 0.039(2) 0.038(3) -0.008(2) 0.001(2) -0.004(2) N(4) 0.036(3) 0.033(2) 0.034(2) 0.001(2) 0.002(2) -0.003(2) N(5) 0.050(3) 0.043(3) 0.042(3) -0.007(2) 0.003(3) -0.009(2) N(6) 0.19(1) 0.19(1) 0.097(7) 0.085(9) -0.043(8) -0.065(7) C(1) 0.038(3) 0.038(3) 0.044(3) -0.001(2) 0.003(3) -0.001(3) C(2) 0.034(3) 0.051(3) 0.056(4) 0.003(3) 0.001(3) 0.003(3) C(3) 0.043(4) 0.056(4) 0.075(5) 0.011(3) 0.010(4) 0.008(4) C(4) 0.051(4) 0.065(4) 0.064(5) 0.010(3) 0.012(4) -0.015(4) C(5) 0.045(4) 0.056(4) 0.050(4) -0.006(3) 0.007(3) -0.011(3) C(6) 0.058(5) 0.103(7) 0.108(8) 0.037(5) 0.006(5) 0.007(6) C(7) 0.035(3) 0.031(2) 0.046(3) 0.003(2) -0.002(3) -0.003(2) C(8) 0.045(4) 0.036(3) 0.049(4) -0.005(3) 0.006(3) 0.004(3) C(9) 0.050(4) 0.046(3) 0.048(4) 0.004(3) 0.009(3) 0.006(3) C(10) 0.065(5) 0.058(4) 0.037(3) 0.002(4) 0.002(3) 0.006(3) C(11) 0.045(4) 0.052(4) 0.042(3) -0.001(3) -0.002(3) -0.007(3) C(12) 0.095(7) 0.071(5) 0.067(5) -0.010(5) 0.021(5) 0.018(4) C(13) 0.039(3) 0.039(3) 0.036(3) -0.006(2) 0.002(3) -0.003(2) C(14) 0.035(3) 0.053(4) 0.050(4) 0.006(3) 0.004(3) 0.004(3) C(15) 0.034(3) 0.074(4) 0.041(3) 0.000(3) 0.004(3) 0.008(3) C(16) 0.038(4) 0.066(4) 0.050(4) -0.016(3) -0.003(3) 0.000(3) C(17) 0.040(3) 0.047(3) 0.046(4) -0.014(3) -0.001(3) -0.002(3) C(18) 0.034(4) 0.110(7) 0.089(6) 0.008(4) -0.002(4) 0.010(5) C(19) 0.034(3) 0.032(3) 0.032(3) 0.002(2) -0.001(2) -0.005(2) C(20) 0.046(4) 0.038(3) 0.039(3) 0.000(3) 0.007(3) -0.003(2) C(21) 0.044(3) 0.041(3) 0.040(3) -0.009(3) 0.005(3) -0.001(3) C(22) 0.058(4) 0.032(3) 0.050(4) -0.004(3) 0.002(3) -0.004(3) C(23) 0.047(4) 0.035(3) 0.043(3) 0.007(3) 0.004(3) -0.006(2) C(24) 0.083(6) 0.047(4) 0.091(6) -0.009(4) 0.031(5) -0.002(4) C(25) 0.174(10) 0.038(4) 0.051(4) 0.011(5) -0.012(6) -0.004(3) C(26) 0.068(5) 0.045(3) 0.034(3) -0.006(3) -0.005(3) 0.001(3) C(27) 0.051(5) 0.100(6) 0.091(6) -0.012(5) 0.013(5) -0.005(5) C(28) 0.077(6) 0.088(6) 0.089(7) 0.025(5) -0.011(6) -0.028(5) #------------------------------------------------------------------------------ _refine_special_details ; ? ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme 'w = 1/[\s^2^(Fo) + 0.00040|Fo|^2^]' _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 5375 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0321 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0386 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.134 _refine_ls_shift/esd_max 0.0010 _refine_ls_shift/esd_mean 0.0000 _refine_diff_density_min -1.31 _refine_diff_density_max 0.60 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt Ni 2.5314(7) 1_555 1_555 yes Pt S(1) 2.321(2) 1_555 1_555 yes Pt S(2) 2.322(2) 1_555 1_555 yes Pt S(3) 2.324(2) 1_555 1_555 yes Pt S(4) 2.321(2) 1_555 1_555 yes Ni N(1) 2.130(5) 1_555 1_555 yes Ni N(2) 2.104(5) 1_555 1_555 yes Ni N(3) 2.119(5) 1_555 1_555 yes Ni N(4) 2.124(4) 1_555 1_555 yes Ni N(5) 2.119(5) 1_555 1_555 yes S(1) C(1) 1.748(6) 1_555 1_555 yes S(2) C(7) 1.760(6) 1_555 1_555 yes S(3) C(13) 1.761(6) 1_555 1_555 yes S(4) C(19) 1.749(5) 1_555 1_555 yes N(1) C(1) 1.357(7) 1_555 1_555 yes N(1) C(5) 1.352(7) 1_555 1_555 yes N(2) C(7) 1.356(7) 1_555 1_555 yes N(2) C(11) 1.348(7) 1_555 1_555 yes N(3) C(13) 1.354(7) 1_555 1_555 yes N(3) C(17) 1.361(7) 1_555 1_555 yes N(4) C(19) 1.370(7) 1_555 1_555 yes N(4) C(23) 1.357(7) 1_555 1_555 yes N(5) C(26) 1.130(7) 1_555 1_555 yes N(6) C(28) 1.12(1) 1_555 1_555 yes C(1) C(2) 1.401(8) 1_555 1_555 yes C(2) C(3) 1.377(9) 1_555 1_555 yes C(2) H(1) 1.114 1_555 1_555 no C(3) C(4) 1.392(10) 1_555 1_555 yes C(3) C(6) 1.532(10) 1_555 1_555 yes C(4) C(5) 1.385(9) 1_555 1_555 yes C(4) H(2) 0.977 1_555 1_555 no C(5) H(3) 1.115 1_555 1_555 no C(6) H(4) 1.022 1_555 1_555 no C(6) H(5) 0.916 1_555 1_555 no C(6) H(6) 0.919 1_555 1_555 no C(7) C(8) 1.392(8) 1_555 1_555 yes C(8) C(9) 1.378(9) 1_555 1_555 yes C(8) H(7) 0.975 1_555 1_555 no C(9) C(10) 1.389(9) 1_555 1_555 yes C(9) C(12) 1.505(9) 1_555 1_555 yes C(10) C(11) 1.376(9) 1_555 1_555 yes C(10) H(8) 1.033 1_555 1_555 no C(11) H(9) 1.058 1_555 1_555 no C(12) H(10) 0.960 1_555 1_555 no C(12) H(11) 0.961 1_555 1_555 no C(12) H(12) 0.925 1_555 1_555 no C(13) C(14) 1.382(8) 1_555 1_555 yes C(14) C(15) 1.377(9) 1_555 1_555 yes C(14) H(13) 1.030 1_555 1_555 no C(15) C(16) 1.403(9) 1_555 1_555 yes C(15) C(18) 1.494(9) 1_555 1_555 yes C(16) C(17) 1.378(9) 1_555 1_555 yes C(16) H(14) 0.978 1_555 1_555 no C(17) H(15) 1.036 1_555 1_555 no C(18) H(16) 0.976 1_555 1_555 no C(18) H(17) 0.952 1_555 1_555 no C(18) H(18) 0.955 1_555 1_555 no C(19) C(20) 1.383(8) 1_555 1_555 yes C(20) C(21) 1.381(7) 1_555 1_555 yes C(20) H(19) 1.018 1_555 1_555 no C(21) C(22) 1.371(8) 1_555 1_555 yes C(21) C(24) 1.503(9) 1_555 1_555 yes C(22) C(23) 1.375(9) 1_555 1_555 yes C(22) H(20) 1.128 1_555 1_555 no C(23) H(21) 1.106 1_555 1_555 no C(24) H(22) 0.961 1_555 1_555 no C(24) H(23) 1.071 1_555 1_555 no C(24) H(24) 1.033 1_555 1_555 no C(25) C(26) 1.458(9) 1_555 1_555 yes C(25) H(25) 0.956 1_555 1_555 no C(25) H(26) 0.942 1_555 1_555 no C(25) H(27) 0.963 1_555 1_555 no C(27) C(28) 1.42(1) 1_555 1_555 yes C(27) H(28) 0.985 1_555 1_555 no C(27) H(29) 0.920 1_555 1_555 no C(27) H(30) 0.986 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ni Pt S(1) 89.51(4) 1_555 1_555 1_555 yes Ni Pt S(2) 89.03(4) 1_555 1_555 1_555 yes Ni Pt S(3) 89.62(4) 1_555 1_555 1_555 yes Ni Pt S(4) 90.10(4) 1_555 1_555 1_555 yes S(1) Pt S(2) 90.85(6) 1_555 1_555 1_555 yes S(1) Pt S(3) 178.32(5) 1_555 1_555 1_555 yes S(1) Pt S(4) 89.74(6) 1_555 1_555 1_555 yes S(2) Pt S(3) 90.58(6) 1_555 1_555 1_555 yes S(2) Pt S(4) 178.94(5) 1_555 1_555 1_555 yes S(3) Pt S(4) 88.82(6) 1_555 1_555 1_555 yes Pt Ni N(1) 88.0(1) 1_555 1_555 1_555 yes Pt Ni N(2) 89.2(1) 1_555 1_555 1_555 yes Pt Ni N(3) 88.0(1) 1_555 1_555 1_555 yes Pt Ni N(4) 87.2(1) 1_555 1_555 1_555 yes Pt Ni N(5) 177.5(1) 1_555 1_555 1_555 yes N(1) Ni N(2) 89.6(2) 1_555 1_555 1_555 yes N(1) Ni N(3) 175.9(2) 1_555 1_555 1_555 yes N(1) Ni N(4) 89.4(2) 1_555 1_555 1_555 yes N(1) Ni N(5) 90.5(2) 1_555 1_555 1_555 yes N(2) Ni N(3) 91.2(2) 1_555 1_555 1_555 yes N(2) Ni N(4) 176.3(2) 1_555 1_555 1_555 yes N(2) Ni N(5) 92.9(2) 1_555 1_555 1_555 yes N(3) Ni N(4) 89.5(2) 1_555 1_555 1_555 yes N(3) Ni N(5) 93.4(2) 1_555 1_555 1_555 yes N(4) Ni N(5) 90.7(2) 1_555 1_555 1_555 yes Pt S(1) C(1) 104.8(2) 1_555 1_555 1_555 yes Pt S(2) C(7) 104.2(2) 1_555 1_555 1_555 yes Pt S(3) C(13) 103.5(2) 1_555 1_555 1_555 yes Pt S(4) C(19) 104.4(2) 1_555 1_555 1_555 yes Ni N(1) C(1) 122.4(4) 1_555 1_555 1_555 yes Ni N(1) C(5) 119.4(4) 1_555 1_555 1_555 yes C(1) N(1) C(5) 117.7(5) 1_555 1_555 1_555 yes Ni N(2) C(7) 123.6(4) 1_555 1_555 1_555 yes Ni N(2) C(11) 119.5(4) 1_555 1_555 1_555 yes C(7) N(2) C(11) 116.8(5) 1_555 1_555 1_555 yes Ni N(3) C(13) 124.5(4) 1_555 1_555 1_555 yes Ni N(3) C(17) 119.2(4) 1_555 1_555 1_555 yes C(13) N(3) C(17) 116.3(5) 1_555 1_555 1_555 yes Ni N(4) C(19) 123.8(3) 1_555 1_555 1_555 yes Ni N(4) C(23) 119.8(4) 1_555 1_555 1_555 yes C(19) N(4) C(23) 115.9(5) 1_555 1_555 1_555 yes Ni N(5) C(26) 164.3(5) 1_555 1_555 1_555 yes S(1) C(1) N(1) 120.5(4) 1_555 1_555 1_555 yes S(1) C(1) C(2) 118.3(5) 1_555 1_555 1_555 yes N(1) C(1) C(2) 121.3(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 120.4(6) 1_555 1_555 1_555 yes C(1) C(2) H(1) 118.0(6) 1_555 1_555 1_555 no C(3) C(2) H(1) 120.7(6) 1_555 1_555 1_555 no C(2) C(3) C(4) 118.2(6) 1_555 1_555 1_555 yes C(2) C(3) C(6) 120.9(7) 1_555 1_555 1_555 yes C(4) C(3) C(6) 120.8(7) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.0(6) 1_555 1_555 1_555 yes C(3) C(4) H(2) 120.9(7) 1_555 1_555 1_555 no C(5) C(4) H(2) 120.1(7) 1_555 1_555 1_555 no N(1) C(5) C(4) 123.3(6) 1_555 1_555 1_555 yes N(1) C(5) H(3) 118.9(6) 1_555 1_555 1_555 no C(4) C(5) H(3) 117.3(6) 1_555 1_555 1_555 no C(3) C(6) H(4) 105.7(8) 1_555 1_555 1_555 no C(3) C(6) H(5) 111.0(7) 1_555 1_555 1_555 no C(3) C(6) H(6) 111.7(8) 1_555 1_555 1_555 no H(4) C(6) H(5) 106.2(9) 1_555 1_555 1_555 no H(4) C(6) H(6) 106.0(8) 1_555 1_555 1_555 no H(5) C(6) H(6) 115.4(10) 1_555 1_555 1_555 no S(2) C(7) N(2) 119.9(4) 1_555 1_555 1_555 yes S(2) C(7) C(8) 118.2(4) 1_555 1_555 1_555 yes N(2) C(7) C(8) 121.9(5) 1_555 1_555 1_555 yes C(7) C(8) C(9) 120.8(6) 1_555 1_555 1_555 yes C(7) C(8) H(7) 120.9(6) 1_555 1_555 1_555 no C(9) C(8) H(7) 116.5(6) 1_555 1_555 1_555 no C(8) C(9) C(10) 117.0(6) 1_555 1_555 1_555 yes C(8) C(9) C(12) 121.9(6) 1_555 1_555 1_555 yes C(10) C(9) C(12) 121.1(6) 1_555 1_555 1_555 yes C(9) C(10) C(11) 119.9(6) 1_555 1_555 1_555 yes C(9) C(10) H(8) 113.3(6) 1_555 1_555 1_555 no C(11) C(10) H(8) 126.5(7) 1_555 1_555 1_555 no N(2) C(11) C(10) 123.5(6) 1_555 1_555 1_555 yes N(2) C(11) H(9) 118.8(6) 1_555 1_555 1_555 no C(10) C(11) H(9) 117.7(6) 1_555 1_555 1_555 no C(9) C(12) H(10) 108.1(7) 1_555 1_555 1_555 no C(9) C(12) H(11) 108.4(7) 1_555 1_555 1_555 no C(9) C(12) H(12) 110.9(7) 1_555 1_555 1_555 no H(10) C(12) H(11) 107.8(8) 1_555 1_555 1_555 no H(10) C(12) H(12) 110.8(8) 1_555 1_555 1_555 no H(11) C(12) H(12) 110.7(8) 1_555 1_555 1_555 no S(3) C(13) N(3) 119.3(4) 1_555 1_555 1_555 yes S(3) C(13) C(14) 117.9(5) 1_555 1_555 1_555 yes N(3) C(13) C(14) 122.8(5) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120.9(6) 1_555 1_555 1_555 yes C(13) C(14) H(13) 122.8(6) 1_555 1_555 1_555 no C(15) C(14) H(13) 115.9(6) 1_555 1_555 1_555 no C(14) C(15) C(16) 117.0(6) 1_555 1_555 1_555 yes C(14) C(15) C(18) 121.7(7) 1_555 1_555 1_555 yes C(16) C(15) C(18) 121.3(6) 1_555 1_555 1_555 yes C(15) C(16) C(17) 119.5(6) 1_555 1_555 1_555 yes C(15) C(16) H(14) 131.5(7) 1_555 1_555 1_555 no C(17) C(16) H(14) 108.0(6) 1_555 1_555 1_555 no N(3) C(17) C(16) 123.5(6) 1_555 1_555 1_555 yes N(3) C(17) H(15) 120.5(6) 1_555 1_555 1_555 no C(16) C(17) H(15) 116.0(6) 1_555 1_555 1_555 no C(15) C(18) H(16) 110.5(7) 1_555 1_555 1_555 no C(15) C(18) H(17) 111.5(7) 1_555 1_555 1_555 no C(15) C(18) H(18) 111.7(8) 1_555 1_555 1_555 no H(16) C(18) H(17) 107.1(8) 1_555 1_555 1_555 no H(16) C(18) H(18) 106.9(8) 1_555 1_555 1_555 no H(17) C(18) H(18) 108.9(8) 1_555 1_555 1_555 no S(4) C(19) N(4) 119.4(4) 1_555 1_555 1_555 yes S(4) C(19) C(20) 118.4(4) 1_555 1_555 1_555 yes N(4) C(19) C(20) 122.1(5) 1_555 1_555 1_555 yes C(19) C(20) C(21) 120.4(5) 1_555 1_555 1_555 yes C(19) C(20) H(19) 112.5(5) 1_555 1_555 1_555 no C(21) C(20) H(19) 126.7(6) 1_555 1_555 1_555 no C(20) C(21) C(22) 117.9(5) 1_555 1_555 1_555 yes C(20) C(21) C(24) 121.6(6) 1_555 1_555 1_555 yes C(22) C(21) C(24) 120.6(5) 1_555 1_555 1_555 yes C(21) C(22) C(23) 119.8(5) 1_555 1_555 1_555 yes C(21) C(22) H(20) 128.3(6) 1_555 1_555 1_555 no C(23) C(22) H(20) 111.7(6) 1_555 1_555 1_555 no N(4) C(23) C(22) 123.8(5) 1_555 1_555 1_555 yes N(4) C(23) H(21) 108.3(5) 1_555 1_555 1_555 no C(22) C(23) H(21) 127.9(6) 1_555 1_555 1_555 no C(21) C(24) H(22) 113.1(6) 1_555 1_555 1_555 no C(21) C(24) H(23) 112.7(7) 1_555 1_555 1_555 no C(21) C(24) H(24) 104.4(7) 1_555 1_555 1_555 no H(22) C(24) H(23) 108.1(7) 1_555 1_555 1_555 no H(22) C(24) H(24) 125.4(9) 1_555 1_555 1_555 no H(23) C(24) H(24) 91.1(6) 1_555 1_555 1_555 no C(26) C(25) H(25) 110.0(7) 1_555 1_555 1_555 no C(26) C(25) H(26) 110.8(7) 1_555 1_555 1_555 no C(26) C(25) H(27) 109.4(8) 1_555 1_555 1_555 no H(25) C(25) H(26) 109.7(9) 1_555 1_555 1_555 no H(25) C(25) H(27) 107.9(8) 1_555 1_555 1_555 no H(26) C(25) H(27) 109.0(7) 1_555 1_555 1_555 no N(5) C(26) C(25) 174.6(7) 1_555 1_555 1_555 yes C(28) C(27) H(28) 110.0(9) 1_555 1_555 1_555 no C(28) C(27) H(29) 114.5(9) 1_555 1_555 1_555 no C(28) C(27) H(30) 110.1(8) 1_555 1_555 1_555 no H(28) C(27) H(29) 109.0(8) 1_555 1_555 1_555 no H(28) C(27) H(30) 103.8(9) 1_555 1_555 1_555 no H(29) C(27) H(30) 108.9(9) 1_555 1_555 1_555 no N(6) C(28) C(27) 176(1) 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Pt Ni 2.5314(7) 1_555 1_555 ? S(3) C(22) 3.517(6) 1_555 6_545 ? S(4) C(25) 3.527(8) 1_555 7_554 ? N(6) C(16) 3.48(1) 1_555 2_456 ? C(15) C(24) 3.522(10) 1_555 7_555 ? #------------------------------------------------------------------------------ _publ_requested_journal ' Dalton Transactions' _publ_contact_author ; Isamu Kinoshita Graduate School of Science, Osaka City University, Sumiyoshi-ku, Osaka 558-8 585, JAPAN ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+81-6-605-3146' _publ_contact_author_fax '+81-6-690-2753' _publ_contact_author_email 'isamu@sci.osaka-cu.ac.jp' loop_ _publ_author_name 'Ken'ichi Kitano' _publ_author_address ; 'Graduate School of Science, Osaka City University, Sumiyoshi-ku, Osaka 558- 8585, JAPAN' ; _publ_section_title ; ENTER SECTION TITLE ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #=END