#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003683.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003683 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1291 _journal_page_last 1293 _publ_section_title ;Isothiocyanatobis(1,10-phenanthroline)copper(II) Dicyanonitrosomethanide ; _chemical_formula_moiety '[Cu (NCS)(C12 H8 N2 )2 ][ONC(CN)2 ]' _chemical_formula_sum 'C28 H16 Cu N8 O S' _chemical_formula_structural '[Cu (NCS)(C12 H8 N2 )2 ][ONC(CN)2 ]' _chemical_formula_weight 576.09 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 7.937(4) _cell_length_b 11.249(6) _cell_length_c 15.144(6) _cell_angle_alpha 99.59(4) _cell_angle_beta 98.00(4) _cell_angle_gamma 110.59(4) _cell_volume 1219.1(10) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_meas 1.54(1) _exptl_crystal_density_method 'flotation in CCl~4~-CHBr~3~' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 4.60 _cell_measurement_theta_max 10.68 _exptl_absorpt_coefficient_mu 1.023 _cell_measurement_temperature 295(2) _exptl_crystal_description 'prism' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_colour 'dark green' _chemical_compound_source synthesis _diffrn_measurement_device 'Syntex P21 diffractometer' _diffrn_measurement_method \q-2\q _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 5656 _reflns_number_total 5656 _reflns_number_observed 3721 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_theta_max 27.57 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0506 _refine_ls_wR_factor_obs 0.1112 _refine_ls_wR_factor_all 0.1318 _refine_ls_goodness_of_fit_obs 1.083 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_number_reflns 5656 _refine_ls_number_parameters 400 _refine_ls_hydrogen_treatment refxyz _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0661P)^2^ + 0.3278P] _refine_ls_shift/esd_max 0.007 _refine_diff_density_max .438 _refine_diff_density_min -.469 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'N' 'N' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0061 0.003 'S' 'S' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.1246 0.123 'Cu' 'Cu' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.3201 1.2 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Cu1 1 0.36811(5) 0.42657(4) 0.22709(3) 0.04323(14) N11 1 0.5757(4) 0.5334(3) 0.3318(2) 0.0425(6) N12 1 0.3393(4) 0.2917(3) 0.3084(2) 0.0437(6) N13 1 0.1782(3) 0.3036(3) 0.1185(2) 0.0424(6) N14 1 0.5368(3) 0.4228(2) 0.1322(2) 0.0394(6) S1 1 0.1668(2) 0.77364(12) 0.24807(9) 0.0841(4) C1 1 0.2226(5) 0.6491(4) 0.2391(2) 0.0458(8) N1 1 0.2624(4) 0.5605(3) 0.2303(2) 0.0566(8) C111 1 0.6045(4) 0.4686(3) 0.3960(2) 0.0412(7) C112 1 0.6873(5) 0.6564(4) 0.3431(2) 0.0534(9) C113 1 0.8339(6) 0.7191(4) 0.4163(3) 0.0610(10) C114 1 0.8653(5) 0.6540(4) 0.4805(3) 0.0593(10) C115 1 0.7489(5) 0.5248(4) 0.4724(2) 0.0494(8) C116 1 0.7686(6) 0.4486(5) 0.5362(3) 0.0620(11) C121 1 0.4776(5) 0.3382(3) 0.3832(2) 0.0425(7) C122 1 0.2180(6) 0.1721(4) 0.2970(3) 0.0559(9) C123 1 0.2284(7) 0.0952(4) 0.3577(3) 0.0679(11) C124 1 0.3676(7) 0.1412(5) 0.4316(3) 0.0693(12) C125 1 0.4994(6) 0.2668(4) 0.4470(2) 0.0542(9) C126 1 0.6512(7) 0.3274(5) 0.5238(3) 0.0682(12) C131 1 0.2464(4) 0.2738(3) 0.0449(2) 0.0379(7) C132 1 -0.0005(5) 0.2474(4) 0.1125(3) 0.0523(9) C133 1 -0.1190(5) 0.1575(4) 0.0353(3) 0.0558(9) C134 1 -0.0512(5) 0.1262(4) -0.0384(3) 0.0544(9) C135 1 0.1366(4) 0.1857(3) -0.0359(2) 0.0428(7) C136 1 0.2209(5) 0.1623(4) -0.1100(3) 0.0556(9) C141 1 0.4382(4) 0.3391(3) 0.0518(2) 0.0378(7) C142 1 0.7143(5) 0.4841(4) 0.1394(2) 0.0503(9) C143 1 0.8017(5) 0.4669(4) 0.0691(3) 0.0592(10) C144 1 0.7049(5) 0.3824(4) -0.0111(2) 0.0548(9) C145 1 0.5167(4) 0.3148(3) -0.0219(2) 0.0430(7) C146 1 0.4017(5) 0.2223(4) -0.1037(2) 0.0542(9) O100 1 0.1742(4) 0.6516(3) 0.7155(2) 0.0734(8) N100 1 0.1715(4) 0.7427(3) 0.6791(2) 0.0595(8) C100 1 0.2965(5) 0.8619(4) 0.7198(2) 0.0511(8) C101 1 0.4286(5) 0.8878(4) 0.8004(3) 0.0566(9) N101 1 0.5300(5) 0.9044(4) 0.8654(3) 0.0812(11) C102 1 0.2905(7) 0.9631(5) 0.6775(3) 0.0758(12) N102 1 0.2803(8) 1.0415(5) 0.6431(4) 0.125(2) H112 1 0.6526(46) 0.7001(33) 0.2997(24) 0.050 H113 1 0.9140(49) 0.8073(36) 0.4230(24) 0.050 H114 1 0.9576(49) 0.6860(33) 0.5248(25) 0.050 H116 1 0.8595(51) 0.4856(35) 0.5821(26) 0.050 H122 1 0.1293(48) 0.1435(33) 0.2425(25) 0.050 H123 1 0.1358(49) 0.0137(36) 0.3474(24) 0.050 H124 1 0.3819(48) 0.0940(34) 0.4671(25) 0.050 H126 1 0.6632(47) 0.2784(34) 0.5588(25) 0.050 H132 1 -0.0441(46) 0.2791(33) 0.1633(24) 0.050 H133 1 -0.2421(51) 0.1142(34) 0.0343(23) 0.050 H134 1 -0.1194(48) 0.0697(34) -0.0871(25) 0.050 H136 1 0.1466(50) 0.1068(36) -0.1537(25) 0.050 H142 1 0.7744(49) 0.5304(35) 0.1882(25) 0.050 H143 1 0.9233(50) 0.5112(34) 0.0753(24) 0.050 H144 1 0.7584(48) 0.3614(33) -0.0585(25) 0.050 H146 1 0.4641(48) 0.2086(33) -0.1491(25) 0.050 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Cu1 0.0446(2) 0.0140(2) 0.0021(2) 0.0454(2) 0.0055(2) 0.0335(2) N11 0.0463(15) 0.0150(13) 0.0064(11) 0.0445(15) 0.0078(11) 0.0337(13) N12 0.051(2) 0.0169(13) 0.0141(12) 0.0408(15) 0.0074(12) 0.0392(14) N13 0.0369(14) 0.0139(12) 0.0049(11) 0.051(2) 0.0079(12) 0.0356(13) N14 0.0379(14) 0.0117(12) 0.0024(11) 0.0426(14) 0.0083(11) 0.0326(13) S1 0.1111(10) 0.0559(7) 0.0173(7) 0.0708(7) 0.0172(6) 0.0866(8) C1 0.043(2) 0.014(2) 0.0014(13) 0.055(2) 0.0073(14) 0.032(2) N1 0.065(2) 0.032(2) 0.0038(15) 0.060(2) 0.0100(15) 0.047(2) C111 0.043(2) 0.023(2) 0.0108(13) 0.053(2) 0.0052(14) 0.0306(15) C112 0.057(2) 0.014(2) 0.004(2) 0.052(2) 0.008(2) 0.042(2) C113 0.056(2) 0.008(2) 0.003(2) 0.056(2) -0.003(2) 0.051(2) C114 0.046(2) 0.025(2) -0.001(2) 0.080(3) -0.009(2) 0.040(2) C115 0.048(2) 0.030(2) 0.0082(14) 0.070(2) 0.001(2) 0.032(2) C116 0.064(3) 0.044(3) 0.008(2) 0.095(3) 0.015(2) 0.038(2) C121 0.052(2) 0.029(2) 0.0132(14) 0.051(2) 0.0101(14) 0.034(2) C122 0.063(2) 0.019(2) 0.017(2) 0.048(2) 0.008(2) 0.054(2) C123 0.092(3) 0.023(2) 0.030(3) 0.043(2) 0.018(2) 0.072(3) C124 0.103(4) 0.054(3) 0.038(3) 0.073(3) 0.037(2) 0.063(3) C125 0.074(2) 0.043(2) 0.024(2) 0.065(2) 0.021(2) 0.045(2) C126 0.094(3) 0.065(3) 0.019(2) 0.099(4) 0.031(2) 0.041(2) C131 0.041(2) 0.0139(13) 0.0043(13) 0.036(2) 0.0102(13) 0.036(2) C132 0.041(2) 0.018(2) 0.011(2) 0.065(2) 0.013(2) 0.049(2) C133 0.034(2) 0.009(2) 0.005(2) 0.067(2) 0.013(2) 0.056(2) C134 0.048(2) 0.007(2) -0.004(2) 0.052(2) 0.006(2) 0.047(2) C135 0.042(2) 0.0135(14) 0.0008(14) 0.043(2) 0.0072(14) 0.038(2) C136 0.054(2) 0.010(2) 0.000(2) 0.052(2) -0.007(2) 0.042(2) C141 0.041(2) 0.0151(14) 0.0035(13) 0.039(2) 0.0110(13) 0.034(2) C142 0.041(2) 0.008(2) 0.0032(15) 0.056(2) 0.008(2) 0.041(2) C143 0.037(2) 0.007(2) 0.008(2) 0.076(3) 0.013(2) 0.052(2) C144 0.049(2) 0.021(2) 0.017(2) 0.076(3) 0.017(2) 0.041(2) C145 0.043(2) 0.0159(15) 0.0066(14) 0.047(2) 0.0106(14) 0.038(2) C146 0.055(2) 0.019(2) 0.009(2) 0.065(2) 0.004(2) 0.037(2) O100 0.081(2) 0.017(2) 0.019(2) 0.063(2) 0.0103(15) 0.068(2) N100 0.057(2) 0.024(2) 0.0131(15) 0.074(2) 0.006(2) 0.045(2) C100 0.048(2) 0.021(2) 0.009(2) 0.059(2) 0.007(2) 0.044(2) C101 0.051(2) 0.015(2) 0.013(2) 0.056(2) 0.013(2) 0.058(2) N101 0.064(2) 0.009(2) -0.015(2) 0.081(3) 0.016(2) 0.073(2) C102 0.084(3) 0.027(3) 0.004(2) 0.074(3) 0.019(2) 0.064(3) N102 0.161(5) 0.054(4) -0.005(4) 0.102(4) 0.050(3) 0.113(4)