#------------------------------------------------------------------------------ #$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003470.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003470 loop_ _publ_author_name 'Tahirov, T. H.' 'Lu, T.-H.' 'Luh, H.' 'Lai, C.-Y.' 'Chung, C.-S.' _publ_section_title ; [3,9-Dimethyl-4,8-diaza-3,8-undecadiene-2,10-dione dioximato(1--)](thiocyanato)copper(II) and [3,6,6,9-Tetramethyl-4,8-diaza-3,8-undecadiene-2,10-dione dioximato(1--)](isothiocyanato)copper(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 846 _journal_page_last 849 _journal_volume 51 _journal_year 1995 _chemical_formula_sum 'C12 H19 Cu N5 O2 S' _chemical_formula_weight 360.92 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.152(7) _cell_angle_beta 98.770(10) _cell_angle_gamma 100.49(2) _cell_formula_units_Z 2 _cell_length_a 7.275(3) _cell_length_b 7.7110(7) _cell_length_c 14.2930(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 298(3) _cell_measurement_theta_max 21.53 _cell_measurement_theta_min 8.05 _cell_volume 778.8(3) _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 7252 _diffrn_reflns_theta_max 35 _diffrn_standards_decay_% 1.5 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.54 _exptl_absorpt_correction_T_max 0.9990 _exptl_absorpt_correction_T_min 0.7861 _exptl_absorpt_correction_type 'psi scan (Northe, Phillips & Mathews, 1968)' _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.539 _exptl_crystal_description parallelepiped _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.28 _refine_diff_density_max 1.32(18) _refine_diff_density_min -1.12(18) _refine_ls_extinction_coef 0.70(10) _refine_ls_extinction_method 'Zachariasen (1967)' _refine_ls_goodness_of_fit_obs 2.37 _refine_ls_hydrogen_treatment noref _refine_ls_number_parameters 191 _refine_ls_number_reflns 4193 _refine_ls_R_factor_obs 0.064 _refine_ls_shift/esd_max 0.001 _refine_ls_structure_factor_coef F _refine_ls_weighting_scheme 'w = 1/[\s^2^(F) + 0.0008F^2^]' _refine_ls_wR_factor_obs 0.099 _reflns_number_observed 4193 _reflns_number_total 6839 _reflns_observed_criterion I>2.5\s(I) _[local]_cod_data_source_file kh1000.cif _[local]_cod_data_source_block kh1000a _cod_original_cell_volume 778.9(4) _cod_database_code 2003470 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Cu .09269(6) .38415(6) .31118(3) S .3526(2) .2739(2) .24394(11) O1 -.1156(5) .0200(4) .3228(2) O2 .0984(5) .1546(4) .4713(2) N1 -.1005(5) .1709(4) .2730(2) N2 -.0426(5) .4676(5) .1954(3) N3 .2160(5) .6172(4) .3682(3) N4 .1474(5) .3183(4) .4432(2) N5 .1756(6) .1752(6) .0643(2) C1 -.3309(7) .0146(8) .1432(4) C2 -.1995(5) .1708(6) .1902(3) C3 -.1674(6) .3489(7) .1475(3) C4 -.2872(8) .3726(11) .0548(4) C5 .0032(7) .6530(7) .1684(4) C6 .2040(8) .7374(7) .2081(4) C7 .2464(8) .7787(6) .3131(4) C8 .3595(7) .7786(6) .5170(4) C9 .2688(5) .6180(5) .4581(3) C10 .2298(5) .4441(5) .5034(3) C11 .2797(7) .4160(7) .6067(3) C12 .2471(7) .2319(7) .1364(5) HO1 -.024 .062 .384 H1 -.283 -.048 .092 H2 -.360 -.093 .190 H3 -.439 .036 .108 H4 -.240 .450 .020 H5 -.405 .306 .041 H6 -.229 .275 .020 H7 -.050 .674 .103 H8 -.099 .709 .189 H9 .303 .657 .184 H10 .225 .866 .176 H11 .150 .850 .328 H12 .383 .856 .344 H13 .481 .822 .504 H14 .352 .775 .578 H15 .276 .873 .488 H16 .409 .464 .638 H17 .259 .273 .616 H18 .183 .469 .643 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag S Cu N1 95.10(10) yes S Cu N2 100.00(10) yes S Cu N3 103.90(10) yes S Cu N4 100.20(10) yes N1 Cu N2 80.30(10) yes N1 Cu N3 161.00(10) yes N1 Cu N4 94.80(10) yes N2 Cu N3 97.5(2) yes N2 Cu N4 159.50(10) yes N3 Cu N4 80.80(10) yes Cu S C12 98.8(2) yes Cu N1 O1 123.8(2) yes Cu N1 C2 116.3(3) yes O1 N1 C2 119.3(3) yes Cu N2 C3 114.6(3) yes Cu N2 C5 120.7(3) yes C3 N2 C5 124.7(4) yes Cu N3 C7 123.4(3) yes Cu N3 C9 114.4(3) yes C7 N3 C9 122.1(4) yes Cu N4 O2 122.6(2) yes Cu N4 C10 116.5(3) yes O2 N4 C10 120.8(3) yes N1 C2 C1 124.4(4) yes N1 C2 C3 111.7(4) yes C1 C2 C3 124.0(4) yes N2 C3 C2 116.1(4) yes N2 C3 C4 126.4(5) yes C2 C3 C4 117.5(5) yes N2 C5 C6 112.0(4) yes C5 C6 C7 116.8(5) yes N3 C7 C6 111.5(4) yes N3 C9 C8 124.2(4) yes N3 C9 C10 115.8(3) yes C8 C9 C10 120.0(4) yes N4 C10 C9 112.5(3) yes N4 C10 C11 123.1(4) yes C9 C10 C11 124.4(4) yes S C12 N5 168.9(5) yes loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Cu S 2.521(2) yes Cu N1 1.974(3) yes Cu N2 1.965(3) yes Cu N3 1.970(3) yes Cu N4 1.956(3) yes S C12 1.613(7) yes O1 N1 1.362(4) yes O2 N4 1.329(4) yes N1 C2 1.288(5) yes N2 C3 1.278(6) yes N2 C5 1.474(6) yes N3 C7 1.476(5) yes N3 C9 1.284(6) yes N4 C10 1.292(5) yes N5 C12 1.129(8) yes C1 C2 1.482(7) yes C2 C3 1.499(7) yes C3 C4 1.502(6) yes C5 C6 1.509(8) yes C6 C7 1.507(8) yes C8 C9 1.485(6) yes C9 C10 1.490(5) yes C10 C11 1.491(6) yes