#------------------------------------------------------------------------------ #$Date: 2011-01-02 22:00:31 +0200 (Sun, 02 Jan 2011) $ #$Revision: 5310 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2216639.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_2216639 loop_ _publ_author_name 'Kelan Li' 'Feihua Luo' 'Xuegang Song' 'Zongqiu Hu' _publ_section_title ;\ catena-Poly[copper(II)-di-\m~2~-1,1-azido-copper(II)-\m~2~-acetato-\ \m~2~-1,1-azido-\m~2~-(dimethyl sulfoxide)-copper(II)-di-\m~2~-1,1-azido] ; _journal_coeditor_code LH2563 _journal_issue 12 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m3156 _journal_page_last m3156 _journal_volume 63 _journal_year 2007 _chemical_formula_iupac '[Cu3 (C2 H3 O2)2 (N3)4 (C2 H6 O S)2]' _chemical_formula_moiety 'C8 H18 Cu3 N12 O6 S2' _chemical_formula_sum 'C8 H18 Cu3 N12 O6 S2' _chemical_formula_weight 633.13 _chemical_name_systematic ; catena-Poly[copper(II)-di-\m~2~-1,1-azido-copper(II)-\m~2~-acetato- \m~2~-1,1-azido-\m~2~-(dimethyl sulfoxide)-copper(II)-di-\m~2~-1,1-azido] ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.386(2) _cell_angle_beta 112.6870(10) _cell_angle_gamma 116.2610(10) _cell_formula_units_Z 1 _cell_length_a 8.5205(9) _cell_length_b 8.6624(9) _cell_length_c 9.4999(10) _cell_measurement_reflns_used 2542 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.00 _cell_measurement_theta_min 2.38 _cell_volume 566.66(10) _computing_cell_refinement 'SAINT-Plus (Bruker, 2001)' _computing_data_collection 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus (Bruker, 2001)' _computing_molecular_graphics 'SHELXTL (Bruker, 2001)' _computing_publication_material 'SHELXTL (Bruker, 2001)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.970 _diffrn_measurement_device_type 'Bruker SMART-CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 3467 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 2.38 _exptl_absorpt_coefficient_mu 3.024 _exptl_absorpt_correction_type none _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 317 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.602 _refine_diff_density_min -0.646 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 145 _refine_ls_number_reflns 2404 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.106 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0346 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.3521P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.0988 _reflns_number_gt 2182 _reflns_number_total 2404 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file lh2563.cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2216639 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy Cu Cu1 0.81687(5) 0.81565(4) -0.06003(4) 0.03025(14) Uani d . 1 Cu Cu2 0.5000 0.5000 0.0000 0.03156(15) Uani d S 1 C C1 0.7810(8) 1.1353(5) 0.2360(6) 0.0673(12) Uani d . 1 H H1A 0.8966 1.1839 0.2199 0.101 Uiso calc R 1 H H1B 0.8111 1.1893 0.3382 0.101 Uiso calc R 1 H H1C 0.6854 1.1577 0.1586 0.101 Uiso calc R 1 C C2 0.4761(7) 0.8594(7) 0.2395(6) 0.0707(13) Uani d . 1 H H2A 0.4049 0.9054 0.1643 0.106 Uiso calc R 1 H H2B 0.5099 0.9132 0.3429 0.106 Uiso calc R 1 H H2C 0.3974 0.7341 0.2218 0.106 Uiso calc R 1 C C3 0.2979(6) 0.5365(6) -0.4771(4) 0.0630(12) Uani d . 1 H H3A 0.2879 0.4330 -0.5259 0.095 Uiso calc R 1 H H3B 0.3458 0.6318 -0.5264 0.095 Uiso calc R 1 H H3C 0.1722 0.5130 -0.4879 0.095 Uiso calc R 1 C C4 0.4350(5) 0.5860(4) -0.3071(4) 0.0361(6) Uani d . 1 N N1 1.0712(4) 0.9551(4) 0.1239(3) 0.0449(7) Uani d . 1 N N2 1.1240(4) 0.9351(4) 0.2578(3) 0.0421(6) Uani d . 1 N N3 1.1756(6) 0.9171(6) 0.3806(4) 0.0691(11) Uani d . 1 N N4 0.2460(4) 0.4183(3) 0.0089(3) 0.0328(5) Uani d . 1 N N5 0.1232(4) 0.4496(4) -0.0825(3) 0.0379(6) Uani d . 1 N N6 0.0095(5) 0.4816(5) -0.1649(5) 0.0624(9) Uani d . 1 O O1 0.6009(3) 0.7171(3) -0.2653(3) 0.0432(6) Uani d . 1 O O2 0.3755(3) 0.4928(3) -0.2207(3) 0.0406(5) Uani d . 1 O O3 0.6177(4) 0.8295(3) 0.0499(3) 0.0430(5) Uani d . 1 S S1 0.68907(12) 0.90584(11) 0.22039(10) 0.0401(2) Uani d . 1 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 Cu1 0.0237(2) 0.0250(2) 0.0280(2) 0.00378(15) 0.00743(15) 0.00848(14) Cu2 0.0225(3) 0.0298(3) 0.0332(3) 0.0057(2) 0.0115(2) 0.0083(2) C1 0.080(3) 0.0306(19) 0.068(3) 0.009(2) 0.031(2) -0.0018(18) C2 0.057(3) 0.079(3) 0.062(3) 0.014(2) 0.035(2) -0.008(2) C3 0.046(2) 0.071(3) 0.0320(18) 0.007(2) 0.0030(16) 0.0070(17) C4 0.0317(15) 0.0350(16) 0.0304(14) 0.0103(13) 0.0097(12) 0.0041(12) N1 0.0338(14) 0.0375(15) 0.0345(14) 0.0031(12) 0.0040(11) 0.0176(11) N2 0.0356(14) 0.0370(15) 0.0372(15) 0.0090(12) 0.0101(12) 0.0122(11) N3 0.071(2) 0.076(3) 0.0393(18) 0.026(2) 0.0150(17) 0.0256(17) N4 0.0251(12) 0.0272(12) 0.0428(14) 0.0099(10) 0.0148(11) 0.0109(10) N5 0.0316(13) 0.0317(13) 0.0458(15) 0.0109(11) 0.0175(12) 0.0118(11) N6 0.052(2) 0.070(2) 0.073(2) 0.0381(19) 0.0230(18) 0.0342(19) O1 0.0344(12) 0.0334(11) 0.0305(11) -0.0018(10) 0.0059(9) 0.0056(9) O2 0.0282(11) 0.0391(12) 0.0337(11) 0.0031(10) 0.0094(9) 0.0067(9) O3 0.0450(13) 0.0400(13) 0.0407(12) 0.0177(11) 0.0188(11) 0.0008(10) S1 0.0395(4) 0.0351(4) 0.0384(4) 0.0163(4) 0.0118(3) 0.0031(3) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 N4 . 2_665 92.49(11) n O1 Cu1 N1 . . 166.25(11) n N4 Cu1 N1 2_665 . 98.17(11) n O1 Cu1 N1 . 2_775 89.72(10) n N4 Cu1 N1 2_665 2_775 165.71(13) n N1 Cu1 N1 . 2_775 77.84(12) n O1 Cu1 O3 . . 91.09(10) n N4 Cu1 O3 2_665 . 87.19(10) n N1 Cu1 O3 . . 98.06(12) n N1 Cu1 O3 2_775 . 106.90(12) n O2 Cu2 O2 . 2_665 180.00(15) n O2 Cu2 N4 . 2_665 90.66(10) n O2 Cu2 N4 2_665 2_665 89.34(10) n O2 Cu2 N4 . . 89.34(10) n O2 Cu2 N4 2_665 . 90.66(10) n N4 Cu2 N4 2_665 . 180.0 n S1 C1 H1A . . 109.5 ? S1 C1 H1B . . 109.5 ? H1A C1 H1B . . 109.5 ? S1 C1 H1C . . 109.5 ? H1A C1 H1C . . 109.5 ? H1B C1 H1C . . 109.5 ? S1 C2 H2A . . 109.5 ? S1 C2 H2B . . 109.5 ? H2A C2 H2B . . 109.5 ? S1 C2 H2C . . 109.5 ? H2A C2 H2C . . 109.5 ? H2B C2 H2C . . 109.5 ? C4 C3 H3A . . 109.5 ? C4 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C4 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? O2 C4 O1 . . 126.0(3) ? O2 C4 C3 . . 117.2(3) ? O1 C4 C3 . . 116.8(3) ? N2 N1 Cu1 . . 129.6(2) ? N2 N1 Cu1 . 2_775 124.8(2) ? Cu1 N1 Cu1 . 2_775 102.16(11) ? N3 N2 N1 . . 178.7(4) ? N5 N4 Cu1 . 2_665 122.3(2) ? N5 N4 Cu2 . . 120.7(2) ? Cu1 N4 Cu2 2_665 . 104.04(11) ? N6 N5 N4 . . 178.3(4) ? C4 O1 Cu1 . . 128.8(2) ? C4 O2 Cu2 . . 131.9(2) ? S1 O3 Cu1 . . 124.36(14) ? O3 S1 C2 . . 104.30(19) ? O3 S1 C1 . . 105.62(19) ? C2 S1 C1 . . 97.6(3) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 . 1.933(2) yes Cu1 N4 2_665 1.970(2) yes Cu1 N1 . 1.986(3) yes Cu1 N1 2_775 2.002(3) yes Cu1 O3 . 2.351(2) yes Cu2 O2 . 1.936(2) yes Cu2 O2 2_665 1.936(2) ? Cu2 N4 2_665 1.995(2) ? Cu2 N4 . 1.995(2) yes Cu2 O3 . 2.542(2) yes C1 S1 . 1.765(4) ? C1 H1A . 0.9600 ? C1 H1B . 0.9600 ? C1 H1C . 0.9600 ? C2 S1 . 1.760(5) ? C2 H2A . 0.9600 ? C2 H2B . 0.9600 ? C2 H2C . 0.9600 ? C3 C4 . 1.500(4) ? C3 H3A . 0.9600 ? C3 H3B . 0.9600 ? C3 H3C . 0.9600 ? C4 O2 . 1.245(4) ? C4 O1 . 1.259(4) ? N1 N2 . 1.217(4) ? N1 Cu1 2_775 2.002(3) ? N2 N3 . 1.116(4) ? N4 N5 . 1.215(4) ? N4 Cu1 2_665 1.970(2) ? N5 N6 . 1.133(4) ? O3 S1 . 1.517(2) ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion O1 Cu1 N1 N2 . . -175.2(4) N4 Cu1 N1 N2 2_665 . -34.7(4) N1 Cu1 N1 N2 2_775 . 159.2(5) O3 Cu1 N1 N2 . . 53.6(4) O1 Cu1 N1 Cu1 . 2_775 25.6(6) N4 Cu1 N1 Cu1 2_665 2_775 166.06(14) N1 Cu1 N1 Cu1 2_775 2_775 0.0 O3 Cu1 N1 Cu1 . 2_775 -105.65(14) O2 Cu2 N4 N5 . . -27.1(3) O2 Cu2 N4 N5 2_665 . 152.9(3) O2 Cu2 N4 Cu1 . 2_665 114.98(12) O2 Cu2 N4 Cu1 2_665 2_665 -65.02(12) O2 C4 O1 Cu1 . . 1.1(5) C3 C4 O1 Cu1 . . -178.1(3) N4 Cu1 O1 C4 2_665 . 35.2(3) N1 Cu1 O1 C4 . . 176.1(5) N1 Cu1 O1 C4 2_775 . -158.9(3) O3 Cu1 O1 C4 . . -52.0(3) O1 C4 O2 Cu2 . . -1.5(6) C3 C4 O2 Cu2 . . 177.6(3) N4 Cu2 O2 C4 2_665 . -34.0(3) N4 Cu2 O2 C4 . . 146.0(3) O1 Cu1 O3 S1 . . -177.11(17) N4 Cu1 O3 S1 2_665 . 90.44(18) N1 Cu1 O3 S1 . . -7.41(19) N1 Cu1 O3 S1 2_775 . -87.08(18) Cu1 O3 S1 C2 . . -173.7(2) Cu1 O3 S1 C1 . . 83.9(2)