#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/27/2012762.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_2012762 loop_ _publ_author_name 'Poto\catena-Poly[[(2,2'-bipyridine-\k^2^N:N')(dicyanamido-\kN)copper(II)]-\m-dicyanamido-\k^2^N:N'] ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m327 _journal_page_last m329 _journal_paper_doi 10.1107/S0108270102006625 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu (C10 H8 N2) (C2 N3)2]' _chemical_formula_moiety 'C14 H8 Cu N8' _chemical_formula_sum 'C14 H8 Cu N8' _chemical_formula_weight 351.82 _chemical_name_systematic ; catena-Poly[[(2,2'-bipyridine-\k^2^N:N')(dicyanamide-\kN)copper(II)]- \m-dicyanamide-\k^2^N:N'] ; _space_group_IT_number 9 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall 'C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 113.85(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.6495(18) _cell_length_b 17.118(4) _cell_length_c 10.568(2) _cell_measurement_reflns_used 7754 _cell_measurement_temperature 220(2) _cell_measurement_theta_max 26.05 _cell_measurement_theta_min 1.65 _cell_volume 1431.1(6) _computing_cell_refinement 'CELL in IPDS (Stoe & Cie, 1999)' _computing_data_collection 'EXPOSE in IPDS (Stoe & Cie, 1999)' _computing_data_reduction 'INTEGRATE in IPDS (Stoe & Cie, 1999)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990)' _diffrn_ambient_temperature 220(2) _diffrn_measured_fraction_theta_full 0.913 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\f scan' _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 0.028 _diffrn_reflns_av_sigmaI/netI 0.021 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 5294 _diffrn_reflns_theta_full 25.87 _diffrn_reflns_theta_max 25.87 _diffrn_reflns_theta_min 2.84 _diffrn_standards_decay_% none _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 1.538 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'FACE in IPDS (Stoe & Cie, 1999)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.633 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 708 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.25 _refine_diff_density_min -0.39 _refine_ls_abs_structure_details '(Flack, 1983), 1224 Friedel pairs' _refine_ls_abs_structure_Flack -0.012(11) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 2491 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.024 _refine_ls_R_factor_gt 0.023 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.6066P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.060 _refine_ls_wR_factor_ref 0.064 _reflns_number_gt 2434 _reflns_number_total 2491 _reflns_threshold_expression I>2\s(I) _cod_data_source_file gg1106.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_cell_volume 1431.1(5) _cod_original_sg_symbol_H-M 'C c' _cod_database_code 2012762 _cod_database_fobs_code 2012762 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+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_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cu1 -0.07395(2) -0.183633(13) -0.71806(2) 0.03066(10) Uani d . 1 . . Cu N10 -0.3290(5) -0.18665(12) -0.7987(4) 0.0323(7) Uani d . 1 . . N N20 -0.1092(3) -0.30078(12) -0.7266(3) 0.0336(6) Uani d . 1 . . N C11 -0.3984(3) -0.25867(13) -0.8158(3) 0.0298(5) Uani d . 1 . . C C12 -0.4277(4) -0.12434(15) -0.8421(3) 0.0390(6) Uani d . 1 . . C H12 -0.3785 -0.0752 -0.8326 0.047 Uiso calc R 1 . . H C13 -0.6031(4) -0.13072(19) -0.9014(3) 0.0441(7) Uani d . 1 . . C H13 -0.6704 -0.0864 -0.9307 0.053 Uiso calc R 1 . . H C14 -0.6749(4) -0.2032(2) -0.9161(4) 0.0443(7) Uani d . 1 . . C H14 -0.7919 -0.2085 -0.9542 0.053 Uiso calc R 1 . . H C15 -0.5725(3) -0.26869(17) -0.8740(3) 0.0411(6) Uani d . 1 . . C H15 -0.6195 -0.3184 -0.8845 0.049 Uiso calc R 1 . . H C21 -0.2736(3) -0.32352(13) -0.7709(3) 0.0303(6) Uani d . 1 . . C C22 0.0126(4) -0.35507(18) -0.6876(3) 0.0447(7) Uani d . 1 . . C H22 0.1248 -0.3395 -0.6572 0.054 Uiso calc R 1 . . H C23 -0.0251(4) -0.43418(18) -0.6915(4) 0.0528(10) Uani d . 1 . . C H23 0.0611 -0.4711 -0.6661 0.063 Uiso calc R 1 . . H C24 -0.1886(5) -0.45744(16) -0.7325(4) 0.0510(8) Uani d . 1 . . C H24 -0.2142 -0.5102 -0.7321 0.061 Uiso calc R 1 . . H C25 -0.3183(4) -0.40172(15) -0.7753(3) 0.0398(6) Uani d . 1 . . C H25 -0.4310 -0.4166 -0.8058 0.048 Uiso calc R 1 . . H C2 0.3182(4) -0.17978(16) -0.5806(3) 0.0382(6) Uani d . 1 . . C N2 0.1728(5) -0.19182(16) -0.6217(5) 0.0477(9) Uani d . 1 . . N N1 0.4790(5) -0.17500(18) -0.5413(5) 0.0586(10) Uani d . 1 . . N C3 0.5685(4) -0.11258(16) -0.4834(3) 0.0426(6) Uani d . 1 . . C N3 0.6617(4) -0.06218(15) -0.4330(4) 0.0617(8) Uani d . 1 . . N C5 -0.0472(4) -0.01411(18) -0.6014(3) 0.0445(7) Uani d . 1 . . C N5 -0.0680(3) -0.07777(15) -0.6359(3) 0.0484(6) Uani d . 1 . . N N4 -0.0121(6) 0.05849(19) -0.5707(4) 0.0804(12) Uani d . 1 . . N C6 -0.0491(3) -0.09740(14) -0.9821(3) 0.0338(5) Uani d . 1 . . C N6 -0.0722(3) -0.13972(14) -0.9090(3) 0.0437(5) Uani d . 1 . . N 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 0.02391(16) 0.03166(14) 0.03519(17) 0.00042(15) 0.01067(13) 0.00155(15) N10 0.0292(17) 0.0326(14) 0.0361(17) 0.0000(9) 0.0143(15) 0.0017(8) N20 0.0330(18) 0.0359(10) 0.0323(12) 0.0022(9) 0.0136(14) 0.0010(10) C11 0.0295(13) 0.0323(12) 0.0287(13) 0.0000(9) 0.0129(12) 0.0006(9) C12 0.0345(15) 0.0342(14) 0.0480(17) 0.0028(11) 0.0162(14) 0.0013(11) C13 0.0285(15) 0.0475(16) 0.0507(19) 0.0087(12) 0.0100(15) -0.0040(13) C14 0.0211(15) 0.0587(17) 0.050(2) 0.0004(14) 0.0111(16) -0.0101(16) C15 0.0275(14) 0.0446(15) 0.0487(18) -0.0072(11) 0.0130(14) -0.0085(12) C21 0.0298(15) 0.0325(12) 0.0302(14) 0.0001(9) 0.0139(14) 0.0002(9) C22 0.0392(18) 0.0465(16) 0.0471(19) 0.0153(13) 0.0160(16) 0.0103(12) C23 0.061(2) 0.0383(15) 0.060(3) 0.0210(13) 0.026(2) 0.0085(14) C24 0.072(2) 0.0273(14) 0.055(2) 0.0046(14) 0.027(2) 0.0028(11) C25 0.0472(16) 0.0343(13) 0.0388(15) -0.0038(11) 0.0182(14) 0.0005(11) C2 0.0282(16) 0.0410(16) 0.0415(18) 0.0040(10) 0.0102(15) 0.0007(10) N2 0.0279(19) 0.0478(17) 0.062(3) -0.0015(11) 0.0133(18) -0.0005(13) N1 0.0269(17) 0.0531(17) 0.087(3) 0.0008(12) 0.0139(18) -0.0168(15) C3 0.0373(16) 0.0421(14) 0.0493(18) 0.0101(12) 0.0185(15) 0.0076(12) N3 0.0462(15) 0.0441(14) 0.080(2) -0.0021(13) 0.0109(17) -0.0041(14) C5 0.0362(15) 0.0534(17) 0.0468(16) -0.0083(12) 0.0198(14) -0.0175(13) N5 0.0365(14) 0.0504(14) 0.0519(17) -0.0028(10) 0.0114(14) -0.0183(11) N4 0.117(3) 0.0609(18) 0.104(3) -0.0418(19) 0.086(3) -0.0455(18) C6 0.0284(13) 0.0347(12) 0.0388(15) 0.0044(10) 0.0140(12) 0.0029(10) N6 0.0468(14) 0.0434(12) 0.0470(14) 0.0057(10) 0.0253(13) 0.0106(10) 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' 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 N2 Cu1 N5 . . 90.46(12) yes N2 Cu1 N10 . . 172.06(15) yes N5 Cu1 N10 . . 92.19(10) yes N2 Cu1 N20 . . 93.72(11) yes N5 Cu1 N20 . . 153.26(11) yes N10 Cu1 N20 . . 80.60(9) yes N2 Cu1 N6 . . 95.29(15) yes N5 Cu1 N6 . . 94.67(11) yes N10 Cu1 N6 . . 91.95(12) yes N20 Cu1 N6 . . 111.18(11) yes C12 N10 C11 . . 119.9(3) ? C12 N10 Cu1 . . 124.5(2) ? C11 N10 Cu1 . . 115.5(2) ? C22 N20 C21 . . 119.3(2) ? C22 N20 Cu1 . . 126.0(2) ? C21 N20 Cu1 . . 114.58(16) ? N10 C11 C15 . . 121.1(3) ? N10 C11 C21 . . 114.4(3) ? C15 C11 C21 . . 124.5(2) ? N10 C12 C13 . . 121.6(3) ? N10 C12 H12 . . 119.2 ? C13 C12 H12 . . 119.2 ? C14 C13 C12 . . 119.0(3) ? C14 C13 H13 . . 120.5 ? C12 C13 H13 . . 120.5 ? C13 C14 C15 . . 119.7(3) ? C13 C14 H14 . . 120.2 ? C15 C14 H14 . . 120.2 ? C11 C15 C14 . . 118.7(3) ? C11 C15 H15 . . 120.6 ? C14 C15 H15 . . 120.6 ? N20 C21 C25 . . 121.7(2) ? N20 C21 C11 . . 114.8(2) ? C25 C21 C11 . . 123.6(2) ? N20 C22 C23 . . 121.5(3) ? N20 C22 H22 . . 119.3 ? C23 C22 H22 . . 119.3 ? C24 C23 C22 . . 119.7(3) ? C24 C23 H23 . . 120.1 ? C22 C23 H23 . . 120.1 ? C23 C24 C25 . . 119.8(3) ? C23 C24 H24 . . 120.1 ? C25 C24 H24 . . 120.1 ? C21 C25 C24 . . 118.0(3) ? C21 C25 H25 . . 121.0 ? C24 C25 H25 . . 121.0 ? N2 C2 N1 . . 172.9(3) yes C2 N2 Cu1 . . 163.6(3) yes C2 N1 C3 . . 124.0(3) yes N3 C3 N1 . . 172.6(3) yes N5 C5 N4 . . 173.0(3) yes C5 N5 Cu1 . . 167.8(2) yes C6 N4 C5 2 . 125.3(3) yes N6 C6 N4 . 2_554 171.0(3) yes C6 N6 Cu1 . . 158.2(2) yes 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 N2 . 1.963(4) yes Cu1 N5 . 2.001(2) yes Cu1 N6 . 2.159(2) yes Cu1 N10 . 2.018(4) yes Cu1 N20 . 2.025(2) yes N10 C12 . 1.327(4) ? N10 C11 . 1.351(3) ? N20 C22 . 1.339(4) ? N20 C21 . 1.362(4) ? C11 C15 . 1.387(4) ? C11 C21 . 1.486(3) ? C12 C13 . 1.392(4) ? C12 H12 . 0.9300 ? C13 C14 . 1.368(5) ? C13 H13 . 0.9300 ? C14 C15 . 1.386(5) ? C14 H14 . 0.9300 ? C15 H15 . 0.9300 ? C21 C25 . 1.389(3) ? C22 C23 . 1.389(5) ? C22 H22 . 0.9300 ? C23 C24 . 1.361(5) ? C23 H23 . 0.9300 ? C24 C25 . 1.401(4) ? C24 H24 . 0.9300 ? C25 H25 . 0.9300 ? N1 C2 . 1.283(5) yes N1 C3 . 1.316(5) yes N2 C2 . 1.171(5) yes N3 C3 . 1.154(4) yes N4 C5 . 1.289(4) yes N4 C6 2 1.291(4) yes N5 C5 . 1.140(4) yes N6 C6 . 1.134(3) yes