#------------------------------------------------------------------------------ #$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $ #$Revision: 25271 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2012585.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_2012585 loop_ _publ_author_name 'N\"ather, Christian' 'Je\&s, Inke' _publ_section_title ; catena-Poly[[bis(nicotinamide-\kN^1^)copper(I)]-\m-thiocyanato-\k^2^N:S] ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m190 _journal_page_last m192 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Cu (C6 H6 N2 O)2 (C N S)]' _chemical_formula_moiety 'C13 H12 Cu N5 O2 S' _chemical_formula_sum 'C13 H12 Cu N5 O2 S' _chemical_formula_weight 365.88 _chemical_name_common ; poly[(\m~2~-thiocyanato-N,S)-bis(nicotinamide-N)copper(I) ; _chemical_name_systematic ; catena-Poly[[bis(nicotinamide-\kN^1^)copper(I)]-\m-thiocyanato-\k^2^N:S] ; _space_group_IT_number 62 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2n' _symmetry_space_group_name_H-M 'P n m a' _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 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9304(4) _cell_length_b 21.3533(12) _cell_length_c 7.5895(3) _cell_measurement_reflns_used 8000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26 _cell_measurement_theta_min 3 _cell_volume 1447.27(12) _computing_cell_refinement IPDS _computing_data_collection 'IPDS (Stoe & Cie, 1998)' _computing_data_reduction IPDS _computing_molecular_graphics 'XP in SHELXTL (Bruker AXS, 1997)' _computing_publication_material 'CIFTAB in SHELXL97' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full .992 _diffrn_measured_fraction_theta_max .992 _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method '\f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .044 _diffrn_reflns_av_sigmaI/netI .022 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 11282 _diffrn_reflns_theta_full 25.98 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_min 1.91 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 1.667 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.679 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 744 _exptl_crystal_size_max .12 _exptl_crystal_size_mid .09 _exptl_crystal_size_min .05 _refine_diff_density_max .30 _refine_diff_density_min -.43 _refine_ls_extinction_coef .0084(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL97 (Sheldrick, 1997)' _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 107 _refine_ls_number_reflns 1446 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.104 _refine_ls_R_factor_all .042 _refine_ls_R_factor_gt .030 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0398P)^2^+0.7777P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .073 _refine_ls_wR_factor_ref .078 _reflns_number_gt 1172 _reflns_number_total 1446 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ln1135.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M Pnma _cod_database_code 2012585 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -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_type_symbol Cu1 .75590(4) .2500 .62891(6) .03028(17) Uani d S 1 Cu S1 .76638(9) .2500 .93515(13) .0400(3) Uani d S 1 S C1 .5462(2) .36175(10) .6268(3) .0243(5) Uani d . 1 C H1 .5456 .3559 .7482 .029 Uiso calc R 1 H C2 .4521(2) .40667(10) .5560(3) .0236(5) Uani d . 1 C C3 .4507(3) .41488(11) .3753(3) .0361(6) Uani d . 1 C H3 .3860 .4435 .3229 .043 Uiso calc R 1 H C4 .5480(4) .37949(13) .2744(4) .0477(7) Uani d . 1 C H4 .5517 .3848 .1529 .057 Uiso calc R 1 H C5 .6390(3) .33648(12) .3552(3) .0392(6) Uani d . 1 C H5 .7045 .3132 .2860 .047 Uiso calc R 1 H C6 .3485(2) .44396(10) .6696(3) .0263(5) Uani d . 1 C N1 .6378(2) .32644(8) .5295(3) .0276(4) Uani d . 1 N N2 .3939(2) .45502(10) .8325(3) .0350(5) Uani d . 1 N H1N2 .4850 .4483 .8643 .053 Uiso d R 1 H H2N2 .3416 .4779 .9023 .053 Uiso d R 1 H O1 .22639(18) .46248(9) .6120(2) .0380(4) Uani d . 1 O C7 .5838(3) .2500 .9612(4) .0254(7) Uani d S 1 C N3 .4560(3) .2500 .9782(4) .0385(7) Uani d S 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 .0233(2) .0290(2) .0385(3) .000 .00260(17) .000 S1 .0241(4) .0657(6) .0302(5) .000 .0001(3) .000 C1 .0258(10) .0245(10) .0226(12) .0013(9) -.0003(9) .0012(9) C2 .0219(10) .0220(10) .0268(12) -.0014(8) .0000(9) .0016(9) C3 .0447(13) .0328(12) .0306(14) .0103(11) -.0037(11) .0069(11) C4 .076(2) .0462(16) .0209(14) .0174(15) .0056(13) .0042(11) C5 .0530(15) .0335(13) .0310(16) .0112(12) .0120(11) -.0025(11) C6 .0225(10) .0248(10) .0315(13) .0015(8) .0022(9) .0065(9) N1 .0307(10) .0224(9) .0298(12) .0028(7) .0018(8) -.0011(8) N2 .0280(10) .0438(12) .0333(12) .0130(9) -.0011(8) -.0078(9) O1 .0244(8) .0497(11) .0399(11) .0132(7) -.0014(7) .0074(8) C7 .0290(17) .0269(15) .0202(17) .000 -.0043(13) .000 N3 .0243(15) .0511(19) .0401(19) .000 -.0056(13) .000 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu .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 N3 Cu1 N1 6_657 . 108.10(8) y N1 Cu1 N1 7_565 . 103.05(10) y N3 Cu1 S1 6_657 . 112.15(10) y N1 Cu1 S1 . . 112.46(6) y C7 S1 Cu1 . . 94.61(12) n N1 C1 C2 . . 123.3(2) n N1 C1 H1 . . 118.4 n C2 C1 H1 . . 118.4 n C3 C2 C1 . . 118.6(2) n C3 C2 C6 . . 120.0(2) n C1 C2 C6 . . 121.4(2) n C4 C3 C2 . . 118.3(2) n C4 C3 H3 . . 120.8 n C2 C3 H3 . . 120.8 n C5 C4 C3 . . 119.4(2) n C5 C4 H4 . . 120.3 n C3 C4 H4 . . 120.3 n N1 C5 C4 . . 123.0(2) n N1 C5 H5 . . 118.5 n C4 C5 H5 . . 118.5 n O1 C6 N2 . . 122.9(2) n O1 C6 C2 . . 120.7(2) n N2 C6 C2 . . 116.39(19) n C1 N1 C5 . . 117.4(2) n C1 N1 Cu1 . . 123.47(16) n C5 N1 Cu1 . . 118.59(16) n C6 N2 H1N2 . . 121.5 n C6 N2 H2N2 . . 120.8 n H1N2 N2 H2N2 . . 115.9 n N3 C7 S1 . . 179.5(3) n C7 N3 Cu1 . 6_557 149.1(3) n 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 N3 6_657 1.963(3) y Cu1 N1 . 2.0848(18) y Cu1 S1 . 2.3261(11) y S1 C7 . 1.642(3) n C1 N1 . 1.336(3) n C1 C2 . 1.384(3) n C1 H1 . .9300 n C2 C3 . 1.383(3) n C2 C6 . 1.494(3) n C3 C4 . 1.383(4) n C3 H3 . .9300 n C4 C5 . 1.371(4) n C4 H4 . .9300 n C5 N1 . 1.339(3) n C5 H5 . .9300 n C6 O1 . 1.240(3) n C6 N2 . 1.322(3) n N2 H1N2 . .8600 n N2 H2N2 . .8600 n C7 N3 . 1.149(4) n loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N2 H1N2 O1 6_657 .86 2.18 3.003(3) 159 N2 H2N2 O1 2_565 .86 2.13 2.959(3) 163 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 _geom_torsion_publ_flag N3 Cu1 S1 C7 6_657 180.0 n N1 Cu1 S1 C7 . 57.91(6) n N1 C1 C2 C3 . 1.1(3) n N1 C1 C2 C6 . 178.4(2) n C1 C2 C3 C4 . -2.6(4) n C6 C2 C3 C4 . -179.9(2) n C2 C3 C4 C5 . 1.8(4) n C3 C4 C5 N1 . .5(5) n C3 C2 C6 O1 . 28.7(3) n C1 C2 C6 O1 . -148.6(2) n C3 C2 C6 N2 . -152.0(2) n C1 C2 C6 N2 . 30.7(3) n C2 C1 N1 C5 . 1.2(3) n C2 C1 N1 Cu1 . -170.54(16) n C4 C5 N1 C1 . -2.1(4) n C4 C5 N1 Cu1 . 170.1(2) n N3 Cu1 N1 C1 6_657 -140.89(18) n N1 Cu1 N1 C1 7_565 104.82(17) n S1 Cu1 N1 C1 . -16.54(19) n N3 Cu1 N1 C5 6_657 47.4(2) n N1 Cu1 N1 C5 7_565 -66.9(2) n S1 Cu1 N1 C5 . 171.77(17) n