#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/22/2202249.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_2202249 loop_ _publ_author_name 'Lyakhov, Alexander S.' 'Gaponik, Pavel N.' 'Degtyarik, Michail M.' 'Ivashkevich, Ludmila S.' _publ_section_title ;The chain structure of catena-poly[[(2-tert-butyltetrazole-\kN^4^)copper(II)]-di-\m-chloro] ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m38 _journal_page_last m40 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Cu Cl2 (C5 H10 N4)]' _chemical_formula_moiety 'C5 H10 Cl2 Cu N4' _chemical_formula_sum 'C5 H10 Cl2 Cu N4' _chemical_formula_weight 260.61 _chemical_name_systematic ; catena-poly[[(2-tert-butyltetrazole-\kN^4^)copper(II)]-di-\m-chloro] ; _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_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 108.92(2) _cell_angle_beta 106.899(19) _cell_angle_gamma 97.39(2) _cell_formula_units_Z 2 _cell_length_a 6.1054(15) _cell_length_b 9.598(3) _cell_length_c 9.813(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.1 _cell_measurement_theta_min 19.2 _cell_volume 504.5(3) _computing_cell_refinement 'R3m Software' _computing_data_collection 'R3m Software (Nicolet, 1980)' _computing_data_reduction 'R3m Software' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2002)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Nicolet R3m four-circle' _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.028 _diffrn_reflns_av_sigmaI/netI 0.019 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3216 _diffrn_reflns_theta_full 30.1 _diffrn_reflns_theta_max 30.1 _diffrn_reflns_theta_min 2.3 _diffrn_standards_decay_% 0.6 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 2.65 _exptl_absorpt_correction_T_max 0.778 _exptl_absorpt_correction_T_min 0.299 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 262 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.04 _refine_diff_density_min -0.87 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 2961 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.06 _refine_ls_R_factor_all 0.039 _refine_ls_R_factor_gt 0.035 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0593P)^2^+0.2094P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.095 _refine_ls_wR_factor_ref 0.098 _reflns_number_gt 2663 _reflns_number_total 2961 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6146.cif _[local]_cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times). Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (10 times). Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 504.5(2) _cod_database_code 2202249 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 _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 0.22407(4) 0.41412(3) 0.49362(3) 0.03175(10) Uani d . 1 . . Cu Cl1 0.59253(8) 0.45976(6) 0.66413(6) 0.03636(12) Uani d . 1 . . Cl Cl2 0.16180(9) 0.62584(6) 0.65569(6) 0.04406(15) Uani d . 1 . . Cl N1 0.3290(4) -0.0171(3) 0.3036(3) 0.0648(7) Uani d . 1 . . N N2 0.0982(3) -0.03464(19) 0.2408(2) 0.0350(3) Uani d . 1 . . N N3 0.0305(3) 0.0903(2) 0.2848(2) 0.0417(4) Uani d . 1 . . N N4 0.2226(3) 0.1962(2) 0.3855(2) 0.0369(4) Uani d . 1 . . N C5 0.4010(5) 0.1278(3) 0.3940(4) 0.0607(8) Uani d . 1 . . C H5 0.5573 0.1769 0.4563 0.073 Uiso calc R 1 . . H C6 -0.0690(4) -0.1850(2) 0.1303(3) 0.0394(4) Uani d . 1 . . C C7 -0.2789(5) -0.1530(3) 0.0281(4) 0.0599(7) Uani d . 1 . . C H7A -0.3599 -0.0984 0.0898 0.090 Uiso calc R 1 . . H H7B -0.3846 -0.2472 -0.0475 0.090 Uiso calc R 1 . . H H7C -0.2250 -0.0931 -0.0228 0.090 Uiso calc R 1 . . H C8 0.0642(6) -0.2725(3) 0.0382(4) 0.0661(8) Uani d . 1 . . C H8A 0.1124 -0.2173 -0.0184 0.099 Uiso calc R 1 . . H H8B -0.0365 -0.3704 -0.0323 0.099 Uiso calc R 1 . . H H8C 0.2011 -0.2854 0.1069 0.099 Uiso calc R 1 . . H C9 -0.1393(7) -0.2653(4) 0.2264(4) 0.0780(10) Uani d . 1 . . C H9A -0.0004 -0.2756 0.2956 0.117 Uiso calc R 1 . . H H9B -0.2407 -0.3641 0.1599 0.117 Uiso calc R 1 . . H H9C -0.2215 -0.2071 0.2845 0.117 Uiso calc R 1 . . H 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 0.02355(13) 0.03013(14) 0.03111(14) 0.00532(9) 0.00740(9) 0.00112(10) Cl1 0.0283(2) 0.0393(3) 0.0319(2) 0.00523(18) 0.00467(17) 0.00819(19) Cl2 0.0266(2) 0.0424(3) 0.0398(3) 0.00939(19) 0.00530(19) -0.0082(2) N1 0.0396(11) 0.0377(11) 0.0812(17) 0.0125(9) -0.0026(11) -0.0019(11) N2 0.0344(8) 0.0298(8) 0.0328(8) 0.0065(6) 0.0080(7) 0.0059(6) N3 0.0314(8) 0.0319(8) 0.0458(10) 0.0053(7) 0.0086(7) 0.0002(7) N4 0.0316(8) 0.0305(8) 0.0370(8) 0.0053(6) 0.0075(7) 0.0032(7) C5 0.0364(12) 0.0378(12) 0.0744(19) 0.0097(9) -0.0034(12) -0.0005(12) C6 0.0376(10) 0.0292(9) 0.0383(10) 0.0011(8) 0.0081(8) 0.0039(8) C7 0.0442(13) 0.0483(14) 0.0569(15) 0.0058(11) -0.0026(12) 0.0026(12) C8 0.0578(16) 0.0510(15) 0.0569(16) 0.0118(12) 0.0136(13) -0.0136(12) C9 0.085(2) 0.0624(19) 0.081(2) -0.0088(17) 0.0273(19) 0.0328(17) 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 Cl1 . 2.2661(9) yes Cu1 Cl2 2_566 2.2892(9) yes Cu1 Cl2 . 2.2931(9) yes Cu1 Cl1 2_666 2.6438(8) yes Cu1 N4 . 2.0131(19) yes N1 N2 . 1.327(3) yes N1 C5 . 1.316(3) yes N2 N3 . 1.300(2) yes N2 C6 . 1.504(3) ? N3 N4 . 1.324(2) yes N4 C5 . 1.339(3) yes C5 H5 . 0.9300 ? C6 C9 . 1.512(4) ? C6 C8 . 1.515(4) ? C6 C7 . 1.516(4) ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? C8 H8A . 0.9600 ? C8 H8B . 0.9600 ? C8 H8C . 0.9600 ? C9 H9A . 0.9600 ? C9 H9B . 0.9600 ? C9 H9C . 0.9600 ? 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' Cl Cl 0.1484 0.1585 '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 N4 Cu1 Cl1 . . 91.54(6) N4 Cu1 Cl2 . 2_566 91.39(6) Cl1 Cu1 Cl2 . 2_566 173.63(2) N4 Cu1 Cl2 . . 161.22(6) Cl1 Cu1 Cl2 . . 90.59(4) Cl2 Cu1 Cl2 2_566 . 84.83(4) N4 Cu1 Cl1 . 2_666 99.64(6) Cl1 Cu1 Cl1 . 2_666 89.26(3) Cl2 Cu1 Cl1 2_566 2_666 95.82(3) Cl2 Cu1 Cl1 . 2_666 99.05(3) Cu1 Cl1 Cu1 . 2_666 90.74(3) Cu1 Cl2 Cu1 2_566 . 95.17(4) C5 N1 N2 . . 102.2(2) N3 N2 N1 . . 113.55(18) N3 N2 C6 . . 123.33(18) N1 N2 C6 . . 123.12(18) N2 N3 N4 . . 106.15(18) N3 N4 C5 . . 106.08(19) N3 N4 Cu1 . . 123.85(14) C5 N4 Cu1 . . 130.06(16) N1 C5 N4 . . 111.9(2) N1 C5 H5 . . 124.0 N4 C5 H5 . . 124.0 N2 C6 C9 . . 106.9(2) N2 C6 C8 . . 107.18(19) C9 C6 C8 . . 111.1(3) N2 C6 C7 . . 107.66(19) C9 C6 C7 . . 112.1(3) C8 C6 C7 . . 111.6(2) C6 C7 H7A . . 109.5 C6 C7 H7B . . 109.5 H7A C7 H7B . . 109.5 C6 C7 H7C . . 109.5 H7A C7 H7C . . 109.5 H7B C7 H7C . . 109.5 C6 C8 H8A . . 109.5 C6 C8 H8B . . 109.5 H8A C8 H8B . . 109.5 C6 C8 H8C . . 109.5 H8A C8 H8C . . 109.5 H8B C8 H8C . . 109.5 C6 C9 H9A . . 109.5 C6 C9 H9B . . 109.5 H9A C9 H9B . . 109.5 C6 C9 H9C . . 109.5 H9A C9 H9C . . 109.5 H9B C9 H9C . . 109.5 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 N4 Cu1 Cl1 Cu1 . 2_666 99.62(6) Cl2 Cu1 Cl1 Cu1 . 2_666 -99.04(3) Cl1 Cu1 Cl1 Cu1 2_666 2_666 0.0 N4 Cu1 Cl2 Cu1 . 2_566 -79.02(17) Cl1 Cu1 Cl2 Cu1 . 2_566 -175.57(2) Cl2 Cu1 Cl2 Cu1 2_566 2_566 0.0 Cl1 Cu1 Cl2 Cu1 2_666 2_566 95.08(3) C5 N1 N2 N3 . . 1.6(3) C5 N1 N2 C6 . . -177.9(2) N1 N2 N3 N4 . . -2.0(3) C6 N2 N3 N4 . . 177.52(18) N2 N3 N4 C5 . . 1.4(3) N2 N3 N4 Cu1 . . -179.71(14) Cl1 Cu1 N4 N3 . . 166.62(18) Cl2 Cu1 N4 N3 2_566 . -7.73(18) Cl2 Cu1 N4 N3 . . 70.2(3) Cl1 Cu1 N4 N3 2_666 . -103.87(18) Cl1 Cu1 N4 C5 . . -14.8(3) Cl2 Cu1 N4 C5 2_566 . 170.8(3) Cl2 Cu1 N4 C5 . . -111.2(3) Cl1 Cu1 N4 C5 2_666 . 74.7(3) N2 N1 C5 N4 . . -0.7(4) N3 N4 C5 N1 . . -0.5(4) Cu1 N4 C5 N1 . . -179.2(2) N3 N2 C6 C9 . . -93.3(3) N1 N2 C6 C9 . . 86.2(3) N3 N2 C6 C8 . . 147.5(2) N1 N2 C6 C8 . . -33.0(3) N3 N2 C6 C7 . . 27.3(3) N1 N2 C6 C7 . . -153.2(3) _cod_database_fobs_code 2202249 _journal_paper_doi 10.1107/S1600536802023085