#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/05/2200570.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_2200570 loop_ _publ_author_name 'Ivashkevich, Dmitry O.' 'Lyakhov, Alexander S.' 'Gaponik, Pavel N.' 'Bogatikov, Andrey N.' 'Govorova, Alla A.' _publ_section_title ;Layered structure of catena-poly[[bis[1-(2-azidoethyl)tetrazole-N^4^]copper(II)]-di-\m-chloro] ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m335 _journal_page_last m337 _journal_paper_doi 10.1107/S1600536801009965 _journal_volume 57 _journal_year 2001 _chemical_formula_iupac '[Cu Cl2 (C3 H5 N7)2]' _chemical_formula_sum 'C6 H10 Cl2 Cu N14' _chemical_formula_weight 412.72 _chemical_name_systematic ; catena-poly[[bis(1-(2-azidoethyl)tetrazole-N^4^)-copper(II)]-di-\m-chloro] ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 91.87(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 15.616(2) _cell_length_b 6.702(2) _cell_length_c 7.208(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.2 _cell_measurement_theta_min 17.2 _cell_volume 754.0(7) _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)' _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 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 .71073 _diffrn_reflns_av_R_equivalents .018 _diffrn_reflns_av_sigmaI/netI .0201 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1880 _diffrn_reflns_theta_full 27.5 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 1.3 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.83 _exptl_absorpt_correction_T_max .964 _exptl_absorpt_correction_T_min .323 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_process_details '(North et al., 1968)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 414 _exptl_crystal_size_max .80 _exptl_crystal_size_mid .46 _exptl_crystal_size_min .02 _refine_diff_density_max .47 _refine_diff_density_min -.34 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 106 _refine_ls_number_reflns 1734 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.04 _refine_ls_R_factor_all .039 _refine_ls_R_factor_gt .033 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0690P)^2^+0.2230P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .097 _reflns_number_gt 1529 _reflns_number_total 1734 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ya6036.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 2200570 _cod_database_fobs_code 2200570 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 .0000 .5000 .5000 .02654(15) Uani d S 1 . . Cu Cl1 -.05746(3) .71706(7) .28493(7) .02841(16) Uani d . 1 . . Cl N1 .20604(11) .8732(3) .4690(3) .0315(4) Uani d . 1 . . N N2 .24478(14) .6972(3) .4424(4) .0463(6) Uani d . 1 . . N N3 .18738(13) .5609(3) .4586(4) .0427(5) Uani d . 1 . . N N4 .11123(10) .6469(3) .4928(2) .0259(4) Uani d . 1 . . N C5 .12436(13) .8398(3) .4984(3) .0301(4) Uani d . 1 . . C H5 .0832 .9367 .5196 .036 Uiso calc R 1 . . H C6 .25272(17) 1.0620(4) .4532(5) .0462(6) Uani d . 1 . . C H6A .2165 1.1709 .4920 .055 Uiso calc R 1 . . H H6B .2664 1.0841 .3245 .055 Uiso calc R 1 . . H C7 .33252(18) 1.0609(5) .5685(5) .0493(7) Uani d . 1 . . C H7A .3692 .9516 .5327 .059 Uiso calc R 1 . . H H7B .3198 1.0459 .6986 .059 Uiso calc R 1 . . H N5 .37491(16) 1.2541(4) .5364(5) .0634(8) Uani d . 1 . . N N6 .44506(17) 1.2736(4) .6084(4) .0605(7) Uani d . 1 . . N N7 .5109(2) 1.3094(7) .6666(6) .1060(14) 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 .0247(2) .0269(2) .0280(2) -.00358(12) .00057(14) .00865(13) Cl1 .0346(3) .0283(3) .0223(3) .00035(17) .00029(19) .00461(18) N1 .0296(9) .0286(9) .0364(11) -.0046(7) .0016(7) .0013(7) N2 .0326(10) .0355(10) .0718(17) -.0034(8) .0140(10) -.0078(10) N3 .0303(9) .0305(9) .0679(16) -.0010(8) .0093(9) -.0085(10) N4 .0263(8) .0268(8) .0248(9) -.0013(6) .0034(6) .0033(7) C5 .0285(10) .0282(9) .0337(12) -.0016(8) .0008(8) .0018(8) C6 .0394(13) .0352(12) .0635(18) -.0136(11) -.0071(12) .0120(12) C7 .0439(14) .0448(13) .0585(18) -.0159(12) -.0088(13) .0069(13) N5 .0509(15) .0575(14) .081(2) -.0275(12) -.0146(14) .0163(13) N6 .0510(14) .0704(17) .0600(17) -.0302(13) .0016(12) .0021(13) N7 .064(2) .141(4) .111(3) -.052(2) -.024(2) .010(3) 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' Cl Cl .1484 .1585 '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' N N .0061 .0033 '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 N4 Cu1 Cl1 . . 89.49(5) yes N4 Cu1 Cl1 3_566 2_545 89.18(6) yes Cl1 Cu1 Cl1 . 2_545 93.35(5) yes C5 N1 N2 . . 108.5(2) yes C5 N1 C6 . . 130.1(2) yes N2 N1 C6 . . 121.3(2) yes N3 N2 N1 . . 107.0(2) yes N2 N3 N4 . . 109.5(2) yes C5 N4 N3 . . 106.8(2) yes C5 N4 Cu1 . . 128.40(10) yes N3 N4 Cu1 . . 124.40(10) yes N4 C5 N1 . . 108.3(2) yes N4 C5 H5 . . 125.9 ? N1 C5 H5 . . 125.9 ? N1 C6 C7 . . 111.4(2) yes N1 C6 H6A . . 109.3 ? C7 C6 H6A . . 109.3 ? N1 C6 H6B . . 109.3 ? C7 C6 H6B . . 109.3 ? H6A C6 H6B . . 108.0 ? C6 C7 N5 . . 106.4(2) yes C6 C7 H7A . . 110.4 ? N5 C7 H7A . . 110.4 ? C6 C7 H7B . . 110.4 ? N5 C7 H7B . . 110.4 ? H7A C7 H7B . . 108.6 ? N6 N5 C7 . . 115.7(3) yes N7 N6 N5 . . 173.1(4) 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 Cl1 . 2.2880(10) yes Cu1 Cl1 2_545 2.9560(10) yes Cu1 N4 . 1.999(2) yes N1 N2 . 1.342(3) yes N1 C5 . 1.319(3) yes N1 C6 . 1.467(3) yes N2 N3 . 1.288(3) yes N3 N4 . 1.351(3) yes N4 C5 . 1.309(3) yes C5 H5 . .9300 ? C6 C7 . 1.475(4) yes C6 H6A . .9700 ? C6 H6B . .9700 ? C7 N5 . 1.476(3) yes C7 H7A . .9700 ? C7 H7B . .9700 ? N5 N6 . 1.204(4) yes N6 N7 . 1.123(4) yes 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 C5 H5 Cl1 3_576 .93 2.75 3.529(3) 141.8 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 C5 N1 N2 N3 . -.9(3) C6 N1 N2 N3 . -177.7(2) N1 N2 N3 N4 . .9(3) N2 N3 N4 C5 . -.5(3) N2 N3 N4 Cu1 . 172.71(18) Cl1 Cu1 N4 C5 . 46.07(19) Cl1 Cu1 N4 C5 3_566 -133.93(19) Cl1 Cu1 N4 C5 2_545 139.41(18) Cl1 Cu1 N4 N3 . -125.63(19) Cl1 Cu1 N4 N3 3_566 54.37(19) Cl1 Cu1 N4 N3 2_545 -32.29(18) N3 N4 C5 N1 . -.1(3) Cu1 N4 C5 N1 . -172.95(15) N2 N1 C5 N4 . .6(3) C6 N1 C5 N4 . 177.0(2) C5 N1 C6 C7 . 132.1(3) N2 N1 C6 C7 . -51.9(4) N1 C6 C7 N5 . 178.1(3) C6 C7 N5 N6 . -174.3(3)