#------------------------------------------------------------------------------ #$Date: 2015-04-02 12:22:18 +0100 (Thu, 02 Apr 2015) $ #$Revision: 134621 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/62/2006214.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_2006214 loop_ _publ_author_name 'Parvez, Masood' 'Sabir, Aaliya P.' _publ_section_title ; Clemizole Tetrachlorocuprate(II) and Clemizole Tetrachlorocobaltate(II) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 675 _journal_page_last 677 _journal_paper_doi 10.1107/S0108270196015922 _journal_volume 53 _journal_year 1997 _chemical_formula_analytical 'C19 H22 Cl5 Co N3 ' _chemical_formula_moiety '[C19 H22 Cl N3][Co Cl4]' _chemical_formula_structural '[C19 H22 Cl N3][Co Cl4]' _chemical_formula_sum 'C19 H22 Cl5 Co N3' _chemical_formula_weight 528.60 _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' _cell_angle_alpha 90.00 _cell_angle_beta 91.110(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 7.0400(10) _cell_length_b 23.282(3) _cell_length_c 13.7300(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 200 _cell_measurement_theta_max 20.0 _cell_measurement_theta_min 10.0 _cell_volume 2250.0(5) _computing_cell_refinement 'MSC/AFC Diffractometer Control Software' _computing_data_collection ;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1988) ; _computing_data_reduction 'TEXSAN (Molecular Structure Corporation, 1995)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material TEXSAN _computing_structure_refinement TEXSAN _computing_structure_solution 'SAPI91 (Fan, 1991)' _diffrn_ambient_temperature 200 _diffrn_measurement_device 'Rigaku AFC-6S' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0855 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 4465 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 2.0 _diffrn_standards_decay_% 1.39 _diffrn_standards_interval_count 200 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.367 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_correction_T_min 0.75 _exptl_absorpt_correction_type ' empirical (North, Phillips & Mathews, 1968) ' _exptl_absorpt_process_details ' \y-scan (3 reflections) ' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_meas ? _exptl_crystal_description needle _exptl_crystal_F_000 1076.00 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.36 _refine_diff_density_min -0.42 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 2.31 _refine_ls_goodness_of_fit_obs 1.67 _refine_ls_hydrogen_treatment 'Geometrically idealized with C-H and N-H 0.95 \%A' _refine_ls_matrix_type full _refine_ls_number_parameters 253 _refine_ls_number_reflns 3992 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1134 _refine_ls_R_factor_obs .0566 _refine_ls_shift/esd_max 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.014(Fo^2^)]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1568 _refine_ls_wR_factor_obs .0809 _reflns_number_observed 2129 _reflns_number_total 4116 _reflns_observed_criterion '[I > 2.0\s(I)]' _[local]_cod_data_source_file fg1248.cif _[local]_cod_data_source_block 2 _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_chemical_formula_sum_orig 'C19 H22 Cl5 Co N3 ' _cod_depositor_comments ; The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 50 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'w = 1/[\s^2^(Fo) + 0.014(Fo^2^)] ' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo) + 0.014(Fo^2^)]'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_cell_volume 2250.0(4) _cod_database_code 2006214 loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' 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 Co1 .0297(5) .0276(5) .0298(5) .0008(5) -.0013(4) .0024(5) Cl1 .0670(10) .0270(10) .0540(10) .0034(10) .0190(10) -.0008(9) Cl2 .0460(10) .0410(10) .0300(10) -.0003(9) -.0054(8) .0050(9) Cl3 .0380(10) .0320(10) .0330(10) -.0064(8) -.0005(8) .0039(8) Cl4 .0340(10) .0420(10) .0280(10) .0029(9) -.0041(8) .0077(8) Cl5 .0480(10) .077(2) .062(2) .0120(10) -.0150(10) .0170(10) N1 .031(3) .017(3) .024(3) .000(2) .000(2) .004(2) N2 .028(3) .027(3) .020(3) .004(3) -.001(2) .001(3) N3 .048(4) .033(4) .023(3) .004(3) -.006(3) .002(3) C1 .020(4) .035(4) .019(4) .004(3) -.003(3) -.002(3) C2 .024(4) .020(4) .025(4) -.003(3) -.003(3) .000(3) C3 .041(4) .033(5) .025(4) -.002(3) .004(3) -.004(3) C4 .033(4) .034(5) .040(5) .003(3) .005(3) -.019(4) C5 .033(4) .020(4) .053(5) .002(3) -.001(4) -.010(4) C6 .029(4) .024(4) .036(4) .005(3) .000(3) .005(3) C7 .019(4) .020(4) .028(4) .001(3) .000(3) -.003(3) C8 .033(4) .029(4) .022(4) .000(3) .006(3) .003(3) C9 .034(4) .019(4) .021(4) .003(3) .003(3) -.001(3) C10 .041(4) .028(4) .031(4) -.002(3) .004(3) .003(3) C11 .048(5) .031(4) .030(4) .010(4) .004(4) .013(3) C12 .033(4) .041(5) .023(4) .005(4) -.006(3) .002(3) C13 .040(5) .027(4) .032(4) -.007(4) -.002(4) -.005(3) C14 .047(5) .020(4) .033(4) .003(3) .003(4) .005(3) C15 .040(4) .031(4) .026(4) .003(3) -.002(3) -.002(3) C16 .069(6) .036(5) .052(5) .019(5) .005(4) -.009(4) C17 .147(11) .041(6) .074(8) .016(7) .017(8) -.007(5) C18 .148(10) .044(6) .064(7) -.043(7) .042(7) -.014(5) C19 .069(6) .036(5) .053(5) -.012(4) .019(5) -.001(4) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Co1 .20782(12) .19251(4) .36375(7) .0291(3) Uani ? ? Cl1 .3096(3) .11385(8) .28750(10) .0493(6) Uani ? ? Cl2 .1835(2) .18262(8) .52840(10) .0392(6) Uani ? ? Cl3 .4188(2) .26756(7) .34450(10) .0344(5) Uani ? ? Cl4 -.0794(2) .21943(7) .29700(10) .0348(5) Uani ? ? Cl5 .3180(3) .02820(10) .9298(2) .0626(8) Uani ? ? N1 -.2858(7) .1539(2) .4672(4) .024(2) Uani ? ? N2 -.3416(7) .1100(2) .6044(4) .025(2) Uani ? ? N3 -.3818(8) .2682(2) .5501(4) .035(2) Uani ? ? C1 -.3342(9) .1612(3) .5601(4) .025(2) Uani ? ? C2 -.2565(8) .0954(3) .4498(5) .023(2) Uani ? ? C3 -.2041(9) .0654(3) .3672(5) .033(2) Uani ? ? C4 -.1895(9) .0067(3) .3767(5) .035(2) Uani ? ? C5 -.2276(9) -.0211(3) .4651(5) .035(2) Uani ? ? C6 -.2790(9) .0089(3) .5470(5) .030(2) Uani ? ? C7 -.2917(8) .0675(3) .5370(5) .022(2) Uani ? ? C8 -.3870(9) .0991(3) .7067(4) .028(2) Uani ? ? C9 -.2125(9) .0819(3) .7661(4) .025(2) Uani ? ? C10 -.2002(10) .0282(3) .8082(5) .033(2) Uani ? ? C11 -.0389(10) .0120(3) .8596(5) .036(2) Uani ? ? C12 .1107(9) .0495(3) .8685(5) .032(2) Uani ? ? C13 .1015(10) .1040(3) .8283(5) .033(2) Uani ? ? C14 -.0596(10) .1197(3) .7760(5) .033(2) Uani ? ? C15 -.3799(9) .2161(3) .6121(5) .032(2) Uani ? ? C16 -.4864(11) .3162(3) .6014(6) .052(3) Uani ? ? C17 -.3918(18) .3683(4) .5667(7) .087(4) Uani ? ? C18 -.1900(17) .3539(4) .5538(7) .085(4) Uani ? ? C19 -.1888(11) .2911(3) .5232(6) .052(3) Uani ? ? H1 -.2732 .1837 .4205 .0288 Uani ? ? H3 -.4498 .2594 .4915 .0417 Uani ? ? H31 -.1796 .0843 .3075 .0398 Uani ? ? H41 -.1528 -.0155 .3222 .0423 Uani ? ? H51 -.2176 -.0617 .4684 .0422 Uani ? ? H61 -.3043 -.0099 .6068 .0356 Uani ? ? H81 -.4392 .1330 .7338 .0332 Uani ? ? H82 -.4777 .0689 .7093 .0332 Uani ? ? H101 -.3036 .0022 .8016 .0397 Uani ? ? H111 -.0312 -.0250 .8886 .0437 Uani ? ? H131 .2044 .1301 .8365 .0399 Uani ? ? H141 -.0665 .1566 .7466 .0398 Uani ? ? H151 -.2875 .2215 .6627 .0386 Uani ? ? H152 -.5019 .2121 .6397 .0386 Uani ? ? H161 -.6173 .3163 .5834 .0624 Uani ? ? H162 -.4732 .3127 .6701 .0624 Uani ? ? H171 -.4474 .3801 .5064 .1047 Uani ? ? H172 -.4035 .3982 .6132 .1047 Uani ? ? H181 -.1369 .3774 .5047 .1020 Uani ? ? H182 -.1207 .3590 .6132 .1020 Uani ? ? H191 -.0908 .2709 .5572 .0628 Uani ? ? H192 -.1704 .2879 .4551 .0628 Uani ? ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.003 0.002 'International Tables' H 0.000 0.000 'International Tables' N 0.006 0.003 'International Tables' Cl 0.148 0.159 'International Tables' Co 0.349 0.972 'International Tables' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl1 Co1 Cl2 114.36(8) yes Cl1 Co1 Cl3 110.70(8) yes Cl1 Co1 Cl4 108.99(8) yes Cl2 Co1 Cl3 104.48(7) yes Cl2 Co1 Cl4 109.94(7) yes Cl3 Co1 Cl4 108.16(7) yes C1 N1 C2 109.1(5) yes C1 N2 C7 108.4(5) yes C1 N2 C8 126.9(5) yes C7 N2 C8 124.7(5) yes C15 N3 C16 109.6(5) yes C15 N3 C19 115.5(5) yes C16 N3 C19 107.4(5) yes N1 C1 N2 109.5(6) no N1 C1 C15 128.5(6) no N2 C1 C15 122.0(6) no N1 C2 C3 132.2(6) no N1 C2 C7 106.2(5) no C3 C2 C7 121.6(6) no C2 C3 C4 116.3(6) no C3 C4 C5 121.6(6) no C4 C5 C6 121.9(6) no C5 C6 C7 116.0(6) no N2 C7 C2 106.8(5) no N2 C7 C6 130.6(6) no C2 C7 C6 122.6(6) no N2 C8 C9 111.8(5) no C8 C9 C10 120.5(6) no C8 C9 C14 120.2(6) no C10 C9 C14 119.3(6) no C9 C10 C11 120.5(6) no C10 C11 C12 119.6(6) no Cl5 C12 C11 119.6(5) no Cl5 C12 C13 119.1(5) no C11 C12 C13 121.2(6) no C12 C13 C14 118.8(6) no C9 C14 C13 120.6(6) no N3 C15 C1 115.0(5) no N3 C16 C17 103.3(7) no C16 C17 C18 107.2(8) no C17 C18 C19 105.2(8) no N3 C19 C18 105.2(7) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 Cl1 ? ? 2.234(2) yes Co1 Cl2 ? ? 2.282(2) yes Co1 Cl3 ? ? 2.312(2) yes Co1 Cl4 ? ? 2.291(2) yes Cl5 C12 ? ? 1.743(7) yes N1 C1 ? ? 1.337(7) yes N1 C2 ? ? 1.400(7) yes N2 C1 ? ? 1.339(8) yes N2 C7 ? ? 1.405(7) yes N2 C8 ? ? 1.469(7) yes N3 C15 ? ? 1.483(8) yes N3 C16 ? ? 1.518(8) yes N3 C19 ? ? 1.512(9) yes C1 C15 ? ? 1.502(8) no C2 C3 ? ? 1.387(8) no C2 C7 ? ? 1.388(8) no C3 C4 ? ? 1.375(9) no C4 C5 ? ? 1.406(9) no C5 C6 ? ? 1.378(9) no C6 C7 ? ? 1.374(8) no C8 C9 ? ? 1.515(8) no C9 C10 ? ? 1.380(8) no C9 C14 ? ? 1.395(9) no C10 C11 ? ? 1.378(9) no C11 C12 ? ? 1.373(9) no C12 C13 ? ? 1.384(9) no C13 C14 ? ? 1.380(9) no C16 C17 ? ? 1.468(12) no C17 C18 ? ? 1.474(13) no C18 C19 ? ? 1.521(10) no