#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/66/2006616.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_2006616 loop_ _publ_author_name 'Land, John M.' 'Baughman, Russell G.' 'Hester, Colin A.' _publ_section_title ; Bis[2-(dimethylamino)pyridinium] Tetrachlorocobaltate(II) ; _journal_issue 10 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first IUC9700016 _journal_paper_doi 10.1107/S0108270197099435 _journal_volume 53 _journal_year 1997 _chemical_formula_iupac '(C7 H11 N2)2 [Co Cl4]' _chemical_formula_moiety 'C14 H22 Cl4 Co N4' _chemical_formula_sum 'C14 H22 Cl4 Co N4' _chemical_formula_weight 447.09 _chemical_name_systematic ; Bis(N,N-dimethyl-2-pyridin-1H-iumamine) Tetrachlorocobaltate(II) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _audit_creation_method SHELXL _cell_angle_alpha 90.00 _cell_angle_beta 102.090(12) _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 31.441(5) _cell_length_b 8.3824(11) _cell_length_c 15.409(2) _cell_measurement_reflns_used 50 _cell_measurement_temperature 288(2) _cell_measurement_theta_max 19.67 _cell_measurement_theta_min 6.29 _cell_volume 3971.0(10) _computing_cell_refinement 'P3/P4-PC Diffractometer Program' _computing_data_collection 'P3/P4-PC Diffractometer Program (Siemens, 1991a)' _computing_data_reduction 'XDISK (Siemens, 1991b)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990b)' _computing_publication_material 'SHELXTL/PC and SHELXL93' _computing_structure_refinement 'SHELXL93 (Sheldrick, 1993)' _computing_structure_solution 'SHELXS86 (Sheldrick, 1990a)' _diffrn_ambient_temperature 288(2) _diffrn_measurement_device 'Siemens P3' _diffrn_measurement_method \q/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.020 _diffrn_reflns_av_sigmaI/netI 0.0410 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 3522 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_min 2.52 _diffrn_standards_decay_% 'average of 1.7% in \s(I)'s' _diffrn_standards_interval_count 47 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.405 _exptl_absorpt_correction_T_max 0.704 _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_type 'empirical, 7 \y scans, 10 degree steps' _exptl_absorpt_process_details 'North, Phillips & Mathews (1968)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'block cut from needle' _exptl_crystal_F_000 1832 _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.277 _refine_diff_density_min -0.311 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.045 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_hydrogen_treatment ; H atoms riding, C---H 0.96 and N---H 0.90\%A; H1a & H1aa first observed in difference map ; _refine_ls_matrix_type full _refine_ls_number_parameters 212 _refine_ls_number_reflns 3444 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.095 _refine_ls_R_factor_all 0.066 _refine_ls_R_factor_obs .040 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.8355P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.096 _refine_ls_wR_factor_obs .083 _reflns_number_observed 2512 _reflns_number_total 3457 _reflns_observed_criterion >2sigma(I) _cod_data_source_file qb0019.cif _cod_data_source_block cocldmap _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0428P)^2^+1.8355P] where P = (Fo^2^+2Fc^2^)/3' 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^2^)+(0.0428P)^2^+1.8355P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 2006616 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' '-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_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 Co .0369(3) .0360(3) .0380(3) .0002(2) .0059(2) -.0013(2) Cl1 .0535(6) .0431(5) .0632(6) -.0111(5) .0025(5) .0002(5) Cl2 .0522(5) .0648(7) .0449(5) .0006(5) .0160(4) .0011(5) Cl3 .0602(6) .0471(6) .0577(6) .0175(5) .0214(5) .0099(5) Cl4 .0551(5) .0409(5) .0512(6) .0001(5) -.0096(4) -.0040(5) N1 .043(2) .061(2) .037(2) -.002(2) .0086(13) .000(2) N2 .041(2) .067(2) .043(2) .000(2) .0014(14) -.003(2) C2 .036(2) .044(2) .036(2) .006(2) .011(2) -.004(2) C3 .049(2) .063(3) .053(2) .006(2) .024(2) .009(2) C4 .062(3) .095(4) .038(2) .019(3) .017(2) .013(2) C5 .048(2) .104(4) .043(2) .015(2) .004(2) -.008(2) C6 .040(2) .077(3) .047(2) -.002(2) .006(2) -.008(2) C7 .042(2) .078(3) .075(3) -.005(2) .008(2) -.018(3) C8 .060(3) .096(4) .040(2) .005(3) .001(2) -.002(2) N1A .0375(15) .037(2) .039(2) -.0005(14) .0106(13) -.0003(14) N2A .045(2) .047(2) .045(2) .004(2) .0024(14) -.001(2) C2A .034(2) .044(2) .034(2) .002(2) .0136(15) -.003(2) C3A .048(2) .046(2) .044(2) -.009(2) .011(2) -.004(2) C4A .064(3) .036(2) .057(2) .002(2) .021(2) .004(2) C5A .050(2) .047(2) .059(2) .008(2) .016(2) .007(2) C6A .037(2) .051(2) .044(2) .003(2) .009(2) .003(2) C7A .048(2) .080(3) .061(3) .011(2) -.005(2) -.002(3) C8A .066(3) .058(3) .049(2) .016(2) .006(2) .005(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_thermal_displace_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_group _atom_site_type_symbol Co .374527(14) .16462(6) .14327(3) .03727(15) Uani d . 1 . Co Cl1 .40945(3) .40296(12) .15054(7) .0547(3) Uani d . 1 . Cl Cl2 .34522(3) .11653(13) .26298(6) .0531(3) Uani d . 1 . Cl Cl3 .42086(3) -.03770(12) .12734(7) .0537(3) Uani d . 1 . Cl Cl4 .32279(3) .16688(12) .01412(6) .0521(3) Uani d . 1 . Cl N1 .45967(9) .1773(4) -.0079(2) .0471(8) Uani d . 1 . N H1A .45750 .1345 .0446 .080 Uiso d R 1 . H N2 .52857(9) .2644(4) .0599(2) .0512(8) Uani d . 1 . N C2 .49674(11) .2552(4) -.0132(2) .0383(8) Uani d . 1 . C C3 .49872(12) .3217(5) -.0959(3) .0532(10) Uani d . 1 . C H3A .52405 .3801 -.1029 .080 Uiso d R 1 . H C4 .46455(13) .3028(6) -.1665(3) .0641(13) Uani d . 1 . C H4A .46626 .3476 -.2230 .080 Uiso d R 1 . H C5 .42739(13) .2208(6) -.1572(3) .0655(13) Uani d . 1 . C H5A .40352 .2083 -.2071 .080 Uiso d R 1 . H C6 .42547(12) .1582(5) -.0782(3) .0553(11) Uani d . 1 . C H6A .39986 .1014 -.0714 .080 Uiso d R 1 . H C7 .57040(12) .3365(6) .0561(3) .0655(12) Uani d . 1 . C H7A .56614 .4464 .0389 .050 Uiso calc R 1 . H H7B .5831 .2806 .0134 .050 Uiso calc R 1 . H H7C .5895 .3299 .1134 .050 Uiso calc R 1 . H C8 .52281(13) .2042(6) .1450(2) .0666(13) Uani d . 1 . C H8A .4969 .2491 .1586 .050 Uiso calc R 1 . H H8B .5475 .2335 .1903 .050 Uiso calc R 1 . H H8C .5203 .0901 .1424 .050 Uiso calc R 1 . H N1A .28810(8) -.1591(4) -.0702(2) .0375(7) Uani d . 1 . N H1AA .29201 -.0531 -.0637 .080 Uiso d R 1 . H N2A .22314(10) -.1069(4) -.1686(2) .0469(8) Uani d . 1 . N C2A .25122(10) -.2121(4) -.1245(2) .0361(8) Uani d . 1 . C C3A .24554(12) -.3802(5) -.1305(2) .0457(9) Uani d . 1 . C H3AA .21972 -.4251 -.1666 .080 Uiso d R 1 . H C4A .27694(13) -.4768(5) -.0847(3) .0511(10) Uani d . 1 . C H4AA .27301 -.5902 -.0893 .080 Uiso d R 1 . H C5A .31508(13) -.4159(5) -.0315(3) .0512(10) Uani d . 1 . C H5AA .33734 -.4857 -.0004 .080 Uiso d R 1 . H C6A .31954(11) -.2567(5) -.0250(2) .0437(9) Uani d . 1 . C H6AA .34510 -.2115 .0119 .080 Uiso d R 1 . H C7A .18113(12) -.1572(6) -.2211(3) .0656(12) Uani d . 1 . C H7AA .18555 -.2197 -.2707 .050 Uiso calc R 1 . H H7AB .1640 -.0648 -.2424 .050 Uiso calc R 1 . H H7AC .1661 -.2200 -.1849 .050 Uiso calc R 1 . H C8A .23107(14) .0636(5) -.1583(3) .0582(11) Uani d . 1 . C H8AA .2094 .1205 -.2001 .050 Uiso calc R 1 . H H8AB .2594 .0879 -.1691 .050 Uiso calc R 1 . H H8AC .2297 .0952 -.0991 .050 Uiso calc R 1 . H 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 5 1 -5 0 2 0 0 0 4 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 Cl2 Co Cl1 113.05(4) yes Cl2 Co Cl3 109.46(4) yes Cl1 Co Cl3 110.25(4) yes Cl2 Co Cl4 111.90(4) yes Cl1 Co Cl4 106.47(4) yes Cl3 Co Cl4 105.41(4) yes C2 N1 C6 123.6(3) yes C2 N2 C8 121.7(3) yes C2 N2 C7 120.6(3) yes C8 N2 C7 117.7(3) yes N2 C2 N1 118.5(3) yes N2 C2 C3 124.8(3) yes N1 C2 C3 116.7(3) yes C4 C3 C2 119.9(4) yes C3 C4 C5 120.9(4) yes C6 C5 C4 119.1(4) yes C5 C6 N1 119.8(4) yes C2A N1A C6A 123.8(3) yes C2A N2A C8A 121.1(3) yes C2A N2A C7A 121.3(3) yes C8A N2A C7A 117.3(3) yes N2A C2A N1A 119.3(3) yes N2A C2A C3A 124.3(3) yes N1A C2A C3A 116.4(3) yes C4A C3A C2A 119.4(4) yes C3A C4A C5A 121.9(4) yes C6A C5A C4A 118.0(4) yes C5A C6A N1A 120.4(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 Co Cl2 . 2.2641(10) yes Co Cl1 . 2.2711(11) yes Co Cl3 . 2.2821(10) yes Co Cl4 . 2.2914(10) yes N1 C2 . 1.353(4) yes N1 C6 . 1.366(5) yes N2 C2 . 1.343(4) yes N2 C8 . 1.451(5) yes N2 C7 . 1.460(5) yes C2 C3 . 1.404(5) yes C3 C4 . 1.369(6) yes C4 C5 . 1.388(6) yes C5 C6 . 1.340(6) yes N1A C2A . 1.356(4) yes N1A C6A . 1.357(4) yes N2A C2A . 1.329(4) yes N2A C8A . 1.454(5) yes N2A C7A . 1.459(5) yes C2A C3A . 1.421(5) yes C3A C4A . 1.355(5) yes C4A C5A . 1.399(5) yes C5A C6A . 1.343(5) yes