#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/06/2240609.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_2240609
loop_
_publ_author_name
'Mghandef, Marwa'
'Boughzala, Habib'
_publ_section_title
;
 Crystal structure of bis(2-amino-5-chloropyridinium)
 tetrachloridocobaltate(II)
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              555
_journal_page_last               557
_journal_paper_doi               10.1107/S2056989015007707
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '(C5 H6 Cl N2)2 [Co Cl4]'
_chemical_formula_moiety         '2(C5 H6 Cl N2 +), Cl4 Co 2-'
_chemical_formula_sum            'C10 H12 Cl6 Co N4'
_chemical_formula_weight         459.87
_chemical_name_systematic
;
Bis(2-amino-5-chloropyridinium) tetrachloridocobaltate(II)
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.858(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.519(2)
_cell_length_b                   14.945(3)
_cell_length_c                   8.725(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1760.6(6)
_computing_cell_refinement
;
CAD-4 EXPRESS (Enraf--Nonius, 1994)
;
_computing_data_collection
;
CAD-4 EXPRESS (Enraf--Nonius, 1994)
;
_computing_data_reduction
;
XCAD4 (Harms & Wocadlo, 1995)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2008)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       'non-profiled ω/2τ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6241
_diffrn_reflns_theta_full        26.96
_diffrn_reflns_theta_max         26.96
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        6
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_T_max  0.6489
_exptl_absorpt_correction_T_min  0.4232
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al., 1968)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             916
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.335
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0443P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                2121
_reflns_number_total             3707
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5146sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C10 H12 Cl6 Co1 N4'
_cod_database_code               2240609
_cod_database_fobs_code          2240609
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_type_symbol
_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_symmetry_multiplicity
Co Co 0.75262(3) 0.48488(3) 0.01742(6) 0.03927(16) Uani d . 1 1
Cl Cl1 0.66040(7) 0.47789(7) -0.20888(12) 0.0475(3) Uani d . 1 1
Cl Cl2 0.64020(8) 0.48540(8) 0.20135(13) 0.0580(3) Uani d . 1 1
Cl Cl3 0.85951(8) 0.60044(7) 0.05556(14) 0.0580(3) Uani d . 1 1
Cl Cl4 0.84305(8) 0.35504(7) 0.03059(15) 0.0690(4) Uani d . 1 1
Cl Cl5 0.83772(8) 0.37281(8) 0.53616(14) 0.0646(3) Uani d . 1 1
Cl Cl6 0.68358(8) 0.75291(9) 0.29194(14) 0.0672(4) Uani d . 1 1
N N1 0.9792(2) 0.7278(2) 0.7188(4) 0.0616(11) Uani d . 1 1
H H1A 1.0247 0.7306 0.7912 0.074 Uiso calc R 1 1
H H1B 0.9565 0.7762 0.6768 0.074 Uiso calc R 1 1
N N2 0.9798(2) 0.5740(2) 0.7372(4) 0.0430(8) Uani d . 1 1
H HN2 1.0261 0.5790 0.8078 0.052 Uiso calc R 1 1
N N3 0.4647(2) 0.8197(2) 0.5514(4) 0.0444(8) Uani d . 1 1
H HN3 0.4394 0.8686 0.5834 0.053 Uiso calc R 1 1
N N4 0.3491(2) 0.7428(2) 0.6902(4) 0.0557(9) Uani d . 1 1
H H4A 0.3264 0.7931 0.7210 0.067 Uiso calc R 1 1
H H4B 0.3233 0.6935 0.7195 0.067 Uiso calc R 1 1
C C1 0.8770(3) 0.4802(3) 0.5868(5) 0.0427(9) Uani d . 1 1
C C2 0.8694(3) 0.6385(3) 0.5537(5) 0.0498(11) Uani d . 1 1
H H2 0.8425 0.6887 0.5045 0.060 Uiso calc R 1 1
C C3 0.8370(3) 0.5557(3) 0.5125(5) 0.0503(11) Uani d . 1 1
H H3 0.7880 0.5492 0.4346 0.060 Uiso calc R 1 1
C C4 0.9472(3) 0.4907(2) 0.6989(5) 0.0458(10) Uani d . 1 1
H H4 0.9736 0.4411 0.7504 0.055 Uiso calc R 1 1
C C5 0.9440(3) 0.6484(2) 0.6714(5) 0.0418(9) Uani d . 1 1
C C6 0.5837(3) 0.7483(3) 0.4092(4) 0.0451(10) Uani d . 1 1
C C7 0.5437(3) 0.6658(3) 0.4521(5) 0.0550(11) Uani d . 1 1
H H7 0.5707 0.6129 0.4168 0.066 Uiso calc R 1 1
C C8 0.4669(3) 0.6625(3) 0.5436(5) 0.0536(11) Uani d . 1 1
H H8 0.4413 0.6075 0.5720 0.064 Uiso calc R 1 1
C C9 0.4253(3) 0.7413(3) 0.5959(4) 0.0444(10) Uani d . 1 1
C C10 0.5418(3) 0.8250(3) 0.4591(4) 0.0433(9) Uani d . 1 1
H H10 0.5659 0.8804 0.4301 0.052 Uiso calc R 1 1
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'
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'
N N 0.0061 0.0033 '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
-2 8 2
1 8 1
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
Cl2 Co Cl3 109.81(5)
Cl2 Co Cl1 104.84(5)
Cl3 Co Cl1 118.58(5)
Cl2 Co Cl4 110.02(5)
Cl3 Co Cl4 107.65(5)
Cl1 Co Cl4 105.73(4)
C5 N1 H1A 120.0
C5 N1 H1B 120.0
H1A N1 H1B 120.0
C5 N2 C4 123.6(3)
C5 N2 HN2 118.2
C4 N2 HN2 118.2
C10 N3 C9 123.3(3)
C10 N3 HN3 118.4
C9 N3 HN3 118.4
C9 N4 H4A 120.0
C9 N4 H4B 120.0
H4A N4 H4B 120.0
C4 C1 C3 119.2(4)
C4 C1 Cl5 119.4(3)
C3 C1 Cl5 121.4(3)
C3 C2 C5 119.9(4)
C3 C2 H2 120.0
C5 C2 H2 120.0
C2 C3 C1 120.1(4)
C2 C3 H3 119.9
C1 C3 H3 119.9
C1 C4 N2 119.9(4)
C1 C4 H4 120.1
N2 C4 H4 120.1
N2 C5 N1 119.5(3)
N2 C5 C2 117.2(3)
N1 C5 C2 123.3(3)
C10 C6 C7 118.8(4)
C10 C6 Cl6 120.2(3)
C7 C6 Cl6 120.9(3)
C8 C7 C6 120.7(4)
C8 C7 H7 119.7
C6 C7 H7 119.7
C7 C8 C9 120.1(4)
C7 C8 H8 120.0
C9 C8 H8 120.0
N4 C9 N3 118.9(4)
N4 C9 C8 123.1(4)
N3 C9 C8 117.9(4)
N3 C10 C6 119.2(4)
N3 C10 H10 120.4
C6 C10 H10 120.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co Cl2 2.2645(12) y
Co Cl3 2.2657(11) y
Co Cl1 2.2843(12) y
Co Cl4 2.2934(12) y
Cl5 C1 1.741(4) ?
Cl6 C6 1.735(4) ?
N1 C5 1.337(5) ?
N1 H1A 0.8600 ?
N1 H1B 0.8600 ?
N2 C5 1.331(4) ?
N2 C4 1.357(5) ?
N2 HN2 0.8600 ?
N3 C10 1.351(5) ?
N3 C9 1.352(5) ?
N3 HN3 0.8600 ?
N4 C9 1.351(5) ?
N4 H4A 0.8600 ?
N4 H4B 0.8600 ?
C1 C4 1.337(5) ?
C1 C3 1.397(6) ?
C2 C3 1.355(6) ?
C2 C5 1.410(5) ?
C2 H2 0.9300 ?
C3 H3 0.9300 ?
C4 H4 0.9300 ?
C6 C10 1.360(5) ?
C6 C7 1.405(6) ?
C7 C8 1.342(6) ?
C7 H7 0.9300 ?
C8 C9 1.392(6) ?
C8 H8 0.9300 ?
C10 H10 0.9300 ?
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
N1 H1A Cl4 3_766 0.860 2.641 3.400(4) 147.94
N1 H1B Cl3 4_576 0.860 2.470 3.317(3) 168.71
N2 HN2 Cl4 3_766 0.860 2.417 3.238(3) 159.98
N3 HN3 Cl1 2_655 0.860 2.415 3.251(3) 164.25
N4 H4A Cl1 2_655 0.860 2.769 3.519(4) 146.60
N4 H4B Cl2 3_666 0.860 2.799 3.541(4) 145.38
