#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/97/2229728.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_2229728
loop_
_publ_author_name
'Feng, Miao'
'Mi, Huai-Feng'
'Hu, Tong-Liang'
_publ_section_title
;
 Bis[μ-1,1'-methylenebis(1H-imidazole)-κ²N³:N^3'^]bis[dichloridocobalt(II)]
;
_journal_coeditor_code           JH2275
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m491
_journal_paper_doi               10.1107/S1600536811010610
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co2 Cl4 (C7 H8 N4)2]'
_chemical_formula_moiety         'C14 H16 Cl4 Co2 N8'
_chemical_formula_sum            'C14 H16 Cl4 Co2 N8'
_chemical_formula_weight         556.01
_chemical_name_systematic
;
Bis[μ-1,1'-methylenebis(1H-imidazole)-
κ²N³:N^3'^]bis[dichloridocobalt(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                 98.75(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.7137(17)
_cell_length_b                   8.7948(18)
_cell_length_c                   14.560(3)
_cell_measurement_reflns_used    9628
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.3
_cell_volume                     1102.8(4)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku SCX-mini'
_diffrn_measurement_method       ω
_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  0.0396
_diffrn_reflns_av_sigmaI/netI    0.0316
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11057
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         3.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.7892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0402
_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/[σ²(Fo²)+(0.0240P)²+0.5905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0748
_reflns_number_gt                2004
_reflns_number_total             2501
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            jh2275.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2229728
_cod_database_fobs_code          2229728
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_disorder_assembly
_atom_site_disorder_group
Co Co1 0.71310(4) 0.17519(4) 0.29288(2) 0.03334(12) Uani d . 1 . .
Cl Cl1 0.67525(10) 0.16673(10) 0.13677(5) 0.0560(2) Uani d . 1 . .
Cl Cl2 0.86129(8) 0.37006(8) 0.35849(5) 0.04539(19) Uani d . 1 . .
N N1 0.7895(3) -0.0223(3) 0.35434(15) 0.0392(5) Uani d . 1 . .
N N2 0.2068(2) 0.2229(2) 0.55419(15) 0.0376(5) Uani d . 1 . .
N N3 0.3271(2) 0.2738(2) 0.41927(15) 0.0345(5) Uani d . 1 . .
N N4 0.5028(2) 0.2027(2) 0.33439(14) 0.0349(5) Uani d . 1 . .
C C1 0.4789(3) 0.2715(3) 0.41130(18) 0.0355(6) Uani d . 1 . .
H H1 0.5570 0.3132 0.4546 0.043 Uiso calc R 1 . .
C C2 0.3577(3) 0.1591(4) 0.2905(2) 0.0465(7) Uani d . 1 . .
H H2 0.3378 0.1069 0.2344 0.056 Uiso calc R 1 . .
C C3 0.2496(3) 0.2042(4) 0.3417(2) 0.0502(8) Uani d . 1 . .
H H3 0.1429 0.1906 0.3272 0.060 Uiso calc R 1 . .
C C4 0.2601(3) 0.3409(3) 0.4956(2) 0.0432(7) Uani d . 1 . .
H H4A 0.1734 0.4054 0.4708 0.052 Uiso calc R 1 . .
H H4B 0.3373 0.4037 0.5328 0.052 Uiso calc R 1 . .
C C5 0.7094(3) -0.1052(3) 0.4060(2) 0.0441(7) Uani d . 1 . .
H H5 0.6075 -0.0847 0.4139 0.053 Uiso calc R 1 . .
C C6 0.9327(3) -0.0932(3) 0.3608(2) 0.0459(7) Uani d . 1 . .
H H6 1.0142 -0.0610 0.3312 0.055 Uiso calc R 1 . .
C C7 0.0639(3) 0.2160(3) 0.5834(2) 0.0454(7) Uani d . 1 . .
H H7 -0.0186 0.2829 0.5678 0.054 Uiso calc R 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_
_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
N1 Co1 N4 . . 102.85(9) ?
N1 Co1 Cl1 . . 114.03(7) ?
N4 Co1 Cl1 . . 107.75(7) ?
N1 Co1 Cl2 . . 109.58(7) ?
N4 Co1 Cl2 . . 105.46(7) ?
Cl1 Co1 Cl2 . . 115.95(4) ?
C5 N1 C6 . . 105.2(2) ?
C5 N1 Co1 . . 124.02(18) ?
C6 N1 Co1 . . 130.55(18) ?
C5 N2 C7 3_656 . 106.9(2) ?
C5 N2 C4 3_656 . 126.6(2) ?
C7 N2 C4 . . 126.4(2) ?
C1 N3 C3 . . 106.9(2) ?
C1 N3 C4 . . 125.8(2) ?
C3 N3 C4 . . 127.3(2) ?
C1 N4 C2 . . 105.6(2) ?
C1 N4 Co1 . . 125.08(18) ?
C2 N4 Co1 . . 129.31(18) ?
N4 C1 N3 . . 111.4(2) ?
N4 C1 H1 . . 124.3 ?
N3 C1 H1 . . 124.3 ?
C3 C2 N4 . . 109.3(3) ?
C3 C2 H2 . . 125.4 ?
N4 C2 H2 . . 125.4 ?
C2 C3 N3 . . 106.9(2) ?
C2 C3 H3 . . 126.6 ?
N3 C3 H3 . . 126.6 ?
N3 C4 N2 . . 111.0(2) ?
N3 C4 H4A . . 109.4 ?
N2 C4 H4A . . 109.4 ?
N3 C4 H4B . . 109.4 ?
N2 C4 H4B . . 109.4 ?
H4A C4 H4B . . 108.0 ?
N1 C5 N2 . 3_656 111.7(2) ?
N1 C5 H5 . . 124.1 ?
N2 C5 H5 3_656 . 124.1 ?
C7 C6 N1 3_656 . 109.8(2) ?
C7 C6 H6 3_656 . 125.1 ?
N1 C6 H6 . . 125.1 ?
C6 C7 N2 3_656 . 106.4(2) ?
C6 C7 H7 3_656 . 126.8 ?
N2 C7 H7 . . 126.8 ?
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
Co1 N1 . 2.020(2) ?
Co1 N4 . 2.029(2) ?
Co1 Cl1 . 2.2478(9) ?
Co1 Cl2 . 2.2676(9) ?
N1 C5 . 1.320(3) ?
N1 C6 . 1.385(3) ?
N2 C5 3_656 1.346(3) ?
N2 C7 . 1.377(3) ?
N2 C4 . 1.464(3) ?
N3 C1 . 1.346(3) ?
N3 C3 . 1.369(4) ?
N3 C4 . 1.456(3) ?
N4 C1 . 1.317(3) ?
N4 C2 . 1.381(3) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.347(4) ?
C2 H2 . 0.9300 ?
C3 H3 . 0.9300 ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 N2 3_656 1.346(3) ?
C5 H5 . 0.9300 ?
C6 C7 3_656 1.349(4) ?
C6 H6 . 0.9300 ?
C7 C6 3_656 1.349(4) ?
C7 H7 . 0.9300 ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N4 Co1 N1 C5 . . . . 1.3(3) ?
Cl1 Co1 N1 C5 . . . . -115.1(2) ?
Cl2 Co1 N1 C5 . . . . 113.1(2) ?
N4 Co1 N1 C6 . . . . -172.0(2) ?
Cl1 Co1 N1 C6 . . . . 71.6(3) ?
Cl2 Co1 N1 C6 . . . . -60.2(3) ?
N1 Co1 N4 C1 . . . . 88.2(2) ?
Cl1 Co1 N4 C1 . . . . -151.0(2) ?
Cl2 Co1 N4 C1 . . . . -26.6(2) ?
N1 Co1 N4 C2 . . . . -93.2(2) ?
Cl1 Co1 N4 C2 . . . . 27.6(3) ?
Cl2 Co1 N4 C2 . . . . 152.0(2) ?
C2 N4 C1 N3 . . . . 0.3(3) ?
Co1 N4 C1 N3 . . . . 179.13(17) ?
C3 N3 C1 N4 . . . . -1.0(3) ?
C4 N3 C1 N4 . . . . -179.9(2) ?
C1 N4 C2 C3 . . . . 0.6(3) ?
Co1 N4 C2 C3 . . . . -178.2(2) ?
N4 C2 C3 N3 . . . . -1.2(4) ?
C1 N3 C3 C2 . . . . 1.3(3) ?
C4 N3 C3 C2 . . . . -179.8(3) ?
C1 N3 C4 N2 . . . . -108.0(3) ?
C3 N3 C4 N2 . . . . 73.3(4) ?
C5 N2 C4 N3 3_656 . . . 53.1(4) ?
C7 N2 C4 N3 . . . . -130.9(3) ?
C6 N1 C5 N2 . . . 3_656 0.8(3) ?
Co1 N1 C5 N2 . . . 3_656 -173.89(18) ?
C5 N1 C6 C7 . . . 3_656 -0.5(3) ?
Co1 N1 C6 C7 . . . 3_656 173.8(2) ?
C5 N2 C7 C6 3_656 . . 3_656 -0.5(3) ?
C4 N2 C7 C6 . . . 3_656 -177.2(3) ?
