#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:50:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178826 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/80/4108042.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4108042
loop_
_publ_author_name
'Guillermo Mínguez Espallargas'
'Lee Brammer'
'David R. Allan'
'Colin R. Pulham'
'Neil Robertson'
'John E. Warren'
_publ_section_title
;
 Noncovalent Interactions under Extreme Conditions: High-Pressure and
 Low-Temperature Diffraction Studies of the Isostructural Metal-Organic
 Networks (4-Chloropyridinium)2[CoX4] (X = Cl, Br)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9058
_journal_page_last               9071
_journal_paper_doi               10.1021/ja8010868
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         '2(C5 H5 Cl N), Cl4 Co'
_chemical_formula_sum            'C10 H10 Cl6 Co N2'
_chemical_formula_weight         429.83
_chemical_name_systematic
;
 ?
;
_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'
_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                 101.164(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4411(7)
_cell_length_b                   6.9803(6)
_cell_length_c                   13.3444(6)
_cell_measurement_reflns_used    1096
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      19.38
_cell_measurement_theta_min      2.93
_cell_volume                     1502.47(16)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.537
_diffrn_measured_fraction_theta_max 0.537
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           X-rays
_diffrn_radiation_wavelength     0.48800
_diffrn_reflns_av_R_equivalents  0.0618
_diffrn_reflns_av_sigmaI/netI    0.0590
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            4761
_diffrn_reflns_theta_full        20.50
_diffrn_reflns_theta_max         20.50
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    0.754
_exptl_absorpt_correction_T_max  0.8959
_exptl_absorpt_correction_T_min  0.8234
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_description       block
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     87
_refine_ls_number_reflns         1250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0722
_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)+(0.0475P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.1015
_reflns_number_gt                855
_reflns_number_total             1250
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8010868-file002_23.cif
_cod_data_source_block           cocl05s
_cod_database_code               4108042
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_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.5000 0.44359(19) 0.2500 0.0293(4) Uani 1 2 d S
Cl1 Cl 0.40736(5) 0.2714(3) 0.31338(8) 0.0431(6) Uani 1 1 d .
Cl2 Cl 0.57505(5) 0.6573(3) 0.35913(8) 0.0429(6) Uani 1 1 d .
N1 N 0.90026(17) 0.3068(8) 0.3835(3) 0.0373(17) Uani 1 1 d .
H1 H 0.9331 0.2609 0.3465 0.045 Uiso 1 1 calc R
C2 C 0.8249(2) 0.3625(10) 0.3377(3) 0.038(2) Uani 1 1 d .
H2 H 0.8081 0.3486 0.2675 0.045 Uiso 1 1 calc R
C3 C 0.7718(2) 0.4404(10) 0.3942(3) 0.036(2) Uani 1 1 d .
H3 H 0.7191 0.4813 0.3633 0.043 Uiso 1 1 calc R
C4 C 0.79893(19) 0.4563(9) 0.4978(3) 0.0267(18) Uani 1 1 d .
Cl4 Cl 0.73362(5) 0.5509(3) 0.57145(7) 0.0362(5) Uani 1 1 d .
C5 C 0.8772(2) 0.3941(11) 0.5441(3) 0.034(2) Uani 1 1 d .
H5 H 0.8952 0.4033 0.6145 0.041 Uiso 1 1 calc R
C6 C 0.9270(2) 0.3189(11) 0.4834(3) 0.038(2) Uani 1 1 d .
H6 H 0.9799 0.2760 0.5123 0.046 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0245(3) 0.0291(13) 0.0354(4) 0.000 0.0084(3) 0.000
Cl1 0.0379(5) 0.0482(19) 0.0465(6) 0.0061(7) 0.0166(4) -0.0080(6)
Cl2 0.0243(4) 0.0473(19) 0.0545(6) -0.0180(7) 0.0015(4) 0.0014(5)
N1 0.0300(14) 0.043(6) 0.0426(18) 0.003(2) 0.0161(13) 0.0032(18)
C2 0.0395(19) 0.045(8) 0.0290(18) -0.003(3) 0.0092(14) 0.000(2)
C3 0.0273(15) 0.045(7) 0.0355(19) 0.000(3) 0.0056(13) -0.001(2)
C4 0.0277(15) 0.021(6) 0.0332(18) 0.003(2) 0.0109(13) -0.0007(19)
Cl4 0.0378(4) 0.0379(17) 0.0363(5) -0.0027(6) 0.0153(4) 0.0010(5)
C5 0.0357(18) 0.035(8) 0.0302(18) -0.003(3) 0.0010(14) 0.000(2)
C6 0.0263(16) 0.037(8) 0.049(2) 0.001(3) 0.0043(15) 0.003(2)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0020 0.0007 '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 -0.0030 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.0646 0.0747 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.1848 0.4883 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Cl1 Co1 Cl1 114.82(10) 2_655 .
Cl1 Co1 Cl2 105.70(4) 2_655 .
Cl1 Co1 Cl2 115.85(4) . .
Cl1 Co1 Cl2 115.86(4) 2_655 2_655
Cl1 Co1 Cl2 105.69(4) . 2_655
Cl2 Co1 Cl2 98.01(9) . 2_655
C6 N1 C2 122.8(3) . .
C6 N1 H1 118.6 . .
C2 N1 H1 118.6 . .
N1 C2 C3 120.0(3) . .
N1 C2 H2 120.0 . .
C3 C2 H2 120.0 . .
C2 C3 C4 118.0(4) . .
C2 C3 H3 121.0 . .
C4 C3 H3 121.0 . .
C3 C4 C5 121.1(4) . .
C3 C4 Cl4 119.3(3) . .
C5 C4 Cl4 119.6(3) . .
C6 C5 C4 117.9(3) . .
C6 C5 H5 121.0 . .
C4 C5 H5 121.0 . .
N1 C6 C5 120.2(4) . .
N1 C6 H6 119.9 . .
C5 C6 H6 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Cl1 2.2311(13) 2_655
Co1 Cl1 2.2312(13) .
Co1 Cl2 2.2746(16) .
Co1 Cl2 2.2746(16) 2_655
N1 C6 1.324(5) .
N1 C2 1.330(5) .
N1 H1 0.8600 .
C2 C3 1.370(6) .
C2 H2 0.9300 .
C3 C4 1.372(5) .
C3 H3 0.9300 .
C4 C5 1.386(5) .
C4 Cl4 1.722(4) .
C5 C6 1.364(6) .
C5 H5 0.9300 .
C6 H6 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
C6 N1 C2 C3 1.5(10)
N1 C2 C3 C4 -0.7(10)
C2 C3 C4 C5 -0.5(10)
C2 C3 C4 Cl4 -179.3(5)
C3 C4 C5 C6 0.9(10)
Cl4 C4 C5 C6 179.6(5)
C2 N1 C6 C5 -1.2(10)
C4 C5 C6 N1 -0.1(10)
