#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:50:35 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178826 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/80/4108048.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_4108048
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), Br4 Co'
_chemical_formula_sum            'C10 H10 Br4 Cl2 Co N2'
_chemical_formula_weight         607.67
_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                 100.381(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.211(2)
_cell_length_b                   7.3392(4)
_cell_length_c                   13.7246(7)
_cell_measurement_reflns_used    1443
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      18.55
_cell_measurement_theta_min      3.04
_cell_volume                     1705.2(2)
_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 0.416
_diffrn_measured_fraction_theta_max 0.416
_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  0.0748
_diffrn_reflns_av_sigmaI/netI    0.0554
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5562
_diffrn_reflns_theta_full        20.41
_diffrn_reflns_theta_max         20.41
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    3.885
_exptl_absorpt_correction_T_max  0.3957
_exptl_absorpt_correction_T_min  0.3957
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.367
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.692
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         1090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.692
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0549
_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)+(0.0354P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1381
_reflns_number_gt                740
_reflns_number_total             1090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8010868-file002_29.cif
_cod_data_source_block           cobr02s
_cod_database_code               4108048
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 0.44533(19) 0.2500 0.0327(15) Uani 1 2 d S
Br1 Br 0.40650(13) 0.26931(12) 0.31681(7) 0.0573(11) Uani 1 1 d .
Br2 Br 0.57656(12) 0.65541(11) 0.36297(7) 0.0490(11) Uani 1 1 d .
N1 N 0.89691(12) 0.30284(11) 0.38350(7) 0.0425(18) Uiso 1 1 d R
H1 H 0.9274 0.2568 0.3468 0.051 Uiso 1 1 calc R
C2 C 0.82448(12) 0.35752(11) 0.34021(7) 0.0336(18) Uiso 1 1 d R
H2 H 0.8080 0.3442 0.2722 0.040 Uiso 1 1 calc R
C3 C 0.77452(12) 0.43382(11) 0.39735(7) 0.0344(18) Uiso 1 1 d R
H3 H 0.7240 0.4720 0.3689 0.041 Uiso 1 1 calc R
C4 C 0.80181(12) 0.45187(11) 0.49838(7) 0.0353(19) Uiso 1 1 d R
Cl4 Cl 0.74067(12) 0.54669(11) 0.57126(7) 0.039(2) Uani 1 1 d R
C5 C 0.87681(12) 0.39205(11) 0.54207(7) 0.041(2) Uiso 1 1 d R
H5 H 0.8944 0.4027 0.6100 0.049 Uiso 1 1 calc R
C6 C 0.92425(12) 0.31641(11) 0.48147(7) 0.053(3) Uiso 1 1 d R
H6 H 0.9747 0.2752 0.5082 0.063 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 0.033(5) 0.0294(8) 0.0369(8) 0.000 0.0092(16) 0.000
Br1 0.073(3) 0.0530(6) 0.0509(6) 0.0079(4) 0.0241(11) -0.0142(8)
Br2 0.032(3) 0.0543(6) 0.0580(6) -0.0207(4) 0.0015(10) 0.0015(8)
Cl4 0.033(7) 0.0425(11) 0.0450(11) -0.0041(8) 0.017(2) 0.0052(16)
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'
Br Br 0.2378 1.2974 '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
Br1 Co1 Br1 114.03(8) 2_655 .
Br1 Co1 Br2 105.51(6) 2_655 .
Br1 Co1 Br2 115.52(4) . .
Br1 Co1 Br2 115.53(4) 2_655 2_655
Br1 Co1 Br2 105.50(6) . 2_655
Br2 Co1 Br2 100.23(8) . 2_655
C2 N1 C6 123.4 . .
C2 N1 H1 118.3 . .
C6 N1 H1 118.3 . .
N1 C2 C3 119.5 . .
N1 C2 H2 120.2 . .
C3 C2 H2 120.2 . .
C2 C3 C4 118.2 . .
C2 C3 H3 120.9 . .
C4 C3 H3 120.9 . .
C3 C4 C5 121.4 . .
C3 C4 Cl4 119.1 . .
C5 C4 Cl4 119.5 . .
C6 C5 C4 118.0 . .
C6 C5 H5 121.0 . .
C4 C5 H5 121.0 . .
N1 C6 C5 119.5 . .
N1 C6 H6 120.2 . .
C5 C6 H6 120.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 Br1 2.3729(17) 2_655
Co1 Br1 2.3730(17) .
Co1 Br2 2.4044(16) .
Co1 Br2 2.4045(16) 2_655
N1 C2 1.3420 .
N1 C6 1.3458 .
N1 H1 0.8600 .
C2 C3 1.3824 .
C2 H2 0.9300 .
C3 C4 1.3878 .
C3 H3 0.9300 .
C4 C5 1.3927 .
C4 Cl4 1.7238 .
C5 C6 1.3825 .
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 0.7
N1 C2 C3 C4 0.3
C2 C3 C4 C5 -1.2
C2 C3 C4 Cl4 180.0
C3 C4 C5 C6 1.1
Cl4 C4 C5 C6 179.9
C2 N1 C6 C5 -0.8
C4 C5 C6 N1 -0.1
