Bis[2-(dimethylamino)pyridinium] Tetrachlorocobaltate(II)
Land, John M.; Baughman, Russell G.; Hester, Colin A.; Acta Crystallographica Section C 53 (1997) IUC9700016–; doi:10.1107/S0108270197099435

data_2006616
_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