<i>trans</i>-Dichloridotetrakis[(dimethylphosphoryl)methanaminium-κ<i>O</i>]cobalt(II) tetrachloridocobaltate(II)
Reiss, Guido J.; Acta Crystallographica Section E 69 (2013) m248–m249; doi:10.1107/S1600536813008945

data_2238021
_publ_section_title
;
 <i>trans</i>-Dichloridotetrakis[(dimethylphosphoryl)methanaminium-\k<i>O</i>]cobalt(II)
 tetrachloridocobaltate(II)
;
_journal_coeditor_code           SJ5313
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m248
_journal_page_last               m249
_journal_paper_doi               10.1107/S1600536813008945
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co Cl2 (C3 H11 N O P)4] [Co Cl4]2'
_chemical_formula_moiety         'C12 H44 Cl2 Co1 N4 O4 P4 4+, 2(Cl4 Co 2-)'
_chemical_formula_sum            'C12 H44 Cl10 Co3 N4 O4 P4'
_chemical_formula_weight         963.68
_chemical_name_systematic
'<i>trans</i>-Dichloridotetrakis[(dimethylphosphoryl)methanaminium-\k<i>O</i>]cobalt(II) bis[tetrachloridocobaltate(II)]'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                110.738(4)
_cell_angle_beta                 97.688(4)
_cell_angle_gamma                104.331(5)
_cell_formula_units_Z            1
_cell_length_a                   7.7748(3)
_cell_length_b                   11.1557(5)
_cell_length_c                   12.1205(5)
_cell_measurement_reflns_used    13303
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      32.6097
_cell_measurement_theta_min      2.8862
_cell_volume                     923.67(8)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2009)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2012)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0(10)
_diffrn_detector_area_resol_mean 16.2711
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Oxford Xcalibur'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15687
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         2.892
_exptl_absorpt_coefficient_mu    2.254
_exptl_absorpt_correction_T_max  0.838
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Oxford Diffraction, 2009), based on expressions derived
by Clark & Reid (1995)]
;
_exptl_crystal_colour            blue
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_exptl_crystal_description       block
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_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.381
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         4920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.012P)^2^+0.50P], where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0405
_refine_ls_wR_factor_ref         0.0416
_reflns_number_gt                4552
_reflns_number_total             4920
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj5313.cif
_cod_data_source_block           I
_cod_original_cell_volume        923.66(8)
_cod_database_code               2238021
_cod_database_fobs_code          2238021
_shelxl_version_number           20.13