Tris[hexaamminecobalt(III)] bis[trioxalatocobaltate(II)] chloride dodecahydrate
Tian, Ruijng; Yan, Yan; Zhang, Cailing; Wang, Liyan; Pan, Qinhe; Acta Crystallographica Section E 68 (2012) m914–m915; doi:10.1107/S1600536812026414

data_2235708
_publ_section_title
;
 Tris[hexaamminecobalt(III)] bis[trioxalatocobaltate(II)] chloride
 dodecahydrate
;
_journal_coeditor_code           YK2060
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m914
_journal_page_last               m915
_journal_paper_doi               10.1107/S1600536812026414
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Co (N H3)6] [Co (C2 O4)3] Cl, 12H2 O'
_chemical_formula_moiety
'3(Co H18 N6 3+), 2(C6 Co O12 4-), Cl -, 12(H2 O)'
_chemical_formula_sum            'C12 H78 Cl Co5 N18 O36'
_chemical_formula_weight         1381.02
_chemical_name_systematic
;
Tris[hexaamminecobalt(III)] bis[trioxalatocobaltate(II)] chloride
dodecahydrate
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   12.2138(4)
_cell_length_b                   12.2138(4)
_cell_length_c                   9.9090(8)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.06
_cell_volume                     1280.15(12)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 5.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7736
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(<i>SADABS</i>; Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.613
_refine_diff_density_min         -1.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1923
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0482P)^2^+0.6892P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                1514
_reflns_number_total             1923
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yk2060.cif
_cod_data_source_block           I
_cod_database_code               2235708
_cod_database_fobs_code          2235708