Polymorphism of <i>mer</i>-μ-oxalato-bis[chloridotripyridinecobalt(II)] pyridine disolvate
Modec, Barbara; Acta Crystallographica Section C 69 (2013) 340–343; doi:10.1107/S010827011300499X

data_2018930
_publ_section_title
;
 Polymorphism of <i>mer</i>-\m-oxalato-bis[chloridotripyridinecobalt(II)]
 pyridine disolvate
;
_journal_coeditor_code           SK3477
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              340
_journal_page_last               343
_journal_paper_doi               10.1107/S010827011300499X
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co2 (C2 O4) Cl2 (C5 H5 N)6], 2C5 H5 N'
_chemical_formula_moiety         'C32 H30 Cl2 Co2 N6 O4, 2(C5 H5 N)'
_chemical_formula_sum            'C42 H40 Cl2 Co2 N8 O4'
_chemical_formula_weight         909.58
_chemical_name_systematic
;
<i>mer</i>-\m-Oxalato-bis[chloridotripyridinecobalt(II)] pyridine disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                78.8340(10)
_cell_angle_beta                 82.8560(10)
_cell_angle_gamma                89.7040(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6402(7)
_cell_length_b                   9.9899(7)
_cell_length_c                   10.7775(7)
_cell_measurement_reflns_used    6588
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.50
_cell_measurement_theta_min      1.94
_cell_volume                     1010.18(12)
_computing_cell_refinement       'SMART (Siemens, 1994)'
_computing_data_collection       'SMART (Siemens, 1994)'
_computing_data_reduction        'SAINT (Siemens, 1994)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008), PLATON (Spek, 2009) and Mercury
(Macrae
<i>et al.</i>, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Siemens P4 diffractometer with a 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  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10108
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  0.9329
_exptl_absorpt_correction_T_min  0.9060
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             468
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.545
_refine_diff_density_min         -0.278
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4614
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0377
_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/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0774
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                3467
_reflns_number_total             4614
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3477.cif
_cod_data_source_block           I
_cod_database_code               2018930
_cod_database_fobs_code          2018930