Tetraethylammonium (2,2'-bipyridine)tetracyanidocobaltate(III) sesquihydrate acetonitrile solvate
Lyubartseva, Ganna; Parkin, Sean; Acta Crystallographica Section E 66 (2010) m475–m476; doi:10.1107/S1600536810011311

data_2225627
_publ_section_title
;
 Tetraethylammonium (2,2'-bipyridine)tetracyanidocobaltate(III)
 sesquihydrate acetonitrile solvate
;
_journal_coeditor_code           KP2254
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m475
_journal_page_last               m476
_journal_paper_doi               10.1107/S1600536810011311
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'(C8 H20 N) [Co (C N)4 (C10 H8 N2)], C2 H3 N, 1.5H2 O'
_chemical_formula_moiety
'C8 H20 N +, C14 H8 Co N6 -, C2 H3 N, 1.5(H2 O)'
_chemical_formula_sum            'C24 H34 Co N8 O1.5'
_chemical_formula_weight         517.52
_chemical_name_systematic
;
Tetraethylammonium (2,2'-bipyridine)tetracyanidocobaltate(III)
sesquihydrate acetonitrile solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.3080(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.15910(10)
_cell_length_b                   23.4015(3)
_cell_length_c                   11.3422(2)
_cell_measurement_reflns_used    6273
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2674.57(6)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and local procedures
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            28623
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.675
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SCALEPACK; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1092
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         4704
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0414
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0481P)^2^+2.6305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                3689
_reflns_number_total             4704
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            kp2254.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C24 H34 Co N8 O1.50'
_cod_database_code               2225627
_cod_database_fobs_code          2225627