Tris(3,4,7,8-tetramethyl-1,10-phenanthrolin-1-ium) hexacyanidocobaltate(III) pentahydrate
Hu, Ai-Yun; Yu, Deng-Yong; Yuan, Ai-Hua; Acta Crystallographica Section E 69 (2013) m142–; doi:10.1107/S1600536813003632

data_2237551
_publ_section_title
;
 Tris(3,4,7,8-tetramethyl-1,10-phenanthrolin-1-ium)
 hexacyanidocobaltate(III) pentahydrate
;
_journal_coeditor_code           RZ5042
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m142
_journal_paper_doi               10.1107/S1600536813003632
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C16 H17 N2)3 [Co (C N)6], 5H2 O'
_chemical_formula_moiety         '3(C16 H17 N2 +), C6 Co N6 3-, 5(H2 O)'
_chemical_formula_sum            'C54 H61 Co N12 O5'
_chemical_formula_weight         1017.08
_chemical_name_systematic
;
Tris(3,4,7,8-tetramethyl-1,10-phenanthrolin-1-ium) hexacyanidocobaltate(III)
pentahydrate
;
_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           SHELXL-97
_cell_angle_alpha                97.216(2)
_cell_angle_beta                 110.934(2)
_cell_angle_gamma                112.179(2)
_cell_formula_units_Z            2
_cell_length_a                   12.836(2)
_cell_length_b                   14.458(2)
_cell_length_c                   16.645(3)
_cell_measurement_reflns_used    2791
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.57
_cell_measurement_theta_min      2.40
_cell_volume                     2547.6(7)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'SMART (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'phi and omega 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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19411
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.398
_exptl_absorpt_correction_T_max  0.9501
_exptl_absorpt_correction_T_min  0.9391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.528
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         9402
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0575
_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^)+(0.0725P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1384
_refine_ls_wR_factor_ref         0.1545
_reflns_number_gt                6096
_reflns_number_total             9402
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            rz5042.cif
_cod_data_source_block           I
_cod_database_code               2237551
_cod_database_fobs_code          2237551