Tris(2,2'-bi-1<i>H</i>-imidazole-κ^2^<i>N</i>^3^,<i>N</i>^3'^)cobalt(II) hydrogen phosphate
Liang, Zhiqiang; Wang, Fuxiang; Wu, Qihui; Zhi, Xia; Pan, Qinhe; Acta Crystallographica Section E 67 (2011) m1399–; doi:10.1107/S1600536811037299

data_2231799
_publ_section_title
;
 Tris(2,2'-bi-1<i>H</i>-imidazole-\k^2^<i>N</i>^3^,<i>N</i>^3'^)cobalt(II)
 hydrogen phosphate
;
_journal_coeditor_code           AA2021
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1399
_journal_paper_doi               10.1107/S1600536811037299
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Co (C6 H6 N4)3] H P O4'
_chemical_formula_moiety         'C18 H18 Co N12 +, H P O4 -'
_chemical_formula_sum            'C18 H19 Co N12 O4 P'
_chemical_formula_weight         557.35
_chemical_name_systematic
;
Tris(2,2'-bi-1<i>H</i>-imidazole-\k^2^<i>N</i>^3^,<i>N</i>^3'^)cobalt(II)
hydrogen phosphate
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 95.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.700(3)
_cell_length_b                   21.447(4)
_cell_length_c                   9.1140(18)
_cell_measurement_reflns_used    12761
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.05
_cell_volume                     2469.6(9)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID-S'
_diffrn_measurement_method       \w
_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  0.0978
_diffrn_reflns_av_sigmaI/netI    0.1382
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12597
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.05
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.810
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Crystalclear; Rigaku/MSC, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.316
_refine_ls_abs_structure_details 'Flack (1983), <b>2755 Friedel pairs</b>'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5593
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1428
_refine_ls_R_factor_gt           0.0765
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                3373
_reflns_number_total             5593
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            aa2021.cif
_cod_data_source_block           I
_cod_original_cell_volume        2469.6(8)
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               2231799
_cod_database_fobs_code          2231799