Second-sphere coordination in anion binding: sodium hexaamminecobalt(III) tetrakis(4-fluorobenzoate) monohydrate
Sharma, Raj Pal; Bala, Ritu; Sharma, Rajni; Bond, Andrew D.; Acta Crystallographica Section C 61 (2005) m356–m358; doi:10.1107/S0108270105018500

data_2014965
_publ_section_title
;
 Second-sphere coordination in anion binding: sodium
 hexaamminecobalt(III) tetrakis(4-fluorobenzoate) monohydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m356
_journal_page_last               m358
_journal_paper_doi               10.1107/S0108270105018500
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'Na [Co (N H3)6] (C7 H4 F O2)4 , H2 O'
_chemical_formula_moiety         'Na + , Co N6 H18 3+ , 4C7 H4 F O2 - , H2 O'
_chemical_formula_sum            'C28 H36 Co F4 N6 Na O9'
_chemical_formula_weight         758.55
_chemical_melting_point          478
_chemical_name_systematic
;
sodium hexaamminecobalt(III) tetrakis(4-fluorobenzoate) monohydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 112.3490(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1930(4)
_cell_length_b                   33.4500(9)
_cell_length_c                   6.5169(2)
_cell_measurement_reflns_used    6005
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.02
_cell_measurement_theta_min      2.28
_cell_volume                     3264.77(16)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'APEX2 (Bruker Nonius, 2003)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker Nonius X8APEX-II CCD area-detector'
_diffrn_measurement_method       'thin-slice \w and \f'
_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  0.0188
_diffrn_reflns_av_sigmaI/netI    0.0183
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            11474
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         28.02
_diffrn_reflns_theta_min         3.59
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2003) Ratio of minimum to maximum apparent
transmission 0.788976
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         3531
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0506P)^2^+1.8227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0791
_refine_ls_wR_factor_ref         0.0853
_reflns_number_gt                2909
_reflns_number_total             3531
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg1006.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2014965
_cod_database_fobs_code          2014965