Bis[tris(2,2'-bipyridyl-κ^2^<i>N,N</i>')iron(II)] <i>cyclo</i>-tetravanadate decahydrate
Ming-Hua Huang; Li-Hua Bi; Shao-Jun Dong; Acta Crystallographica Section E 60 (2004) m153–m155; doi:10.1107/S1600536803029532

data_2203220
_publ_section_title
;
 Bis[tris(2,2'-bipyridyl-\k^2^<i>N,N</i>')iron(II)]
 <i>cyclo</i>-tetravanadate decahydrate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m153
_journal_page_last               m155
_journal_paper_doi               10.1107/S1600536803029532
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Fe (C10 H8 N2)3]2 [V4 O12], 10H2 O'
_chemical_formula_moiety         'C60 H48 Fe2 N12, V4 O12, 10(H2 O)'
_chemical_formula_sum            'C60 H68 Fe2 N12 O22 V4'
_chemical_formula_weight         1624.72
_chemical_name_systematic
;
Bis[tris(2,2'-bipyridyl-\k^2^N,N')iron(II)] cyclo-tetravanadate decahydrate
;
_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                 103.296(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.619(3)
_cell_length_b                   13.656(3)
_cell_length_c                   23.517(4)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.17
_cell_measurement_theta_min      5.20
_cell_volume                     6757(2)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS  (Siemens, 1994)'
_computing_data_reduction        'SHELXTL (Siemens, 1994)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    SHELXTL
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0800
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            7943
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.622
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(SHELXTL; Siemens, 1994)'
_exptl_crystal_colour            Black--red
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3328
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.549
_refine_diff_density_min         -1.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.1116
_refine_ls_R_factor_gt           0.0741
_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^)+(0.1P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1950
_refine_ls_wR_factor_ref         0.2111
_reflns_number_gt                4004
_reflns_number_total             6634
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6193.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2203220
_cod_database_fobs_code          2203220