Tris[tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II)] dodecatungstoferrate dihydrate
Ma, Feng-Xia; Chen, Ya-Guang; Shi, Dong-Mei; Acta Crystallographica Section E 64 (2008) m672–; doi:10.1107/S1600536808009896

data_2218160
_publ_section_title
;
 Tris[tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)]
 dodecatungstoferrate dihydrate
;
_journal_coeditor_code           HY2126
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m672
_journal_paper_doi               10.1107/S1600536808009896
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Fe (C12 H8 N2)3]3 [Fe W12 O40], 2H2 O'
_chemical_formula_moiety         '3(C36 H24 Fe1 N6 2+), Fe O40 W12 6-, 2H2 O'
_chemical_formula_sum            'C108 H76 Fe4 N18 O42 W12'
_chemical_formula_weight         4727.47
_chemical_name_systematic
;
Tris[tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)]
dodecatungstoferrate dihydrate
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                120.000
_cell_formula_units_Z            3
_cell_length_a                   25.088(5)
_cell_length_b                   25.088(5)
_cell_length_c                   17.231(5)
_cell_measurement_reflns_used    5571
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      1.5
_cell_volume                     9392(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\f and \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  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16084
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         1.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.506
_exptl_absorpt_correction_T_max  0.104
_exptl_absorpt_correction_T_min  0.075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6593.7
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.616
_refine_diff_density_min         -1.551
_refine_ls_abs_structure_details 'Flack (1983), 3713 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.006(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6154
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0566P)^2^+7.5378P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0933
_reflns_number_gt                5557
_reflns_number_total             6154
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2126.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2218160
_cod_database_fobs_code          2218160