Tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II) bis(2,4,5-tricarboxybenzoate) monohydrate and tris(2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')iron(II) 2,5-dicarboxybenzene-1,4-dicarboxylate–benzene-1,2,4,5-tetracarboxylic acid–water (1/1/2)
Zhong, Kai-Long; Acta Crystallographica Section C 68 (2012) m259–m264; doi:10.1107/S0108270112034567

data_2018651
_publ_section_title
;
 Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
 bis(2,4,5-tricarboxybenzoate) monohydrate and
 tris(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')iron(II)
 2,5-dicarboxybenzene-1,4-dicarboxylate--benzene-1,2,4,5-tetracarboxylic
 acid--water (1/1/2)
;
_journal_coeditor_code           SF3175
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m259
_journal_page_last               m264
_journal_paper_doi               10.1107/S0108270112034567
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Fe (C10 H8 N2)3] (C10 H4 O8) , C10 H6 O8 , 2H2 O'
_chemical_formula_moiety
'C30 H24 Fe N6 2+, C10 H4 O8 2-, C10 H6 O8, 2(H2 O)'
_chemical_formula_sum            'C50 H38 Fe N6 O18'
_chemical_formula_weight         1066.71
_chemical_name_systematic
;
tris(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')iron(II)
2,5-dicarboxybenzene-1,4-dicarboxylate--benzene-1,2,4,5-tetracarboxylic
acid--water (1/1/2)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.68(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.767(3)
_cell_length_b                   13.911(3)
_cell_length_c                   24.202(5)
_cell_measurement_reflns_used    19949
_cell_measurement_temperature    223.15
_cell_measurement_theta_max      27.5165
_cell_measurement_theta_min      3.0334
_cell_volume                     4521.9(18)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'graphite monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_sigmaI/netI    0.0902
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22163
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.424
_exptl_absorpt_correction_T_max  0.9588
_exptl_absorpt_correction_T_min  0.8488
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2200
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.329
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.226
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         7925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.226
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0932
_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^)+(0.0284P)^2^+7.0361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1478
_refine_ls_wR_factor_ref         0.1598
_reflns_number_gt                6272
_reflns_number_total             7925
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3175.cif
_cod_data_source_block           II
_cod_original_cell_volume        4521.7(16)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_database_code               2018651