Triclinic modification of diaquabis(5-carboxy-1<i>H</i>-imidazole-4-carboxylato-κ^2^<i>N</i>^3^,<i>O</i>^4^)iron(II)
Ohshima, Eriko; Yoshida, Kazuki; Sugiyama, Kazumasa; Uekusa, Hidehiro; Acta Crystallographica Section E 68 (2012) m1093–m1094; doi:10.1107/S1600536812031753

data_2235790
_publ_section_title
;
 Triclinic modification of
 diaquabis(5-carboxy-1<i>H</i>-imidazole-4-carboxylato-\k^2^<i>N</i>^3^,<i>O</i>^4^)iron(II)
;
_journal_coeditor_code           FJ2571
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1093
_journal_page_last               m1094
_journal_paper_doi               10.1107/S1600536812031753
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Fe (C5 H3 N2 O4)2 (H2 O)2]'
_chemical_formula_moiety         'C10 H10 Fe N4 O10 '
_chemical_formula_sum            'C10 H10 Fe N4 O10'
_chemical_formula_weight         402.08
_chemical_name_systematic
;
Diaquabis(5-carboxy-1<i>H</i>-imidazole-4-
carboxylato-\k^2^<i>N</i>^3^,<i>O</i>^4^)iron(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                78.161(3)
_cell_angle_beta                 85.175(3)
_cell_angle_gamma                72.776(4)
_cell_formula_units_Z            1
_cell_length_a                   4.9290(5)
_cell_length_b                   6.4258(6)
_cell_length_c                   12.2812(10)
_cell_measurement_reflns_used    3918
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.49
_cell_measurement_theta_min      3.38
_cell_volume                     363.52(6)
_computing_cell_refinement       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'RAPID-AUTO (Rigaku, 1998)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 100
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0925
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3655
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    1.104
_exptl_absorpt_correction_T_max  0.8976
_exptl_absorpt_correction_T_min  0.8518
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.837
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.916
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1668
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.916
_refine_ls_R_factor_all          0.0819
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0339P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                1066
_reflns_number_total             1668
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fj2571.cif
_cod_data_source_block           I
_cod_database_code               2235790
_cod_database_fobs_code          2235790