Tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II) squarate octahydrate
Uçar, İbrahim; Paşaoĝlu, Hümeyra; Büyükgüngör, Orhan; Bulut, Ahmet; Acta Crystallographica Section E 61 (2005) m1405–m1407; doi:10.1107/S1600536805019550

data_2206157
_publ_section_title
;
 Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II) squarate
 octahydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1405
_journal_page_last               m1407
_journal_paper_doi               10.1107/S1600536805019550
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe (C12 H8 N2)3] (C4 O4), 8H2 O'
_chemical_formula_moiety         'C36 H24 Fe N6 2+, C4 O4 2-, 8H2 O'
_chemical_formula_sum            'C40 H40 Fe N6 O12'
_chemical_formula_weight         852.63
_chemical_name_systematic
;
Tris(1,10-phenanthroline-\k^2^N,N')iron(II) squarate octahydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.804(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9285(6)
_cell_length_b                   21.3431(7)
_cell_length_c                   16.8988(8)
_cell_measurement_reflns_used    5187
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      1.65
_cell_volume                     3895.2(3)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2002)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2002)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS-2'
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            42766
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.460
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(X-RED32; Stoe & Cie, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1776
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.402
_refine_ls_extinction_coef       0.0023(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         8612
_refine_ls_number_restraints     25
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0679P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1128
_reflns_number_gt                5723
_reflns_number_total             8612
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ci6598.cif
_cod_data_source_block           I
_cod_original_cell_volume        3895.4(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2206157