Crystal structure of tris(1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')iron(II) bis[bis(trifluoromethylsulfonyl)imide] monohydrate
Teramoto, Kazunori; Kawasaki, Takeshi; Nishide, Toshikazu; Ikeda, Yasuhisa; Acta Crystallographica Section E 71 (2015) m8–m9; doi:10.1107/S2056989014026966

data_2240273
_publ_section_title
;
 Crystal structure of
 tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
 bis[bis(trifluoromethylsulfonyl)imide] monohydrate
;
_journal_coeditor_code           WM5100
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m8
_journal_page_last               m9
_journal_paper_doi               10.1107/S2056989014026966
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe (C12 H8 N2)3] (C2 F6 N O4 S2)2, H2 O'
_chemical_formula_moiety         'C36 H24 Fe N6 2+, 2(C2 F6 N O4 S2 -), H2 O'
_chemical_formula_sum            'C40 H26 F12 Fe N8 O9 S4'
_chemical_formula_weight         1174.78
_chemical_name_systematic
;
Tris(1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')iron(II)
bis[bis(trifluoromethylsulfonyl)imide] monohydrate
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.6570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.7745(15)
_cell_length_b                   16.0107(12)
_cell_length_c                   13.3084(10)
_cell_measurement_reflns_used    1623
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.47
_cell_measurement_theta_min      2.20
_cell_volume                     4424.7(6)
_computing_cell_refinement
;
SAINT (Bruker, 2007)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
SAINT (Bruker, 2007)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13659
_diffrn_reflns_theta_full        27.17
_diffrn_reflns_theta_max         27.17
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.647
_exptl_absorpt_correction_T_max  0.9381
_exptl_absorpt_correction_T_min  0.7727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>SADABS</i>; Bruker, 2007)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.898
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4910
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0533P)^2^+0.4369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                3247
_reflns_number_total             4910
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5100sup1.cf
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2240273
_cod_database_fobs_code          2240273