Crystal structure of tetrakis(tetrahydrofuran-κ<i>O</i>)bis(trifluoromethanesulfonato-κ<i>O</i>)iron(II)
Riemersma, Charl F.; Monkcom, Emily C.; Klein Gebbink, Robertus J. M.; Lutz, Martin; Acta Crystallographica Section E 75 (2019) 1548–1551; doi:10.1107/S2056989019013094

data_2243119
_publ_section_title
;
 Crystal structure of
 tetrakis(tetrahydrofuran-\k<i>O</i>)bis(trifluoromethanesulfonato-\k<i>O</i>)iron(II)
;
_journal_coeditor_code           VN2153
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1548
_journal_page_last               1551
_journal_paper_doi               10.1107/S2056989019013094
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Fe (C F3 O3 S)2 (C4 H8 O)4]'
_chemical_formula_moiety         'C18 H32 F6 Fe O10 S2'
_chemical_formula_sum            'C18 H32 F6 Fe O10 S2'
_chemical_formula_weight         642.40
_chemical_name_systematic
Tetrakis(tetrahydrofuran-\k<i>O</i>)bis(trifluoromethanesulfonato-\k<i>O</i>)iron(II)
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6618(3)
_cell_length_b                   16.2610(6)
_cell_length_c                   19.0572(4)
_cell_measurement_reflns_used    40729
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      1.63
_cell_volume                     2684.20(15)
_computing_cell_refinement
;
<i>PEAKREF</i> (Schreurs, 2016)
;
_computing_data_collection
;
APEX2 (Bruker, 2007)
;
_computing_data_reduction
;
<i>Eval15</i> (Schreurs <i>et al.</i>,  2010)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and <i>DRAWxtl</i> (Finger <i>et al.</i>,
2007)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
initial coordinates from isostructural Zn complex (Amel'chenkova et al.,
2006)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43720
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         1.646
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause et al., 2015)
;
_exptl_crystal_colour            'light pink'
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.279
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   -0.001(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0198
_refine_ls_R_factor_gt           0.0191
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.6586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0512
_reflns_number_gt                6027
_reflns_number_total             6166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            vn2153sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2684.20(14)
_cod_database_code               2243119
_cod_database_fobs_code          2243119
_shelx_hkl_checksum              38200
_shelx_res_checksum              71175