Crystal structure of bis(acetylacetonato-κ^2^<i>O</i>,<i>O</i>')(tetrahydrofuran-κ<i>O</i>)(trifluoromethanesulfonato-κ<i>O</i>)iron(III)
Richers, Casseday P.; Bertke, Jeffery A.; Rauchfuss, Thomas B.; Acta Crystallographica Section E 71 (2015) 1165–1168; doi:10.1107/S2056989015016849

data_2241149
_publ_contact_author
;
Jeffery A. Bertke
School of Chemical Sciences
University of Illinois at Urbana-Champaign
Urbana, Illinois  61801
USA
;
_publ_section_title
;
 Crystal structure of
 bis(acetylacetonato-\k^2^<i>O</i>,<i>O</i>')(tetrahydrofuran-\k<i>O</i>)(trifluoromethanesulfonato-\k<i>O</i>)iron(III)
;
_journal_coeditor_code           ZS2341
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1165
_journal_page_last               1168
_journal_paper_doi               10.1107/S2056989015016849
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Fe (C F3 O3 S) (C5 H7 O2)2 (C4 H8 O)] '
_chemical_formula_moiety         'C15 H22 F3 Fe O8 S'
_chemical_formula_sum            'C15 H22 F3 Fe O8 S'
_chemical_formula_weight         475.23
_chemical_name_systematic
Bis(acetylacetonato-\k^2^<i>O</i>,<i>O</i>')(tetrahydrofuran-\k<i>O</i>)(trifluoromethanesulfonato-\k<i>O</i>)iron(III)
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.451(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.0118(8)
_cell_length_b                   8.4523(4)
_cell_length_c                   15.9842(9)
_cell_measurement_reflns_used    9821
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.59
_cell_volume                     1994.50(18)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT, XPREP, SADABS and <i>TWINABS</i> (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and CrystalMaker (CrystalMaker, 1994)
;
_computing_publication_material
;
<i>XCIF</i> (Bruker, 2013) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      103(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.156
_diffrn_reflns_theta_min         2.591
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.927
_exptl_absorpt_correction_T_max  0.95448
_exptl_absorpt_correction_T_min  0.72044
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2013)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             980
_exptl_crystal_size_max          0.768
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.079
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.382
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         4417
_refine_ls_number_restraints     344
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0300P)^2^+1.2450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0656
_reflns_number_gt                3800
_reflns_number_total             4417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zs2341sup1.cif
_cod_data_source_block           I
_cod_database_code               2241149
_cod_database_fobs_code          2241149
_shelx_estimated_absorpt_t_min   0.536
_shelx_estimated_absorpt_t_max   0.930
_shelx_hkl_checksum              76107
_shelx_res_checksum              33881
_shelxl_version_number           2014/6