Iron(II) Triflate Salts as Convenient Substitutes for Perchlorate Salts: Crystal Structures of [Fe(H2O)6](CF3SO3)2 and Fe(MeCN)4(CF3SO3)2
Karl S. Hagen; Inorganic Chemistry 39 (2000) 5867–5869; doi:10.1021/ic000444w

data_4321645
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Center
Atlanta GA  30322
USA
;
_publ_contact_author_email       khagen@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Karl S. Hagen'
_publ_contact_author_phone       404-727-6556
_publ_section_title
;
 Iron(II) Triflate Salts as Convenient Substitutes for Perchlorate Salts:
 Crystal Structures of [Fe(H2O)6](CF3SO3)2 and Fe(MeCN)4(CF3SO3)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5867
_journal_page_last               5869
_journal_paper_doi               10.1021/ic000444w
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C2 H12 F6 Fe O12 S2'
_chemical_formula_weight         462.09
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 104.917(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.6643(19)
_cell_length_b                   6.9289(8)
_cell_length_c                   6.5958(9)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      4.36
_cell_volume                     824.24(17)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            1362
_diffrn_reflns_theta_full        28.09
_diffrn_reflns_theta_max         28.09
_diffrn_reflns_theta_min         2.26
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.282
_exptl_absorpt_correction_T_max  0.7836
_exptl_absorpt_correction_T_min  0.6415
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.094(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0644P)^2^+0.4813P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1106
_reflns_number_gt                894
_reflns_number_total             1090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic000444w_1.cif
_cod_data_source_block           fetrifa
_cod_original_sg_symbol_H-M      'C 1 2/c 1'
_cod_database_code               4321645