#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:15:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321645.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4321645
loop_
_publ_author_name
'Karl S. Hagen'
_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
_chemical_name_systematic
;
 ?
;
_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       '2θ/ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0644P)²+0.4813P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe Fe 0.0000 0.0000 0.0000 0.0409(3) Uani 1 4 d S . .
O1 O 0.0492(2) 0.0000 -0.2533(5) 0.0620(8) Uani 1 2 d S . .
H1 H 0.0667(19) 0.091(5) -0.307(5) 0.082(12) Uiso 1 1 d . . .
O2 O 0.07327(15) 0.2166(3) 0.1532(3) 0.0710(7) Uani 1 1 d . . .
H2 H 0.080(2) 0.245(5) 0.268(6) 0.077(11) Uiso 1 1 d . . .
H3 H 0.095(2) 0.286(6) 0.089(7) 0.105(15) Uiso 1 1 d . . .
S S 0.12450(5) 0.5000 -0.31161(12) 0.0463(3) Uani 1 2 d S . .
C C 0.2235(4) 0.5000 -0.2886(10) 0.0922(17) Uani 1 2 d S . .
O3 O 0.11898(19) 0.5000 -0.0984(4) 0.0621(8) Uani 1 2 d S . .
O4 O 0.09866(15) 0.3263(3) -0.4249(3) 0.0750(7) Uani 1 1 d . . .
F1 F 0.2361(3) 0.5000 -0.4740(7) 0.1329(16) Uani 1 2 d S . .
F2 F 0.25305(19) 0.6558(6) -0.1914(6) 0.1795(17) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Fe 0.0612(5) 0.0339(4) 0.0294(3) 0.000 0.0149(3) 0.000
O1 0.105(2) 0.0439(14) 0.0521(14) 0.000 0.0466(16) 0.000
O2 0.1066(17) 0.0672(14) 0.0421(10) -0.0100(10) 0.0241(11) -0.0374(13)
S 0.0685(6) 0.0390(5) 0.0352(4) 0.000 0.0206(4) 0.000
C 0.087(4) 0.109(5) 0.087(4) 0.000 0.034(3) 0.000
O3 0.100(2) 0.0517(15) 0.0423(13) 0.000 0.0314(14) 0.000
O4 0.1240(19) 0.0560(12) 0.0519(10) -0.0146(9) 0.0354(12) -0.0265(13)
F1 0.143(4) 0.151(4) 0.145(3) 0.000 0.109(3) 0.000
F2 0.122(2) 0.241(4) 0.184(3) -0.094(3) 0.056(2) -0.093(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe O1 180.00(16) 5 . ?
O1 Fe O2 91.08(10) 5 5 ?
O1 Fe O2 88.92(10) . 5 ?
O1 Fe O2 88.92(10) 5 . ?
O1 Fe O2 91.08(10) . . ?
O2 Fe O2 180.00(19) 5 . ?
O1 Fe O2 91.08(10) 5 2 ?
O1 Fe O2 88.92(10) . 2 ?
O2 Fe O2 90.94(15) 5 2 ?
O2 Fe O2 89.06(15) . 2 ?
O1 Fe O2 88.92(10) 5 6 ?
O1 Fe O2 91.08(10) . 6 ?
O2 Fe O2 89.06(15) 5 6 ?
O2 Fe O2 90.94(15) . 6 ?
O2 Fe O2 180.00(13) 2 6 ?
O4 S O4 114.2(2) . 6_565 ?
O4 S O3 114.29(10) . . ?
O4 S O3 114.29(10) 6_565 . ?
O4 S C 104.03(15) . . ?
O4 S C 104.03(15) 6_565 . ?
O3 S C 104.2(2) . . ?
F2 C F2 111.9(6) . 6_565 ?
F2 C F1 107.8(4) . . ?
F2 C F1 107.8(4) 6_565 . ?
F2 C S 109.5(3) . . ?
F2 C S 109.5(3) 6_565 . ?
F1 C S 110.3(5) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe O1 2.103(3) 5 ?
Fe O1 2.103(3) . ?
Fe O2 2.105(2) 5 ?
Fe O2 2.105(2) . ?
Fe O2 2.105(2) 2 ?
Fe O2 2.105(2) 6 ?
S O4 1.433(2) . ?
S O4 1.433(2) 6_565 ?
S O3 1.436(2) . ?
S C 1.815(7) . ?
C F2 1.303(5) . ?
C F2 1.303(5) 6_565 ?
C F1 1.304(6) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O4 0.83(3) 1.96(3) 2.790(3) 173(3) .
O2 H2 O4 0.76(4) 2.04(4) 2.805(3) 179(4) 1_556
O2 H3 O3 0.81(5) 2.05(4) 2.840(3) 163(4) .
