#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:53:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179027 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/25/4122580.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_4122580
loop_
_publ_author_name
'Jablonskytė, Aušra'
'Webster, Lee R.'
'Simmons, Trevor R.'
'Wright, Joseph A.'
'Pickett, Christopher J.'
_publ_section_title
;
 Electronic control of the protonation rates of Fe-Fe bonds.
;
_journal_issue                   37
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13038
_journal_page_last               13044
_journal_paper_doi               10.1021/ja506693m
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C12 H23 Fe2 O5 P2 S2, F6 P'
_chemical_formula_structural     '[HFe2(odt)(CO)4(PMe3)2][PF6]'
_chemical_formula_sum            'C12 H23 F6 Fe2 O5 P3 S2'
_chemical_formula_weight         630.03
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 106.854(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.79(2)
_cell_length_b                   8.4769(10)
_cell_length_c                   13.848(16)
_cell_measurement_reflns_used    2191
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.9
_cell_volume                     2336(4)
_computing_cell_refinement       'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_data_collection       'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert (Rigaku, 2011)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
 SHELXL-2014 (Sheldrick, 2014), WinGX (Farrugia, 2012)
 and enCIFer (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5897
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.491
_diffrn_reflns_theta_min         2.612
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.695
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert (Rigaku, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       needle
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2666
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0918
_refine_ls_R_factor_gt           0.0618
_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/[σ²(Fo²)+(0.0663P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1342
_refine_ls_wR_factor_ref         0.1518
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1788
_reflns_number_total             2666
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja506693m_si_002.cif
_cod_data_source_block           '[1H(odt)][PF6]'
_cod_depositor_comments
'Adding full bibliography for 4122577--4122589.cif.'
_cod_database_code               4122580
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.967
_shelxl_version_number           2014-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5319(3) 0.2394(7) 0.0999(4) 0.0431(13) Uani 1 1 d . . . . .
C2 C 0.6003(3) -0.0161(8) 0.1651(4) 0.0558(17) Uani 1 1 d . . . . .
C3 C 0.4720(8) -0.2295(17) 0.1721(12) 0.035(3) Uani 0.5 1 d . . P A -1
H3A H 0.4334 -0.2959 0.1359 0.041 Uiso 0.5 1 calc R U P A -1
H3B H 0.5097 -0.2533 0.1441 0.041 Uiso 0.5 1 calc R U P A -1
C4 C 0.5557(6) -0.2139(16) 0.3261(12) 0.026(3) Uani 0.5 1 d . . P A -1
H4A H 0.5868 -0.2308 0.2850 0.031 Uiso 0.5 1 calc R U P A -1
H4B H 0.5729 -0.2738 0.3898 0.031 Uiso 0.5 1 calc R U P A -1
C5 C 0.6395(4) 0.4564(7) 0.2306(5) 0.0614(18) Uani 1 1 d . . . . .
H5A H 0.6738 0.5222 0.2763 0.092 Uiso 1 1 calc R U . . .
H5B H 0.5961 0.5110 0.2137 0.092 Uiso 1 1 calc R U . . .
H5C H 0.6521 0.4366 0.1687 0.092 Uiso 1 1 calc R U . . .
C6 C 0.6305(5) 0.3297(12) 0.4159(5) 0.105(4) Uani 1 1 d . . . . .
H6A H 0.5884 0.3854 0.4106 0.158 Uiso 1 1 calc R U . . .
H6B H 0.6686 0.3998 0.4460 0.158 Uiso 1 1 calc R U . . .
H6C H 0.6335 0.2361 0.4584 0.158 Uiso 1 1 calc R U . . .
C7 C 0.7142(3) 0.1869(9) 0.3113(6) 0.087(3) Uani 1 1 d . . . . .
H7A H 0.7480 0.2581 0.3532 0.130 Uiso 1 1 calc R U . . .
H7B H 0.7230 0.1717 0.2461 0.130 Uiso 1 1 calc R U . . .
H7C H 0.7163 0.0849 0.3453 0.130 Uiso 1 1 calc R U . . .
F1 F 0.70865(18) 0.7846(4) 0.3856(2) 0.0541(9) Uani 1 1 d . . . . .
F2 F 0.73590(19) 0.9249(3) 0.5316(2) 0.0551(9) Uani 1 1 d . . . . .
F3 F 0.68241(18) 0.6906(4) 0.5220(2) 0.0577(9) Uani 1 1 d . . . . .
Fe1 Fe 0.54748(4) 0.11559(8) 0.20738(5) 0.0326(2) Uani 1 1 d . . . . .
O1 O 0.5221(3) 0.3208(6) 0.0316(3) 0.0699(14) Uani 1 1 d . . . . .
O2 O 0.6323(3) -0.1056(6) 0.1386(3) 0.0762(16) Uani 1 1 d . . . . .
O3 O 0.4909(5) -0.2702(7) 0.2730(6) 0.035(2) Uani 0.5 1 d . . P A -1
P1 P 0.63286(8) 0.27033(19) 0.29154(11) 0.0467(4) Uani 1 1 d . . . . .
P2 P 0.7500 0.7500 0.5000 0.0353(5) Uani 1 2 d S . P . .
S1 S 0.44735(8) -0.00975(15) 0.14634(9) 0.0398(4) Uani 1 1 d . . . . .
H1 H 0.5000 0.244(7) 0.2500 0.033(19) Uiso 1 2 d S . P . .
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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
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
O1 C1 Fe1 179.1(6) . .
O2 C2 Fe1 176.9(7) . .
O3 C3 S1 114.1(9) . .
O3 C3 H3A 108.7 . .
S1 C3 H3A 108.7 . .
O3 C3 H3B 108.7 . .
S1 C3 H3B 108.7 . .
H3A C3 H3B 107.6 . .
O3 C4 S1 110.6(9) . 2_655
O3 C4 H4A 109.5 . .
S1 C4 H4A 109.5 2_655 .
O3 C4 H4B 109.5 . .
S1 C4 H4B 109.5 2_655 .
H4A C4 H4B 108.1 . .
P1 C5 H5A 109.5 . .
P1 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
P1 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
P1 C6 H6A 109.5 . .
P1 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
P1 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
P1 C7 H7A 109.5 . .
P1 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
P1 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C1 Fe1 C2 94.3(3) . .
C1 Fe1 P1 90.8(2) . .
C2 Fe1 P1 93.8(2) . .
C1 Fe1 S1 168.44(18) . 2_655
C2 Fe1 S1 97.3(2) . 2_655
P1 Fe1 S1 89.11(8) . 2_655
C1 Fe1 S1 92.3(2) . .
C2 Fe1 S1 99.8(2) . .
P1 Fe1 S1 165.73(6) . .
S1 Fe1 S1 85.07(7) 2_655 .
C1 Fe1 Fe1 114.03(19) . 2_655
C2 Fe1 Fe1 141.1(2) . 2_655
P1 Fe1 Fe1 110.98(8) . 2_655
S1 Fe1 Fe1 55.51(6) 2_655 2_655
S1 Fe1 Fe1 55.20(7) . 2_655
C1 Fe1 H1 85.9(12) . .
C2 Fe1 H1 177.8(11) . .
P1 Fe1 H1 84.0(11) . .
S1 Fe1 H1 82.6(12) 2_655 .
S1 Fe1 H1 82.3(12) . .
Fe1 Fe1 H1 40.3(16) 2_655 .
C3 O3 C4 112.9(9) . .
C7 P1 C6 104.5(4) . .
C7 P1 C5 102.7(3) . .
C6 P1 C5 103.2(4) . .
C7 P1 Fe1 114.9(3) . .
C6 P1 Fe1 115.0(2) . .
C5 P1 Fe1 115.0(2) . .
F1 P2 F1 180.0(2) . 7_666
F1 P2 F2 90.71(17) . .
F1 P2 F2 89.29(17) 7_666 .
F1 P2 F2 89.29(18) . 7_666
F1 P2 F2 90.71(17) 7_666 7_666
F2 P2 F2 180.0 . 7_666
F1 P2 F3 89.82(19) . .
F1 P2 F3 90.17(19) 7_666 .
F2 P2 F3 89.95(19) . .
F2 P2 F3 90.05(19) 7_666 .
F1 P2 F3 90.18(19) . 7_666
F1 P2 F3 89.83(19) 7_666 7_666
F2 P2 F3 90.05(19) . 7_666
F2 P2 F3 89.95(19) 7_666 7_666
F3 P2 F3 180.0 . 7_666
C3 S1 Fe1 110.2(5) . 2_655
C3 S1 Fe1 102.5(5) . .
Fe1 S1 Fe1 69.30(5) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.140(6) .
C1 Fe1 1.773(6) .
C2 O2 1.137(7) .
C2 Fe1 1.780(6) .
C3 O3 1.380(17) .
C3 S1 1.938(14) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 O3 1.417(14) .
C4 S1 1.777(14) 2_655
C4 H4A 0.9900 .
C4 H4B 0.9900 .
C5 P1 1.813(6) .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9800 .
C6 P1 1.808(7) .
C6 H6A 0.9800 .
C6 H6B 0.9800 .
C6 H6C 0.9800 .
C7 P1 1.779(7) .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
F1 P2 1.596(3) .
F2 P2 1.597(3) .
F3 P2 1.603(4) .
Fe1 P1 2.243(2) .
Fe1 S1 2.262(2) 2_655
Fe1 S1 2.271(2) .
Fe1 Fe1 2.577(2) 2_655
Fe1 H1 1.69(4) .
P2 F1 1.596(3) 7_666
P2 F2 1.597(3) 7_666
P2 F3 1.603(4) 7_666
S1 Fe1 2.262(2) 2_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
S1 C3 O3 C4 -74.4(13) .
S1 C4 O3 C3 77.9(11) 2_655
