#------------------------------------------------------------------------------
#$Date: 2016-03-22 21:53:30 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179027 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/25/4122578.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_4122578
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         'C16 H30 Fe2 O4 P2 S2'
_chemical_formula_structural     Fe2(iPr-pdt)(CO)4(PMe3)2
_chemical_formula_sum            'C16 H30 Fe2 O4 P2 S2'
_chemical_formula_weight         524.16
_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   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 104.937(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7840(7)
_cell_length_b                   11.0945(5)
_cell_length_c                   12.5523(8)
_cell_measurement_reflns_used    12135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.4
_cell_volume                     2258.4(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0737
_diffrn_reflns_av_unetI/netI     0.0728
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14727
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.360
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert (Rigaku, 2011)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2591
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0614
_refine_ls_R_factor_gt           0.0362
_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)+(0.0284P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2004
_reflns_number_total             2591
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja506693m_si_002.cif
_cod_data_source_block           1(iPr-pdt)
_cod_depositor_comments
'Adding full bibliography for 4122577--4122589.cif.'
_cod_database_code               4122578
#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   0.895
_shelx_estimated_absorpt_t_max   0.984
_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 0.41680(15) 0.2669(2) 0.09081(19) 0.0218(6) Uani 1 1 d . . . . .
C2 C 0.34013(16) 0.0640(2) 0.12330(19) 0.0222(6) Uani 1 1 d . . . . .
C3 C 0.4798(6) -0.0904(8) 0.3564(6) 0.0164(18) Uani 0.5 1 d . U P A -1
H3A H 0.5349 -0.1132 0.4025 0.020 Uiso 0.5 1 calc R U P A -1
H3B H 0.4384 -0.1234 0.3922 0.020 Uiso 0.5 1 calc R U P A -1
C4 C 0.4674(3) -0.1500(4) 0.2447(4) 0.0181(11) Uani 0.5 1 d . . P A -1
H4 H 0.4107 -0.1280 0.2007 0.022 Uiso 0.5 1 calc R U P A -1
C5 C 0.5264(6) -0.1064(7) 0.1805(6) 0.0175(17) Uani 0.5 1 d . U P A -1
H5A H 0.5145 -0.1519 0.1104 0.021 Uiso 0.5 1 calc R U P A -1
H5B H 0.5828 -0.1288 0.2227 0.021 Uiso 0.5 1 calc R U P A -1
C6 C 0.4694(3) -0.2902(4) 0.2560(4) 0.0190(12) Uani 0.5 1 d . . P A -1
H6 H 0.4304 -0.3125 0.3009 0.023 Uiso 0.5 1 calc R U P A -1
C7 C 0.4397(8) -0.3532(10) 0.1452(8) 0.024(2) Uani 0.5 1 d . U P A -1
H7A H 0.4789 -0.3385 0.1008 0.036 Uiso 0.5 1 calc R U P A -1
H7B H 0.3854 -0.3216 0.1064 0.036 Uiso 0.5 1 calc R U P A -1
H7C H 0.4355 -0.4400 0.1569 0.036 Uiso 0.5 1 calc R U P A -1
C8 C 0.5538(8) -0.3367(9) 0.3169(7) 0.034(3) Uani 0.5 1 d . U P A -1
H8A H 0.5501 -0.4226 0.3330 0.050 Uiso 0.5 1 calc R U P A -1
H8B H 0.5735 -0.2920 0.3860 0.050 Uiso 0.5 1 calc R U P A -1
H8C H 0.5924 -0.3254 0.2709 0.050 Uiso 0.5 1 calc R U P A -1
C9 C 0.2914(2) 0.1968(2) 0.3587(3) 0.0458(8) Uani 1 1 d . . . . .
H9A H 0.3317 0.1602 0.4209 0.069 Uiso 1 1 calc R U . . .
H9B H 0.2554 0.1339 0.3172 0.069 Uiso 1 1 calc R U . . .
H9C H 0.2580 0.2556 0.3864 0.069 Uiso 1 1 calc R U . . .
C10 C 0.39120(18) 0.3998(2) 0.3512(2) 0.0351(7) Uani 1 1 d . . . . .
H10A H 0.4149 0.4541 0.3060 0.053 Uiso 1 1 calc R U . . .
H10B H 0.4348 0.3718 0.4144 0.053 Uiso 1 1 calc R U . . .
H10C H 0.3491 0.4429 0.3777 0.053 Uiso 1 1 calc R U . . .
C11 C 0.25961(18) 0.3419(3) 0.1702(2) 0.0406(8) Uani 1 1 d . . . . .
H11A H 0.2290 0.3938 0.2089 0.061 Uiso 1 1 calc R U . . .
H11B H 0.2228 0.2793 0.1296 0.061 Uiso 1 1 calc R U . . .
H11C H 0.2809 0.3905 0.1185 0.061 Uiso 1 1 calc R U . . .
O1 O 0.40894(12) 0.33884(15) 0.02218(14) 0.0313(5) Uani 1 1 d . . . . .
O2 O 0.28698(12) 0.00268(14) 0.07659(14) 0.0336(5) Uani 1 1 d . . . . .
P1 P 0.34478(4) 0.27184(5) 0.26938(5) 0.01919(16) Uani 1 1 d . . . . .
S1 S 0.47237(4) 0.06403(5) 0.35523(5) 0.02206(16) Uani 1 1 d . . . . .
Fe1 Fe 0.42298(2) 0.15571(3) 0.19276(2) 0.01674(11) Uani 1 1 d . . . . .
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'
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'
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
O1 C1 Fe1 176.9(2) . .
O2 C2 Fe1 178.5(2) . .
C4 C3 S1 115.8(5) . .
C4 C3 H3A 108.3 . .
S1 C3 H3A 108.3 . .
C4 C3 H3B 108.3 . .
S1 C3 H3B 108.3 . .
H3A C3 H3B 107.4 . .
C5 C4 C3 113.7(6) . .
C5 C4 C6 111.5(5) . .
C3 C4 C6 110.9(5) . .
C5 C4 H4 106.8 . .
C3 C4 H4 106.8 . .
C6 C4 H4 106.8 . .
C4 C5 S1 118.9(6) . 2_655
C4 C5 H5A 107.6 . .
S1 C5 H5A 107.6 2_655 .
C4 C5 H5B 107.6 . .
S1 C5 H5B 107.6 2_655 .
H5A C5 H5B 107.0 . .
C8 C6 C7 110.4(7) . .
C8 C6 C4 112.3(5) . .
C7 C6 C4 112.4(6) . .
C8 C6 H6 107.1 . .
C7 C6 H6 107.1 . .
C4 C6 H6 107.1 . .
C6 C7 H7A 109.5 . .
C6 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C6 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C6 C8 H8A 109.5 . .
C6 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
C6 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
P1 C9 H9A 109.5 . .
P1 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
P1 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
P1 C10 H10A 109.5 . .
P1 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
P1 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
P1 C11 H11A 109.5 . .
P1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
P1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 P1 C9 102.66(14) . .
C10 P1 C11 101.64(13) . .
C9 P1 C11 101.19(16) . .
C10 P1 Fe1 118.97(10) . .
C9 P1 Fe1 116.28(9) . .
C11 P1 Fe1 113.59(9) . .
C3 S1 Fe1 118.0(2) . .
C3 S1 Fe1 113.3(3) . 2_655
Fe1 S1 Fe1 71.39(2) . 2_655
C1 Fe1 C2 98.84(10) . .
C1 Fe1 P1 88.72(8) . .
C2 Fe1 P1 94.00(8) . .
C1 Fe1 S1 156.78(8) . .
C2 Fe1 S1 104.38(7) . .
P1 Fe1 S1 89.46(3) . .
C1 Fe1 S1 91.49(8) . 2_655
C2 Fe1 S1 100.27(8) . 2_655
P1 Fe1 S1 165.52(3) . 2_655
S1 Fe1 S1 84.65(3) . 2_655
C1 Fe1 Fe1 105.31(8) . 2_655
C2 Fe1 Fe1 144.56(7) . 2_655
P1 Fe1 Fe1 111.85(2) . 2_655
S1 Fe1 Fe1 54.38(2) . 2_655
S1 Fe1 Fe1 54.230(18) 2_655 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 1.156(3) .
C1 Fe1 1.761(2) .
C2 O2 1.155(3) .
C2 Fe1 1.762(3) .
C3 C4 1.514(7) .
C3 S1 1.718(9) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
C4 C5 1.508(10) .
C4 C6 1.562(5) .
C4 H4 1.0000 .
C5 S1 1.944(8) 2_655
C5 H5A 0.9900 .
C5 H5B 0.9900 .
C6 C8 1.516(12) .
C6 C7 1.521(7) .
C6 H6 1.0000 .
C7 H7A 0.9800 .
C7 H7B 0.9800 .
C7 H7C 0.9800 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 P1 1.809(3) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 P1 1.807(2) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 P1 1.811(3) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
P1 Fe1 2.2268(7) .
S1 Fe1 2.2381(6) .
S1 Fe1 2.2422(7) 2_655
Fe1 S1 2.2423(7) 2_655
Fe1 Fe1 2.6142(7) 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_4
S1 C3 C4 C5 57.4(10) .
S1 C3 C4 C6 -176.0(5) .
C3 C4 C5 S1 -59.1(9) 2_655
C6 C4 C5 S1 174.7(4) 2_655
C5 C4 C6 C8 61.0(8) .
C3 C4 C6 C8 -66.8(8) .
C5 C4 C6 C7 -64.2(8) .
C3 C4 C6 C7 168.0(8) .
C4 C3 S1 Fe1 11.2(8) .
C4 C3 S1 Fe1 -69.3(7) 2_655
