#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:34:49 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179117 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/79/4307965.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_4307965
loop_
_publ_author_name
'Rongmin Yu'
'Kuppuswamy Arumugam'
'Ashok Manepalli'
'Yvon Tran'
'Russell Schmehl'
'Heiko Jacobsen'
'James P. Donahue'
_publ_contact_author_email       donahue@tulane.edu
_publ_contact_author_fax         504-865-5596
_publ_contact_author_phone       504-862-3562
_publ_section_title
;
Reversible, Electrochemically Controlled Binding of Phosphine to Iron and
Cobalt Bis(dithiolene) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5131
_journal_page_last               5133
_journal_paper_doi               10.1021/ic0624569
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C74 H80 Fe2 O10 S8'
_chemical_formula_weight         1497.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 100.938(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.006(4)
_cell_length_b                   9.3751(15)
_cell_length_c                   27.169(4)
_cell_measurement_reflns_used    8604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.837
_cell_measurement_theta_min      2.2955
_cell_volume                     7003.9(18)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'Bruker-AXS SMART APEX'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0592
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            29967
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.9687
_exptl_absorpt_correction_T_min  0.7862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         8308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0642P)²+6.3709P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1283
_reflns_number_gt                5882
_reflns_number_total             8308
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            ic0624569-file006_01.cif
_cod_data_source_block
'[Fe(S2C2(C6H4-p-OCH3)2)2]2.2(tert-BuOCH3_1a.2(tert-BuOCH3)'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        7003.9(19)
_cod_database_code               4307965
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe -0.018210(14) 0.58633(4) 0.534025(14) 0.01558(11) Uani 1 1 d . . .
S1 S -0.09274(3) 0.50435(8) 0.52532(3) 0.01772(16) Uani 1 1 d . . .
S2 S -0.02391(3) 0.64628(8) 0.61040(3) 0.01821(16) Uani 1 1 d . . .
S3 S 0.03686(3) 0.75562(8) 0.53782(3) 0.01739(16) Uani 1 1 d . . .
S4 S -0.03296(2) 0.61206(8) 0.45172(3) 0.01671(16) Uani 1 1 d . . .
O1 O -0.28465(7) 0.2389(2) 0.59723(8) 0.0276(5) Uani 1 1 d . . .
O2 O -0.11746(10) 0.7356(3) 0.81075(9) 0.0391(6) Uani 1 1 d . . .
O3 O 0.19441(8) 1.1749(2) 0.46787(8) 0.0284(5) Uani 1 1 d . . .
O4 O -0.06031(9) 0.9857(2) 0.24421(8) 0.0339(6) Uani 1 1 d . . .
O5 O -0.26157(9) -0.2215(3) 0.66955(10) 0.0448(7) Uani 1 1 d . . .
C1 C -0.11043(10) 0.5218(3) 0.58180(10) 0.0166(6) Uani 1 1 d . . .
C2 C -0.07892(10) 0.5889(3) 0.62098(10) 0.0174(6) Uani 1 1 d . . .
C3 C 0.03535(10) 0.8136(3) 0.47656(11) 0.0175(6) Uani 1 1 d . . .
C4 C 0.00252(10) 0.7569(3) 0.43762(10) 0.0177(6) Uani 1 1 d . . .
C5 C -0.15760(11) 0.4581(3) 0.58660(10) 0.0179(6) Uani 1 1 d . . .
C6 C -0.16190(11) 0.3737(3) 0.62803(11) 0.0209(6) Uani 1 1 d . . .
H6 H -0.1355 0.3652 0.6544 0.025 Uiso 1 1 calc R . .
C7 C -0.20451(11) 0.3031(3) 0.63041(11) 0.0224(6) Uani 1 1 d . . .
H7 H -0.2066 0.2472 0.6582 0.027 Uiso 1 1 calc R . .
C8 C -0.24455(11) 0.3147(3) 0.59140(11) 0.0214(6) Uani 1 1 d . . .
C9 C -0.24181(11) 0.4007(3) 0.55045(11) 0.0223(6) Uani 1 1 d . . .
H9 H -0.2686 0.4112 0.5246 0.027 Uiso 1 1 calc R . .
C10 C -0.19849(10) 0.4707(3) 0.54864(11) 0.0210(6) Uani 1 1 d . . .
H10 H -0.1967 0.5280 0.5211 0.025 Uiso 1 1 calc R . .
C11 C -0.32716(11) 0.2538(4) 0.55907(13) 0.0316(8) Uani 1 1 d . . .
H11A H -0.3362 0.3526 0.5556 0.047 Uiso 1 1 calc R . .
H11B H -0.3533 0.1998 0.5681 0.047 Uiso 1 1 calc R . .
H11C H -0.3205 0.2191 0.5278 0.047 Uiso 1 1 calc R . .
C12 C -0.09127(10) 0.6226(3) 0.67036(10) 0.0183(6) Uani 1 1 d . . .
C13 C -0.06084(11) 0.5817(4) 0.71464(11) 0.0258(7) Uani 1 1 d . . .
H13 H -0.0331 0.5285 0.7133 0.031 Uiso 1 1 calc R . .
C14 C -0.07140(12) 0.6192(4) 0.76076(11) 0.0290(7) Uani 1 1 d . . .
H14 H -0.0511 0.5895 0.7901 0.035 Uiso 1 1 calc R . .
C15 C -0.11169(12) 0.7001(3) 0.76306(12) 0.0281(7) Uani 1 1 d . . .
C16 C -0.14327(13) 0.7389(4) 0.71926(13) 0.0321(8) Uani 1 1 d . . .
H16 H -0.1712 0.7908 0.7208 0.039 Uiso 1 1 calc R . .
C17 C -0.13279(12) 0.6995(4) 0.67337(12) 0.0284(7) Uani 1 1 d . . .
H17 H -0.1540 0.7252 0.6441 0.034 Uiso 1 1 calc R . .
C18 C -0.14885(15) 0.8499(4) 0.81458(15) 0.0472(10) Uani 1 1 d . . .
H18A H -0.1423 0.9265 0.7934 0.071 Uiso 1 1 calc R . .
H18B H -0.1438 0.8823 0.8487 0.071 Uiso 1 1 calc R . .
H18C H -0.1819 0.8192 0.8043 0.071 Uiso 1 1 calc R . .
C19 C 0.07432(10) 0.9157(3) 0.47125(10) 0.0176(6) Uani 1 1 d . . .
C20 C 0.08514(11) 1.0345(3) 0.50246(11) 0.0202(6) Uani 1 1 d . . .
H20 H 0.0654 1.0561 0.5254 0.024 Uiso 1 1 calc R . .
C21 C 0.12457(12) 1.1199(3) 0.49987(12) 0.0246(7) Uani 1 1 d . . .
H21 H 0.1309 1.1995 0.5205 0.030 Uiso 1 1 calc R . .
C22 C 0.15516(11) 1.0874(3) 0.46635(11) 0.0219(6) Uani 1 1 d . . .
C23 C 0.14468(11) 0.9709(3) 0.43464(11) 0.0230(7) Uani 1 1 d . . .
H23 H 0.1644 0.9496 0.4117 0.028 Uiso 1 1 calc R . .
C24 C 0.10467(10) 0.8866(3) 0.43727(11) 0.0193(6) Uani 1 1 d . . .
H24 H 0.0979 0.8088 0.4159 0.023 Uiso 1 1 calc R . .
C25 C 0.22893(12) 1.1380(4) 0.43686(12) 0.0318(8) Uani 1 1 d . . .
H25A H 0.2397 1.0417 0.4438 0.048 Uiso 1 1 calc R . .
H25B H 0.2563 1.2014 0.4439 0.048 Uiso 1 1 calc R . .
H25C H 0.2138 1.1464 0.4022 0.048 Uiso 1 1 calc R . .
C26 C -0.01011(10) 0.8115(3) 0.38581(11) 0.0190(6) Uani 1 1 d . . .
C27 C -0.00889(11) 0.9582(3) 0.37602(11) 0.0226(6) Uani 1 1 d . . .
H27 H 0.0029 1.0207 0.4021 0.027 Uiso 1 1 calc R . .
C28 C -0.02487(12) 1.0112(3) 0.32865(12) 0.0281(7) Uani 1 1 d . . .
H28 H -0.0232 1.1087 0.3228 0.034 Uiso 1 1 calc R . .
C29 C -0.04350(11) 0.9202(3) 0.28935(11) 0.0243(7) Uani 1 1 d . . .
C30 C -0.04452(11) 0.7742(3) 0.29748(11) 0.0253(7) Uani 1 1 d . . .
H30 H -0.0563 0.7126 0.2711 0.030 Uiso 1 1 calc R . .
C31 C -0.02772(11) 0.7208(3) 0.34569(11) 0.0226(6) Uani 1 1 d . . .
H31 H -0.0283 0.6229 0.3511 0.027 Uiso 1 1 calc R . .
C32 C -0.08356(13) 0.8999(4) 0.20371(12) 0.0334(8) Uani 1 1 d . . .
H32A H -0.0609 0.8308 0.1957 0.050 Uiso 1 1 calc R . .
H32B H -0.0947 0.9591 0.1750 0.050 Uiso 1 1 calc R . .
H32C H -0.1108 0.8518 0.2130 0.050 Uiso 1 1 calc R . .
C33 C -0.27540(18) -0.3622(4) 0.65217(17) 0.0549(11) Uani 1 1 d . . .
H33A H -0.2854 -0.4156 0.6786 0.082 Uiso 1 1 calc R . .
H33B H -0.2482 -0.4088 0.6422 0.082 Uiso 1 1 calc R . .
H33C H -0.3019 -0.3567 0.6240 0.082 Uiso 1 1 calc R . .
C34 C -0.29936(14) -0.1360(4) 0.68284(14) 0.0389(9) Uani 1 1 d . . .
C35 C -0.27266(17) 0.0006(5) 0.70191(19) 0.0610(13) Uani 1 1 d . . .
H35A H -0.2471 -0.0212 0.7298 0.092 Uiso 1 1 calc R . .
H35B H -0.2951 0.0662 0.7125 0.092 Uiso 1 1 calc R . .
H35C H -0.2590 0.0430 0.6755 0.092 Uiso 1 1 calc R . .
C36 C -0.33960(17) -0.1088(5) 0.63780(17) 0.0603(13) Uani 1 1 d . . .
H36A H -0.3259 -0.0688 0.6111 0.090 Uiso 1 1 calc R . .
H36B H -0.3628 -0.0433 0.6470 0.090 Uiso 1 1 calc R . .
H36C H -0.3555 -0.1971 0.6269 0.090 Uiso 1 1 calc R . .
C37 C -0.32005(18) -0.2064(5) 0.72457(17) 0.0608(13) Uani 1 1 d . . .
H37A H -0.3370 -0.2919 0.7121 0.091 Uiso 1 1 calc R . .
H37B H -0.3422 -0.1420 0.7362 0.091 Uiso 1 1 calc R . .
H37C H -0.2940 -0.2297 0.7518 0.091 Uiso 1 1 calc R . .
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'
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
S2 Fe1 S1 87.31(3) . . ?
S2 Fe1 S3 86.96(3) . . ?
S1 Fe1 S3 154.28(3) . . ?
S2 Fe1 S4 154.18(3) . . ?
S1 Fe1 S4 86.43(3) . . ?
S3 Fe1 S4 87.91(3) . . ?
S2 Fe1 S4 101.57(3) . 5_566 ?
S1 Fe1 S4 106.27(3) . 5_566 ?
S3 Fe1 S4 99.44(3) . 5_566 ?
S4 Fe1 S4 104.23(3) . 5_566 ?
S2 Fe1 Fe1 151.63(3) . 5_566 ?
S1 Fe1 Fe1 100.66(3) . 5_566 ?
S3 Fe1 Fe1 96.21(3) . 5_566 ?
S4 Fe1 Fe1 54.16(2) . 5_566 ?
S4 Fe1 Fe1 50.07(2) 5_566 5_566 ?
C1 S1 Fe1 107.56(10) . . ?
C2 S2 Fe1 108.05(10) . . ?
C3 S3 Fe1 106.87(10) . . ?
C4 S4 Fe1 107.37(10) . . ?
C4 S4 Fe1 107.18(10) . 5_566 ?
Fe1 S4 Fe1 75.76(3) . 5_566 ?
C8 O1 C11 117.1(2) . . ?
C15 O2 C18 116.2(3) . . ?
C22 O3 C25 117.6(2) . . ?
C29 O4 C32 118.0(3) . . ?
C34 O5 C33 115.7(3) . . ?
C2 C1 C5 124.1(2) . . ?
C2 C1 S1 118.6(2) . . ?
C5 C1 S1 117.2(2) . . ?
C1 C2 C12 124.3(3) . . ?
C1 C2 S2 118.3(2) . . ?
C12 C2 S2 117.3(2) . . ?
C4 C3 C19 125.1(3) . . ?
C4 C3 S3 120.5(2) . . ?
C19 C3 S3 114.2(2) . . ?
C3 C4 C26 127.3(3) . . ?
C3 C4 S4 116.9(2) . . ?
C26 C4 S4 115.5(2) . . ?
C10 C5 C6 117.3(3) . . ?
C10 C5 C1 121.6(3) . . ?
C6 C5 C1 120.9(3) . . ?
C7 C6 C5 121.2(3) . . ?
C6 C7 C8 120.4(3) . . ?
O1 C8 C9 124.6(3) . . ?
O1 C8 C7 115.6(3) . . ?
C9 C8 C7 119.8(3) . . ?
C8 C9 C10 119.0(3) . . ?
C9 C10 C5 122.3(3) . . ?
C17 C12 C13 118.5(3) . . ?
C17 C12 C2 120.5(3) . . ?
C13 C12 C2 121.0(3) . . ?
C14 C13 C12 120.8(3) . . ?
C15 C14 C13 120.0(3) . . ?
C14 C15 O2 114.9(3) . . ?
C14 C15 C16 120.1(3) . . ?
O2 C15 C16 125.0(3) . . ?
C17 C16 C15 119.5(3) . . ?
C12 C17 C16 121.1(3) . . ?
C24 C19 C20 117.9(3) . . ?
C24 C19 C3 119.5(3) . . ?
C20 C19 C3 122.4(3) . . ?
C21 C20 C19 121.1(3) . . ?
C20 C21 C22 120.2(3) . . ?
O3 C22 C23 124.5(3) . . ?
O3 C22 C21 116.0(3) . . ?
C23 C22 C21 119.5(3) . . ?
C24 C23 C22 119.7(3) . . ?
C23 C24 C19 121.6(3) . . ?
C31 C26 C27 117.8(3) . . ?
C31 C26 C4 121.2(3) . . ?
C27 C26 C4 120.7(3) . . ?
C28 C27 C26 121.2(3) . . ?
C27 C28 C29 120.4(3) . . ?
O4 C29 C30 124.7(3) . . ?
O4 C29 C28 115.3(3) . . ?
C30 C29 C28 120.0(3) . . ?
C29 C30 C31 119.3(3) . . ?
C26 C31 C30 121.3(3) . . ?
O5 C34 C37 110.6(3) . . ?
O5 C34 C36 111.3(3) . . ?
C37 C34 C36 110.1(4) . . ?
O5 C34 C35 102.6(3) . . ?
C37 C34 C35 110.1(4) . . ?
C36 C34 C35 111.9(4) . . ?
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
Fe1 S2 2.1846(8) . ?
Fe1 S1 2.1946(9) . ?
Fe1 S3 2.2019(8) . ?
Fe1 S4 2.2088(8) . ?
Fe1 S4 2.3351(9) 5_566 ?
Fe1 Fe1 2.7917(8) 5_566 ?
S1 C1 1.708(3) . ?
S2 C2 1.707(3) . ?
S3 C3 1.744(3) . ?
S4 C4 1.767(3) . ?
S4 Fe1 2.3350(9) 5_566 ?
O1 C8 1.363(3) . ?
O1 C11 1.430(4) . ?
O2 C15 1.377(4) . ?
O2 C18 1.402(4) . ?
O3 C22 1.366(4) . ?
O3 C25 1.440(4) . ?
O4 C29 1.372(4) . ?
O4 C32 1.418(4) . ?
O5 C34 1.427(4) . ?
O5 C33 1.430(5) . ?
C1 C2 1.397(4) . ?
C1 C5 1.478(4) . ?
C2 C12 1.482(4) . ?
C3 C4 1.371(4) . ?
C3 C19 1.479(4) . ?
C4 C26 1.476(4) . ?
C5 C10 1.393(4) . ?
C5 C6 1.399(4) . ?
C6 C7 1.377(4) . ?
C7 C8 1.393(4) . ?
C8 C9 1.388(4) . ?
C9 C10 1.388(4) . ?
C12 C17 1.384(4) . ?
C12 C13 1.390(4) . ?
C13 C14 1.386(4) . ?
C14 C15 1.371(5) . ?
C15 C16 1.390(5) . ?
C16 C17 1.384(4) . ?
C19 C24 1.395(4) . ?
C19 C20 1.398(4) . ?
C20 C21 1.377(4) . ?
C21 C22 1.397(4) . ?
C22 C23 1.387(4) . ?
C23 C24 1.384(4) . ?
C26 C31 1.397(4) . ?
C26 C27 1.403(4) . ?
C27 C28 1.373(4) . ?
C28 C29 1.389(4) . ?
C29 C30 1.388(4) . ?
C30 C31 1.398(4) . ?
C34 C37 1.518(5) . ?
C34 C36 1.520(5) . ?
C34 C35 1.524(6) . ?
