#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316047.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_4316047
loop_
_publ_author_name
'Yu-Chiao Liu'
'Ling-Kuang Tu'
'Tao-Hung Yen'
'Gene-Hsiang Lee'
'Shu-Ting Yang'
'Ming-Hsi Chiang'
_publ_section_title
;
 Secondary Coordination Sphere Interactions within the Biomimetic Iron
 Azadithiolate Complexes Related to Fe-Only Hydrogenase: Dynamic Measure
 of Electron Density about the Fe Sites
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6409
_journal_page_last               6420
_journal_paper_doi               10.1021/ic100484a
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C60 H60 Fe4 N2 O10 P2 S4'
_chemical_formula_weight         1382.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                112.6151(14)
_cell_angle_beta                 108.4243(14)
_cell_angle_gamma                92.4634(14)
_cell_formula_units_Z            1
_cell_length_a                   10.3639(3)
_cell_length_b                   13.0529(3)
_cell_length_c                   13.5951(3)
_cell_measurement_reflns_used    total
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.00
_cell_volume                     1582.02(7)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_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      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       'ω 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  0.0563
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            26231
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    1.138
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.879
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0017(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         7219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0402P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0809
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                4821
_reflns_number_total             7219
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100484a_si_005.cif
_cod_data_source_block           ic12955
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4316047
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Fe1 Fe 0.23573(4) -0.08364(3) 0.70319(3) 0.03024(11) Uani 1 1 d . . .
Fe2 Fe 0.24535(3) 0.09937(3) 0.86318(3) 0.02490(11) Uani 1 1 d . . .
S1 S 0.05226(6) 0.00322(5) 0.71029(5) 0.02718(15) Uani 1 1 d . . .
S2 S 0.31901(6) 0.08829(6) 0.71842(5) 0.02917(15) Uani 1 1 d . . .
P1 P 0.18339(6) 0.26652(5) 0.92966(5) 0.02552(15) Uani 1 1 d . . .
C1 C 0.4117(3) -0.0990(2) 0.7527(2) 0.0408(7) Uani 1 1 d . . .
C2 C 0.1862(3) -0.1743(2) 0.5544(2) 0.0415(7) Uani 1 1 d . . .
C3 C 0.1779(3) -0.1814(2) 0.7486(2) 0.0382(7) Uani 1 1 d . . .
C4 C 0.4210(3) 0.1322(2) 0.9542(2) 0.0312(6) Uani 1 1 d . . .
C5 C 0.1925(3) 0.0494(2) 0.9502(2) 0.0299(6) Uani 1 1 d . . .
C6 C -0.0831(3) -0.0582(2) 0.7423(2) 0.0323(6) Uani 1 1 d . . .
H6A H -0.0551 -0.1219 0.7612 0.039 Uiso 1 1 calc R . .
H6B H -0.0982 -0.0007 0.8086 0.039 Uiso 1 1 calc R . .
C7 C -0.2161(3) -0.0999(2) 0.6368(2) 0.0370(7) Uani 1 1 d . . .
H7A H -0.2925 -0.1272 0.6548 0.044 Uiso 1 1 calc R . .
H7B H -0.2405 -0.0360 0.6169 0.044 Uiso 1 1 calc R . .
C8 C -0.2879(3) -0.1889(2) 0.4298(2) 0.0411(7) Uani 1 1 d . . .
H8A H -0.3703 -0.1560 0.4380 0.049 Uiso 1 1 calc R . .
H8B H -0.3201 -0.2670 0.3691 0.049 Uiso 1 1 calc R . .
C9 C -0.2031(3) -0.1190(2) 0.3970(2) 0.0345(6) Uani 1 1 d . . .
H9A H -0.1342 -0.1609 0.3710 0.041 Uiso 1 1 calc R . .
H9B H -0.1528 -0.0474 0.4642 0.041 Uiso 1 1 calc R . .
C10 C -0.2263(3) -0.3010(2) 0.5411(2) 0.0440(7) Uani 1 1 d . . .
H10A H -0.3270 -0.3319 0.5066 0.053 Uiso 1 1 calc R . .
H10B H -0.1934 -0.2919 0.6213 0.053 Uiso 1 1 calc R . .
C11 C -0.1535(3) -0.3820(3) 0.4771(3) 0.0522(8) Uani 1 1 d . . .
H11A H -0.0523 -0.3540 0.5154 0.063 Uiso 1 1 calc R . .
H11B H -0.1805 -0.3862 0.3988 0.063 Uiso 1 1 calc R . .
C12 C -0.1887(4) -0.5023(3) 0.4704(3) 0.0623(9) Uani 1 1 d . . .
H12A H -0.1593 -0.4989 0.5477 0.093 Uiso 1 1 calc R . .
H12B H -0.1401 -0.5535 0.4270 0.093 Uiso 1 1 calc R . .
H12C H -0.2888 -0.5304 0.4322 0.093 Uiso 1 1 calc R . .
C13 C 0.2256(3) 0.3711(2) 0.8800(2) 0.0282(6) Uani 1 1 d . . .
C14 C 0.3576(3) 0.3855(2) 0.8762(2) 0.0334(6) Uani 1 1 d . . .
H14 H 0.4185 0.3365 0.8911 0.040 Uiso 1 1 calc R . .
C15 C 0.4001(3) 0.4717(2) 0.8505(2) 0.0398(7) Uani 1 1 d . . .
H15 H 0.4905 0.4817 0.8487 0.048 Uiso 1 1 calc R . .
C16 C 0.3126(3) 0.5421(2) 0.8279(2) 0.0424(7) Uani 1 1 d . . .
H16 H 0.3431 0.6011 0.8111 0.051 Uiso 1 1 calc R . .
C17 C 0.1809(3) 0.5282(2) 0.8293(3) 0.0463(8) Uani 1 1 d . . .
H17 H 0.1198 0.5761 0.8118 0.056 Uiso 1 1 calc R . .
C18 C 0.1379(3) 0.4435(2) 0.8565(2) 0.0381(7) Uani 1 1 d . . .
H18 H 0.0477 0.4348 0.8590 0.046 Uiso 1 1 calc R . .
C19 C 0.2526(2) 0.3520(2) 1.0854(2) 0.0277(5) Uani 1 1 d . . .
C20 C 0.3327(3) 0.3101(2) 1.1588(2) 0.0332(6) Uani 1 1 d . . .
H20 H 0.3509 0.2359 1.1288 0.040 Uiso 1 1 calc R . .
C21 C 0.3867(3) 0.3756(2) 1.2758(2) 0.0409(7) Uani 1 1 d . . .
H21 H 0.4427 0.3465 1.3253 0.049 Uiso 1 1 calc R . .
C22 C 0.3590(3) 0.4828(3) 1.3201(2) 0.0466(8) Uani 1 1 d . . .
H22 H 0.3970 0.5279 1.4002 0.056 Uiso 1 1 calc R . .
C23 C 0.2760(3) 0.5249(2) 1.2485(2) 0.0452(7) Uani 1 1 d . . .
H23 H 0.2545 0.5979 1.2794 0.054 Uiso 1 1 calc R . .
C24 C 0.2246(3) 0.4605(2) 1.1316(2) 0.0378(6) Uani 1 1 d . . .
H24 H 0.1698 0.4904 1.0823 0.045 Uiso 1 1 calc R . .
C25 C -0.0037(2) 0.2502(2) 0.8962(2) 0.0284(6) Uani 1 1 d . . .
C26 C -0.0602(3) 0.2447(2) 0.9744(2) 0.0349(6) Uani 1 1 d . . .
H26 H -0.0010 0.2596 1.0497 0.042 Uiso 1 1 calc R . .
C27 C -0.2024(3) 0.2176(2) 0.9434(2) 0.0423(7) Uani 1 1 d . . .
H27 H -0.2400 0.2134 0.9973 0.051 Uiso 1 1 calc R . .
C28 C -0.2893(3) 0.1966(2) 0.8347(3) 0.0443(7) Uani 1 1 d . . .
H28 H -0.3868 0.1791 0.8139 0.053 Uiso 1 1 calc R . .
C29 C -0.2343(3) 0.2012(2) 0.7562(2) 0.0416(7) Uani 1 1 d . . .
H29 H -0.2943 0.1866 0.6812 0.050 Uiso 1 1 calc R . .
C30 C -0.0925(3) 0.2269(2) 0.7855(2) 0.0333(6) Uani 1 1 d . . .
H30 H -0.0555 0.2287 0.7304 0.040 Uiso 1 1 calc R . .
N1 N -0.2017(2) -0.19055(18) 0.53911(18) 0.0369(5) Uani 1 1 d . . .
O1 O 0.5249(2) -0.1075(2) 0.78399(19) 0.0598(6) Uani 1 1 d . . .
O2 O 0.1579(3) -0.23522(19) 0.46028(17) 0.0653(7) Uani 1 1 d . . .
O3 O 0.1382(2) -0.24416(17) 0.77748(18) 0.0559(6) Uani 1 1 d . . .
O4 O 0.53563(19) 0.14856(18) 1.01212(16) 0.0472(5) Uani 1 1 d . . .
O5 O 0.15696(19) 0.01396(17) 1.00509(16) 0.0435(5) 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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
C3 Fe1 C1 93.23(13) . . ?
C3 Fe1 C2 98.77(13) . . ?
C1 Fe1 C2 99.84(13) . . ?
C3 Fe1 S1 92.21(9) . . ?
C1 Fe1 S1 155.46(10) . . ?
C2 Fe1 S1 102.94(10) . . ?
C3 Fe1 S2 156.71(9) . . ?
C1 Fe1 S2 86.78(10) . . ?
C2 Fe1 S2 104.18(9) . . ?
S1 Fe1 S2 78.94(2) . . ?
C3 Fe1 Fe2 100.44(9) . . ?
C1 Fe1 Fe2 99.58(9) . . ?
C2 Fe1 Fe2 151.73(9) . . ?
S1 Fe1 Fe2 55.882(19) . . ?
S2 Fe1 Fe2 56.762(19) . . ?
C5 Fe2 C4 91.87(11) . . ?
C5 Fe2 P1 94.97(9) . . ?
C4 Fe2 P1 100.70(9) . . ?
C5 Fe2 S1 92.79(8) . . ?
C4 Fe2 S1 158.53(9) . . ?
P1 Fe2 S1 99.77(3) . . ?
C5 Fe2 S2 156.54(9) . . ?
C4 Fe2 S2 88.35(8) . . ?
P1 Fe2 S2 108.05(3) . . ?
S1 Fe2 S2 79.17(2) . . ?
C5 Fe2 Fe1 100.66(8) . . ?
C4 Fe2 Fe1 101.98(8) . . ?
P1 Fe2 Fe1 151.89(2) . . ?
S1 Fe2 Fe1 56.55(2) . . ?
S2 Fe2 Fe1 56.51(2) . . ?
C6 S1 Fe2 114.19(8) . . ?
C6 S1 Fe1 117.99(9) . . ?
Fe2 S1 Fe1 67.57(2) . . ?
C9 S2 Fe1 110.45(9) 2_556 . ?
C9 S2 Fe2 117.45(9) 2_556 . ?
Fe1 S2 Fe2 66.73(2) . . ?
C25 P1 C13 105.28(11) . . ?
C25 P1 C19 102.36(11) . . ?
C13 P1 C19 100.53(11) . . ?
C25 P1 Fe2 111.02(8) . . ?
C13 P1 Fe2 117.99(8) . . ?
C19 P1 Fe2 117.76(8) . . ?
O1 C1 Fe1 179.0(3) . . ?
O2 C2 Fe1 177.3(3) . . ?
O3 C3 Fe1 178.8(3) . . ?
O4 C4 Fe2 177.0(2) . . ?
O5 C5 Fe2 178.3(2) . . ?
C7 C6 S1 108.04(17) . . ?
N1 C7 C6 112.1(2) . . ?
N1 C8 C9 109.3(2) . . ?
C8 C9 S2 109.39(18) . 2_556 ?
N1 C10 C11 111.4(2) . . ?
C10 C11 C12 111.7(3) . . ?
C14 C13 C18 118.7(2) . . ?
C14 C13 P1 117.6(2) . . ?
C18 C13 P1 123.46(19) . . ?
C13 C14 C15 120.0(3) . . ?
C16 C15 C14 120.5(3) . . ?
C15 C16 C17 120.5(3) . . ?
C16 C17 C18 119.6(3) . . ?
C17 C18 C13 120.8(3) . . ?
C20 C19 C24 118.8(2) . . ?
C20 C19 P1 120.90(19) . . ?
C24 C19 P1 120.33(19) . . ?
C19 C20 C21 120.7(3) . . ?
C22 C21 C20 119.9(3) . . ?
C21 C22 C23 120.2(3) . . ?
C22 C23 C24 119.8(3) . . ?
C23 C24 C19 120.5(3) . . ?
C26 C25 C30 118.9(2) . . ?
C26 C25 P1 120.76(19) . . ?
C30 C25 P1 119.71(19) . . ?
C27 C26 C25 120.5(2) . . ?
C28 C27 C26 120.3(3) . . ?
C29 C28 C27 119.7(2) . . ?
C28 C29 C30 120.7(3) . . ?
C29 C30 C25 119.9(2) . . ?
C7 N1 C10 111.9(2) . . ?
C7 N1 C8 111.8(2) . . ?
C10 N1 C8 112.6(2) . . ?
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 C3 1.772(3) . ?
Fe1 C1 1.783(3) . ?
Fe1 C2 1.791(3) . ?
Fe1 S1 2.2645(7) . ?
Fe1 S2 2.2775(7) . ?
Fe1 Fe2 2.5087(5) . ?
Fe2 C5 1.760(3) . ?
Fe2 C4 1.770(3) . ?
Fe2 P1 2.2272(7) . ?
Fe2 S1 2.2469(7) . ?
Fe2 S2 2.2841(7) . ?
S1 C6 1.832(2) . ?
S2 C9 1.844(2) 2_556 ?
P1 C25 1.829(2) . ?
P1 C13 1.831(2) . ?
P1 C19 1.843(2) . ?
C1 O1 1.141(3) . ?
C2 O2 1.147(3) . ?
C3 O3 1.147(3) . ?
C4 O4 1.155(3) . ?
C5 O5 1.154(3) . ?
C6 C7 1.529(3) . ?
C7 N1 1.455(3) . ?
C8 N1 1.482(3) . ?
C8 C9 1.514(3) . ?
C9 S2 1.844(2) 2_556 ?
C10 N1 1.466(3) . ?
C10 C11 1.490(4) . ?
C11 C12 1.559(4) . ?
C13 C14 1.393(3) . ?
C13 C18 1.394(4) . ?
C14 C15 1.393(4) . ?
C15 C16 1.369(4) . ?
C16 C17 1.377(4) . ?
C17 C18 1.390(4) . ?
C19 C20 1.385(3) . ?
C19 C24 1.397(4) . ?
C20 C21 1.387(3) . ?
C21 C22 1.378(4) . ?
C22 C23 1.384(4) . ?
C23 C24 1.384(4) . ?
C25 C26 1.388(3) . ?
C25 C30 1.398(3) . ?
C26 C27 1.386(4) . ?
C27 C28 1.377(4) . ?
C28 C29 1.378(4) . ?
C29 C30 1.385(4) . ?
