#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316044.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_4316044
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            'C26 H30 Fe4 N2 O12 S4'
_chemical_formula_weight         914.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 108.8170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7648(11)
_cell_length_b                   10.8475(5)
_cell_length_c                   16.3427(8)
_cell_measurement_reflns_used    8118
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.32
_cell_volume                     3652.2(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       '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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25504
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         0.99
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_T_max  0.6557
_exptl_absorpt_correction_T_min  0.5899
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         8394
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0350P)²+0.5876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0693
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                7254
_reflns_number_total             8394
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100484a_si_002.cif
_cod_data_source_block           ic12574
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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               4316044
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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 0.111975(14) 1.18389(3) 0.321744(18) 0.01930(7) Uani 1 1 d . . .
Fe2 Fe 0.171429(13) 1.12929(3) 0.475814(17) 0.01779(7) Uani 1 1 d . . .
Fe3 Fe 0.330178(14) 0.56320(3) 0.360976(18) 0.02031(7) Uani 1 1 d . . .
Fe4 Fe 0.394779(14) 0.73275(3) 0.453273(19) 0.02184(8) Uani 1 1 d . . .
S1 S 0.13866(2) 0.98991(4) 0.36761(3) 0.01888(11) Uani 1 1 d . . .
S2 S 0.31441(3) 0.63014(5) 0.48422(3) 0.02285(11) Uani 1 1 d . . .
S3 S 0.22073(2) 1.20784(5) 0.38495(3) 0.02051(11) Uani 1 1 d . . .
S4 S 0.31224(2) 0.76446(5) 0.32956(3) 0.02041(11) Uani 1 1 d . . .
O1 O 0.08961(9) 1.17287(17) 0.13491(11) 0.0418(4) Uani 1 1 d . . .
O2 O 0.09235(9) 1.44879(15) 0.33503(12) 0.0481(5) Uani 1 1 d . . .
O3 O -0.02083(8) 1.14206(17) 0.31942(12) 0.0433(4) Uani 1 1 d . . .
O4 O 0.19283(8) 1.37303(14) 0.55639(10) 0.0339(4) Uani 1 1 d . . .
O5 O 0.06724(9) 1.06917(16) 0.54595(11) 0.0397(4) Uani 1 1 d . . .
O6 O 0.27808(8) 0.99965(16) 0.60396(10) 0.0375(4) Uani 1 1 d . . .
O7 O 0.41040(8) 0.54011(17) 0.24874(10) 0.0385(4) Uani 1 1 d . . .
O8 O 0.38685(8) 0.34176(15) 0.45924(10) 0.0362(4) Uani 1 1 d . . .
O9 O 0.20749(8) 0.45819(16) 0.24862(11) 0.0433(5) Uani 1 1 d . . .
O10 O 0.48408(8) 0.57680(17) 0.58488(12) 0.0460(5) Uani 1 1 d . . .
O11 O 0.49134(9) 0.7994(2) 0.37211(13) 0.0534(5) Uani 1 1 d . . .
O12 O 0.39985(9) 0.96769(17) 0.54488(11) 0.0457(5) Uani 1 1 d . . .
N1 N 0.13554(8) 0.75160(15) 0.47528(11) 0.0215(4) Uani 1 1 d . . .
N2 N 0.33816(8) 1.04019(16) 0.26837(11) 0.0220(4) Uani 1 1 d . . .
C1 C 0.09966(11) 1.1754(2) 0.20761(14) 0.0262(5) Uani 1 1 d . . .
C2 C 0.10198(11) 1.3467(2) 0.33005(14) 0.0293(5) Uani 1 1 d . . .
C3 C 0.03076(11) 1.1589(2) 0.31914(14) 0.0270(5) Uani 1 1 d . . .
C4 C 0.18366(10) 1.2778(2) 0.52568(13) 0.0225(4) Uani 1 1 d . . .
C5 C 0.10799(11) 1.0917(2) 0.51869(13) 0.0257(5) Uani 1 1 d . . .
C6 C 0.23683(10) 1.04876(19) 0.55404(13) 0.0237(4) Uani 1 1 d . . .
C7 C 0.37862(11) 0.5474(2) 0.29121(13) 0.0259(5) Uani 1 1 d . . .
C8 C 0.36457(11) 0.4271(2) 0.42051(13) 0.0256(5) Uani 1 1 d . . .
C9 C 0.25459(11) 0.4986(2) 0.29299(14) 0.0279(5) Uani 1 1 d . . .
C10 C 0.45041(11) 0.6394(2) 0.53429(15) 0.0303(5) Uani 1 1 d . . .
C11 C 0.45447(11) 0.7726(2) 0.40422(15) 0.0327(5) Uani 1 1 d . . .
C12 C 0.39787(11) 0.8768(2) 0.51019(14) 0.0295(5) Uani 1 1 d . . .
C13 C 0.06879(10) 0.89420(18) 0.36400(14) 0.0237(4) Uani 1 1 d . . .
H13A H 0.0481 0.9258 0.4056 0.028 Uiso 1 1 calc R . .
H13B H 0.0364 0.8969 0.3054 0.028 Uiso 1 1 calc R . .
C14 C 0.09149(10) 0.76241(18) 0.38692(14) 0.0253(5) Uani 1 1 d . . .
H14A H 0.0533 0.7089 0.3798 0.030 Uiso 1 1 calc R . .
H14B H 0.1138 0.7330 0.3465 0.030 Uiso 1 1 calc R . .
C15 C 0.18865(10) 0.66416(19) 0.48385(14) 0.0242(4) Uani 1 1 d . . .
H15A H 0.1740 0.5978 0.4403 0.029 Uiso 1 1 calc R . .
H15B H 0.2021 0.6261 0.5420 0.029 Uiso 1 1 calc R . .
C16 C 0.24510(10) 0.73182(19) 0.47057(15) 0.0263(5) Uani 1 1 d . . .
H16A H 0.2581 0.8005 0.5126 0.032 Uiso 1 1 calc R . .
H16B H 0.2316 0.7675 0.4117 0.032 Uiso 1 1 calc R . .
C17 C 0.10231(10) 0.7399(2) 0.54038(15) 0.0275(5) Uani 1 1 d . . .
H17 H 0.0661 0.8014 0.5250 0.033 Uiso 1 1 calc R . .
C18 C 0.14848(12) 0.7760(3) 0.62890(16) 0.0388(6) Uani 1 1 d . . .
H18A H 0.1837 0.7154 0.6476 0.058 Uiso 1 1 calc R . .
H18B H 0.1248 0.7781 0.6707 0.058 Uiso 1 1 calc R . .
H18C H 0.1667 0.8576 0.6255 0.058 Uiso 1 1 calc R . .
C19 C 0.07195(13) 0.6139(2) 0.54246(19) 0.0444(7) Uani 1 1 d . . .
H19A H 0.0434 0.5926 0.4843 0.067 Uiso 1 1 calc R . .
H19B H 0.0466 0.6162 0.5823 0.067 Uiso 1 1 calc R . .
H19C H 0.1063 0.5518 0.5621 0.067 Uiso 1 1 calc R . .
C20 C 0.27247(10) 1.09157(19) 0.35866(13) 0.0236(4) Uani 1 1 d . . .
H20A H 0.3104 1.0749 0.4105 0.028 Uiso 1 1 calc R . .
H20B H 0.2478 1.0138 0.3419 0.028 Uiso 1 1 calc R . .
C21 C 0.29579(10) 1.13401(19) 0.28552(13) 0.0224(4) Uani 1 1 d . . .
H21A H 0.2581 1.1481 0.2329 0.027 Uiso 1 1 calc R . .
H21B H 0.3198 1.2126 0.3014 0.027 Uiso 1 1 calc R . .
C22 C 0.30220(10) 0.94426(18) 0.20927(13) 0.0223(4) Uani 1 1 d . . .
H22A H 0.3019 0.9637 0.1500 0.027 Uiso 1 1 calc R . .
H22B H 0.2566 0.9439 0.2090 0.027 Uiso 1 1 calc R . .
C23 C 0.33134(11) 0.81672(19) 0.23431(13) 0.0238(4) Uani 1 1 d . . .
H23A H 0.3790 0.8201 0.2472 0.029 Uiso 1 1 calc R . .
H23B H 0.3132 0.7585 0.1859 0.029 Uiso 1 1 calc R . .
C24 C 0.39139(11) 1.0901(2) 0.24023(15) 0.0327(5) Uani 1 1 d . . .
H24 H 0.4115 1.0182 0.2202 0.039 Uiso 1 1 calc R . .
C25 C 0.36915(14) 1.1797(3) 0.16430(18) 0.0474(7) Uani 1 1 d . . .
H25A H 0.3359 1.1402 0.1161 0.071 Uiso 1 1 calc R . .
H25B H 0.4063 1.2027 0.1460 0.071 Uiso 1 1 calc R . .
H25C H 0.3510 1.2538 0.1821 0.071 Uiso 1 1 calc R . .
C26 C 0.44384(13) 1.1458(3) 0.31684(19) 0.0514(8) Uani 1 1 d . . .
H26A H 0.4269 1.2199 0.3364 0.077 Uiso 1 1 calc R . .
H26B H 0.4815 1.1678 0.2994 0.077 Uiso 1 1 calc R . .
H26C H 0.4569 1.0857 0.3641 0.077 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'
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'
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 C2 90.47(10) . . ?
C3 Fe1 C1 98.81(10) . . ?
C2 Fe1 C1 98.50(10) . . ?
C3 Fe1 S1 90.75(7) . . ?
C2 Fe1 S1 157.46(7) . . ?
C1 Fe1 S1 103.54(7) . . ?
C3 Fe1 S3 155.76(7) . . ?
C2 Fe1 S3 89.25(7) . . ?
C1 Fe1 S3 105.20(7) . . ?
S1 Fe1 S3 80.56(2) . . ?
C3 Fe1 Fe2 100.11(7) . . ?
C2 Fe1 Fe2 101.14(7) . . ?
C1 Fe1 Fe2 152.47(7) . . ?
S1 Fe1 Fe2 56.529(15) . . ?
S3 Fe1 Fe2 56.275(15) . . ?
C5 Fe2 C4 92.72(10) . . ?
C5 Fe2 C6 98.32(10) . . ?
C4 Fe2 C6 98.41(9) . . ?
C5 Fe2 S1 93.75(7) . . ?
C4 Fe2 S1 157.41(7) . . ?
C6 Fe2 S1 102.03(7) . . ?
C5 Fe2 S3 159.21(7) . . ?
C4 Fe2 S3 85.82(7) . . ?
C6 Fe2 S3 102.42(7) . . ?
S1 Fe2 S3 80.50(2) . . ?
C5 Fe2 Fe1 103.57(7) . . ?
C4 Fe2 Fe1 101.42(7) . . ?
C6 Fe2 Fe1 149.54(7) . . ?
S1 Fe2 Fe1 56.002(15) . . ?
S3 Fe2 Fe1 56.691(16) . . ?
C8 Fe3 C7 92.20(10) . . ?
C8 Fe3 C9 98.78(10) . . ?
C7 Fe3 C9 100.24(10) . . ?
C8 Fe3 S4 159.18(7) . . ?
C7 Fe3 S4 92.40(7) . . ?
C9 Fe3 S4 100.35(7) . . ?
C8 Fe3 S2 86.45(7) . . ?
C7 Fe3 S2 152.03(7) . . ?
C9 Fe3 S2 107.58(8) . . ?
S4 Fe3 S2 80.04(2) . . ?
C8 Fe3 Fe4 102.88(7) . . ?
C7 Fe3 Fe4 97.01(7) . . ?
C9 Fe3 Fe4 151.64(7) . . ?
S4 Fe3 Fe4 56.392(16) . . ?
S2 Fe3 Fe4 56.380(17) . . ?
C11 Fe4 C10 93.01(11) . . ?
C11 Fe4 C12 96.32(11) . . ?
C10 Fe4 C12 101.78(10) . . ?
C11 Fe4 S4 92.59(8) . . ?
C10 Fe4 S4 154.33(8) . . ?
C12 Fe4 S4 102.47(7) . . ?
C11 Fe4 S2 161.03(8) . . ?
C10 Fe4 S2 86.77(8) . . ?
C12 Fe4 S2 102.30(8) . . ?
S4 Fe4 S2 79.98(2) . . ?
C11 Fe4 Fe3 104.83(8) . . ?
C10 Fe4 Fe3 98.29(7) . . ?
C12 Fe4 Fe3 149.90(7) . . ?
S4 Fe4 Fe3 56.078(16) . . ?
S2 Fe4 Fe3 56.573(16) . . ?
C13 S1 Fe1 113.50(7) . . ?
C13 S1 Fe2 117.05(7) . . ?
Fe1 S1 Fe2 67.469(17) . . ?
C16 S2 Fe4 110.10(7) . . ?
C16 S2 Fe3 116.17(8) . . ?
Fe4 S2 Fe3 67.047(18) . . ?
C20 S3 Fe2 110.64(7) . . ?
C20 S3 Fe1 116.35(7) . . ?
Fe2 S3 Fe1 67.034(17) . . ?
C23 S4 Fe3 115.20(7) . . ?
C23 S4 Fe4 118.48(7) . . ?
Fe3 S4 Fe4 67.529(18) . . ?
C14 N1 C15 113.14(17) . . ?
C14 N1 C17 113.79(17) . . ?
C15 N1 C17 115.53(16) . . ?
C21 N2 C22 112.70(16) . . ?
C21 N2 C24 114.28(17) . . ?
C22 N2 C24 111.14(16) . . ?
O1 C1 Fe1 177.2(2) . . ?
O2 C2 Fe1 176.4(2) . . ?
O3 C3 Fe1 178.4(2) . . ?
O4 C4 Fe2 178.01(19) . . ?
O5 C5 Fe2 179.1(2) . . ?
O6 C6 Fe2 179.0(2) . . ?
O7 C7 Fe3 177.9(2) . . ?
O8 C8 Fe3 179.0(2) . . ?
O9 C9 Fe3 178.4(2) . . ?
O10 C10 Fe4 177.5(2) . . ?
O11 C11 Fe4 178.6(2) . . ?
O12 C12 Fe4 179.1(2) . . ?
C14 C13 S1 109.01(14) . . ?
N1 C14 C13 112.18(17) . . ?
N1 C15 C16 109.00(16) . . ?
C15 C16 S2 111.64(14) . . ?
N1 C17 C18 109.69(18) . . ?
N1 C17 C19 114.29(19) . . ?
C18 C17 C19 111.6(2) . . ?
C21 C20 S3 111.35(14) . . ?
N2 C21 C20 109.46(17) . . ?
N2 C22 C23 112.41(17) . . ?
C22 C23 S4 108.76(14) . . ?
N2 C24 C26 110.15(19) . . ?
N2 C24 C25 114.24(19) . . ?
C26 C24 C25 111.9(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 1.775(2) . ?
Fe1 C2 1.790(2) . ?
Fe1 C1 1.799(2) . ?
Fe1 S1 2.2463(6) . ?
Fe1 S3 2.2716(6) . ?
Fe1 Fe2 2.5027(4) . ?
Fe2 C5 1.786(2) . ?
Fe2 C4 1.787(2) . ?
Fe2 C6 1.803(2) . ?
Fe2 S1 2.2601(6) . ?
Fe2 S3 2.2607(6) . ?
Fe3 C8 1.794(2) . ?
Fe3 C7 1.793(2) . ?
Fe3 C9 1.803(2) . ?
Fe3 S4 2.2479(6) . ?
Fe3 S2 2.2689(6) . ?
Fe3 Fe4 2.5033(4) . ?
Fe4 C11 1.786(3) . ?
Fe4 C10 1.792(2) . ?
Fe4 C12 1.808(2) . ?
Fe4 S4 2.2562(6) . ?
Fe4 S2 2.2638(6) . ?
S1 C13 1.826(2) . ?
S2 C16 1.823(2) . ?
S3 C20 1.832(2) . ?
S4 C23 1.826(2) . ?
O1 C1 1.137(3) . ?
O2 C2 1.135(3) . ?
O3 C3 1.139(3) . ?
O4 C4 1.137(2) . ?
O5 C5 1.140(3) . ?
O6 C6 1.133(3) . ?
O7 C7 1.130(3) . ?
O8 C8 1.138(3) . ?
O9 C9 1.136(3) . ?
O10 C10 1.136(3) . ?
O11 C11 1.129(3) . ?
O12 C12 1.131(3) . ?
N1 C14 1.458(3) . ?
N1 C15 1.467(2) . ?
N1 C17 1.472(3) . ?
N2 C21 1.460(3) . ?
N2 C22 1.463(2) . ?
N2 C24 1.480(3) . ?
C13 C14 1.519(3) . ?
C15 C16 1.506(3) . ?
C17 C18 1.523(3) . ?
C17 C19 1.523(3) . ?
C20 C21 1.513(3) . ?
C22 C23 1.522(3) . ?
C24 C26 1.521(3) . ?
C24 C25 1.527(4) . ?
