#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316048.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_4316048
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            'C32 H44 B2 F8 Fe4 N2 O14 S4'
_chemical_formula_weight         1205.95
_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                78.783(2)
_cell_angle_beta                 76.187(2)
_cell_angle_gamma                89.577(2)
_cell_formula_units_Z            1
_cell_length_a                   7.9730(3)
_cell_length_b                   12.1333(5)
_cell_length_c                   13.1870(5)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.00
_cell_volume                     1214.12(8)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0440
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16342
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    1.433
_exptl_absorpt_correction_T_max  0.923
_exptl_absorpt_correction_T_min  0.692
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0374P)²+1.4191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0915
_refine_ls_wR_factor_ref         0.0984
_reflns_number_gt                4300
_reflns_number_total             5510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100484a_si_006.cif
_cod_data_source_block           ic13212
_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               4316048
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 1.30937(5) 0.27516(3) 0.45627(3) 0.02622(11) Uani 1 1 d . . .
Fe2 Fe 1.06290(5) 0.31607(3) 0.36578(3) 0.02550(11) Uani 1 1 d . . .
S1 S 1.07489(9) 0.15936(6) 0.48671(5) 0.02539(15) Uani 1 1 d . . .
S2 S 0.67613(9) -0.25845(6) 0.71353(5) 0.02745(16) Uani 1 1 d . . .
N1 N 0.8130(3) 0.03053(19) 0.79370(17) 0.0270(5) Uani 1 1 d . . .
H1 H 0.7203 0.0724 0.7794 0.032 Uiso 1 1 calc R . .
C1 C 1.4453(4) 0.4006(3) 0.4028(2) 0.0357(7) Uani 1 1 d . . .
C2 C 1.4729(4) 0.1782(3) 0.4891(2) 0.0357(7) Uani 1 1 d . . .
C3 C 1.2304(4) 0.3209(3) 0.5798(2) 0.0327(7) Uani 1 1 d . . .
C4 C 0.9117(4) 0.3766(2) 0.4602(2) 0.0322(7) Uani 1 1 d . . .
C5 C 0.9113(4) 0.2734(3) 0.2956(2) 0.0327(7) Uani 1 1 d . . .
C6 C 1.1283(4) 0.4529(3) 0.2831(2) 0.0347(7) Uani 1 1 d . . .
C7 C 0.9169(4) 0.1539(2) 0.6133(2) 0.0279(6) Uani 1 1 d . . .
H7A H 0.9167 0.2273 0.6354 0.034 Uiso 1 1 calc R . .
H7B H 0.7997 0.1371 0.6057 0.034 Uiso 1 1 calc R . .
C8 C 0.9654(4) 0.0626(3) 0.6962(2) 0.0301(6) Uani 1 1 d . . .
H8A H 1.0654 0.0896 0.7184 0.036 Uiso 1 1 calc R . .
H8B H 0.9997 -0.0045 0.6650 0.036 Uiso 1 1 calc R . .
C9 C 0.7589(4) -0.0913(2) 0.8118(2) 0.0324(7) Uani 1 1 d . . .
H9A H 0.6745 -0.1133 0.8815 0.039 Uiso 1 1 calc R . .
H9B H 0.8608 -0.1383 0.8128 0.039 Uiso 1 1 calc R . .
C10 C 0.6770(4) -0.1100(2) 0.7222(2) 0.0324(7) Uani 1 1 d . . .
H10A H 0.7428 -0.0648 0.6535 0.039 Uiso 1 1 calc R . .
H10B H 0.5569 -0.0845 0.7358 0.039 Uiso 1 1 calc R . .
C11 C 0.8510(4) 0.0596(2) 0.8927(2) 0.0300(6) Uani 1 1 d . . .
H11A H 0.9642 0.0303 0.9009 0.036 Uiso 1 1 calc R . .
H11B H 0.7614 0.0231 0.9561 0.036 Uiso 1 1 calc R . .
C12 C 0.8543(4) 0.1856(3) 0.8862(3) 0.0378(7) Uani 1 1 d . . .
H12A H 0.7471 0.2164 0.8688 0.045 Uiso 1 1 calc R . .
H12B H 0.9536 0.2212 0.8286 0.045 Uiso 1 1 calc R . .
C13 C 0.8696(5) 0.2136(3) 0.9916(3) 0.0502(9) Uani 1 1 d . . .
H13A H 0.7754 0.1745 1.0493 0.075 Uiso 1 1 calc R . .
H13B H 0.8623 0.2949 0.9876 0.075 Uiso 1 1 calc R . .
H13C H 0.9808 0.1893 1.0056 0.075 Uiso 1 1 calc R . .
O1 O 1.5302(3) 0.4806(2) 0.3706(2) 0.0532(7) Uani 1 1 d . . .
O2 O 1.5771(3) 0.1183(2) 0.5043(2) 0.0498(6) Uani 1 1 d . . .
O3 O 1.1760(3) 0.3522(2) 0.65642(18) 0.0447(6) Uani 1 1 d . . .
O4 O 0.8151(3) 0.41477(19) 0.52205(19) 0.0464(6) Uani 1 1 d . . .
O5 O 0.8144(3) 0.2471(2) 0.25378(19) 0.0488(6) Uani 1 1 d . . .
O6 O 1.1702(3) 0.53990(19) 0.2328(2) 0.0525(7) Uani 1 1 d . . .
B1 B 0.3856(5) 0.1108(4) 0.8140(3) 0.0441(9) Uani 1 1 d . . .
F1 F 0.4506(3) 0.0539(3) 0.89583(19) 0.0931(10) Uani 1 1 d . . .
F2 F 0.2682(3) 0.1850(2) 0.8459(2) 0.0830(8) Uani 1 1 d . . .
F3 F 0.3090(3) 0.0342(3) 0.7753(3) 0.1047(11) Uani 1 1 d . . .
F4 F 0.5286(3) 0.1626(2) 0.73809(17) 0.0638(7) Uani 1 1 d . . .
O7 O 0.8272(4) 0.6304(3) -0.0645(2) 0.0668(8) Uani 1 1 d . . .
C14 C 0.7274(5) 0.6008(3) 0.0207(3) 0.0454(8) Uani 1 1 d . . .
C15 C 0.7782(6) 0.5280(4) 0.1121(3) 0.0670(12) Uani 1 1 d . . .
H15A H 0.8962 0.5038 0.0886 0.101 Uiso 1 1 calc R . .
H15B H 0.6987 0.4619 0.1391 0.101 Uiso 1 1 calc R . .
H15C H 0.7731 0.5704 0.1688 0.101 Uiso 1 1 calc R . .
C16 C 0.5455(5) 0.6381(4) 0.0397(4) 0.0739(13) Uani 1 1 d . . .
H16A H 0.5274 0.6875 0.0917 0.111 Uiso 1 1 calc R . .
H16B H 0.4657 0.5723 0.0672 0.111 Uiso 1 1 calc R . .
H16C H 0.5242 0.6792 -0.0275 0.111 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'
F F 0.0171 0.0103 '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'
B B 0.0013 0.0007 '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 90.96(13) . . ?
C3 Fe1 C2 101.31(14) . . ?
C1 Fe1 C2 98.69(15) . . ?
C3 Fe1 S1 91.99(9) . . ?
C1 Fe1 S1 157.62(11) . . ?
C2 Fe1 S1 102.46(10) . . ?
C3 Fe1 S2 157.78(11) . 2_756 ?
C1 Fe1 S2 87.74(10) . 2_756 ?
C2 Fe1 S2 100.81(10) . 2_756 ?
S1 Fe1 S2 81.23(3) . 2_756 ?
C3 Fe1 Fe2 102.71(10) . . ?
C1 Fe1 Fe2 102.06(11) . . ?
C2 Fe1 Fe2 147.76(10) . . ?
S1 Fe1 Fe2 55.68(2) . . ?
S2 Fe1 Fe2 56.09(2) 2_756 . ?
C4 Fe2 C6 91.13(13) . . ?
C4 Fe2 C5 97.58(14) . . ?
C6 Fe2 C5 98.55(14) . . ?
C4 Fe2 S1 92.47(9) . . ?
C6 Fe2 S1 157.94(11) . . ?
C5 Fe2 S1 102.53(10) . . ?
C4 Fe2 S2 156.73(10) . 2_756 ?
C6 Fe2 S2 86.83(10) . 2_756 ?
C5 Fe2 S2 105.66(10) . 2_756 ?
S1 Fe2 S2 81.32(3) . 2_756 ?
C4 Fe2 Fe1 102.07(10) . . ?
C6 Fe2 Fe1 102.02(10) . . ?
C5 Fe2 Fe1 151.09(10) . . ?
S1 Fe2 Fe1 55.96(2) . . ?
S2 Fe2 Fe1 55.96(2) 2_756 . ?
C7 S1 Fe2 113.03(10) . . ?
C7 S1 Fe1 116.00(10) . . ?
Fe2 S1 Fe1 68.36(2) . . ?
C10 S2 Fe1 109.90(10) . 2_756 ?
C10 S2 Fe2 113.69(11) . 2_756 ?
Fe1 S2 Fe2 67.95(2) 2_756 2_756 ?
C9 N1 C11 111.2(2) . . ?
C9 N1 C8 111.2(2) . . ?
C11 N1 C8 112.1(2) . . ?
O1 C1 Fe1 178.8(3) . . ?
O2 C2 Fe1 176.6(3) . . ?
O3 C3 Fe1 177.4(3) . . ?
O4 C4 Fe2 179.1(3) . . ?
O5 C5 Fe2 178.6(3) . . ?
O6 C6 Fe2 178.6(3) . . ?
C8 C7 S1 108.4(2) . . ?
C7 C8 N1 110.6(2) . . ?
N1 C9 C10 109.2(2) . . ?
C9 C10 S2 110.8(2) . . ?
N1 C11 C12 111.1(2) . . ?
C11 C12 C13 110.8(3) . . ?
F2 B1 F3 108.9(3) . . ?
F2 B1 F1 112.3(4) . . ?
F3 B1 F1 108.0(4) . . ?
F2 B1 F4 112.3(3) . . ?
F3 B1 F4 110.3(4) . . ?
F1 B1 F4 105.0(3) . . ?
O7 C14 C15 122.3(4) . . ?
O7 C14 C16 120.8(4) . . ?
C15 C14 C16 116.9(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 C3 1.794(3) . ?
Fe1 C1 1.797(3) . ?
Fe1 C2 1.822(3) . ?
Fe1 S1 2.2564(8) . ?
Fe1 S2 2.2629(8) 2_756 ?
Fe1 Fe2 2.5312(6) . ?
Fe2 C4 1.780(3) . ?
Fe2 C6 1.804(3) . ?
Fe2 C5 1.821(3) . ?
Fe2 S1 2.2490(8) . ?
Fe2 S2 2.2663(8) 2_756 ?
S1 C7 1.825(3) . ?
S2 C10 1.826(3) . ?
S2 Fe1 2.2629(8) 2_756 ?
S2 Fe2 2.2663(8) 2_756 ?
N1 C9 1.500(4) . ?
N1 C11 1.513(3) . ?
N1 C8 1.532(3) . ?
C1 O1 1.138(4) . ?
C2 O2 1.128(4) . ?
C3 O3 1.136(4) . ?
C4 O4 1.147(4) . ?
C5 O5 1.131(4) . ?
C6 O6 1.137(4) . ?
C7 C8 1.516(4) . ?
C9 C10 1.534(4) . ?
C11 C12 1.515(4) . ?
C12 C13 1.524(4) . ?
B1 F2 1.345(5) . ?
B1 F3 1.357(5) . ?
B1 F1 1.371(4) . ?
B1 F4 1.385(4) . ?
O7 C14 1.202(4) . ?
C14 C15 1.486(5) . ?
C14 C16 1.494(5) . ?
