#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:18:24 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179240 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/60/4316052.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_4316052
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            'C48 H84 Fe4 N2 O10 P2 S4'
_chemical_formula_weight         1262.75
_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                113.9135(15)
_cell_angle_beta                 96.2465(16)
_cell_angle_gamma                99.3751(14)
_cell_formula_units_Z            1
_cell_length_a                   10.8266(3)
_cell_length_b                   12.4979(4)
_cell_length_c                   12.5366(4)
_cell_measurement_reflns_used    17778
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.81
_cell_volume                     1500.98(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 0.992
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0447
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            17778
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  0.779
_exptl_absorpt_correction_T_min  0.691
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         6843
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0560P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                5414
_reflns_number_total             6843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100484a_si_010.cif
_cod_data_source_block           ic14339
_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 
;
_cod_original_cell_volume        1500.97(8)
_cod_database_code               4316052
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 0.72882(3) 0.00681(3) 0.22036(3) 0.02040(9) Uani 1 1 d . . .
Fe2 Fe 0.75187(3) -0.17429(3) 0.25551(3) 0.02171(9) Uani 1 1 d U . .
S1 S 0.68165(5) -0.01815(5) 0.38305(5) 0.02270(13) Uani 1 1 d . . .
S2 S 1.08202(5) 0.02083(5) 0.71304(5) 0.02117(13) Uani 1 1 d . . .
P1 P 0.74945(5) 0.20516(5) 0.29356(5) 0.02464(14) Uani 1 1 d . . .
N1 N 0.83881(16) 0.15315(16) 0.73633(15) 0.0224(4) Uani 1 1 d . . .
C1 C 0.7688(2) -0.0154(2) 0.0815(2) 0.0285(5) Uani 1 1 d . . .
C2 C 0.5656(2) -0.0355(2) 0.15415(19) 0.0267(5) Uani 1 1 d . . .
C3 C 0.7865(2) -0.2690(2) 0.1181(2) 0.0272(5) Uani 1 1 d U . .
C4 C 0.5903(2) -0.2581(2) 0.2159(2) 0.0283(5) Uani 1 1 d . . .
C5 C 0.8216(2) -0.2321(2) 0.3523(2) 0.0278(5) Uani 1 1 d U . .
C6 C 0.8042(2) 0.0657(2) 0.51975(18) 0.0270(5) Uani 1 1 d . . .
H6A H 0.8577 0.0119 0.5295 0.032 Uiso 1 1 calc R . .
H6B H 0.8601 0.1330 0.5133 0.032 Uiso 1 1 calc R . .
C7 C 0.7419(2) 0.1150(2) 0.62815(19) 0.0269(5) Uani 1 1 d . . .
H7A H 0.7075 0.1842 0.6296 0.032 Uiso 1 1 calc R . .
H7B H 0.6705 0.0521 0.6242 0.032 Uiso 1 1 calc R . .
C8 C 0.84506(19) 0.0510(2) 0.76404(19) 0.0234(5) Uani 1 1 d . . .
H8A H 0.8169 -0.0241 0.6895 0.028 Uiso 1 1 calc R . .
H8B H 0.7848 0.0482 0.8174 0.028 Uiso 1 1 calc R . .
C9 C 0.97755(19) 0.0555(2) 0.82298(19) 0.0234(5) Uani 1 1 d . . .
H9A H 0.9717 -0.0034 0.8573 0.028 Uiso 1 1 calc R . .
H9B H 1.0140 0.1366 0.8883 0.028 Uiso 1 1 calc R . .
C10 C 0.8145(2) 0.2537(2) 0.8393(2) 0.0293(5) Uani 1 1 d . . .
H10A H 0.8742 0.2667 0.9114 0.035 Uiso 1 1 calc R . .
H10B H 0.7268 0.2302 0.8506 0.035 Uiso 1 1 calc R . .
C11 C 0.8286(2) 0.3715(2) 0.8286(2) 0.0339(6) Uani 1 1 d . . .
H11A H 0.7645 0.3601 0.7600 0.041 Uiso 1 1 calc R . .
H11B H 0.8093 0.4324 0.9010 0.041 Uiso 1 1 calc R . .
C12 C 0.9588(3) 0.4194(3) 0.8127(3) 0.0563(9) Uani 1 1 d . . .
H12A H 1.0240 0.4228 0.8754 0.084 Uiso 1 1 calc R . .
H12B H 0.9639 0.5003 0.8175 0.084 Uiso 1 1 calc R . .
H12C H 0.9733 0.3662 0.7348 0.084 Uiso 1 1 calc R . .
C13 C 0.6579(2) 0.2672(2) 0.4125(2) 0.0307(5) Uani 1 1 d . . .
H13A H 0.6874 0.2486 0.4793 0.037 Uiso 1 1 calc R . .
H13B H 0.6770 0.3558 0.4426 0.037 Uiso 1 1 calc R . .
C14 C 0.5136(2) 0.2191(2) 0.3731(2) 0.0387(6) Uani 1 1 d . . .
H14A H 0.4955 0.1313 0.3230 0.046 Uiso 1 1 calc R . .
H14B H 0.4804 0.2567 0.3236 0.046 Uiso 1 1 calc R . .
C15 C 0.4426(3) 0.2429(2) 0.4772(2) 0.0420(6) Uani 1 1 d . . .
H15A H 0.3504 0.2079 0.4444 0.050 Uiso 1 1 calc R . .
H15B H 0.4720 0.2005 0.5233 0.050 Uiso 1 1 calc R . .
C16 C 0.4597(3) 0.3717(2) 0.5597(2) 0.0452(7) Uani 1 1 d . . .
H16A H 0.5497 0.4059 0.5983 0.068 Uiso 1 1 calc R . .
H16B H 0.4075 0.3788 0.6204 0.068 Uiso 1 1 calc R . .
H16C H 0.4331 0.4154 0.5150 0.068 Uiso 1 1 calc R . .
C17 C 0.9092(2) 0.3002(2) 0.3662(2) 0.0320(5) Uani 1 1 d . . .
H17A H 0.9034 0.3854 0.4012 0.038 Uiso 1 1 calc R . .
H17B H 0.9422 0.2816 0.4320 0.038 Uiso 1 1 calc R . .
C18 C 1.0032(2) 0.2838(2) 0.2824(2) 0.0351(6) Uani 1 1 d . . .
H18A H 0.9717 0.3047 0.2179 0.042 Uiso 1 1 calc R . .
H18B H 1.0073 0.1981 0.2457 0.042 Uiso 1 1 calc R . .
C19 C 1.1371(2) 0.3607(3) 0.3444(2) 0.0463(7) Uani 1 1 d . . .
H19A H 1.1337 0.4465 0.3786 0.056 Uiso 1 1 calc R . .
H19B H 1.1677 0.3418 0.4106 0.056 Uiso 1 1 calc R . .
C20 C 1.2301(3) 0.3404(3) 0.2613(3) 0.0534(8) Uani 1 1 d . . .
H20A H 1.2312 0.2549 0.2245 0.080 Uiso 1 1 calc R . .
H20B H 1.3157 0.3876 0.3060 0.080 Uiso 1 1 calc R . .
H20C H 1.2043 0.3655 0.1993 0.080 Uiso 1 1 calc R . .
C21 C 0.6946(2) 0.2571(2) 0.18260(19) 0.0263(5) Uani 1 1 d . . .
H21A H 0.7404 0.2273 0.1160 0.032 Uiso 1 1 calc R . .
H21B H 0.6027 0.2194 0.1504 0.032 Uiso 1 1 calc R . .
C22 C 0.7125(2) 0.3929(2) 0.2264(2) 0.0320(5) Uani 1 1 d . . .
H22A H 0.8049 0.4308 0.2505 0.038 Uiso 1 1 calc R . .
H22B H 0.6735 0.4248 0.2975 0.038 Uiso 1 1 calc R . .
C23 C 0.6525(2) 0.4279(2) 0.1317(2) 0.0334(6) Uani 1 1 d . . .
H23A H 0.6799 0.5160 0.1600 0.040 Uiso 1 1 calc R . .
H23B H 0.6851 0.3892 0.0578 0.040 Uiso 1 1 calc R . .
C24 C 0.5087(2) 0.3922(2) 0.1036(2) 0.0414(6) Uani 1 1 d . . .
H24A H 0.4808 0.3044 0.0675 0.062 Uiso 1 1 calc R . .
H24B H 0.4761 0.4226 0.0479 0.062 Uiso 1 1 calc R . .
H24C H 0.4757 0.4264 0.1770 0.062 Uiso 1 1 calc R . .
O1 O 0.79503(17) -0.03049(19) -0.00892(15) 0.0462(5) Uani 1 1 d . . .
O2 O 0.46024(15) -0.06740(17) 0.10603(15) 0.0410(4) Uani 1 1 d . . .
O3 O 0.80867(17) -0.32979(16) 0.02813(15) 0.0416(4) Uani 1 1 d . . .
O4 O 0.48658(15) -0.31012(16) 0.19179(16) 0.0422(4) Uani 1 1 d . . .
O5 O 0.86556(16) -0.26761(17) 0.41478(16) 0.0426(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
C1 Fe1 C2 89.57(10) . . ?
C1 Fe1 P1 97.32(8) . . ?
C2 Fe1 P1 97.43(8) . . ?
C1 Fe1 S2 92.26(7) . 2_756 ?
C2 Fe1 S2 156.12(8) . 2_756 ?
P1 Fe1 S2 105.93(2) . 2_756 ?
C1 Fe1 S1 164.18(8) . . ?
C2 Fe1 S1 91.15(7) . . ?
P1 Fe1 S1 98.25(2) . . ?
S2 Fe1 S1 80.82(2) 2_756 . ?
C1 Fe1 Fe2 108.14(8) . . ?
C2 Fe1 Fe2 100.35(8) . . ?
P1 Fe1 Fe2 148.84(2) . . ?
S2 Fe1 Fe2 56.557(17) 2_756 . ?
S1 Fe1 Fe2 56.214(17) . . ?
C3 Fe2 C4 92.02(10) . . ?
C3 Fe2 C5 100.71(10) . . ?
C4 Fe2 C5 100.78(10) . . ?
C3 Fe2 S1 156.51(8) . . ?
C4 Fe2 S1 86.43(7) . . ?
C5 Fe2 S1 102.61(8) . . ?
C3 Fe2 S2 92.77(7) . 2_756 ?
C4 Fe2 S2 157.98(8) . 2_756 ?
C5 Fe2 S2 99.42(7) . 2_756 ?
S1 Fe2 S2 80.69(2) . 2_756 ?
C3 Fe2 Fe1 101.09(8) . . ?
C4 Fe2 Fe1 102.05(7) . . ?
C5 Fe2 Fe1 147.64(8) . . ?
S1 Fe2 Fe1 56.605(17) . . ?
S2 Fe2 Fe1 55.934(16) 2_756 . ?
C6 S1 Fe2 108.97(7) . . ?
C6 S1 Fe1 115.30(7) . . ?
Fe2 S1 Fe1 67.181(18) . . ?
C9 S2 Fe1 113.89(7) . 2_756 ?
C9 S2 Fe2 115.40(8) . 2_756 ?
Fe1 S2 Fe2 67.509(18) 2_756 2_756 ?
C17 P1 C21 104.48(11) . . ?
C17 P1 C13 101.05(11) . . ?
C21 P1 C13 103.75(11) . . ?
C17 P1 Fe1 117.34(8) . . ?
C21 P1 Fe1 113.95(8) . . ?
C13 P1 Fe1 114.53(8) . . ?
C8 N1 C7 109.84(17) . . ?
C8 N1 C10 110.34(16) . . ?
C7 N1 C10 112.45(17) . . ?
O1 C1 Fe1 179.5(2) . . ?
O2 C2 Fe1 176.7(2) . . ?
O3 C3 Fe2 179.3(2) . . ?
O4 C4 Fe2 179.0(2) . . ?
O5 C5 Fe2 179.2(2) . . ?
C7 C6 S1 110.50(15) . . ?
N1 C7 C6 108.65(17) . . ?
N1 C8 C9 113.67(18) . . ?
C8 C9 S2 109.97(14) . . ?
N1 C10 C11 114.84(19) . . ?
C12 C11 C10 114.5(2) . . ?
C14 C13 P1 114.28(16) . . ?
C13 C14 C15 113.5(2) . . ?
C16 C15 C14 115.0(2) . . ?
C18 C17 P1 113.33(17) . . ?
C17 C18 C19 113.0(2) . . ?
C20 C19 C18 112.4(2) . . ?
C22 C21 P1 116.25(15) . . ?
C21 C22 C23 112.90(19) . . ?
C24 C23 C22 113.3(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 C1 1.763(2) . ?
Fe1 C2 1.764(2) . ?
Fe1 P1 2.2290(7) . ?
Fe1 S2 2.2589(6) 2_756 ?
Fe1 S1 2.2821(6) . ?
Fe1 Fe2 2.5195(4) . ?
Fe2 C3 1.772(2) . ?
Fe2 C4 1.788(2) . ?
Fe2 C5 1.804(2) . ?
Fe2 S1 2.2718(6) . ?
Fe2 S2 2.2754(6) 2_756 ?
S1 C6 1.842(2) . ?
S2 C9 1.839(2) . ?
S2 Fe1 2.2589(6) 2_756 ?
S2 Fe2 2.2754(6) 2_756 ?
P1 C17 1.829(2) . ?
P1 C21 1.840(2) . ?
P1 C13 1.856(2) . ?
N1 C8 1.463(3) . ?
N1 C7 1.473(3) . ?
N1 C10 1.477(3) . ?
C1 O1 1.146(3) . ?
C2 O2 1.154(3) . ?
C3 O3 1.153(3) . ?
C4 O4 1.142(3) . ?
C5 O5 1.143(3) . ?
C6 C7 1.529(3) . ?
C8 C9 1.522(3) . ?
C10 C11 1.517(3) . ?
C11 C12 1.506(3) . ?
C13 C14 1.526(3) . ?
C14 C15 1.537(3) . ?
C15 C16 1.485(4) . ?
C17 C18 1.518(3) . ?
C18 C19 1.525(3) . ?
C19 C20 1.504(4) . ?
C21 C22 1.528(3) . ?
C22 C23 1.539(3) . ?
C23 C24 1.508(3) . ?
