#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:15:08 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180130 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/28/7102855.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_7102855
loop_
_publ_author_name
'Xu, Fenfen'
'Tard, Cédric'
'Wang, Xiufeng'
'Ibrahim, Saad K'
'Hughes, David L'
'Zhong, Wei'
'Zeng, Xirui'
'Luo, Qiuyan'
'Liu, Xiaoming'
'Pickett, Christopher J'
_publ_section_title
;
 Controlling carbon monoxide binding at di-iron units related to the
 iron-only hydrogenase sub-site.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              606
_journal_page_last               608
_journal_paper_doi               10.1039/b712805c
_journal_year                    2008
_chemical_formula_moiety         'C10 H11 Fe2 N O5 S2, C2 H3 N'
_chemical_formula_structural     '[Fe2 (CO)5 {MeC(SCH2)CH2NH2}].MeCN'
_chemical_formula_sum            'C12 H14 Fe2 N2 O5 S2'
_chemical_formula_weight         442.07
_chemical_name_common            'Compound A, X=CH2NH2'
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and CrysAlis RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.9779(12)
_cell_length_b                   9.6907(7)
_cell_length_c                   9.6462(5)
_cell_measurement_temperature    140(1)
_cell_volume                     1680.55(19)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28c4 beta
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta
;
_computing_molecular_graphics    'ORTEP (Johnson, 1971)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997b)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      140(1)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_sigmaI/netI    0.0140
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            29453
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.74
_exptl_absorpt_coefficient_mu    1.998
_exptl_absorpt_correction_T_max  1.112
_exptl_absorpt_correction_T_min  0.802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.575
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0233
_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)+(0.0305P)²+0.6602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                2308
_reflns_number_total             2582
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b712805c.txt
_cod_data_source_block           xiaomingl8
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7102855
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x+1/2, -y, z+1/2'
'-x, -y, -z'
'x, -y-1/2, z'
'-x-1/2, y-1/2, z-1/2'
'x-1/2, y, -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 0.459987(15) 0.2500 0.10319(3) 0.01713(7) Uani 1 2 d S . .
Fe2 Fe 0.434517(15) 0.2500 0.35689(3) 0.01792(7) Uani 1 2 d S . .
S1 S 0.506190(17) 0.41095(3) 0.25024(3) 0.01935(8) Uani 1 1 d . . .
C1 C 0.60250(7) 0.37963(15) 0.29964(15) 0.0246(3) Uani 1 1 d . . .
H1A H 0.6321 0.3755 0.2156 0.029 Uiso 1 1 calc R . .
H1B H 0.6197 0.4586 0.3524 0.029 Uiso 1 1 calc R . .
C2 C 0.61846(10) 0.2500 0.38415(19) 0.0188(3) Uani 1 2 d S . .
C21 C 0.70258(10) 0.2500 0.4152(2) 0.0250(4) Uani 1 2 d S . .
H21A H 0.7151 0.3304 0.4685 0.037 Uiso 0.50 1 calc PR . .
H21B H 0.7298 0.2509 0.3296 0.037 Uiso 1 2 calc SR . .
H21C H 0.7152 0.1687 0.4669 0.037 Uiso 0.50 1 calc PR . .
C3 C 0.57929(11) 0.2500 0.5261(2) 0.0249(4) Uani 1 2 d S . .
H3A H 0.5967 0.1696 0.5765 0.030 Uiso 0.50 1 calc PR . .
H3B H 0.5967 0.3304 0.5765 0.030 Uiso 0.50 1 calc PR . .
N4 N 0.49820(10) 0.2500 0.53326(18) 0.0398(5) Uani 1 2 d S . .
H4A H 0.4848 0.3245 0.5830 0.048 Uiso 0.50 1 calc PR . .
H4B H 0.4848 0.1755 0.5830 0.048 Uiso 0.50 1 calc PR . .
C11 C 0.52340(11) 0.2500 -0.0421(2) 0.0218(4) Uani 1 2 d S . .
O11 O 0.56262(9) 0.2500 -0.13458(16) 0.0318(3) Uani 1 2 d S . .
C12 C 0.39788(7) 0.11763(15) 0.04455(14) 0.0220(3) Uani 1 1 d . . .
O12 O 0.35765(6) 0.03298(11) 0.01121(11) 0.0302(2) Uani 1 1 d . . .
C22 C 0.36435(8) 0.12606(15) 0.37817(15) 0.0251(3) Uani 1 1 d . . .
O22 O 0.31423(7) 0.05127(13) 0.38216(14) 0.0406(3) Uani 1 1 d . . .
N5 N 0.37219(11) 0.2500 0.7383(2) 0.0367(4) Uani 1 2 d S . .
C51 C 0.31093(12) 0.2500 0.7093(2) 0.0261(4) Uani 1 2 d S . .
C52 C 0.23285(14) 0.2500 0.6710(3) 0.0438(6) Uani 1 2 d S . .
H52A H 0.2148 0.1568 0.6688 0.066 Uiso 0.50 1 calc PR . .
H52B H 0.2272 0.2911 0.5811 0.066 Uiso 0.50 1 calc PR . .
H52C H 0.2050 0.3021 0.7378 0.066 Uiso 0.50 1 calc PR . .
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
C12 Fe1 C12 91.41(9) . 6_565 ?
C12 Fe1 C11 98.53(6) . . ?
C12 Fe1 C11 98.53(6) 6_565 . ?
C12 Fe1 S1 156.72(5) . . ?
C12 Fe1 S1 86.17(4) 6_565 . ?
C11 Fe1 S1 104.73(4) . . ?
C12 Fe1 S1 86.17(4) . 6_565 ?
C12 Fe1 S1 156.72(5) 6_565 6_565 ?
C11 Fe1 S1 104.73(4) . 6_565 ?
S1 Fe1 S1 86.996(19) . 6_565 ?
C12 Fe1 Fe2 101.28(4) . . ?
C12 Fe1 Fe2 101.28(4) 6_565 . ?
C11 Fe1 Fe2 151.47(6) . . ?
S1 Fe1 Fe2 56.778(11) . . ?
S1 Fe1 Fe2 56.778(11) 6_565 . ?
C22 Fe2 C22 86.45(9) . 6_565 ?
C22 Fe2 N4 107.72(6) . . ?
C22 Fe2 N4 107.72(6) 6_565 . ?
C22 Fe2 S1 89.47(5) . 6_565 ?
C22 Fe2 S1 158.75(5) 6_565 6_565 ?
N4 Fe2 S1 93.39(4) . 6_565 ?
C22 Fe2 S1 158.75(5) . . ?
C22 Fe2 S1 89.47(5) 6_565 . ?
N4 Fe2 S1 93.39(4) . . ?
S1 Fe2 S1 86.819(19) 6_565 . ?
C22 Fe2 Fe1 104.32(5) . . ?
C22 Fe2 Fe1 104.32(5) 6_565 . ?
N4 Fe2 Fe1 135.47(5) . . ?
S1 Fe2 Fe1 56.637(11) 6_565 . ?
S1 Fe2 Fe1 56.637(11) . . ?
C1 S1 Fe1 113.42(5) . . ?
C1 S1 Fe2 107.85(5) . . ?
Fe1 S1 Fe2 66.585(13) . . ?
C2 C1 S1 117.13(10) . . ?
C2 C1 H1A 108.0 . . ?
S1 C1 H1A 108.0 . . ?
C2 C1 H1B 108.0 . . ?
S1 C1 H1B 108.0 . . ?
H1A C1 H1B 107.3 . . ?
C1 C2 C1 110.94(16) 6_565 . ?
C1 C2 C3 112.92(10) 6_565 . ?
C1 C2 C3 112.92(10) . . ?
C1 C2 C21 106.76(10) 6_565 . ?
C1 C2 C21 106.76(10) . . ?
C3 C2 C21 106.01(15) . . ?
C2 C21 H21A 109.5 . . ?
C2 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C2 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N4 C3 C2 119.92(16) . . ?
N4 C3 H3A 107.3 . . ?
C2 C3 H3A 107.3 . . ?
N4 C3 H3B 107.3 . . ?
C2 C3 H3B 107.3 . . ?
H3A C3 H3B 106.9 . . ?
C3 N4 Fe2 121.23(13) . . ?
C3 N4 H4A 107.0 . . ?
Fe2 N4 H4A 107.0 . . ?
C3 N4 H4B 107.0 . . ?
Fe2 N4 H4B 107.0 . . ?
H4A N4 H4B 106.8 . . ?
O11 C11 Fe1 179.19(18) . . ?
O12 C12 Fe1 177.96(13) . . ?
O22 C22 Fe2 173.22(13) . . ?
N5 C51 C52 179.5(2) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
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 C12 1.7922(14) . ?
Fe1 C12 1.7922(14) 6_565 ?
Fe1 C11 1.807(2) . ?
Fe1 S1 2.2660(4) . ?
Fe1 S1 2.2660(4) 6_565 ?
Fe1 Fe2 2.4897(4) . ?
Fe2 C22 1.7538(15) . ?
Fe2 C22 1.7538(15) 6_565 ?
Fe2 N4 2.0507(18) . ?
Fe2 S1 2.2697(4) 6_565 ?
Fe2 S1 2.2697(4) . ?
S1 C1 1.8213(14) . ?
C1 C2 1.5248(17) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C1 1.5248(17) 6_565 ?
C2 C3 1.540(3) . ?
C2 C21 1.542(3) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C3 N4 1.460(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N4 H4A 0.9000 . ?
N4 H4B 0.9000 . ?
C11 O11 1.137(3) . ?
C12 O12 1.1400(17) . ?
C22 O22 1.1570(18) . ?
N5 C51 1.136(3) . ?
C51 C52 1.452(3) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C12 Fe1 Fe2 C22 -1.90(6) . . . . ?
C12 Fe1 Fe2 C22 91.85(7) 6_565 . . . ?
C11 Fe1 Fe2 C22 -135.02(5) . . . . ?
S1 Fe1 Fe2 C22 169.61(5) . . . . ?
S1 Fe1 Fe2 C22 -79.66(5) 6_565 . . . ?
C12 Fe1 Fe2 C22 -91.85(7) . . . 6_565 ?
C12 Fe1 Fe2 C22 1.90(6) 6_565 . . 6_565 ?
C11 Fe1 Fe2 C22 135.02(5) . . . 6_565 ?
S1 Fe1 Fe2 C22 79.66(5) . . . 6_565 ?
S1 Fe1 Fe2 C22 -169.61(5) 6_565 . . 6_565 ?
C12 Fe1 Fe2 N4 133.13(4) . . . . ?
C12 Fe1 Fe2 N4 -133.13(4) 6_565 . . . ?
C11 Fe1 Fe2 N4 0.0 . . . . ?
S1 Fe1 Fe2 N4 -55.367(11) . . . . ?
S1 Fe1 Fe2 N4 55.367(11) 6_565 . . . ?
C12 Fe1 Fe2 S1 77.76(5) . . . 6_565 ?
C12 Fe1 Fe2 S1 171.51(5) 6_565 . . 6_565 ?
C11 Fe1 Fe2 S1 -55.367(11) . . . 6_565 ?
S1 Fe1 Fe2 S1 -110.73(2) . . . 6_565 ?
C12 Fe1 Fe2 S1 -171.51(5) . . . . ?
C12 Fe1 Fe2 S1 -77.76(5) 6_565 . . . ?
C11 Fe1 Fe2 S1 55.367(11) . . . . ?
S1 Fe1 Fe2 S1 110.73(2) 6_565 . . . ?
C12 Fe1 S1 C1 121.66(12) . . . . ?
C12 Fe1 S1 C1 -153.68(7) 6_565 . . . ?
C11 Fe1 S1 C1 -55.86(7) . . . . ?
S1 Fe1 S1 C1 48.59(5) 6_565 . . . ?
Fe2 Fe1 S1 C1 100.16(5) . . . . ?
C12 Fe1 S1 Fe2 21.50(11) . . . . ?
C12 Fe1 S1 Fe2 106.15(4) 6_565 . . . ?
C11 Fe1 S1 Fe2 -156.03(5) . . . . ?
S1 Fe1 S1 Fe2 -51.578(14) 6_565 . . . ?
C22 Fe2 S1 C1 -137.23(14) . . . . ?
C22 Fe2 S1 C1 144.01(7) 6_565 . . . ?
N4 Fe2 S1 C1 36.29(6) . . . . ?
S1 Fe2 S1 C1 -56.93(6) 6_565 . . . ?
Fe1 Fe2 S1 C1 -108.40(5) . . . . ?
C22 Fe2 S1 Fe1 -28.83(14) . . . . ?
C22 Fe2 S1 Fe1 -107.59(5) 6_565 . . . ?
N4 Fe2 S1 Fe1 144.68(4) . . . . ?
S1 Fe2 S1 Fe1 51.473(14) 6_565 . . . ?
Fe1 S1 C1 C2 -65.03(12) . . . . ?
Fe2 S1 C1 C2 6.58(13) . . . . ?
S1 C1 C2 C1 65.52(18) . . . 6_565 ?
S1 C1 C2 C3 -62.41(16) . . . . ?
S1 C1 C2 C21 -178.52(11) . . . . ?
C1 C2 C3 N4 -63.44(11) 6_565 . . . ?
C1 C2 C3 N4 63.44(11) . . . . ?
C21 C2 C3 N4 180.0 . . . . ?
C2 C3 N4 Fe2 0.0 . . . . ?
C22 Fe2 N4 C3 134.03(5) . . . . ?
C22 Fe2 N4 C3 -134.03(5) 6_565 . . . ?
S1 Fe2 N4 C3 43.505(10) 6_565 . . . ?
S1 Fe2 N4 C3 -43.505(10) . . . . ?
Fe1 Fe2 N4 C3 0.0 . . . . ?
C12 Fe1 C11 O11 46.36(5) . . . . ?
C12 Fe1 C11 O11 -46.37(4) 6_565 . . . ?
S1 Fe1 C11 O11 -134.625(17) . . . . ?
S1 Fe1 C11 O11 134.624(18) 6_565 . . . ?
Fe2 Fe1 C11 O11 180.000(4) . . . . ?
C12 Fe1 C12 O12 -100(4) 6_565 . . . ?
C11 Fe1 C12 O12 161(4) . . . . ?
S1 Fe1 C12 O12 -16(4) . . . . ?
S1 Fe1 C12 O12 57(4) 6_565 . . . ?
Fe2 Fe1 C12 O12 2(4) . . . . ?
C22 Fe2 C22 O22 51.4(12) 6_565 . . . ?
N4 Fe2 C22 O22 158.9(12) . . . . ?
S1 Fe2 C22 O22 -107.7(12) 6_565 . . . ?
S1 Fe2 C22 O22 -27.9(13) . . . . ?
Fe1 Fe2 C22 O22 -52.5(12) . . . . ?
