#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:25:19 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180261 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/47/7114796.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_7114796
loop_
_publ_author_name
'Lawrence, Joshua D.'
'Li, Hongxiang'
'Rauchfuss, Thomas B.'
_publ_section_title
;
 Beyond Fe-only hydrogenases: N-functionalized 2-aza-1,3-dithiolates
 Fe2[(SCH2)2NR](CO)x (x = 5, 6)
;
_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1482
_journal_paper_doi               10.1039/b104195a
_journal_year                    2001
_chemical_formula_sum            'C10 H9 Fe2 N O5 S2'
_chemical_formula_weight         399.00
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 91.324(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7450(13)
_cell_length_b                   9.4727(11)
_cell_length_c                   14.1176(16)
_cell_measurement_temperature    193(2)
_cell_volume                     1436.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      193(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0763
_diffrn_reflns_av_sigmaI/netI    0.0888
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11960
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    2.324
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_correction_T_min  0.7248
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platy
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.904
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.914
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0201P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0639
_reflns_number_gt                1918
_reflns_number_total             3222
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b104195a.txt
_cod_data_source_block           4a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114796
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.91275(4) 0.22726(5) 0.61091(3) 0.03227(14) Uani 1 1 d . A .
Fe2 Fe 1.06853(4) 0.31567(5) 0.73250(3) 0.03405(14) Uani 1 1 d . . .
S1 S 0.86014(7) 0.32281(9) 0.75014(6) 0.0352(2) Uani 1 1 d . A .
S2 S 1.04079(7) 0.08527(9) 0.69690(6) 0.0386(2) Uani 1 1 d . A .
O2 O 1.0708(2) 0.1673(3) 0.44909(18) 0.0635(8) Uani 1 1 d . A .
N1 N 0.9186(2) 0.0951(3) 0.8693(2) 0.0436(8) Uani 1 1 d . . .
C7 C 0.9593(3) 0.0020(3) 0.7972(3) 0.0475(10) Uani 1 1 d . A .
H7A H 0.8859 -0.0494 0.7713 0.057 Uiso 1 1 calc R . .
H7B H 1.0158 -0.0687 0.8267 0.057 Uiso 1 1 calc R . .
O1 O 0.8357(2) 0.4891(3) 0.51579(17) 0.0546(7) Uani 1 1 d . A .
O4 O 1.2945(2) 0.2936(3) 0.62268(18) 0.0661(8) Uani 1 1 d . . .
C2 C 1.0078(3) 0.1881(3) 0.5118(3) 0.0419(9) Uani 1 1 d . . .
C6 C 0.8196(3) 0.1873(3) 0.8387(2) 0.0450(9) Uani 1 1 d . A .
H6A H 0.7872 0.2359 0.8951 0.054 Uiso 1 1 calc R . .
H6B H 0.7512 0.1287 0.8117 0.054 Uiso 1 1 calc R . .
C1 C 0.8633(3) 0.3880(4) 0.5538(2) 0.0375(9) Uani 1 1 d . . .
C4 C 1.2075(3) 0.3034(4) 0.6674(2) 0.0441(9) Uani 1 1 d . A .
C5 C 1.0606(3) 0.5001(4) 0.7165(3) 0.0574(11) Uani 1 1 d . A .
O5 O 1.0526(3) 0.6201(3) 0.7032(2) 0.0920(11) Uani 1 1 d . . .
O3 O 0.6935(3) 0.0491(3) 0.57374(18) 0.0767(9) Uani 1 1 d . A .
C3 C 0.7794(3) 0.1175(4) 0.5866(2) 0.0461(10) Uani 1 1 d . . .
C8 C 1.005(2) 0.1770(19) 0.930(2) 0.037(4) Uani 0.485(12) 1 d PD A 1
H8A H 1.0681 0.1112 0.9572 0.045 Uiso 0.485(12) 1 calc PR A 1
H8B H 0.9572 0.2144 0.9842 0.045 Uiso 0.485(12) 1 calc PR A 1
C9 C 1.0708(8) 0.2961(15) 0.8867(7) 0.049(4) Uani 0.485(12) 1 d PD A 1
H9 H 1.0484 0.3876 0.9173 0.059 Uiso 0.485(12) 1 calc PR A 1
C10 C 1.1927(8) 0.2997(16) 0.8535(6) 0.048(3) Uani 0.485(12) 1 d PD A 1
H10A H 1.2410 0.2110 0.8596 0.057 Uiso 0.485(12) 1 calc PR A 1
H10B H 1.2420 0.3850 0.8695 0.057 Uiso 0.485(12) 1 calc PR A 1
C8A C 1.0326(19) 0.1542(19) 0.9168(19) 0.039(4) Uani 0.515(12) 1 d PD A 2
H8A1 H 1.0033 0.2101 0.9712 0.047 Uiso 0.515(12) 1 calc PR A 2
H8A2 H 1.0785 0.0726 0.9440 0.047 Uiso 0.515(12) 1 calc PR A 2
C9A C 1.1264(12) 0.2428(10) 0.8695(7) 0.050(3) Uani 0.515(12) 1 d PD A 2
H9A H 1.2093 0.1949 0.8680 0.060 Uiso 0.515(12) 1 calc PR A 2
C10A C 1.1380(13) 0.3880(10) 0.8652(6) 0.057(3) Uani 0.515(12) 1 d PD A 2
H10C H 1.2239 0.4259 0.8666 0.069 Uiso 0.515(12) 1 calc PR A 2
H10D H 1.0798 0.4434 0.9038 0.069 Uiso 0.515(12) 1 calc PR A 2
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
C2 Fe1 C3 101.40(15)
C2 Fe1 C1 89.60(14)
C3 Fe1 C1 100.28(14)
C2 Fe1 S1 157.89(11)
C3 Fe1 S1 100.62(11)
C1 Fe1 S1 88.48(10)
C2 Fe1 S2 86.86(11)
C3 Fe1 S2 103.36(11)
C1 Fe1 S2 156.33(10)
S1 Fe1 S2 86.11(3)
C2 Fe1 Fe2 102.71(11)
C3 Fe1 Fe2 147.00(10)
C1 Fe1 Fe2 102.09(10)
S1 Fe1 Fe2 56.33(3)
S2 Fe1 Fe2 56.18(3)
C5 Fe2 C4 92.17(16)
C5 Fe2 C10A 78.9(3)
C4 Fe2 C10A 101.3(4)
C5 Fe2 C9A 116.7(3)
C4 Fe2 C9A 102.5(4)
C10A Fe2 C9A 38.0(3)
C5 Fe2 C10 101.5(4)
C4 Fe2 C10 83.9(3)
C10A Fe2 C10 28.1(3)
C9A Fe2 C10 25.0(3)
C5 Fe2 C9 102.2(4)
C4 Fe2 C9 121.3(3)
C10A Fe2 C9 31.7(3)
C9A Fe2 C9 21.9(3)
C10 Fe2 C9 37.7(3)
C5 Fe2 S2 157.44(13)
C4 Fe2 S2 85.96(11)
C10A Fe2 S2 123.5(2)
C9A Fe2 S2 85.6(3)
C10 Fe2 S2 100.7(4)
C9 Fe2 S2 97.9(4)
C5 Fe2 S1 86.51(12)
C4 Fe2 S1 155.03(11)
C10A Fe2 S1 102.9(4)
C9A Fe2 S1 100.3(4)
C10 Fe2 S1 120.9(2)
C9 Fe2 S1 83.2(2)
S2 Fe2 S1 85.84(3)
C5 Fe2 Fe1 102.31(12)
C4 Fe2 Fe1 100.33(11)
C10A Fe2 Fe1 158.3(4)
C9A Fe2 Fe1 133.4(3)
C10 Fe2 Fe1 155.7(4)
C9 Fe2 Fe1 130.1(2)
S2 Fe2 Fe1 56.18(3)
S1 Fe2 Fe1 55.89(3)
C6 S1 Fe1 112.29(12)
C6 S1 Fe2 107.65(10)
Fe1 S1 Fe2 67.77(3)
C7 S2 Fe2 107.64(12)
C7 S2 Fe1 111.76(11)
Fe2 S2 Fe1 67.63(3)
C7 N1 C6 113.6(3)
C7 N1 C8 123.1(7)
C6 N1 C8 107.9(8)
C7 N1 C8A 107.0(7)
C6 N1 C8A 120.1(8)
C8 N1 C8A 16.2(11)
N1 C7 S2 116.1(2)
O2 C2 Fe1 177.6(3)
N1 C6 S1 116.1(2)
O1 C1 Fe1 177.6(3)
O4 C4 Fe2 177.5(3)
O5 C5 Fe2 177.5(4)
O3 C3 Fe1 178.0(4)
N1 C8 C9 117.3(19)
C10 C9 C8 128.3(15)
C10 C9 Fe2 69.7(5)
C8 C9 Fe2 119.2(13)
C9 C10 Fe2 72.5(5)
C9A C8A N1 124.7(19)
C10A C9A C8A 130.2(16)
C10A C9A Fe2 70.3(4)
C8A C9A Fe2 113.9(13)
C9A C10A Fe2 71.7(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 C2 1.790(4)
Fe1 C3 1.796(4)
Fe1 C1 1.797(4)
Fe1 S1 2.2480(9)
Fe1 S2 2.2579(10)
Fe1 Fe2 2.5132(6)
Fe2 C5 1.764(4)
Fe2 C4 1.775(4)
Fe2 C10A 2.115(7)
Fe2 C9A 2.133(9)
Fe2 C10 2.149(8)
Fe2 C9 2.185(10)
Fe2 S2 2.2578(10)
Fe2 S1 2.2596(9)
S1 C6 1.851(3)
S2 C7 1.858(3)
O2 C2 1.144(4)
N1 C7 1.423(4)
N1 C6 1.436(4)
N1 C8 1.47(3)
N1 C8A 1.49(3)
O1 C1 1.135(3)
O4 C4 1.145(4)
C5 O5 1.154(4)
O3 C3 1.140(3)
C8 C9 1.476(12)
C9 C10 1.401(11)
C8A C9A 1.482(11)
C9A C10A 1.383(11)
