#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:55:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179269 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/89/4318961.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_4318961
loop_
_publ_author_name
'Joshua D. Lawrence'
'Thomas B. Rauchfuss'
'Scott R. Wilson'
_publ_contact_author
; 
Scott R. Wilson 
University of Illinois 
School of Chemical Sciences, Box 59-1 
505 South Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_contact_author_email       srwilson@uiuc.edu
_publ_contact_author_fax         '1  217 244 8068'
_publ_contact_author_phone       '1  217 244 1708'
_publ_section_title
;
 New Class of Diiron Dithiolates Related to the Fe-Only Hydrogenase Active
 Site: Synthesis and Characterization of [Fe2(SR)2(CNMe)7]2+
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6193
_journal_page_last               6195
_journal_paper_doi               10.1021/ic025919t
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C9 H14 F6 Fe N4 P S'
_chemical_formula_weight         411.12
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.243(4)
_cell_length_b                   20.985(5)
_cell_length_c                   9.747(2)
_cell_measurement_temperature    193(2)
_cell_volume                     3322.4(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0737
_diffrn_reflns_av_sigmaI/netI    0.0401
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            32660
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    1.187
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3131
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0647P)²+0.5853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                2204
_reflns_number_total             3131
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025919t-3_s1_3.cif
_cod_data_source_block           pnmafac
_cod_database_code               4318961
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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 0.98018(3) 0.31196(2) 0.20072(5) 0.03445(18) Uani 1 1 d . . .
C1 C 0.9467(2) 0.37665(17) 0.0851(4) 0.0383(8) Uani 1 1 d . . .
N1 N 0.92717(17) 0.41752(14) 0.0133(3) 0.0418(7) Uani 1 1 d . . .
C2 C 0.9049(2) 0.46984(18) -0.0747(4) 0.0540(10) Uani 1 1 d . . .
H2A H 0.8919 0.5073 -0.0187 0.081 Uiso 1 1 calc R . .
H2B H 0.8566 0.4581 -0.1294 0.081 Uiso 1 1 calc R . .
H2C H 0.9509 0.4798 -0.1360 0.081 Uiso 1 1 calc R . .
C3 C 1.0839(2) 0.34990(17) 0.2212(4) 0.0400(9) Uani 1 1 d . . .
N2 N 1.14733(19) 0.37225(14) 0.2391(3) 0.0479(8) Uani 1 1 d . . .
C4 C 1.2269(2) 0.3985(2) 0.2717(5) 0.0752(15) Uani 1 1 d . . .
H4A H 1.2217 0.4280 0.3491 0.113 Uiso 1 1 calc R . .
H4B H 1.2485 0.4214 0.1918 0.113 Uiso 1 1 calc R . .
H4C H 1.2647 0.3639 0.2962 0.113 Uiso 1 1 calc R . .
C5 C 0.9400(2) 0.35707(17) 0.3526(4) 0.0402(9) Uani 1 1 d . . .
N3 N 0.91888(18) 0.38612(16) 0.4460(3) 0.0541(9) Uani 1 1 d . . .
C6 C 0.8982(3) 0.4206(2) 0.5695(4) 0.0778(15) Uani 1 1 d . . .
H6A H 0.8633 0.3939 0.6280 0.117 Uiso 1 1 calc R . .
H6B H 0.8686 0.4597 0.5453 0.117 Uiso 1 1 calc R . .
H6C H 0.9488 0.4316 0.6189 0.117 Uiso 1 1 calc R . .
C7 C 1.0234(3) 0.2500 0.3506(6) 0.0437(13) Uani 1 2 d S . .
N4 N 1.0545(3) 0.2500 0.4585(5) 0.0458(11) Uani 1 2 d S . .
C8 C 1.0846(4) 0.2500 0.5942(6) 0.0595(16) Uani 1 2 d S . .
H8A H 1.0459 0.2728 0.6537 0.089 Uiso 0.50 1 calc PR . .
H8B H 1.1383 0.2713 0.5969 0.089 Uiso 0.50 1 calc PR . .
H8C H 1.0905 0.2060 0.6263 0.089 Uiso 0.50 1 calc PR . .
S1 S 1.02290(8) 0.2500 0.02621(13) 0.0421(3) Uani 1 2 d S . .
S2 S 0.86619(7) 0.2500 0.17443(13) 0.0385(3) Uani 1 2 d S . .
C9 C 0.9346(3) 0.2500 -0.0896(6) 0.0524(14) Uani 1 2 d S . .
H9A H 0.9371 0.2881 -0.1492 0.063 Uiso 0.50 1 calc PR . .
H9B H 0.9371 0.2119 -0.1492 0.063 Uiso 0.50 1 calc PR . .
C10 C 0.8526(3) 0.2500 -0.0109(5) 0.0534(15) Uani 1 2 d S . .
H10A H 0.8204 0.2119 -0.0376 0.064 Uiso 0.50 1 calc PR . .
H10B H 0.8204 0.2881 -0.0376 0.064 Uiso 0.50 1 calc PR . .
P1 P 0.84862(6) 0.57357(6) 0.29106(13) 0.0608(4) Uani 1 1 d . . .
F6 F 0.90509(19) 0.61784(13) 0.2019(3) 0.0952(9) Uani 1 1 d . . .
F5 F 0.79682(19) 0.55191(17) 0.1633(3) 0.1224(12) Uani 1 1 d . . .
F4 F 0.89800(15) 0.59349(13) 0.4238(3) 0.0850(8) Uani 1 1 d . . .
F3 F 0.90995(16) 0.51578(12) 0.2652(3) 0.0879(9) Uani 1 1 d . . .
F2 F 0.79378(17) 0.52768(13) 0.3872(4) 0.1106(11) Uani 1 1 d . . .
F1 F 0.78621(16) 0.63052(14) 0.3170(3) 0.1003(10) Uani 1 1 d . . .
C11 C 0.8112(4) 0.2500 -0.4214(6) 0.0702(19) Uani 1 2 d S . .
C12 C 0.7265(4) 0.2500 -0.4564(8) 0.110(3) Uani 1 2 d S . .
H12A H 0.7059 0.2061 -0.4573 0.165 Uiso 0.50 1 calc PR . .
H12B H 0.7193 0.2690 -0.5475 0.165 Uiso 0.50 1 calc PR . .
H12C H 0.6957 0.2749 -0.3886 0.165 Uiso 0.50 1 calc PR . .
N5 N 0.8772(4) 0.2500 -0.3952(6) 0.114(3) Uani 1 2 d S . .
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'
F F 0.0171 0.0103 '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 C3 91.01(14) . . ?
C1 Fe1 C5 90.47(16) . . ?
C3 Fe1 C5 90.82(15) . . ?
C1 Fe1 C7 171.40(15) . . ?
C3 Fe1 C7 83.51(16) . . ?
C5 Fe1 C7 83.00(17) . . ?
C1 Fe1 S1 93.12(11) . . ?
C3 Fe1 S1 92.79(11) . . ?
C5 Fe1 S1 174.86(12) . . ?
C7 Fe1 S1 93.77(12) . . ?
C1 Fe1 S2 96.41(11) . . ?
C3 Fe1 S2 170.26(11) . . ?
C5 Fe1 S2 95.40(11) . . ?
C7 Fe1 S2 89.80(12) . . ?
S1 Fe1 S2 80.54(4) . . ?
C1 Fe1 Fe1 137.34(11) . 7_565 ?
C3 Fe1 Fe1 115.13(10) . 7_565 ?
C5 Fe1 Fe1 120.33(11) . 7_565 ?
C7 Fe1 Fe1 51.26(10) . 7_565 ?
S1 Fe1 Fe1 54.71(2) . 7_565 ?
S2 Fe1 Fe1 55.18(2) . 7_565 ?
N1 C1 Fe1 178.8(3) . . ?
C1 N1 C2 178.2(4) . . ?
N2 C3 Fe1 177.3(3) . . ?
C3 N2 C4 175.8(4) . . ?
N3 C5 Fe1 176.8(3) . . ?
C5 N3 C6 175.2(4) . . ?
N4 C7 Fe1 141.26(10) . 7_565 ?
N4 C7 Fe1 141.26(10) . . ?
Fe1 C7 Fe1 77.5(2) 7_565 . ?
C7 N4 C8 174.6(5) . . ?
C9 S1 Fe1 103.01(15) . . ?
C9 S1 Fe1 103.01(15) . 7_565 ?
Fe1 S1 Fe1 70.58(5) . 7_565 ?
C10 S2 Fe1 102.16(15) . . ?
C10 S2 Fe1 102.16(15) . 7_565 ?
Fe1 S2 Fe1 69.65(4) . 7_565 ?
C10 C9 S1 111.8(4) . . ?
C9 C10 S2 113.0(4) . . ?
F6 P1 F5 92.6(2) . . ?
F6 P1 F4 90.01(16) . . ?
F5 P1 F4 177.4(2) . . ?
F6 P1 F1 90.91(17) . . ?
F5 P1 F1 90.13(17) . . ?
F4 P1 F1 89.67(15) . . ?
F6 P1 F3 89.85(16) . . ?
F5 P1 F3 89.37(17) . . ?
F4 P1 F3 90.80(15) . . ?
F1 P1 F3 179.10(16) . . ?
F6 P1 F2 177.56(19) . . ?
F5 P1 F2 89.5(2) . . ?
F4 P1 F2 87.84(17) . . ?
F1 P1 F2 90.23(17) . . ?
F3 P1 F2 89.02(16) . . ?
N5 C11 C12 179.5(8) . . ?
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 1.846(4) . ?
Fe1 C3 1.875(4) . ?
Fe1 C5 1.875(4) . ?
Fe1 C7 2.078(5) . ?
Fe1 S1 2.2507(12) . ?
Fe1 S2 2.2770(11) . ?
Fe1 Fe1 2.6005(12) 7_565 ?
C1 N1 1.152(4) . ?
N1 C2 1.440(4) . ?
C3 N2 1.145(4) . ?
N2 C4 1.441(5) . ?
C5 N3 1.148(4) . ?
N3 C6 1.443(5) . ?
C7 N4 1.167(6) . ?
C7 Fe1 2.078(5) 7_565 ?
N4 C8 1.410(7) . ?
S1 C9 1.826(5) . ?
S1 Fe1 2.2507(12) 7_565 ?
S2 C10 1.820(5) . ?
S2 Fe1 2.2770(11) 7_565 ?
C9 C10 1.537(7) . ?
P1 F6 1.568(3) . ?
P1 F5 1.570(3) . ?
P1 F4 1.579(3) . ?
P1 F1 1.587(3) . ?
P1 F3 1.590(3) . ?
P1 F2 1.612(3) . ?
C11 N5 1.101(7) . ?
C11 C12 1.418(8) . ?
