#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:48:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179765 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/61/7006142.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_7006142
loop_
_publ_author_name
'Orain, Pierre-Yves'
'Capon, Jean-François'
'Kervarec, Nelly'
'Gloaguen, Frédéric'
'Pétillon, François'
'Pichon, Roger'
'Schollhammer, Philippe'
'Talarmin, Jean'
_publ_section_title
;
 Use of 1,10-phenanthroline in diiron dithiolate derivatives related to
 the [Fe-Fe] hydrogenase active site.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3754
_journal_page_last               3756
_journal_paper_doi               10.1039/b709287c
_journal_year                    2007
_chemical_formula_sum            'C19 H14 Fe2 N2 O4 S2'
_chemical_formula_weight         510.14
_chemical_name_common            pdt-phen
_chemical_name_systematic
;
pdt-phen
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2007-05-02T16:07:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 102.196(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8778(10)
_cell_length_b                   7.5150(6)
_cell_length_c                   18.8451(13)
_cell_measurement_reflns_used    9548
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      32.9753
_cell_measurement_theta_min      2.9157
_cell_volume                     1921.0(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
;
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'Sapphire 2 (CCD)'
_diffrn_measured_fraction_theta_full 0.93
_diffrn_measured_fraction_theta_max 0.93
_diffrn_measurement_device_type  'X-CALIBUR-2 CCD 4-circle diffractometer'
_diffrn_measurement_method
;
omega-scans with kappa -79 deg (chi -58.3 deg), phi 0, 90, 180, 270 deg
;
_diffrn_orient_matrix_UB_11      0.0283258937
_diffrn_orient_matrix_UB_12      -0.0570070313
_diffrn_orient_matrix_UB_13      0.0263518364
_diffrn_orient_matrix_UB_21      -0.032518922
_diffrn_orient_matrix_UB_22      0.0167362882
_diffrn_orient_matrix_UB_23      0.023628804
_diffrn_orient_matrix_UB_31      -0.0295374239
_diffrn_orient_matrix_UB_32      -0.0731369049
_diffrn_orient_matrix_UB_33      -0.0151546347
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            21452
_diffrn_reflns_theta_full        33.08
_diffrn_reflns_theta_max         33.08
_diffrn_reflns_theta_min         2.92
_diffrn_standards_interval_count 50
_exptl_absorpt_coefficient_mu    1.757
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.62103
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0306
_refine_ls_shift/su_max          0.092
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0370P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0771
_reflns_number_gt                4277
_reflns_number_total             6785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b709287c.txt
_cod_data_source_block           pdtphen
_cod_original_cell_volume        1921.0(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7006142
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
C1 C 0.22396(13) 0.2796(2) 0.19903(10) 0.0221(4) Uani 1 1 d . . .
C2 C 0.08570(14) 0.9369(3) 0.09651(10) 0.0262(4) Uani 1 1 d . . .
C3 C 0.17637(14) 0.7320(3) 0.00564(11) 0.0266(4) Uani 1 1 d . . .
C4 C 0.28774(14) 0.8827(2) 0.10974(10) 0.0239(4) Uani 1 1 d . . .
C5 C 0.00479(15) 0.5134(3) 0.15668(12) 0.0301(4) Uani 1 1 d . . .
C6 C 0.02566(16) 0.6497(3) 0.21633(12) 0.0332(5) Uani 1 1 d . . .
C7 C 0.12849(16) 0.6407(3) 0.26266(11) 0.0346(5) Uani 1 1 d . . .
C8 C 0.19078(16) 0.2525(3) -0.00094(11) 0.0280(4) Uani 1 1 d . . .
C9 C 0.21573(19) 0.1679(3) -0.06071(12) 0.0383(5) Uani 1 1 d . . .
C10 C 0.3123(2) 0.1587(3) -0.06628(12) 0.0420(6) Uani 1 1 d . . .
C11 C 0.38560(17) 0.2346(3) -0.01180(12) 0.0344(5) Uani 1 1 d . . .
C12 C 0.4892(2) 0.2302(3) -0.01001(16) 0.0458(7) Uani 1 1 d . . .
C13 C 0.55520(19) 0.3019(3) 0.04458(16) 0.0456(7) Uani 1 1 d . . .
C14 C 0.52535(15) 0.3905(3) 0.10403(13) 0.0349(5) Uani 1 1 d . . .
C15 C 0.58914(16) 0.4728(3) 0.16212(14) 0.0414(6) Uani 1 1 d . . .
C16 C 0.55088(16) 0.5542(3) 0.21501(13) 0.0405(6) Uani 1 1 d . . .
C17 C 0.44955(15) 0.5507(3) 0.21185(12) 0.0322(5) Uani 1 1 d . . .
C18 C 0.42352(14) 0.3960(3) 0.10363(11) 0.0265(4) Uani 1 1 d . . .
C19 C 0.35414(14) 0.3185(2) 0.04585(11) 0.0260(4) Uani 1 1 d . . .
N1 N 0.25771(11) 0.3287(2) 0.05201(8) 0.0228(3) Uani 1 1 d . . .
N2 N 0.38557(11) 0.4734(2) 0.15723(9) 0.0244(3) Uani 1 1 d . . .
O1 O 0.20778(11) 0.1774(2) 0.24058(8) 0.0362(3) Uani 1 1 d . . .
O2 O 0.02793(11) 1.0468(2) 0.09247(9) 0.0417(4) Uani 1 1 d . . .
O3 O 0.18146(12) 0.7097(2) -0.05401(8) 0.0411(4) Uani 1 1 d . . .
O4 O 0.36250(10) 0.95318(19) 0.11707(8) 0.0348(3) Uani 1 1 d . . .
S1 S 0.08419(3) 0.51264(6) 0.09132(2) 0.02083(10) Uani 1 1 d . . .
S2 S 0.22931(3) 0.67580(6) 0.21553(2) 0.02344(11) Uani 1 1 d . . .
Fe1 Fe 0.239295(18) 0.45426(3) 0.140946(13) 0.01847(7) Uani 1 1 d . . .
Fe2 Fe 0.175626(19) 0.76261(3) 0.098399(14) 0.02001(7) Uani 1 1 d . . .
H1 H 0.4271(18) 0.603(3) 0.2482(12) 0.048(7) Uiso 1 1 d . . .
H2 H 0.5922(17) 0.616(3) 0.2567(12) 0.040(6) Uiso 1 1 d . . .
H3 H 0.6583(19) 0.463(3) 0.1629(13) 0.054(7) Uiso 1 1 d . . .
H4 H 0.6209(18) 0.297(3) 0.0451(12) 0.040(6) Uiso 1 1 d . . .
H5 H 0.5053(18) 0.181(3) -0.0487(14) 0.052(8) Uiso 1 1 d . . .
H6 H 0.3273(16) 0.101(3) -0.1046(11) 0.037(6) Uiso 1 1 d . . .
H7 H 0.1645(14) 0.113(3) -0.0954(10) 0.018(5) Uiso 1 1 d . . .
H8 H 0.1172(16) 0.257(2) 0.0036(11) 0.027(5) Uiso 1 1 d . . .
H9 H 0.1379(19) 0.510(4) 0.2874(14) 0.062(8) Uiso 1 1 d . . .
H10 H 0.1355(17) 0.735(3) 0.2980(12) 0.034(6) Uiso 1 1 d . . .
H11 H -0.0236(16) 0.628(3) 0.2469(12) 0.042(6) Uiso 1 1 d . . .
H12 H 0.0130(14) 0.766(3) 0.1934(11) 0.022(5) Uiso 1 1 d . . .
H13 H 0.0122(14) 0.393(3) 0.1755(10) 0.026(5) Uiso 1 1 d . . .
H14 H -0.0636(19) 0.525(3) 0.1259(13) 0.049(7) Uiso 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 0 '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 0.006 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 0 0 0.04
-1 0 0 0.06
-1 0 -2 0.1
0 -1 1 0.365
0 1 0 0.32
-1 0 2 0.145
-1 -1 -1 0.305
1 0 -2 0.145
1 0 2 0.105
2 3 -4 0.275
0 2 -25 0.155
-2 3 4 0.315
1 -1 1 0.31
1 -1 -1 0.335
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
O1 C1 Fe1 172.56(17) . . ?
O2 C2 Fe2 177.37(17) . . ?
O3 C3 Fe2 176.78(19) . . ?
O4 C4 Fe2 176.89(17) . . ?
C6 C5 S1 117.41(15) . . ?
C5 C6 C7 114.31(18) . . ?
C6 C7 S2 116.09(14) . . ?
N1 C8 C9 122.9(2) . . ?
C10 C9 C8 119.8(2) . . ?
C9 C10 C11 119.6(2) . . ?
C19 C11 C10 116.9(2) . . ?
C19 C11 C12 117.9(2) . . ?
C10 C11 C12 125.2(2) . . ?
C13 C12 C11 122.0(2) . . ?
C12 C13 C14 121.5(2) . . ?
C15 C14 C18 117.3(2) . . ?
C15 C14 C13 125.2(2) . . ?
C18 C14 C13 117.5(2) . . ?
C16 C15 C14 119.3(2) . . ?
C15 C16 C17 120.2(2) . . ?
N2 C17 C16 122.6(2) . . ?
N2 C18 C14 123.44(19) . . ?
N2 C18 C19 115.99(16) . . ?
C14 C18 C19 120.57(19) . . ?
N1 C19 C11 124.08(19) . . ?
N1 C19 C18 115.41(17) . . ?
C11 C19 C18 120.50(18) . . ?
C8 N1 C19 116.69(17) . . ?
C8 N1 Fe1 129.71(13) . . ?
C19 N1 Fe1 113.60(13) . . ?
C17 N2 C18 117.15(17) . . ?
C17 N2 Fe1 129.56(14) . . ?
C18 N2 Fe1 113.29(12) . . ?
C5 S1 Fe1 113.01(7) . . ?
C5 S1 Fe2 111.79(7) . . ?
Fe1 S1 Fe2 69.727(16) . . ?
C7 S2 Fe1 111.04(8) . . ?
C7 S2 Fe2 112.71(7) . . ?
Fe1 S2 Fe2 69.438(16) . . ?
C1 Fe1 N1 103.04(7) . . ?
C1 Fe1 N2 102.25(7) . . ?
N1 Fe1 N2 81.71(7) . . ?
C1 Fe1 S2 97.78(6) . . ?
N1 Fe1 S2 159.13(5) . . ?
N2 Fe1 S2 92.67(5) . . ?
C1 Fe1 S1 100.25(6) . . ?
N1 Fe1 S1 91.42(5) . . ?
N2 Fe1 S1 157.42(5) . . ?
S2 Fe1 S1 86.15(2) . . ?
C1 Fe1 Fe2 143.00(6) . . ?
N1 Fe1 Fe2 105.33(4) . . ?
N2 Fe1 Fe2 104.89(5) . . ?
S2 Fe1 Fe2 56.560(15) . . ?
S1 Fe1 Fe2 56.109(14) . . ?
C3 Fe2 C4 89.84(9) . . ?
C3 Fe2 C2 102.94(9) . . ?
C4 Fe2 C2 102.64(9) . . ?
C3 Fe2 S1 87.34(6) . . ?
C4 Fe2 S1 154.17(6) . . ?
C2 Fe2 S1 103.02(6) . . ?
C3 Fe2 S2 148.82(7) . . ?
C4 Fe2 S2 85.96(6) . . ?
C2 Fe2 S2 108.13(6) . . ?
S1 Fe2 S2 83.294(19) . . ?
C3 Fe2 Fe1 96.82(6) . . ?
C4 Fe2 Fe1 100.83(6) . . ?
C2 Fe2 Fe1 149.17(6) . . ?
S1 Fe2 Fe1 54.163(14) . . ?
S2 Fe2 Fe1 54.002(14) . . ?
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
C1 O1 1.153(2) . ?
C1 Fe1 1.7506(19) . ?
C2 O2 1.143(2) . ?
C2 Fe2 1.804(2) . ?
C3 O3 1.153(2) . ?
C3 Fe2 1.765(2) . ?
C4 O4 1.147(2) . ?
C4 Fe2 1.7721(19) . ?
C5 C6 1.503(3) . ?
C5 S1 1.818(2) . ?
C6 C7 1.509(3) . ?
C7 S2 1.828(2) . ?
C8 N1 1.339(2) . ?
C8 C9 1.399(3) . ?
C9 C10 1.368(3) . ?
C10 C11 1.404(3) . ?
C11 C19 1.403(3) . ?
C11 C12 1.432(3) . ?
C12 C13 1.337(4) . ?
C13 C14 1.437(3) . ?
C14 C15 1.398(3) . ?
C14 C18 1.412(3) . ?
C15 C16 1.369(3) . ?
C16 C17 1.395(3) . ?
C17 N2 1.341(3) . ?
C18 N2 1.364(2) . ?
C18 C19 1.418(3) . ?
C19 N1 1.370(2) . ?
N1 Fe1 1.9864(15) . ?
N2 Fe1 1.9931(15) . ?
S1 Fe1 2.2023(5) . ?
S1 Fe2 2.2551(5) . ?
S2 Fe1 2.2020(5) . ?
S2 Fe2 2.2712(5) . ?
Fe1 Fe2 2.5483(4) . ?
