#------------------------------------------------------------------------------
#$Date: 2019-12-19 13:00:35 +0200 (Thu, 19 Dec 2019) $
#$Revision: 245390 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/66/1556672.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_1556672
loop_
_publ_author_name
'Tard, C.'
'Borg, S.J.'
'Fairhurst, S.A.'
'Pickett, C.J.'
'Best, S.P.'
_publ_section_title
;
 Electronic Communication between Dithiolato-Bridged Diiron Carbonyl and
 S-Bridged Redox-Active Centres
;
_journal_name_full               Inorganics
_journal_page_first              37
_journal_paper_doi               10.3390/inorganics7030037
_journal_volume                  7
_journal_year                    2019
_chemical_formula_moiety         'C16 H15 Fe2 N O5 S3'
_chemical_formula_structural     MeC(CH2S)3,-Fe(CO)3,-Fe(CO)2,-C6H4NH2
_chemical_formula_sum            'C16 H15 Fe2 N O5 S3'
_chemical_formula_weight         509.2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0(0)
_cell_angle_beta                 94.30(2)
_cell_angle_gamma                90.0(0)
_cell_formula_units_Z            4
_cell_length_a                   8.797(3)
_cell_length_b                   12.528(4)
_cell_length_c                   18.181(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11
_cell_measurement_theta_min      10
_cell_volume                     1998.1(10)
_computing_cell_refinement       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_collection       'CAD4/EXPRESS (Enraf-Nonius, 1992)'
_computing_data_reduction        'CAD4 (Hursthouse, 1976)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976 and Farrugia, 2012)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997) and WINGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Enraf-Nonius CAD4 diffractometer'
_diffrn_measurement_method       'scintillation counter; ω/θ 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  0.0138
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            5779
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.5
_diffrn_standards_decay_%        1.11
_diffrn_standards_interval_time  167
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.792
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.092
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'EMPABS, (Sheldrick et al, 1977)'
_exptl_crystal_colour            'dark orange-brown'
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         3517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0291P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0660
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2632
_reflns_number_total             3517
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            Inorganics-2019-7-37.cif
_cod_data_source_block           cedric10
_cod_original_cell_volume        1998.0(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1556672
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, 1/2+y, 1/2-z'
'-x, -y, -z'
'x, -1/2-y, -1/2+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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.07247(5) 0.30743(3) 0.44381(2) 0.04954(13) Uani 1 1 d . . . . .
Fe2 Fe 0.24431(5) 0.15985(3) 0.40597(2) 0.04273(12) Uani 1 1 d . . . . .
S1 S 0.12116(8) 0.27361(5) 0.32590(4) 0.0474(2) Uani 1 1 d . . . . .
S2 S 0.01546(8) 0.13210(5) 0.45020(4) 0.0483(2) Uani 1 1 d . . . . .
S3 S 0.24469(7) 0.04298(5) 0.31236(4) 0.0480(2) Uani 1 1 d . . . . .
C1 C 0.0818(4) 0.3064(3) 0.5415(2) 0.0799(10) Uani 1 1 d . . . . .
O1 O 0.0888(4) 0.3035(3) 0.6041(2) 0.1427(15) Uani 1 1 d . . . . .
C2 C -0.1011(4) 0.3809(3) 0.4235(2) 0.0728(9) Uani 1 1 d . . . . .
O2 O -0.2078(3) 0.4292(2) 0.4069(2) 0.1114(10) Uani 1 1 d . . . . .
C3 C 0.2125(4) 0.4098(3) 0.4451(2) 0.0702(9) Uani 1 1 d . . . . .
O3 O 0.3057(3) 0.4735(2) 0.4467(2) 0.1088(10) Uani 1 1 d . . . . .
C4 C 0.3247(3) 0.0928(2) 0.4858(2) 0.0561(7) Uani 1 1 d . . . . .
O4 O 0.3721(3) 0.0498(2) 0.5378(1) 0.0842(7) Uani 1 1 d . . . . .
C5 C 0.4215(4) 0.2220(2) 0.3950(2) 0.0610(8) Uani 1 1 d . . . . .
O5 O 0.5368(3) 0.2628(2) 0.3907(2) 0.1000(8) Uani 1 1 d . . . . .
C11 C -0.0370(4) 0.2049(2) 0.2754(2) 0.0553(7) Uani 1 1 d . . . . .
C12 C -0.1238(3) 0.0914(3) 0.3767(2) 0.0593(8) Uani 1 1 d . . . . .
C13 C 0.0448(3) 0.0096(3) 0.2854(2) 0.0640(9) Uani 1 1 d . . . . .
C14 C -0.0779(3) 0.0930(2) 0.2984(2) 0.0500(7) Uani 1 1 d . . . . .
C15 C -0.2197(4) 0.0576(3) 0.2493(3) 0.0766(11) Uani 1 1 d . . . . .
C31 C 0.3241(3) -0.0847(2) 0.3333(1) 0.0447(6) Uani 1 1 d . . . . .
C32 C 0.2851(3) -0.1466(2) 0.3919(2) 0.0546(7) Uani 1 1 d . . . . .
C33 C 0.3570(4) -0.2427(2) 0.4066(2) 0.0590(8) Uani 1 1 d . . . . .
C34 C 0.4719(3) -0.2785(2) 0.3643(2) 0.0548(7) Uani 1 1 d . . . . .
C35 C 0.5097(3) -0.2161(2) 0.3061(2) 0.0592(8) Uani 1 1 d . . . . .
C36 C 0.4363(3) -0.1211(2) 0.2904(2) 0.0509(7) Uani 1 1 d . . . . .
N31 N 0.5465(4) -0.3744(3) 0.3795(3) 0.0842(10) Uani 1 1 d . . . . .
H11A H -0.1190(30) 0.2480(20) 0.2766(15) 0.054(8) Uiso 1 1 d . . . . .
H11B H -0.0050(30) 0.2060(20) 0.2270(18) 0.068(9) Uiso 1 1 d . . . . .
H12A H -0.1480(30) 0.0210(20) 0.3862(16) 0.065(9) Uiso 1 1 d . . . . .
H12B H -0.2060(30) 0.1360(20) 0.3783(15) 0.064(9) Uiso 1 1 d . . . . .
H13A H 0.0480(40) -0.0070(20) 0.2350(20) 0.086(11) Uiso 1 1 d . . . . .
H13B H 0.0240(40) -0.0510(30) 0.3131(18) 0.090(12) Uiso 1 1 d . . . . .
H15A H -0.1970(40) 0.0660(30) 0.2000(20) 0.101(15) Uiso 1 1 d . . . . .
H15B H -0.3020(40) 0.1000(20) 0.2589(15) 0.064(9) Uiso 1 1 d . . . . .
H15C H -0.2410(40) -0.0150(30) 0.2584(17) 0.077(11) Uiso 1 1 d . . . . .
H32 H 0.2170(30) -0.1250(20) 0.4216(14) 0.048(8) Uiso 1 1 d . . . . .
H33 H 0.3350(40) -0.2810(20) 0.4439(18) 0.075(10) Uiso 1 1 d . . . . .
H35 H 0.5870(40) -0.2410(20) 0.2792(17) 0.076(10) Uiso 1 1 d . . . . .
H36 H 0.4520(30) -0.0788(19) 0.2513(13) 0.041(7) Uiso 1 1 d . . . . .
H31A H 0.6150(50) -0.3930(30) 0.3550(20) 0.105(17) Uiso 1 1 d . . . . .
H31B H 0.5050(40) -0.4060(30) 0.4150(20) 0.096(15) 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 0.0000 0.0000 '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'
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'
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
Fe2 S1 Fe1 67.78(3) . .
Fe2 S2 Fe1 67.86(2) . .
S1 Fe1 S2 85.70(3) . .
C1 Fe1 S1 162.28(13) . .
C2 Fe1 S1 96.86(11) . .
C3 Fe1 S1 88.10(10) . .
C1 Fe1 S2 86.27(11) . .
C2 Fe1 S2 108.68(11) . .
C3 Fe1 S2 149.06(12) . .
C1 Fe1 C2 100.67(17) . .
C1 Fe1 C3 90.72(14) . .
C3 Fe1 C2 102.15(16) . .
C5 Fe2 S3 98.66(10) . .
S2 Fe2 S1 85.93(3) . .
S3 Fe2 S1 87.18(3) . .
C4 Fe2 S3 106.71(10) . .
C5 Fe2 C4 90.01(13) . .
C4 Fe2 S1 165.52(9) . .
C5 Fe2 S1 91.93(10) . .
S3 Fe2 S2 102.85(3) . .
C4 Fe2 S2 86.96(9) . .
C5 Fe2 S2 158.24(10) . .
C11 S1 Fe1 111.9812) . .
C11 S1 Fe2 109.73(10) . .
C12 S2 Fe1 112.02(12) . .
C12 S2 Fe2 110.63(11) . .
C13 S3 Fe2 107.15(11) . .
C31 S3 Fe2 116.60(9) . .
C31 S3 C13 101.86(14) . .
O1 C1 Fe1 178.6(4) . .
O2 C2 Fe1 176.1(4) . .
O3 C3 Fe1 178.0(3) . .
O4 C4 Fe2 177.9(3) . .
O5 C5 Fe2 177.5(3) . .
C14 C11 S1 119.1(2) . .
C14 C12 S2 118.5(2) . .
C14 C13 S3 118.3(2) . .
C12 C14 C11 110.9(2) . .
C11 C14 C13 113.8(3) . .
C11 C14 C15 107.8(3) . .
C12 C14 C13 112.2(3) . .
C12 C14 C15 106.3(3) . .
C13 C14 C15 105.3(2) . .
C32 C31 S3 123.7(2) . .
C36 C31 S3 117.5(2) . .
C36 C31 C32 118.7(3) . .
C33 C32 C31 120.2(3) . .
C35 C34 N31 120.5(3) . .
C35 C34 C33 118.0(3) . .
N31 C34 C33 121.5(3) . .
C36 C35 C34 121.0(3) . .
C35 C36 C31 120.9(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 Fe2 2.5165(8) .
Fe1 S1 2.2574(9) .
Fe1 S2 2.2580(10) .
Fe1 C1 1.771(4) .
Fe1 C2 1.798(4) .
Fe2 S1 2.2555(9) .
Fe2 S2 2.2501(10) .
Fe2 S3 2.2452(8) .
Fe2 C4 1.778(3) .
Fe2 C5 1.767(3) .
S1 C11 1.824(3) .
S2 C12 1.817(3) .
S3 C13 1.838(3) .
S3 C31 1.775(3) .
C1 O1 1.136(4) .
C2 O2 1.138(4) .
C3 O3 1.142(4) .
C4 O4 1.139(3) .
C5 O5 1.143(3) .
C11 C14 1.514(4) .
C12 C14 1.509(4) .
C13 C14 1.533(4) .
C14 C15 1.543(4) .
C31 C32 1.382(4) .
C31 C36 1.381(4) .
C32 C33 1.377(4) .
C33 C34 1.389(4) .
C34 C35 1.377(4) .
C34 N31 1.387(4) .
C35 C36 1.374(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N31 H31B O3 0.861 2.416 3.162 145.23 1_545
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
Fe1 S1 C11 C14 -65.5(3) . . . .
Fe2 S1 C11 C14 7.7(3) . . . .
S1 C11 C14 C15 177.0(3) . . . .
Fe1 S2 C12 C14 67.2(3) . . . .
Fe2 S2 C12 C14 -6.4(3) . . . .
S2 C12 C14 C15 -178.6(2) . . . .
Fe2 S3 C13 C14 28.1(3) . . . .
C31 S3 C13 C14 151.0(3) . . . .
S3 C13 C14 C15 162.6(3) . . . .
