#------------------------------------------------------------------------------
#$Date: 2017-09-12 06:07:22 +0300 (Tue, 12 Sep 2017) $
#$Revision: 200589 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/41/7044185.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_7044185
loop_
_publ_author_name
'Halder, Partha'
'Ghorai, Santanu'
'Banerjee, Sridhar'
'Mondal, Biswajit'
'Rana, Atanu'
_publ_section_title
;
 Iron(II) Complexes of 2-Mercaptopyridine as Rubredoxin Site Analogues
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02645E
_journal_year                    2017
_chemical_formula_sum            'C20 H16 Fe2 N4 S4'
_chemical_formula_weight         552.31
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-05-25 deposited with the CCDC.
2017-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   27.8033(10)
_cell_length_b                   27.8033(10)
_cell_length_c                   21.6926(15)
_cell_measurement_reflns_used    3801
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      19.27
_cell_measurement_theta_min      2.43
_cell_volume                     14522.3(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.612
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.612
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32398
_diffrn_reflns_point_group_measured_fraction_full 0.612
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.34
_diffrn_reflns_theta_min         1.263
_exptl_absorpt_coefficient_mu    1.168
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.137
_exptl_crystal_description       needle
_exptl_crystal_F_000             5040
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.070
_platon_squeeze_details          1348
_refine_diff_density_max         0.194
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0171P)²+58.7656P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2884
_reflns_number_total             3576
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt02645e2.cif
_cod_data_source_block           ph221_0m_sq_sqd
_cod_original_cell_volume        14522.3(14)
_cod_database_code               7044185
_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.
;
_shelx_estimated_absorpt_t_min   0.844
_shelx_estimated_absorpt_t_max   0.923
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Fe1 Fe 0.35165(3) 0.01067(3) 0.36326(3) 0.0429(2) Uani 1 1 d . .
Fe2 Fe 0.35155(3) -0.00308(3) 0.53025(3) 0.0418(2) Uani 1 1 d . .
S3 S 0.37905(5) 0.07729(5) 0.44873(5) 0.0460(3) Uani 1 1 d . .
S4 S 0.34073(5) -0.06558(5) 0.43153(5) 0.0482(3) Uani 1 1 d . .
S1 S 0.28895(5) -0.05403(5) 0.27352(5) 0.0499(3) Uani 1 1 d . .
N3 N 0.43880(14) 0.04831(14) 0.51510(15) 0.0392(9) Uani 1 1 d . .
C15 C 0.44305(18) 0.08333(17) 0.46895(19) 0.0409(11) Uani 1 1 d . .
C14 C 0.4933(2) 0.11806(19) 0.4415(2) 0.0525(13) Uani 1 1 d . .
H14 H 0.4955 0.1412 0.4093 0.063 Uiso 1 1 calc R U
C11 C 0.4852(2) 0.0494(2) 0.5343(2) 0.0534(13) Uani 1 1 d . .
H11 H 0.4824 0.0258 0.5661 0.064 Uiso 1 1 calc R U
C12 C 0.5360(2) 0.0835(2) 0.5093(2) 0.0622(14) Uani 1 1 d . .
H12 H 0.5674 0.0833 0.5238 0.075 Uiso 1 1 calc R U
C13 C 0.5399(2) 0.1183(2) 0.4620(2) 0.0659(15) Uani 1 1 d . .
H13 H 0.5741 0.1420 0.4441 0.079 Uiso 1 1 calc R U
N1 N 0.27053(16) 0.00015(16) 0.35858(17) 0.0505(10) Uani 1 1 d . .
C1 C 0.2420(2) 0.0196(2) 0.3906(2) 0.0659(15) Uani 1 1 d . .
H1 H 0.2581 0.0412 0.4255 0.079 Uiso 1 1 calc R U
C5 C 0.2469(2) -0.0314(2) 0.3082(2) 0.0514(13) Uani 1 1 d . .
C4 C 0.1948(2) -0.0430(2) 0.2877(3) 0.0694(16) Uani 1 1 d . .
H4 H 0.1794 -0.0642 0.2524 0.083 Uiso 1 1 calc R U
C2 C 0.1898(3) 0.0084(3) 0.3729(3) 0.0873(19) Uani 1 1 d . .
H2 H 0.1707 0.0217 0.3960 0.105 Uiso 1 1 calc R U
C3 C 0.1664(2) -0.0227(3) 0.3204(3) 0.0881(19) Uani 1 1 d . .
H3 H 0.1316 -0.0299 0.3072 0.106 Uiso 1 1 calc R U
N4 N 0.26819(15) -0.05897(15) 0.50086(16) 0.0446(9) Uani 1 1 d . .
C20 C 0.27279(19) -0.08730(19) 0.4529(2) 0.0499(12) Uani 1 1 d . .
C16 C 0.2175(2) -0.0719(2) 0.5218(2) 0.0572(14) Uani 1 1 d . .
H16 H 0.2147 -0.0520 0.5547 0.069 Uiso 1 1 calc R U
C17 C 0.1698(2) -0.1138(3) 0.4958(3) 0.0775(17) Uani 1 1 d . .
H17 H 0.1352 -0.1223 0.5111 0.093 Uiso 1 1 calc R U
C19 C 0.2250(2) -0.1303(2) 0.4246(2) 0.0641(15) Uani 1 1 d . .
H19 H 0.2282 -0.1495 0.3913 0.077 Uiso 1 1 calc R U
C7 C 0.5132(2) 0.0288(2) 0.3055(2) 0.0554(14) Uani 1 1 d . .
H7 H 0.5363 0.0141 0.3128 0.067 Uiso 1 1 calc R U
C6 C 0.4630(2) 0.0077(2) 0.33494(19) 0.0490(12) Uani 1 1 d . .
H6 H 0.4525 -0.0213 0.3627 0.059 Uiso 1 1 calc R U
C8 C 0.5289(2) 0.0726(2) 0.2643(2) 0.0581(14) Uani 1 1 d . .
H8 H 0.5630 0.0880 0.2443 0.070 Uiso 1 1 calc R U
N2 N 0.42831(14) 0.02763(15) 0.32516(14) 0.0388(9) Uani 1 1 d . .
S2 S 0.39430(5) 0.09114(5) 0.27477(5) 0.0408(3) Uani 1 1 d . .
C10 C 0.44305(18) 0.06972(18) 0.28496(19) 0.0400(11) Uani 1 1 d . .
C9 C 0.49369(19) 0.09276(19) 0.2537(2) 0.0517(13) Uani 1 1 d . .
H9 H 0.5034 0.1216 0.2259 0.062 Uiso 1 1 calc R U
C18 C 0.1738(2) -0.1434(2) 0.4464(3) 0.0795(18) Uani 1 1 d . .
H18 H 0.1419 -0.1718 0.4283 0.095 Uiso 1 1 calc R U
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'
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
N2 Fe1 N1 153.66(13) . .
N2 Fe1 S3 103.27(9) . .
N1 Fe1 S3 92.72(12) . .
N2 Fe1 S4 95.93(10) . .
N1 Fe1 S4 104.07(10) . .
S3 Fe1 S4 93.05(4) . .
N2 Fe1 S1 96.49(9) . .
N1 Fe1 S1 64.93(11) . .
S3 Fe1 S1 157.36(5) . .
S4 Fe1 S1 95.82(4) . .
N2 Fe1 S2 64.18(10) . .
N1 Fe1 S2 94.32(10) . .
S3 Fe1 S2 93.95(4) . .
S4 Fe1 S2 159.96(4) . .
S1 Fe1 S2 84.71(4) . .
N3 Fe2 N4 153.33(14) . .
N3 Fe2 S2 93.63(10) . 6
N4 Fe2 S2 100.39(9) . 6
N3 Fe2 S1 107.46(10) . 6
N4 Fe2 S1 94.19(11) . 6
S2 Fe2 S1 93.92(4) 6 6
N3 Fe2 S3 65.19(10) . .
N4 Fe2 S3 99.48(9) . .
S2 Fe2 S3 158.80(4) 6 .
S1 Fe2 S3 91.93(4) 6 .
N3 Fe2 S4 91.87(9) . .
N4 Fe2 S4 64.00(11) . .
S2 Fe2 S4 97.60(4) 6 .
S1 Fe2 S4 156.81(5) 6 .
S3 Fe2 S4 84.54(4) . .
C15 S3 Fe1 100.25(14) . .
C15 S3 Fe2 76.40(15) . .
Fe1 S3 Fe2 91.02(4) . .
C20 S4 Fe1 95.96(15) . .
C20 S4 Fe2 76.21(17) . .
Fe1 S4 Fe2 89.82(4) . .
C5 S1 Fe2 98.83(15) . 8_544
C5 S1 Fe1 76.68(17) . .
Fe2 S1 Fe1 91.58(4) 8_544 .
C11 N3 C15 118.3(4) . .
C11 N3 Fe2 136.4(3) . .
C15 N3 Fe2 104.8(3) . .
N3 C15 C14 121.1(4) . .
N3 C15 S3 113.2(3) . .
C14 C15 S3 125.7(4) . .
C13 C14 C15 119.4(4) . .
C13 C14 H14 120.3 . .
C15 C14 H14 120.3 . .
N3 C11 C12 123.0(4) . .
N3 C11 H11 118.5 . .
C12 C11 H11 118.5 . .
C11 C12 C13 118.3(5) . .
C11 C12 H12 120.8 . .
C13 C12 H12 120.8 . .
C14 C13 C12 119.9(5) . .
C14 C13 H13 120.1 . .
C12 C13 H13 120.1 . .
C1 N1 C5 118.9(4) . .
C1 N1 Fe1 135.5(4) . .
C5 N1 Fe1 105.4(3) . .
N1 C1 C2 121.9(5) . .
N1 C1 H1 119.0 . .
C2 C1 H1 119.0 . .
N1 C5 C4 121.4(5) . .
N1 C5 S1 112.8(4) . .
C4 C5 S1 125.8(4) . .
C3 C4 C5 119.1(5) . .
C3 C4 H4 120.4 . .
C5 C4 H4 120.4 . .
C3 C2 C1 119.0(6) . .
C3 C2 H2 120.5 . .
C1 C2 H2 120.5 . .
C4 C3 C2 119.6(5) . .
C4 C3 H3 120.2 . .
C2 C3 H3 120.2 . .
C16 N4 C20 119.8(4) . .
C16 N4 Fe2 134.5(3) . .
C20 N4 Fe2 105.6(3) . .
N4 C20 C19 120.4(5) . .
N4 C20 S4 114.1(3) . .
C19 C20 S4 125.5(4) . .
N4 C16 C17 121.7(5) . .
N4 C16 H16 119.2 . .
C17 C16 H16 119.2 . .
C16 C17 C18 119.2(5) . .
C16 C17 H17 120.4 . .
C18 C17 H17 120.4 . .
C18 C19 C20 119.4(5) . .
C18 C19 H19 120.3 . .
C20 C19 H19 120.3 . .
C6 C7 C8 118.7(4) . .
C6 C7 H7 120.7 . .
C8 C7 H7 120.7 . .
N2 C6 C7 122.4(4) . .
N2 C6 H6 118.8 . .
C7 C6 H6 118.8 . .
C9 C8 C7 119.3(5) . .
C9 C8 H8 120.3 . .
C7 C8 H8 120.3 . .
C6 N2 C10 119.3(4) . .
C6 N2 Fe1 134.2(3) . .
C10 N2 Fe1 106.4(3) . .
C10 S2 Fe2 97.48(14) . 8_544
C10 S2 Fe1 74.00(16) . .
Fe2 S2 Fe1 89.49(4) 8_544 .
N2 C10 C9 120.7(4) . .
N2 C10 S2 115.3(3) . .
C9 C10 S2 124.0(4) . .
C8 C9 C10 119.6(5) . .
C8 C9 H9 120.2 . .
C10 C9 H9 120.2 . .
C19 C18 C17 119.5(5) . .
C19 C18 H18 120.3 . .
C17 C18 H18 120.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N2 2.108(3) .
Fe1 N1 2.127(4) .
Fe1 S3 2.4571(13) .
Fe1 S4 2.4770(13) .
Fe1 S1 2.6323(13) .
Fe1 S2 2.7285(13) .
Fe2 N3 2.137(3) .
Fe2 N4 2.143(4) .
Fe2 S2 2.4673(12) 6
Fe2 S1 2.4752(13) 6
Fe2 S3 2.6453(12) .
Fe2 S4 2.6783(13) .
S3 C15 1.757(4) .
S4 C20 1.734(5) .
S1 C5 1.749(5) .
S1 Fe2 2.4751(13) 8_544
N3 C11 1.340(5) .
N3 C15 1.360(5) .
C15 C14 1.374(6) .
C14 C13 1.366(6) .
C14 H14 0.9300 .
C11 C12 1.360(6) .
C11 H11 0.9300 .
C12 C13 1.379(6) .
C12 H12 0.9300 .
C13 H13 0.9300 .
N1 C1 1.355(6) .
N1 C5 1.349(6) .
C1 C2 1.376(7) .
C1 H1 0.9300 .
C5 C4 1.391(6) .
C4 C3 1.375(7) .
C4 H4 0.9300 .
C2 C3 1.382(8) .
C2 H2 0.9300 .
C3 H3 0.9300 .
N4 C16 1.348(6) .
N4 C20 1.349(5) .
C20 C19 1.409(6) .
C16 C17 1.375(7) .
C16 H16 0.9300 .
C17 C18 1.390(8) .
C17 H17 0.9300 .
C19 C18 1.364(7) .
C19 H19 0.9300 .
C7 C6 1.373(6) .
C7 C8 1.392(6) .
C7 H7 0.9300 .
C6 N2 1.347(5) .
C6 H6 0.9300 .
C8 C9 1.370(6) .
C8 H8 0.9300 .
N2 C10 1.348(5) .
S2 C10 1.746(4) .
S2 Fe2 2.4673(12) 8_544
C10 C9 1.396(6) .
C9 H9 0.9300 .
C18 H18 0.9300 .
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
C7 H7 S2 0.93 2.96 3.606(5) 127.5 18_545
C12 H12 S4 0.93 2.99 3.917(5) 172.1 10_656
C7 H7 S2 0.93 2.96 3.606(5) 127.5 18_545
C12 H12 S4 0.93 2.99 3.917(5) 172.1 10_656
C7 H7 S2 0.93 2.96 3.606(5) 127.5 18_545
C1 H1 S3 0.93 3.03 3.546(6) 116.4 .
C12 H12 S4 0.93 2.99 3.917(5) 172.1 10_656
C7 H7 S2 0.93 2.96 3.606(5) 127.5 18_545
C1 H1 S3 0.93 3.03 3.546(6) 116.4 .
C12 H12 S4 0.93 2.99 3.917(5) 172.1 10_656
C12 H12 S4 0.93 2.99 3.917(5) 172.1 10_656
C7 H7 S2 0.93 2.96 3.606(5) 127.5 18_545
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.004 1944 449 ' '
2 0.333 0.667 0.061 1939 449 ' '
3 0.667 0.333 0.728 1939 450 ' '
