#------------------------------------------------------------------------------
#$Date: 2019-11-24 13:01:21 +0200 (Sun, 24 Nov 2019) $
#$Revision: 237963 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/00/4350049.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_4350049
loop_
_publ_author_name
'Chen, Xiu-Qin'
'Cai, You-De'
'Ye, Yi-Shan'
'Tong, Ming-Liang'
'Bao, Xin'
_publ_section_title
;
 Investigation of SCO property--structural relationships in a family of
 mononuclear Fe(ii) complexes
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              2194
_journal_paper_doi               10.1039/C9QI00577C
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C26 H26 Fe N6 S2'
_chemical_formula_sum            'C26 H26 Fe N6 S2'
_chemical_formula_weight         542.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-06-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2019-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7067(15)
_cell_length_b                   18.4252(18)
_cell_length_c                   8.8199(8)
_cell_measurement_reflns_used    1658
_cell_measurement_temperature    123
_cell_measurement_theta_max      24.5475
_cell_measurement_theta_min      2.2107
_cell_volume                     2552.5(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'PHOTON 100 CMOS detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.471
_diffrn_reflns_theta_min         2.211
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6171
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     161
_refine_ls_number_reflns         2221
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0335
_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)+(0.0253P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.872
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.986
_reflns_number_gt                1893
_reflns_number_total             2221
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9qi00577c2.cif
_cod_data_source_block           151109f_0m_pl
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_database_code               4350049
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 1.00(3) 0.00(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y, z+1/2'
'x+1/2, -y, z+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1'
'x+1/2, -y+1/2, z+1'
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
Fe1 Fe 0.0000 0.5000 -0.18688(9) 0.01809(18) Uani 1 2 d S T P
S1 S 0.07997(7) 0.31878(5) -0.56040(13) 0.0333(3) Uani 1 1 d . . .
N1 N -0.1440(2) 0.46875(17) -0.1472(3) 0.0235(8) Uani 1 1 d . . .
N2 N -0.0453(3) 0.56781(17) 0.0061(3) 0.0256(9) Uani 1 1 d . . .
N3 N 0.0387(2) 0.42405(18) -0.3463(4) 0.0258(8) Uani 1 1 d . . .
C1 C -0.1504(3) 0.3525(2) -0.2705(4) 0.0286(10) Uani 1 1 d . . .
H1 H -0.0916 0.3563 -0.2941 0.034 Uiso 1 1 calc R . .
C0AA C 0.0556(3) 0.3805(2) -0.4357(4) 0.0200(9) Uani 1 1 d . . .
C2 C -0.1956(3) 0.2923(2) -0.3156(5) 0.0373(12) Uani 1 1 d . . .
H2 H -0.1681 0.2548 -0.3706 0.045 Uiso 1 1 calc R . .
C3 C -0.2829(3) 0.2863(3) -0.2802(6) 0.0476(15) Uani 1 1 d . . .
H3 H -0.3139 0.2448 -0.3126 0.057 Uiso 1 1 calc R . .
C4 C -0.3231(3) 0.3390(3) -0.2007(6) 0.0471(13) Uani 1 1 d . . .
H4 H -0.3817 0.3337 -0.1766 0.057 Uiso 1 1 calc R . .
C5 C -0.2786(3) 0.4019(2) -0.1532(5) 0.0332(11) Uani 1 1 d . . .
C6 C -0.1908(2) 0.40839(19) -0.1899(5) 0.0249(8) Uani 1 1 d . . .
C7 C -0.1847(3) 0.5203(2) -0.0708(5) 0.0300(10) Uani 1 1 d . . .
C8 C -0.2708(3) 0.5173(3) -0.0312(5) 0.0388(12) Uani 1 1 d . . .
H8 H -0.2963 0.5560 0.0235 0.047 Uiso 1 1 calc R . .
C9 C -0.3173(3) 0.4585(3) -0.0719(6) 0.0415(12) Uani 1 1 d . . .
H9 H -0.3758 0.4557 -0.0456 0.050 Uiso 1 1 calc R . .
C10 C -0.1341(3) 0.5863(2) -0.0252(5) 0.0355(12) Uani 1 1 d . . .
H10A H -0.1364 0.6227 -0.1077 0.043 Uiso 1 1 calc R . .
H10B H -0.1599 0.6083 0.0664 0.043 Uiso 1 1 calc R . .
C11 C -0.0404(3) 0.5223(2) 0.1455(5) 0.0325(11) Uani 1 1 d . . .
H11A H -0.0904 0.4896 0.1500 0.039 Uiso 1 1 calc R . .
H11B H -0.0416 0.5539 0.2363 0.039 Uiso 1 1 calc R . .
C12 C 0.0039(3) 0.6360(2) 0.0262(5) 0.0350(11) Uani 1 1 d . . .
H12A H 0.0637 0.6243 0.0466 0.053 Uiso 1 1 calc GR . .
H12B H -0.0195 0.6636 0.1115 0.053 Uiso 1 1 calc GR . .
H12C H 0.0001 0.6652 -0.0665 0.053 Uiso 1 1 calc GR . .
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'
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
N1 Fe1 N1 162.95(15) 2_565 .
N2 Fe1 N1 93.19(13) 2_565 .
N2 Fe1 N1 73.61(13) 2_565 2_565
N2 Fe1 N1 73.61(13) . .
N2 Fe1 N1 93.19(13) . 2_565
N2 Fe1 N2 80.36(17) 2_565 .
N3 Fe1 N1 102.51(13) . .
N3 Fe1 N1 102.51(13) 2_565 2_565
N3 Fe1 N1 89.10(12) . 2_565
N3 Fe1 N1 89.09(12) 2_565 .
N3 Fe1 N2 92.64(12) . 2_565
N3 Fe1 N2 92.64(12) 2_565 .
N3 Fe1 N2 171.68(13) . .
N3 Fe1 N2 171.68(13) 2_565 2_565
N3 Fe1 N3 94.68(19) . 2_565
C6 N1 Fe1 131.6(3) . .
C7 N1 Fe1 111.2(3) . .
C7 N1 C6 117.1(4) . .
C10 N2 Fe1 106.9(3) . .
C10 N2 C11 109.6(3) . .
C10 N2 C12 108.7(3) . .
C11 N2 Fe1 107.4(2) . .
C12 N2 Fe1 113.5(3) . .
C12 N2 C11 110.6(3) . .
C0AA N3 Fe1 176.2(3) . .
C2 C1 H1 119.9 . .
C2 C1 C6 120.3(4) . .
C6 C1 H1 119.9 . .
N3 C0AA S1 179.4(4) . .
C1 C2 H2 120.0 . .
C1 C2 C3 120.1(5) . .
C3 C2 H2 120.0 . .
C2 C3 H3 119.6 . .
C4 C3 C2 120.8(5) . .
C4 C3 H3 119.6 . .
C3 C4 H4 119.7 . .
C3 C4 C5 120.7(5) . .
C5 C4 H4 119.7 . .
C4 C5 C6 118.7(4) . .
C9 C5 C4 123.1(4) . .
C9 C5 C6 118.2(4) . .
N1 C6 C1 119.1(3) . .
N1 C6 C5 121.4(4) . .
C1 C6 C5 119.5(4) . .
N1 C7 C8 124.4(4) . .
N1 C7 C10 117.3(4) . .
C8 C7 C10 118.4(4) . .
C7 C8 H8 120.4 . .
C9 C8 C7 119.1(5) . .
C9 C8 H8 120.4 . .
C5 C9 H9 120.1 . .
C8 C9 C5 119.8(4) . .
C8 C9 H9 120.1 . .
N2 C10 C7 111.4(3) . .
N2 C10 H10A 109.3 . .
N2 C10 H10B 109.3 . .
C7 C10 H10A 109.3 . .
C7 C10 H10B 109.3 . .
H10A C10 H10B 108.0 . .
N2 C11 C11 110.4(3) . 2_565
N2 C11 H11A 109.6 . .
N2 C11 H11B 109.6 . .
C11 C11 H11A 109.6 2_565 .
C11 C11 H11B 109.6 2_565 .
H11A C11 H11B 108.1 . .
N2 C12 H12A 109.5 . .
N2 C12 H12B 109.5 . .
N2 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 2.359(3) .
Fe1 N1 2.359(3) 2_565
Fe1 N2 2.228(3) 2_565
Fe1 N2 2.228(3) .
Fe1 N3 2.075(3) 2_565
Fe1 N3 2.075(3) .
S1 C0AA 1.627(4) .
N1 C6 1.386(5) .
N1 C7 1.329(5) .
N2 C10 1.463(6) .
N2 C11 1.490(5) .
N2 C12 1.486(5) .
N3 C0AA 1.156(5) .
C1 H1 0.9500 .
C1 C2 1.376(6) .
C1 C6 1.403(6) .
C2 H2 0.9500 .
C2 C3 1.410(7) .
C3 H3 0.9500 .
C3 C4 1.353(8) .
C4 H4 0.9500 .
C4 C5 1.415(6) .
C5 C6 1.422(5) .
C5 C9 1.404(6) .
C7 C8 1.397(6) .
C7 C10 1.508(6) .
C8 H8 0.9500 .
C8 C9 1.355(7) .
C9 H9 0.9500 .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C11 1.513(9) 2_565
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
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_4
Fe1 N1 C6 C1 0.8(6) .
Fe1 N1 C6 C5 -179.5(3) .
Fe1 N1 C7 C8 179.6(4) .
Fe1 N1 C7 C10 0.0(5) .
Fe1 N2 C10 C7 48.2(4) .
Fe1 N2 C11 C11 40.9(5) 2_565
N1 C7 C8 C9 0.1(7) .
N1 C7 C10 N2 -32.6(5) .
C1 C2 C3 C4 -0.6(7) .
C2 C1 C6 N1 -179.4(4) .
C2 C1 C6 C5 0.9(6) .
C2 C3 C4 C5 0.9(7) .
C3 C4 C5 C6 -0.3(7) .
C3 C4 C5 C9 179.3(5) .
C4 C5 C6 N1 179.7(4) .
C4 C5 C6 C1 -0.6(6) .
C4 C5 C9 C8 -179.5(4) .
C6 N1 C7 C8 0.1(6) .
C6 N1 C7 C10 -179.5(4) .
C6 C1 C2 C3 -0.3(6) .
C6 C5 C9 C8 0.1(6) .
C7 N1 C6 C1 -179.9(4) .
C7 N1 C6 C5 -0.2(5) .
C7 C8 C9 C5 -0.2(7) .
C8 C7 C10 N2 147.8(4) .
C9 C5 C6 N1 0.1(6) .
C9 C5 C6 C1 179.8(4) .
C10 N2 C11 C11 156.7(4) 2_565
C10 C7 C8 C9 179.7(4) .
C11 N2 C10 C7 -67.9(4) .
C12 N2 C10 C7 171.1(3) .
C12 N2 C11 C11 -83.5(5) 2_565
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 1.00(3)
2 0.00(3)
