#------------------------------------------------------------------------------
#$Date: 2019-11-23 06:42:44 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232347 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/75/4347503.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_4347503
loop_
_publ_author_name
'Arroyave, Alejandra'
'Lennartson, Anders'
'Dragulescu-Andrasi, Alina'
'Pedersen, Kasper S.'
'Piligkos, Stergios'
'Stoian, Sebastian A.'
'Greer, Samuel M.'
'Pak, Chongin'
'Hietsoi, Oleksandr'
'Phan, Hoa'
'Hill, Stephen'
'McKenzie, Christine J.'
'Shatruk, Michael'
_publ_section_title
;
 Spin Crossover in Fe(II) Complexes with N4S2 Coordination.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5904
_journal_page_last               5913
_journal_paper_doi               10.1021/acs.inorgchem.6b00246
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C16 H22 B2 Fe N4 S2'
_chemical_formula_weight         411.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 122.860(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.824(10)
_cell_length_b                   8.093(4)
_cell_length_c                   14.260(7)
_cell_measurement_reflns_used    6163
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.23
_cell_measurement_theta_min      2.77
_cell_volume                     2018.7(17)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    'X-Seed 2.0 (Barbour, 2001)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'Bruker APEX II CCD area-detector'
_diffrn_measurement_method       'profile data from ω scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8234
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.256
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    0.960
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6100
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            dark-grey
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0254
_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)+(0.0335P)²+1.1076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0706
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2171
_reflns_number_total             2355
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00246_si_005.cif
_cod_data_source_block
;
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347503
_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   0.689
_shelx_estimated_absorpt_t_max   0.910
_shelxl_version_number           2013-4
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.5000 0.39862(3) 0.2500 0.03142(10) Uani 1 2 d S T P
S1 S 0.44942(2) 0.63001(5) 0.31100(3) 0.04252(11) Uani 1 1 d . . .
N2 N 0.38594(7) 0.42040(15) 0.10272(10) 0.0353(3) Uani 1 1 d . . .
N1 N 0.46087(7) 0.23805(17) 0.32358(12) 0.0450(3) Uani 1 1 d . . .
C7 C 0.35008(9) 0.5769(2) 0.21507(14) 0.0467(4) Uani 1 1 d . . .
H7A H 0.3353 0.4982 0.2514 0.056 Uiso 1 1 calc R U .
H7B H 0.3195 0.6756 0.1998 0.056 Uiso 1 1 calc R U .
C6 C 0.33090(8) 0.50424(19) 0.10539(12) 0.0369(3) Uani 1 1 d . . .
C5 C 0.25734(9) 0.5180(2) 0.01266(15) 0.0479(4) Uani 1 1 d . . .
H5 H 0.2209 0.5791 0.0162 0.058 Uiso 1 1 calc R U .
C3 C 0.29394(10) 0.3520(2) -0.08836(14) 0.0479(4) Uani 1 1 d . . .
H3 H 0.2825 0.2976 -0.1531 0.057 Uiso 1 1 calc R U .
C2 C 0.36652(9) 0.3460(2) 0.00615(13) 0.0422(3) Uani 1 1 d . . .
H2 H 0.4039 0.2878 0.0033 0.051 Uiso 1 1 calc R U .
C1 C 0.42784(9) 0.1858(2) 0.35975(13) 0.0418(3) Uani 1 1 d . . .
C4 C 0.23839(10) 0.4402(2) -0.08528(15) 0.0518(4) Uani 1 1 d . . .
H4 H 0.1890 0.4470 -0.1482 0.062 Uiso 1 1 calc R U .
C8 C 0.46040(10) 0.8044(2) 0.24060(16) 0.0525(4) Uani 1 1 d . . .
H8A H 0.4220 0.7983 0.1612 0.063 Uiso 1 1 calc R U .
H8B H 0.4527 0.9066 0.2688 0.063 Uiso 1 1 calc R U .
B1 B 0.37884(14) 0.1174(3) 0.4058(2) 0.0658(6) Uani 1 1 d . . .
H1A H 0.3449 0.2022 0.4008 0.099 Uiso 1 1 calc R U .
H1B H 0.4124 0.0847 0.4823 0.099 Uiso 1 1 calc R U .
H1C H 0.3496 0.0237 0.3622 0.099 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'
B B 0.0013 0.0007 '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 103.25(8) 2_655 .
N1 Fe1 N2 90.93(6) 2_655 2_655
N1 Fe1 N2 94.88(6) . 2_655
N1 Fe1 N2 94.88(6) 2_655 .
N1 Fe1 N2 90.93(6) . .
N2 Fe1 N2 170.64(7) 2_655 .
N1 Fe1 S1 169.23(4) 2_655 .
N1 Fe1 S1 86.51(5) . .
N2 Fe1 S1 92.79(5) 2_655 .
N2 Fe1 S1 80.22(4) . .
N1 Fe1 S1 86.51(5) 2_655 2_655
N1 Fe1 S1 169.23(4) . 2_655
N2 Fe1 S1 80.22(5) 2_655 2_655
N2 Fe1 S1 92.79(5) . 2_655
S1 Fe1 S1 84.17(4) . 2_655
C7 S1 C8 101.67(9) . .
C7 S1 Fe1 94.76(6) . .
C8 S1 Fe1 100.65(7) . .
C2 N2 C6 117.68(13) . .
C2 N2 Fe1 121.23(10) . .
C6 N2 Fe1 121.05(10) . .
C1 N1 Fe1 161.87(14) . .
C6 C7 S1 115.35(10) . .
C6 C7 H7A 108.4 . .
S1 C7 H7A 108.4 . .
C6 C7 H7B 108.4 . .
S1 C7 H7B 108.4 . .
H7A C7 H7B 107.5 . .
N2 C6 C5 122.05(14) . .
N2 C6 C7 118.30(13) . .
C5 C6 C7 119.57(13) . .
C4 C5 C6 119.44(15) . .
C4 C5 H5 120.3 . .
C6 C5 H5 120.3 . .
C2 C3 C4 118.78(16) . .
C2 C3 H3 120.6 . .
C4 C3 H3 120.6 . .
N2 C2 C3 123.09(14) . .
N2 C2 H2 118.5 . .
C3 C2 H2 118.5 . .
N1 C1 B1 177.53(18) . .
C3 C4 C5 118.94(15) . .
C3 C4 H4 120.5 . .
C5 C4 H4 120.5 . .
C8 C8 S1 110.62(11) 2_655 .
C8 C8 H8A 109.5 2_655 .
S1 C8 H8A 109.5 . .
C8 C8 H8B 109.5 2_655 .
S1 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
C1 B1 H1A 109.5 . .
C1 B1 H1B 109.5 . .
H1A B1 H1B 109.5 . .
C1 B1 H1C 109.5 . .
H1A B1 H1C 109.5 . .
H1B B1 H1C 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 2.0931(15) 2_655
Fe1 N1 2.0931(15) .
Fe1 N2 2.1611(14) 2_655
Fe1 N2 2.1611(14) .
Fe1 S1 2.5233(9) .
Fe1 S1 2.5233(9) 2_655
S1 C7 1.8069(18) .
S1 C8 1.8170(19) .
N2 C2 1.349(2) .
N2 C6 1.3501(18) .
N1 C1 1.141(2) .
C7 C6 1.508(2) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C6 C5 1.382(2) .
C5 C4 1.380(3) .
C5 H5 0.9300 .
C3 C2 1.376(2) .
C3 C4 1.380(3) .
C3 H3 0.9300 .
C2 H2 0.9300 .
C1 B1 1.583(3) .
C4 H4 0.9300 .
C8 C8 1.521(4) 2_655
C8 H8A 0.9700 .
C8 H8B 0.9700 .
B1 H1A 0.9600 .
B1 H1B 0.9600 .
B1 H1C 0.9600 .
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
C8 S1 C7 C6 69.15(14) .
Fe1 S1 C7 C6 -32.78(13) .
C2 N2 C6 C5 -1.4(2) .
Fe1 N2 C6 C5 -179.15(12) .
C2 N2 C6 C7 175.31(14) .
Fe1 N2 C6 C7 -2.40(18) .
S1 C7 C6 N2 27.98(19) .
S1 C7 C6 C5 -155.18(14) .
N2 C6 C5 C4 1.9(3) .
C7 C6 C5 C4 -174.86(16) .
C6 N2 C2 C3 0.0(2) .
Fe1 N2 C2 C3 177.70(13) .
C4 C3 C2 N2 1.0(3) .
C2 C3 C4 C5 -0.6(3) .
C6 C5 C4 C3 -0.8(3) .
C7 S1 C8 C8 -144.80(15) 2_655
Fe1 S1 C8 C8 -47.62(16) 2_655
