#------------------------------------------------------------------------------
#$Date: 2019-11-23 06:42:13 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232345 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/75/4347501.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_4347501
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                 123.2050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.3243(13)
_cell_length_b                   7.9693(5)
_cell_length_c                   14.0085(9)
_cell_measurement_reflns_used    4559
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.82
_cell_volume                     1898.5(2)
_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      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0259
_diffrn_reflns_av_unetI/netI     0.0249
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7294
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.395
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            dark-grey
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1934
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0263
_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)+(0.0327P)²+1.7020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0667
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1698
_reflns_number_total             1934
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00246_si_004.cif
_cod_data_source_block
;
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4347501
_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   0.838
_shelx_estimated_absorpt_t_max   0.980
_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 0.0000 0.42275(4) 0.2500 0.01172(11) Uani 1 2 d S T P
S1 S 0.04242(3) 0.62286(6) 0.18274(4) 0.01700(13) Uani 1 1 d . . .
N1 N 0.03769(8) 0.26026(19) 0.18538(12) 0.0157(3) Uani 1 1 d . . .
N2 N 0.10968(8) 0.42734(18) 0.39025(12) 0.0144(3) Uani 1 1 d . . .
C1 C 0.06874(10) 0.1933(2) 0.14813(14) 0.0164(4) Uani 1 1 d . . .
C2 C 0.13000(10) 0.3531(2) 0.48949(15) 0.0173(4) Uani 1 1 d . . .
H2 H 0.0904 0.2971 0.4938 0.021 Uiso 1 1 calc R U .
C3 C 0.20582(11) 0.3553(2) 0.58501(15) 0.0199(4) Uani 1 1 d . . .
H3 H 0.2180 0.2995 0.6528 0.024 Uiso 1 1 calc R U .
C4 C 0.26378(11) 0.4392(2) 0.58124(16) 0.0224(4) Uani 1 1 d . . .
H4 H 0.3161 0.4438 0.6464 0.027 Uiso 1 1 calc R U .
C5 C 0.24402(11) 0.5165(3) 0.48048(16) 0.0207(4) Uani 1 1 d . . .
H5 H 0.2826 0.5763 0.4757 0.025 Uiso 1 1 calc R U .
C6 C 0.16737(10) 0.5059(2) 0.38648(15) 0.0162(4) Uani 1 1 d . . .
C7 C 0.14624(10) 0.5767(2) 0.27365(16) 0.0196(4) Uani 1 1 d . . .
H7A H 0.1607 0.4950 0.2349 0.023 Uiso 1 1 calc R U .
H7B H 0.1767 0.6807 0.2867 0.023 Uiso 1 1 calc R U .
C8 C 0.03858(11) 0.8111(2) 0.25369(17) 0.0226(4) Uani 1 1 d . . .
H8A H 0.0831 0.8117 0.3346 0.027 Uiso 1 1 calc R U .
H8B H 0.0423 0.9125 0.2161 0.027 Uiso 1 1 calc R U .
BB1 B 0.11650(14) 0.1102(3) 0.1010(2) 0.0276(5) Uani 1 1 d . . .
HB1A H 0.1588 0.1860 0.1146 0.041 Uiso 1 1 calc R U .
HB1B H 0.0811 0.0897 0.0190 0.041 Uiso 1 1 calc R U .
HB1C H 0.1392 0.0036 0.1405 0.041 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'
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
N1 Fe1 N1 97.31(8) 2 .
N1 Fe1 N2 93.75(6) 2 .
N1 Fe1 N2 87.63(6) . .
N1 Fe1 N2 87.63(6) 2 2
N1 Fe1 N2 93.75(6) . 2
N2 Fe1 N2 177.91(8) . 2
N1 Fe1 S1 176.12(4) 2 .
N1 Fe1 S1 86.48(4) . .
N2 Fe1 S1 85.54(4) . .
N2 Fe1 S1 92.98(4) 2 .
N1 Fe1 S1 86.48(4) 2 2
N1 Fe1 S1 176.12(4) . 2
N2 Fe1 S1 92.98(4) . 2
N2 Fe1 S1 85.54(4) 2 2
S1 Fe1 S1 89.75(3) . 2
C7 S1 C8 99.51(9) . .
C7 S1 Fe1 97.35(6) . .
C8 S1 Fe1 102.36(6) . .
C1 N1 Fe1 165.66(15) . .
C2 N2 C6 117.31(15) . .
C2 N2 Fe1 123.29(12) . .
C6 N2 Fe1 119.39(12) . .
N1 C1 BB1 175.9(2) . .
N2 C2 C3 122.82(16) . .
C4 C3 C2 119.45(17) . .
C3 C4 C5 118.56(17) . .
C4 C5 C6 119.30(17) . .
N2 C6 C5 122.51(16) . .
N2 C6 C7 117.35(16) . .
C5 C6 C7 120.09(16) . .
C6 C7 S1 111.62(12) . .
C8 C8 S1 108.33(10) 2 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.9602(15) 2
Fe1 N1 1.9602(15) .
Fe1 N2 2.0084(15) .
Fe1 N2 2.0084(15) 2
Fe1 S1 2.2503(5) .
Fe1 S1 2.2503(5) 2
S1 C7 1.8074(18) .
S1 C8 1.8246(19) .
N1 C1 1.147(2) .
N2 C2 1.351(2) .
N2 C6 1.355(2) .
C1 BB1 1.586(3) .
C2 C3 1.381(2) .
C3 C4 1.381(3) .
C4 C5 1.383(3) .
C5 C6 1.386(3) .
C6 C7 1.503(2) .
C8 C8 1.514(4) 2
