#------------------------------------------------------------------------------
#$Date: 2015-11-29 04:24:02 +0200 (Sun, 29 Nov 2015) $
#$Revision: 170606 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/13/2241374.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241374
loop_
_publ_author_name
'Kraft, Bradley M.'
'Brennessel, William W.'
'Ryan, Amy E.'
'Benjamin, Candace K.'
_publ_section_title
;
 Crystal structures of tris[1-oxopyridine-2-olato(1{-})]silicon(IV)
 chloride chloroform-d₁ disolvate,
 tris[1-oxopyridine-2-olato(1{-})]silicon(IV) chloride acetonitrile
 unquantified solvate, and
 fac-tris[1-oxopyridine-2-thiolato(1{-})]silicon(IV) chloride
 chloroform-d₁ disolvate
;
_journal_coeditor_code           HG5464
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1531
_journal_page_last               1535
_journal_paper_doi               10.1107/S2056989015022203
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          'C15 H12 N3 O3 S3 Si +, Cl -, 2C D Cl3'
_chemical_formula_moiety         'C15 H12 N3 O3 S3 Si +, Cl -, 2(C D Cl3)'
_chemical_formula_sum            'C17 H12 Cl7 D2 N3 O3 S3 Si'
_chemical_formula_weight         682.74
_chemical_name_common            sjfbk44
_chemical_name_systematic
;
fac-Tris[1-oxopyridine-2-thiolato(1-)]silicon(IV) chloride
chloroform-d₁ disolvate
;
_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_Hall           'P 2ac 2ab 3'
_space_group_name_H-M_alt        'P 21 3'
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9483(12)
_cell_length_b                   13.9483(12)
_cell_length_c                   13.9483(12)
_cell_measurement_reflns_used    4002
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      33.81
_cell_measurement_theta_min      2.53
_cell_volume                     2713.7(4)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2014)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2011 (Burla et al.,  2012)
;
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD Platform'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66318
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.537
_diffrn_reflns_theta_min         2.065
_exptl_absorpt_coefficient_mu    1.034
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2014)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       tetrahedron
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.668
_refine_ls_abs_structure_details
;
Flack x determined using 1775 quotients
[(I⁺)-(I⁻)]/[(I⁺)+(I⁻)]
(Parsons et al.,  2013)
;
_refine_ls_abs_structure_Flack   -0.018(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         5067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0370
_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)+(0.0387P)²+1.2622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0879
_reflns_number_gt                4360
_reflns_number_total             5067
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hg5464sup1.cif
_cod_data_source_block           III
_cod_original_cell_volume        2713.7(7)
_cod_database_code               2241374
_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   0.836
_shelx_estimated_absorpt_t_max   0.836
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Cl Cl1 0.47976(3) -0.02024(3) 0.52024(3) 0.01864(13) Uani d 1
Si Si1 0.48307(3) 0.48307(3) 0.48307(3) 0.01248(14) Uani d 1
S S1 0.47110(3) 0.49896(3) 0.64425(3) 0.01526(8) Uani d 1
O O1 0.45832(11) 0.35879(9) 0.49722(10) 0.0153(2) Uani d 1
N N1 0.46124(12) 0.31975(11) 0.58645(11) 0.0138(2) Uani d 1
C C1 0.46796(14) 0.37754(13) 0.66485(13) 0.0146(3) Uani d 1
C C2 0.47203(16) 0.33345(14) 0.75505(14) 0.0190(3) Uani d 1
H H2 0.4772 0.3713 0.8114 0.023 Uiso calc 1
C C3 0.46853(18) 0.23462(15) 0.76169(15) 0.0220(4) Uani d 1
H H3 0.4708 0.2045 0.8228 0.026 Uiso calc 1
C C4 0.46163(15) 0.17883(14) 0.67861(15) 0.0187(3) Uani d 1
H H4 0.4592 0.1109 0.6831 0.022 Uiso calc 1
C C5 0.45834(14) 0.22276(13) 0.59068(14) 0.0161(3) Uani d 1
H H5 0.4541 0.1858 0.5337 0.019 Uiso calc 1
C C6 0.30918(15) 0.30918(15) 0.30918(15) 0.0212(6) Uani d 1
D D6 0.3506 0.3506 0.3506 0.025 Uiso calc 1
Cl Cl2 0.30061(7) 0.19603(5) 0.36357(6) 0.04462(19) Uani d 1
C C7 0.12879(19) 0.37121(19) 0.62879(19) 0.0264(7) Uani d 1
D D7 0.0874 0.4126 0.5874 0.032 Uiso calc 1
Cl Cl3 0.21080(7) 0.44529(6) 0.68782(8) 0.0511(2) Uani d 1
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'
D D 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Cl Cl 0.1484 0.1585 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Si1 O1 9 5 86.60(7) ?
O1 Si1 O1 9 . 86.59(7) ?
O1 Si1 O1 5 . 86.59(7) ?
O1 Si1 S1 9 . 96.31(5) ?
O1 Si1 S1 5 . 174.00(5) ?
O1 Si1 S1 . . 88.33(4) y
O1 Si1 S1 9 9 88.33(4) ?
O1 Si1 S1 5 9 96.31(5) ?
O1 Si1 S1 . 9 174.00(5) y
S1 Si1 S1 . 9 89.04(3) ?
O1 Si1 S1 9 5 174.00(5) ?
O1 Si1 S1 5 5 88.33(4) ?
O1 Si1 S1 . 5 96.31(5) ?
S1 Si1 S1 . 5 89.04(3) ?
S1 Si1 S1 9 5 89.04(3) ?
C1 S1 Si1 . . 94.09(6) ?
N1 O1 Si1 . . 119.10(11) ?
C5 N1 O1 . . 116.05(15) ?
C5 N1 C1 . . 123.93(16) ?
O1 N1 C1 . . 120.02(14) ?
N1 C1 C2 . . 117.64(16) ?
N1 C1 S1 . . 116.80(13) ?
C2 C1 S1 . . 125.56(14) ?
C3 C2 C1 . . 119.75(18) ?
C3 C2 H2 . . 120.1 ?
C1 C2 H2 . . 120.1 ?
C2 C3 C4 . . 120.09(18) ?
C2 C3 H3 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C5 C4 C3 . . 119.64(17) ?
C5 C4 H4 . . 120.2 ?
C3 C4 H4 . . 120.2 ?
N1 C5 C4 . . 118.94(17) ?
N1 C5 H5 . . 120.5 ?
C4 C5 H5 . . 120.5 ?
Cl2 C6 Cl2 9 5 110.91(11) ?
Cl2 C6 Cl2 9 . 110.91(11) ?
Cl2 C6 Cl2 5 . 110.91(11) ?
Cl2 C6 D6 9 . 108.0 ?
Cl2 C6 D6 5 . 108.0 ?
Cl2 C6 D6 . . 108.0 ?
Cl3 C7 Cl3 6_456 12_565 110.93(14) ?
Cl3 C7 Cl3 6_456 . 110.93(14) ?
Cl3 C7 Cl3 12_565 . 110.93(14) ?
Cl3 C7 D7 6_456 . 108.0 ?
Cl3 C7 D7 12_565 . 108.0 ?
Cl3 C7 D7 . . 108.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Si1 O1 9 1.7784(14) ?
Si1 O1 5 1.7784(14) ?
Si1 O1 . 1.7784(14) y
Si1 S1 . 2.2654(7) y
Si1 S1 9 2.2654(7) ?
Si1 S1 5 2.2654(7) ?
S1 C1 . 1.7184(19) ?
O1 N1 . 1.359(2) ?
N1 C5 . 1.355(2) ?
N1 C1 . 1.362(2) ?
C1 C2 . 1.402(3) ?
C2 C3 . 1.383(3) ?
C2 H2 . 0.9500 ?
C3 C4 . 1.399(3) ?
C3 H3 . 0.9500 ?
C4 C5 . 1.372(3) ?
C4 H4 . 0.9500 ?
C5 H5 . 0.9500 ?
C6 Cl2 9 1.7552(13) ?
C6 Cl2 5 1.7552(13) ?
C6 Cl2 . 1.7552(13) ?
C6 D6 . 1.0000 ?
C7 Cl3 6_456 1.7476(16) ?
C7 Cl3 12_565 1.7476(16) ?
C7 Cl3 . 1.7476(16) ?
C7 D7 . 1.0000 ?
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_site_symmetry_1
_geom_torsion
O1 Si1 O1 N1 9 -108.75(16)
O1 Si1 O1 N1 5 164.47(14)
S1 Si1 O1 N1 . -12.32(12)
S1 Si1 O1 N1 5 76.53(13)
Si1 O1 N1 C5 . -168.92(13)
Si1 O1 N1 C1 . 10.3(2)
C5 N1 C1 C2 . 0.0(3)
O1 N1 C1 C2 . -179.14(18)
C5 N1 C1 S1 . 179.76(15)
O1 N1 C1 S1 . 0.7(2)
Si1 S1 C1 N1 . -7.82(15)
Si1 S1 C1 C2 . 171.97(18)
N1 C1 C2 C3 . -0.4(3)
S1 C1 C2 C3 . 179.79(18)
C1 C2 C3 C4 . 0.5(4)
C2 C3 C4 C5 . 0.0(4)
O1 N1 C5 C4 . 179.61(17)
C1 N1 C5 C4 . 0.5(3)
C3 C4 C5 N1 . -0.4(3)

_cod_database_fobs_code 2241374
