Crystal structures of tris[1-oxopyridine-2-olato(1{-})]silicon(IV) chloride chloroform-<i>d</i>~1~ disolvate, tris[1-oxopyridine-2-olato(1{-})]silicon(IV) chloride acetonitrile unquantified solvate, and <i>fac</i>-tris[1-oxopyridine-2-thiolato(1{-})]silicon(IV) chloride chloroform-<i>d</i>~1~ disolvate
Kraft, Bradley M.; Brennessel, William W.; Ryan, Amy E.; Benjamin, Candace K.; Acta Crystallographica Section E 71 (2015) 1531–1535; doi:10.1107/S2056989015022203

data_2241372
_publ_section_title
;
 Crystal structures of tris[1-oxopyridine-2-olato(1{-})]silicon(IV)
 chloride chloroform-<i>d</i>~1~ disolvate,
 tris[1-oxopyridine-2-olato(1{-})]silicon(IV) chloride acetonitrile
 unquantified solvate, and
 <i>fac</i>-tris[1-oxopyridine-2-thiolato(1{-})]silicon(IV) chloride
 chloroform-<i>d</i>~1~ 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 O6 Si +, Cl -, 2C D Cl3'
_chemical_formula_moiety         'C15 H12 N3 O6 Si +, Cl -, 2(C D Cl3)'
_chemical_formula_sum            'C17 H12 Cl7 D2 N3 O6 Si'
_chemical_formula_weight         634.56
_chemical_name_common            sjfbk16
_chemical_name_systematic
;
Tris[1-oxopyridine-2-olato(1-)]silicon(IV) chloride chloroform-<i>d</i>~1~
disolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 101.8660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5133(7)
_cell_length_b                   13.5039(7)
_cell_length_c                   13.7752(7)
_cell_measurement_reflns_used    3986
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      37.03
_cell_measurement_theta_min      2.37
_cell_volume                     2460.0(2)
_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
;
SHELXL2012 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2011 (Burla <i>et al.</i>,  2012)
;
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \f'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            61259
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.722
_diffrn_reflns_theta_min         1.923
_exptl_absorpt_coefficient_mu    0.897
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6674
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Sheldrick, 2014)
;
_exptl_crystal_colour            'pale red-yellow'
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.811
_refine_diff_density_min         -0.851
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         13615
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0438
_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/[\s^2^(Fo^2^)+(0.0513P)^2^+0.4945P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                9035
_reflns_number_total             13615
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hg5464sup1.cif
_cod_data_source_block           I
_cod_database_code               2241372
_cod_database_fobs_code          2241372
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.870
_shelx_hkl_checksum              18520
_shelx_res_checksum              55845
_shelxl_version_number           .2012