Synthesis and crystal structures of bis-[1-oxopyridin-2-olato(1-)]bis-(penta-fluoro-phen-yl)silicon(IV)-tetra-hydro-furan-pentane (2/1/1), bis-[1-oxopyridin-2-olato(1-)]bis-(<i>p</i>-tol-yl)silicon(IV), and dimesitylbis[1-oxopyridin-2-olato(1-)]silicon(IV).
Kraft, Bradley M.; Brennessel, William W.; Andrews, Jordan W.; Viggiani, Michael T.; Kittrell, Nathan F.; Heckman, Matthew T.; Acta crystallographica. Section E, Crystallographic communications 80 (2024) 318–324; doi:10.1107/S2056989024001543

data_2023038
_publ_section_title
;
 Synthesis and crystal structures of
 bis-[1-oxopyridin-2-olato(1-)]bis-(penta-fluoro-phen-yl)silicon(IV)-tetra-hydro-furan-pentane
 (2/1/1), bis-[1-oxopyridin-2-olato(1-)]bis-(<i>p</i>-tol-yl)silicon(IV),
 and dimesitylbis[1-oxopyridin-2-olato(1-)]silicon(IV).
;
_journal_coeditor_code           EE2004
_journal_issue                   'Pt 3'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              318
_journal_page_last               324
_journal_paper_doi               10.1107/S2056989024001543
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          'C22 H8 F10 N2 O4 Si, 0.5C5 H12, 0.5C4 H8 O'
_chemical_formula_moiety
'C22 H8 F10 N2 O4 Si, 0.5(C5 H12), 0.5(C4 H8 O)'
_chemical_formula_sum            'C26.5 H18 F10 N2 O4.5 Si'
_chemical_formula_weight         654.52
_chemical_name_common
'Bis[1-oxopyridin-2-olato(1-)]bis(pentafluorophenyl)silicon(IV)--tetrahydrofuran--pentane (2/1/1)'
_chemical_name_systematic
'Bis[1-oxopyridin-2-olato(1-)]bis(pentafluorophenyl)silicon(IV)--tetrahydrofuran--pentane (2/1/1)'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_cell_angle_alpha                90
_cell_angle_beta                 105.7674(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6809(9)
_cell_length_b                   12.1217(9)
_cell_length_c                   17.7335(13)
_cell_measurement_reflns_used    3989
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      37.40
_cell_measurement_theta_min      2.30
_cell_volume                     2623.3(3)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX3 (Bruker, 2016)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            97594
_diffrn_reflns_theta_full        37.785
_diffrn_reflns_theta_max         38.755
_diffrn_reflns_theta_min         1.768
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  0.7476
_exptl_absorpt_correction_T_min  0.6935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Krause <i>et al.</i>,  2015)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       plate
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.579
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         14595
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0822P)^2^+0.9141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1629
_reflns_number_gt                9977
_reflns_number_total             14595
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ee2004sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2023038--2023040.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2023038
_cod_database_fobs_code          2023038
_shelx_estimated_absorpt_t_min   0.923
_shelx_estimated_absorpt_t_max   0.972
_shelx_hkl_checksum              51442
_shelx_res_checksum              44336