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_2023040
_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_absolute_configuration ad
_chemical_formula_moiety         'C28 H30 N2 O4 Si'
_chemical_formula_sum            'C28 H30 N2 O4 Si'
_chemical_formula_weight         486.63
_chemical_name_common
;
Bis[1-oxopyridin-2-olato(1-)]bis(2,4,6-trimethylphenyl)silicon(IV)
;
_chemical_name_systematic
;
Dimesitylbis[1-oxopyridin-2-olato(1-)]silicon(IV)
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5710(2)
_cell_length_b                   12.68898(19)
_cell_length_c                   15.3580(2)
_cell_measurement_reflns_used    11827
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.9300
_cell_measurement_theta_min      4.5080
_cell_volume                     2449.80(6)
_computing_cell_refinement
;
CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)
;
_computing_data_collection
;
CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)
;
_computing_data_reduction
;
CrysAlisPro 1.171.40.68a (Rigaku OD, 2019)
;
_computing_molecular_graphics
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22120
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         77.689
_diffrn_reflns_theta_min         4.520
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.154
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2019)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.094
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.249
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1985 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons et al., 2013)
;
_refine_ls_abs_structure_Flack   -0.034(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0316
_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/[\s^2^(Fo^2^)+(0.0363P)^2^+0.5221P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0787
_reflns_number_gt                4847
_reflns_number_total             5138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ee2004sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2023038--2023040.cif.'
_cod_original_cell_volume        2449.80(7)
_cod_database_code               2023040
_cod_database_fobs_code          2023040
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.936
_shelx_hkl_checksum              24327
_shelx_res_checksum              39681