Neutral and Cationic Bis-Chelate Monoorganosilicon(IV) Complexes of 1-Hydroxy-2-pyridinone
Koch, James G.; Brennessel, William W.; Kraft, Bradley M.; Organometallics 36 (2017) 594–; doi:10.1021/acs.organomet.6b00796

data_4086929
_publ_section_title
;
 Neutral and Cationic Bis-Chelate Monoorganosilicon(IV) Complexes of
 1-Hydroxy-2-pyridinone
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              594
_journal_paper_doi               10.1021/acs.organomet.6b00796
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C17 H15 N2 O4 Si, C F3 O3 S, C4 H8 O'
_chemical_formula_sum            'C22 H23 F3 N2 O8 S Si'
_chemical_formula_weight         560.57
_chemical_name_common            sjfbk53
_space_group_crystal_system      orthorhombic
_space_group_IT_number           58
_space_group_name_Hall           '-P 2 2n'
_space_group_name_H-M_alt        'P n n m'
_symmetry_space_group_name_Hall  '-P 2 2n'
_symmetry_space_group_name_H-M   'P n n m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.663(4)
_cell_length_b                   9.2503(15)
_cell_length_c                   10.0619(17)
_cell_measurement_reflns_used    4050
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      31.29
_cell_measurement_theta_min      2.16
_cell_volume                     2481.7(7)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX3 (Bruker, 2016)'
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_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
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_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016b)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            53183
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        31.506
_diffrn_reflns_theta_max         31.589
_diffrn_reflns_theta_min         2.163
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.252
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2016a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       needle
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4356
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0633P)^2^+1.1874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1252
_refine_ls_wR_factor_ref         0.1395
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3236
_reflns_number_total             4356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            20161212_Combined.cif
_cod_data_source_block           08r
_cod_depositor_comments
'Adding full bibliography for 4086922--4086931.cif.'
_cod_database_code               4086929
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.924
_shelx_estimated_absorpt_t_max   0.970
_shelx_res_checksum              26895
_shelx_hkl_checksum              12568