Mono- and bimetallic pentacoordinate silicon complexes of a chelating bis(catecholimine) ligand.
Do, Thomas H.; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11565–11574; doi:10.1039/c9dt02475a

data_7700467
_publ_section_title
;
 Mono- and bimetallic pentacoordinate silicon complexes of a chelating
 bis(catecholimine) ligand.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11565
_journal_page_last               11574
_journal_paper_doi               10.1039/c9dt02475a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C55 H65 N2 Na O6 Si, 2(C4 H8 O)'
_chemical_formula_sum            'C63 H81 N2 Na O8 Si'
_chemical_formula_weight         1045.37
_chemical_name_common            '(THF)Na[(Xbic)SiPh] . 2 THF'
_chemical_name_systematic
'(Tetrahydrofuran)sodium(9,9-dimethylxanthene-4,5-bis(4,6-di-tert-butyl-2,3-dioxybenzaldimine)(phenyl)silicate) bis(tetrahydrofuran) solvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2019-06-11 deposited with the CCDC.    2019-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.068(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.104(2)
_cell_length_b                   19.806(3)
_cell_length_c                   17.777(2)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.36
_cell_volume                     5655.8(13)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            129520
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.452
_diffrn_reflns_theta_min         1.268
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6960
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             2248
_exptl_crystal_recrystallization_method
'Crystals were deposited by diffusion of acetonitrile into a solution of the compound in THF.'
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.196
_exptl_transmission_factor_max   0.795700
_exptl_transmission_factor_min   0.696000
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         14183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0721P)^2^+5.5303P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1440
_refine_ls_wR_factor_ref         0.1616
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10326
_reflns_number_total             14183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02475a2.cif
_cod_data_source_block           sina
_cod_depositor_comments
'Adding full bibliography for 7700466--7700470.cif.'
_cod_original_cell_volume        5656.0(13)
_cod_database_code               7700467
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.975
_shelx_estimated_absorpt_t_max   0.980
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelxl_version_number           2013-4
_shelx_res_checksum              9745