Crown ether adducts of light alkali metal triphenylsilyls: synthesis, structure and hydrosilylation catalysis.
Leich, Valeri; Lamberts, Kevin; Spaniol, Thomas P.; Okuda, Jun; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14315–14321; doi:10.1039/c4dt00916a

data_7030819
_publ_section_title
;
 Crown ether adducts of light alkali metal triphenylsilyls: synthesis,
 structure and hydrosilylation catalysis.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14315
_journal_page_last               14321
_journal_paper_doi               10.1039/c4dt00916a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C28 H35 Na O5 Si, 0.5 (C4 H8 O)'
_chemical_formula_sum            'C30 H39 Na O5.5 Si'
_chemical_formula_weight         538.69
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   12.858(5)
_cell_length_b                   12.858(5)
_cell_length_c                   10.756(5)
_cell_measurement_temperature    220(2)
_cell_volume                     1540.0(11)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      220(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4593
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         1.829
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         1817
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1155
_refine_ls_shift/su_max          0.047
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0100P)^2^+4.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1900
_refine_ls_wR_factor_ref         0.2141
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1052
_reflns_number_total             1817
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00916a2.cif
_cod_data_source_block           3beta
_cod_depositor_comments
'Adding full bibliography for 7030818--7030820.cif.'
_cod_original_cell_volume        1540.1(14)
_cod_original_formula_sum        'C30 H39 Na O5.50 Si'
_cod_database_code               7030819
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2013-2
_shelx_res_checksum              29647