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_7030820
_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         'C34 H47 K O7 Si'
_chemical_formula_sum            'C34 H47 K O7 Si'
_chemical_formula_weight         634.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
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_cell_angle_beta                 112.535(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_length_c                   12.752(4)
_cell_measurement_temperature    100(2)
_cell_volume                     3435.6(18)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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
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_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12783
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.361
_diffrn_reflns_theta_min         1.775
_exptl_absorpt_coefficient_mu    0.234
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   TWINABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.450
_exptl_crystal_size_min          0.420
_refine_diff_density_max         0.751
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.00(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         7033
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+4.0000P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1862
_refine_ls_wR_factor_ref         0.1944
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_reflns_Friedel_fraction_full    0.800
_reflns_Friedel_fraction_max     0.776
_reflns_number_gt                6143
_reflns_number_total             7033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt00916a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7030818--7030820.cif.'
_cod_database_code               7030820
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.908
_shelxl_version_number           2013-2
_shelx_res_checksum              45807