Preparation and structural characterisation of methoxybis(trimethylsilyl)silyl potassium and its condensation product
Likhar, Pravin R.; Zirngast, Michaela; Baumgartner, Judith; Marschner, Christoph; Chemical Communications  (2004) 1764–1765; doi:10.1039/b406074a

data_7111337
_publ_section_title
;
 Preparation and structural characterisation of
 methoxybis(trimethylsilyl)silyl potassium and its condensation product
;
_journal_issue                   15
_journal_name_full               'Chemical Communications'
_journal_page_first              1764
_journal_page_last               1765
_journal_paper_doi               10.1039/b406074a
_journal_year                    2004
_chemical_formula_sum            'C19 H45 K O7 Si3'
_chemical_formula_weight         508.92
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.6523(19)
_cell_length_b                   18.092(4)
_cell_length_c                   34.297(7)
_cell_measurement_temperature    100(2)
_cell_volume                     5989(2)
_computing_cell_refinement       'Bruker SAINT (1998)'
_computing_data_collection       'Bruker SMART (1998)'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0938
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            40265
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_type   SADABS
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            'slight yellow'
_exptl_crystal_density_diffrn    1.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.184
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.184
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0741
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0559P)^2^+6.5766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1520
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                4350
_reflns_number_total             5291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b406074asup1.cif
_cod_data_source_block           147j
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               7111337