Synthesis and Isolation of a Silylsilicate Containing Two Pentacoordinated Silicon Atoms by Monoprotonation of a Disilicate and Monodeprotonation of a Disilane
Kano, Naokazu; Sasaki, Keishi; Miyake, Hideaki; Kawashima, Takayuki; Organometallics 33 (2014) 2358–; doi:10.1021/om500291k

data_4083102
_publ_section_title
;
 Synthesis and Isolation of a Silylsilicate Containing Two
 Pentacoordinated Silicon Atoms by Monoprotonation of a Disilicate and
 Monodeprotonation of a Disilane
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2358
_journal_paper_doi               10.1021/om500291k
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C45 H36 F24 O9 Si2'
_chemical_formula_weight         1232.91
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            32
_cell_length_a                   39.272(14)
_cell_length_b                   28.384(9)
_cell_length_c                   36.443(12)
_cell_measurement_reflns_used    24363
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4835
_cell_measurement_theta_min      3.0494
_cell_volume                     40623(2)
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_collection       'CrystalClear (Rigaku Corp., 2000)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2000)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.5666
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
Mercury CCD (2x2 bin mode)
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Sealed Tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0948
_diffrn_reflns_av_unetI/netI     0.1241
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            65390
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.050
_exptl_absorpt_coefficient_mu    0.212
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Jacobson, R. (1998) Private communication
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.613
_exptl_crystal_description       Block
_exptl_crystal_F_000             19904
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 3400 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.5(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1469
_refine_ls_number_reflns         17290
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0658
_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^)+(0.0454P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1660
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.909
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                11807
_reflns_number_total             17290
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500291k_si_002.cif
_cod_data_source_block           sisi8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083102--4083103.cif.
;
_cod_original_cell_volume        40622(23)
_cod_database_code               4083102
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2013-4
_shelx_res_checksum              93075
_shelx_hkl_checksum              32484