A hydrogen bonded molecular capsule versus a 3D network of tripodal organopolysilanols
Marina Fukawa; Takayuki Sato; Yoshio Kabe; Chem.Commun. 51 (2015) 14746–; doi:10.1039/C5cc04515K

data_7117823
_publ_section_title
;
 A hydrogen bonded molecular capsule versus a 3D network of tripodal
 organopolysilanols
;
_journal_name_full               Chem.Commun.
_journal_page_first              14746
_journal_paper_doi               10.1039/C5cc04515K
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C33 H66 Si3'
_chemical_formula_sum            'C33 H66 Si3'
_chemical_formula_weight         547.13
_chemical_melting_point          338
_chemical_name_common            tris(diisopropylsilylmethyl)triethylbenzene
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-02 deposited with the CCDC.
2015-08-10 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.236(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.388(3)
_cell_length_b                   9.4848(9)
_cell_length_c                   27.972(3)
_cell_measurement_reflns_used    17512
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      3.0342
_cell_volume                     7254.7(13)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
;
'Saturn724+ (4x4 bin mode)'
;
_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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            57106
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.03
_exptl_absorpt_coefficient_mu    0.149
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chip
_exptl_crystal_F_000             2448
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.282
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         16329
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0843P)^2^+2.3620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1535
_refine_ls_wR_factor_ref         0.1677
_reflns_number_gt                12569
_reflns_number_total             16329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc04515k2.cif.txt
_cod_data_source_block           Et3C6(CH2SiiPr2H)3_2b
_cod_depositor_comments
;

2017-03-09
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        7254.9(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C66 H132 Si6'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1094.26
_cod_database_code               7117823