Synthesis and Structure of Ladder Oligosilsesquioxanes: Tricyclic Ladder Oligomethylsilsesquioxanes
Suyama, Ken-ichi; Gunji, Takahiro; Arimitsu, Koji; Abe, Yoshimoto; Organometallics 25 (2006) 5587–; doi:10.1021/om060705v

data_4074494
_publ_section_title
;
 Synthesis and Structure of Ladder Oligosilsesquioxanes:&#x00A0; Tricyclic
 Ladder Oligomethylsilsesquioxanes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5587
_journal_paper_doi               10.1021/om060705v
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C24 H60 O14 Si8'
_chemical_formula_sum            'C24 H60 O14 Si8'
_chemical_formula_weight         797.44
_chemical_name_common            5a
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.091(3)
_cell_angle_beta                 101.413(4)
_cell_angle_gamma                96.798(4)
_cell_formula_units_Z            2
_cell_length_a                   8.6034(16)
_cell_length_b                   13.100(2)
_cell_length_c                   19.985(4)
_cell_measurement_reflns_used    8896
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.44
_cell_volume                     2118.8(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15064
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    0.307
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9273
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         10239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.046
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1129P)^2^+0.6598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1843
_reflns_number_gt                8644
_reflns_number_total             10239
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060705vsi20060804_054045.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        2118.7(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4074494