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_4074495
_publ_section_title
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 Synthesis and Structure of Ladder Oligosilsesquioxanes:&#x00A0; Tricyclic
 Ladder Oligomethylsilsesquioxanes
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_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            5d
_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                76.599(2)
_cell_angle_beta                 78.407(2)
_cell_angle_gamma                83.239(2)
_cell_formula_units_Z            2
_cell_length_a                   8.5654(14)
_cell_length_b                   13.721(2)
_cell_length_c                   19.278(3)
_cell_measurement_reflns_used    5041
_cell_measurement_temperature    90
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.43
_cell_volume                     2153.0(6)
_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 8.333
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0324
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       11
_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       -25
_diffrn_reflns_number            27810
_diffrn_reflns_theta_full        27.93
_diffrn_reflns_theta_max         27.93
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.302
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.9618
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         10054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0309P)^2^+3.9317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                8202
_reflns_number_total             10054
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060705vsi20060804_054045.cif
_cod_data_source_block           5d
_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_sg_symbol_H-M      P-1
_cod_database_code               4074495