Silsesquioxane Chemistry: Synthesis and Structure of the Novel Anionic Aluminosilsesquioxane [HNEt3][{Cy7Si7O9(OSiMe3)O2}2Al].C6H14 (Cy = c-C6H11)
Frank T. Edelmann; Yurii K. Gun'ko; Stephan Giessmann; Falk Olbrich; Klaus Jacob; Inorganic Chemistry 38 (1999) 210–211; doi:10.1021/ic9808100

data_4321743
_publ_contact_author
;
      Frank T. Edelmann
      Chemisches Institut 
      Otto-von-Guericke Universit\"at Magdeburg
      Universit\"atsplatz 2
      D-39106 Magdeburg
      GERMANY
;
_publ_contact_author_email       frank.edelmann@chemie.uni-magdeburg.de
_publ_contact_author_fax         '+49 391 67 12933'
_publ_contact_author_phone       '+49 391 67 18327'
_publ_section_title
;
 Silsesquioxane Chemistry: Synthesis and Structure of the Novel Anionic
 Aluminosilsesquioxane [HNEt3][{Cy7Si7O9(OSiMe3)O2}2Al].C6H14 (Cy =
 c-C6H11)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              210
_journal_page_last               211
_journal_paper_doi               10.1021/ic9808100
_journal_volume                  38
_journal_year                    1999
_chemical_formula_moiety         '[HNEt3][{(C6H11)7Si7O9(OSiMe3)O2}2Al]*C6H14'
_chemical_formula_sum            'C102 H202 Al N O24 Si16'
_chemical_formula_weight         2303.07
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.078(4)
_cell_length_b                   28.954(6)
_cell_length_c                   31.740(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      21.15
_cell_volume                     13665(6)
_computing_molecular_graphics    'SHELXTL PLUS (Siemens, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Hilger&Watts diffractometer'
_diffrn_measurement_method       '2\q/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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.1880
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            20185
_diffrn_reflns_theta_full        22.55
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.41
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 97
_diffrn_standards_interval_time  'not applied'
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_correction_T_min  0.9790
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5000
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       'not applied'
_refine_ls_extinction_method     'not applied'
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1362
_refine_ls_number_reflns         17926
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1949
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2018
_refine_ls_wR_factor_ref         0.2599
_reflns_number_gt                8611
_reflns_number_total             17926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9808100.cif
_cod_data_source_block           IURI
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1201P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4321743