A convenient route to anionic and cyclic aluminosiloxanes: crystal structures of [PyH][Al{OSiPh2(OSiPh2)2O}2] and the first twelve-membered organic aluminosilicate Al2Si4O6 ring
Gun'ko, Yurii K.; Reilly, Roisin; Kessler, Vadim G.; New Journal of Chemistry 25 (2001) 528–530; doi:10.1039/b009556g

data_7052515
_publ_section_title
;
 A convenient route to anionic and cyclic aluminosiloxanes: crystal
 structures of [PyH][&#xE010;Al{OSiPh2(OSiPh2)2O&#xE011;}2] and the first
 twelve-membered organic aluminosilicate Al2Si4O6 ring
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              528
_journal_page_last               530
_journal_paper_doi               10.1039/b009556g
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C77 H66 Al N O8 Si6'
_chemical_formula_weight         1328.83
_chemical_name_systematic        ?
_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                93.716(2)
_cell_angle_beta                 93.872(2)
_cell_angle_gamma                107.226(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8800(9)
_cell_length_b                   15.0636(12)
_cell_length_c                   20.7172(17)
_cell_measurement_reflns_used    999(I>10sigma(I))
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      1.42
_cell_volume                     3519.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINTPLUS'
_computing_molecular_graphics    'Bruker SHELXTL-NT'
_computing_publication_material  'Bruker SHELXTL-NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'SMART CCD 1K'
_diffrn_measurement_method       'Bruker SMART'
_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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0856
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14160
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_type   'not applied'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.925
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         9181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.925
_refine_ls_R_factor_all          0.1150
_refine_ls_R_factor_gt           0.0540
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0651P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1284
_reflns_number_gt                5292
_reflns_number_total             9181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009556g.txt
_cod_data_source_block           alsi11m
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               7052515