Nano Building Blocks via Iodination of [PhSiO1.5]n, Forming [p-I-C6H4SiO1.5]n (n = 8, 10, 12), and a New Route to High-Surface-Area, Thermally Stable, Microporous Materials via Thermal Elimination of I2
M. F. Roll; J. W. Kampf; Y. Kim; E. Yi; R. M. Laine; Journal of the American Chemical Society 132 (2010) 10171–10183; doi:10.1021/ja102453s

data_4102695
_publ_section_title
;
 Nano Building Blocks via Iodination of [PhSiO1.5]n, Forming
 [p-I-C6H4SiO1.5]n (n = 8, 10, 12), and a New Route to High-Surface-Area,
 Thermally Stable, Microporous Materials via Thermal Elimination of I2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10171
_journal_page_last               10183
_journal_paper_doi               10.1021/ja102453s
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C60 H50 O15 Si10, C7 H8'
_chemical_formula_sum            'C67 H58 O15 Si10'
_chemical_formula_weight         1384.03
_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                72.7060(1)
_cell_angle_beta                 80.4340(1)
_cell_angle_gamma                81.3950(1)
_cell_formula_units_Z            6
_cell_length_a                   12.5377(9)
_cell_length_b                   24.6836(17)
_cell_length_c                   35.061(2)
_cell_measurement_reflns_used    9252
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.22
_cell_volume                     10157.9(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART-APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            228543
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.9475
_exptl_absorpt_correction_T_min  0.9215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Blessing, R. Acta Cryst. (1995) A51 33-38.
  Sheldrick, G.  SADABS (Version 2008/1) Bruker AXS area
  detector absorption and other corrections, University of
  Gottingen, Germany 2008.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2636
_refine_ls_number_reflns         50482
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0486P)^2^+3.9986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                40257
_reflns_number_total             50482
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102453s_si_003.cif
_cod_data_source_block           decap
_cod_original_cell_volume        10157.8(12)
_cod_database_code               4102695