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_4102694
_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         'C72 H48 I12 O18 Si12, 4(C8 H10)'
_chemical_formula_sum            'C104 H88 I12 O18 Si12'
_chemical_formula_weight         3485.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.438(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.082(9)
_cell_length_b                   14.704(4)
_cell_length_c                   28.755(8)
_cell_measurement_reflns_used    9454
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      29.58
_cell_measurement_theta_min      2.42
_cell_volume                     11928(6)
_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  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0202
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            173661
_diffrn_reflns_theta_full        29.67
_diffrn_reflns_theta_max         29.67
_diffrn_reflns_theta_min         1.44
_exptl_absorpt_coefficient_mu    3.297
_exptl_absorpt_correction_T_max  0.4379
_exptl_absorpt_correction_T_min  0.3248
_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    1.941
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6640
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.30
_refine_diff_density_max         4.370
_refine_diff_density_min         -4.306
_refine_diff_density_rms         0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         16839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1457P)^2^+5.4809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2732
_refine_ls_wR_factor_ref         0.2885
_reflns_number_gt                13867
_reflns_number_total             16839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102453s_si_002.cif
_cod_data_source_block           12i5a
_cod_original_cell_volume        11928(5)
_cod_database_code               4102694