1,8-Bis[3-(triethoxysilyl)propyl]-1,8-diazoniatricyclo[9.3.1.1^4,8^]hexadecane diiodide
Rousselin, Yoann; Denat, Franck; Lebeau, Benedicte; Walcarius, Alain; Acta Crystallographica Section E 65 (2009) o2531–; doi:10.1107/S1600536809038112

data_2223537
_publ_section_title
;1,8-Bis[3-(triethoxysilyl)propyl]-1,8-diazoniatricyclo[9.3.1.1^4,8^]hexadecane
 diiodide
;
_journal_coeditor_code           RK2168
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2531
_journal_paper_doi               10.1107/S1600536809038112
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C30 H66 N4 O6 Si2 2+, 2I -'
_chemical_formula_moiety         'C30 H66 N4 O6 Si2 2+, 2(I -)'
_chemical_formula_sum            'C30 H66 I2 N4 O6 Si2'
_chemical_formula_weight         888.85
_chemical_name_systematic
;1,8-Bis[3-(triethoxysilyl)propyl]-1,8-diazoniatricyclo[9.3.1.1^4,8^]hexadecane
diiodide
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.8080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.0484(2)
_cell_length_b                   8.42290(10)
_cell_length_c                   16.5921(3)
_cell_measurement_reflns_used    4978
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2058.56(5)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'WinGX    (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1993)'
_diffrn_ambient_temperature      115(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w'
_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  0.0304
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8944
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.94
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.837
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    16
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0299
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+1.6474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0714
_refine_ls_wR_factor_ref         0.0758
_reflns_number_gt                3900
_reflns_number_total             4686
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2168.cif
_cod_data_source_block           I
_cod_original_cell_volume        2058.57(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2223537
_cod_database_fobs_code          2223537