Hexakis(adamantyltrimethylammonium) cyclooctasilicate tetratetracontahydrate
Verlooy, Pieter L. H.; Robeyns, Koen; Van Meervelt, Luc; Kirschhock, Christine E. A.; Martens, Johan A.; Acta Crystallographica Section C 66 (2010) o619–o622; doi:10.1107/S0108270110044549

data_2017896
_publ_section_title
;
 Hexakis(adamantyltrimethylammonium) cyclooctasilicate
 tetratetracontahydrate
;
_journal_coeditor_code           SF3136
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o619
_journal_page_last               o622
_journal_paper_doi               10.1107/S0108270110044549
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '6C13 H24 N + , H2 O20 Si8 6- , 44H2 O'
_chemical_formula_moiety         '6(C13 H24 N +), H2 O20 Si8 6-, 44(H2 O)'
_chemical_formula_sum            'C78 H234 N6 O64 Si8'
_chemical_formula_weight         2505.44
_chemical_name_systematic
;
Hexakis(adamantyltrimethylammonium) cyclooctasilicate
tetratetracontahydrate
;
_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           SHELXL97
_cell_angle_alpha                60.863(2)
_cell_angle_beta                 72.511(3)
_cell_angle_gamma                82.119(2)
_cell_formula_units_Z            1
_cell_length_a                   15.5889(8)
_cell_length_b                   15.9297(8)
_cell_length_c                   16.2269(11)
_cell_measurement_temperature    100(2)
_cell_volume                     3356.8(3)
_computing_cell_refinement       'SAINT (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SAINT (Bruker, 1997)'
_computing_molecular_graphics    'PLUTON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  'crossed Goebel mirrors'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0277
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66631
_diffrn_reflns_theta_full        67.70
_diffrn_reflns_theta_max         71.23
_diffrn_reflns_theta_min         2.97
_exptl_absorpt_coefficient_mu    1.532
_exptl_absorpt_correction_T_max  0.858
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.692
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         12596
_refine_ls_number_restraints     399
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.1073P)^2^+3.7976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                10388
_reflns_number_total             12596
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sf3136.cif
_cod_data_source_block           I
_cod_database_code               2017896
_cod_database_fobs_code          2017896