Naked Deltahedral Silicon Clusters in Solution: Synthesis and Characterization of Si93- and Si52-
Jose M. Goicoechea; Slavi C. Sevov; Journal of the American Chemical Society 126 (2004) 6860–6861; doi:10.1021/ja0488075

data_4112631
_publ_section_title
;
 Naked Deltahedral Silicon Clusters in Solution: Synthesis and
 Characterization of Si93- and Si52-
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6860
_journal_page_last               6861
_journal_paper_doi               10.1021/ja0488075
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C54 H108 K3 N15 O18 Si9'
_chemical_formula_weight         1625.66
_chemical_name_systematic
; 
 [K-(2,2,2-crypt)]3(Si9)*8(NH3)
;
_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                80.518(4)
_cell_angle_beta                 84.853(4)
_cell_angle_gamma                66.374(4)
_cell_formula_units_Z            2
_cell_length_a                   14.077(4)
_cell_length_b                   15.061(4)
_cell_length_c                   22.746(6)
_cell_measurement_temperature    100(2)
_cell_volume                     4356(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL-V5.1'
_computing_molecular_graphics    'Bruker SHELXTL-V5.1'
_computing_publication_material  'Bruker SHELXTL-V5.1'
_computing_structure_refinement  'Bruker SHELXTL-V5.1'
_computing_structure_solution    'Bruker SHELXTL-V5.1'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0757
_diffrn_reflns_av_sigmaI/netI    0.1057
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37105
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.92
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.7125
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-orange
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.829
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.308
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         15210
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.308
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.0791
_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^)+(0.0419P)^2^+4.6490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1782
_reflns_number_gt                9342
_reflns_number_total             15210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0488075si20040414_051604_1.cif
_cod_data_source_block           '[K-(2,2,2-crypt)]3(Si9)*8(NH3)'
_cod_original_cell_volume        4356.4(19)
_cod_database_code               4112631