Silicon Clusters with Six and Seven Unsubstituted Vertices via a Two-step Reaction from Elemental Silicon
Schiegerl, Lorenz; Karttunen, Antti J.; Klein, Wilhelm; Fässler, Thomas F; Chemical Science  (2019) –; doi:10.1039/C9SC03324F

data_1552236
_publ_section_title
;
 Silicon Clusters with Six and Seven Unsubstituted Vertices via a Two-step
 Reaction from Elemental Silicon
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC03324F
_journal_year                    2019
_chemical_formula_moiety         'C18 H54 Si17, 2(C18 H36 K N2 O6), C6 H5 F'
_chemical_formula_sum            'C60 H131 F K2 N4 O12 Si17'
_chemical_formula_weight         1675.41
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-02-11 deposited with the CCDC.    2019-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.756(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4939(9)
_cell_length_b                   25.3561(17)
_cell_length_c                   22.6197(12)
_cell_measurement_reflns_used    37570
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.07
_cell_measurement_theta_min      1.94
_cell_volume                     9459.2(10)
_computing_cell_refinement       'STOE X-AREA 1.76'
_computing_data_collection       'STOE X-AREA 1.76'
_computing_data_reduction        'STOE X-AREA 1.76'
_computing_molecular_graphics    'DIAMOND 3.2k'
_computing_structure_refinement  SHELXL-2014/7
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.893
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.1377
_diffrn_reflns_Laue_measured_fraction_full 0.893
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60136
_diffrn_reflns_point_group_measured_fraction_full 0.893
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.708
_diffrn_source                   'Genix 3D HF Mo'
_diffrn_source_current           1.000
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.944
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_description       block
_exptl_crystal_F_000             3600
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Fluorobenzene'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.67(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1892
_refine_ls_number_reflns         24142
_refine_ls_number_restraints     422
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1880
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.894
_reflns_Friedel_fraction_max     0.882
_reflns_number_gt                12835
_reflns_number_total             24142
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc03324f2.cif
_cod_data_source_block           LSP-413
_cod_database_code               1552236
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              61318