Boron and phosphorus containing heterosiliconoids: stable p- and n-doped unsaturated silicon clusters.
Heider, Yannic; Willmes, Philipp; Huch, Volker; Zimmer, Michael; Scheschkewitz, David; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b11181

data_4133735
_publ_section_title
;
 Boron and phosphorus containing heterosiliconoids: stable p- and n-doped
 unsaturated silicon clusters.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b11181
_journal_year                    2019
_chemical_formula_moiety         'C66 H119 Si7, C5 H12'
_chemical_formula_sum            'C71 H122 Si7'
_chemical_formula_weight         1172.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 113.3692(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7021(9)
_cell_length_b                   27.0801(8)
_cell_length_c                   24.4934(7)
_cell_measurement_reflns_used    9915
_cell_measurement_temperature    142(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.25
_cell_volume                     15040.4(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0930
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            133330
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.689
_diffrn_reflns_theta_min         1.171
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       block
_exptl_crystal_F_000             5168
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.494
_exptl_crystal_size_min          0.376
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1522
_refine_ls_number_reflns         42515
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+15.6048P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23475
_reflns_number_total             42515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11181_si_003.cif
_cod_data_source_block           sh4075
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4133735
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.941
_shelx_res_checksum              4220
_shelx_hkl_checksum              4829