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_4133737
_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 H106 B N Si5'
_chemical_formula_sum            'C66 H106 B N Si5'
_chemical_formula_weight         1064.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                98.387(2)
_cell_angle_beta                 92.938(2)
_cell_angle_gamma                106.305(2)
_cell_formula_units_Z            2
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_cell_length_b                   13.5798(6)
_cell_length_c                   18.9871(8)
_cell_measurement_reflns_used    9672
_cell_measurement_temperature    132(2)
_cell_measurement_theta_max      30.76
_cell_measurement_theta_min      2.47
_cell_volume                     3289.7(3)
_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      132(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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  0.0277
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            76421
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.988
_diffrn_reflns_theta_min         1.089
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7190
_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            orange
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.652
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.228
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1082
_refine_ls_number_reflns         20730
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.8406P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0889
_refine_ls_wR_factor_ref         0.0965
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16525
_reflns_number_total             20730
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b11181_si_004.cif
_cod_data_source_block           sh4060
_cod_database_code               4133737
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              27151
_shelx_hkl_checksum              67735