FLP-type Nitrile Activation and Cyclic Ether Ring Opening by Halo-Borane Nonagermanide-Cluster Lewis Acid-Base-Pairs
Wallach, Chistoph; Geitner, Felix; Fässler, Thomas F; Chemical Science  (2021) –; doi:10.1039/D1SC00811K

data_1561547
_publ_section_title
;
 FLP-type Nitrile Activation and Cyclic Ether Ring Opening by Halo-Borane
 Nonagermanide-Cluster Lewis Acid-Base-Pairs
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC00811K
_journal_year                    2021
_chemical_formula_moiety         'C42 H88 B Ge9 K N2 O Si8, 1.5(C7 H8)'
_chemical_formula_sum            'C52.5 H100 B Ge9 K N2 O Si8'
_chemical_formula_weight         1703.28
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-03-31 deposited with the CCDC.	2021-04-03 downloaded from the CCDC.
;
_cell_angle_alpha                65.966(3)
_cell_angle_beta                 67.528(4)
_cell_angle_gamma                88.951(3)
_cell_formula_units_Z            2
_cell_length_a                   14.7094(7)
_cell_length_b                   16.9327(6)
_cell_length_c                   18.7377(9)
_cell_measurement_reflns_used    187049
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.02
_cell_measurement_theta_min      2.62
_cell_volume                     3886.2(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            74106
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.670
_diffrn_source                   'Genix 3D HF Mo'
_exptl_absorpt_coefficient_mu    3.638
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_description       block
_exptl_crystal_F_000             1722
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.445
_refine_diff_density_min         -1.265
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     682
_refine_ls_number_reflns         15237
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0265P)^2^+18.8354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0880
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                10831
_reflns_number_total             15237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00811k2.cif
_cod_data_source_block           FSG-1131
_cod_original_formula_sum        'C52.50 H100 B Ge9 K N2 O Si8'
_cod_database_code               1561547
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              58632
_shelx_hkl_checksum              56203