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_1561548
_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         'C40 H83 B Ge9 K N3 Si8, C7 H8'
_chemical_formula_sum            'C47 H91 B Ge9 K N3 Si8'
_chemical_formula_weight         1626.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 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                90.000(3)
_cell_angle_beta                 94.438(3)
_cell_angle_gamma                90.000(2)
_cell_formula_units_Z            2
_cell_length_a                   13.7573(4)
_cell_length_b                   9.2613(3)
_cell_length_c                   28.4239(10)
_cell_measurement_reflns_used    135436
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.00
_cell_measurement_theta_min      2.52
_cell_volume                     3610.6(2)
_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  0.0405
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            78148
_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         25.996
_diffrn_reflns_theta_min         2.522
_diffrn_source                   'Genix 3D HF Mo'
_exptl_absorpt_coefficient_mu    3.911
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'STOE X-AREA 1.76'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       needle
_exptl_crystal_F_000             1636
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 5870 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         14199
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+1.8949P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.879
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                13310
_reflns_number_total             14199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00811k2.cif
_cod_data_source_block           FSG-1196
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               1561548
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              52424
_shelx_hkl_checksum              70388