Facile activation of alkynes with a boraguanidinato-stabilized germylene: a combined experimental and theoretical study
Böserle, Jiří; Zhigulin, Grigory; Štěpnička, Petr; Horký, Filip; Erben, Milan; Jambor, Roman; R°užička, Aleš; Ketkov, Sergey; Dostál, Libor; Dalton Transactions 46 (2017) 12339–12353; doi:10.1039/C7DT01950E

data_1546891
_publ_section_title
;
 Facile activation of alkynes with a boraguanidinato-stabilized germylene:
 a combined experimental and theoretical study
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              12339
_journal_page_last               12353
_journal_paper_doi               10.1039/C7DT01950E
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C60 H74 B2 Ge2 N6, 0.5(C6 H14)'
_chemical_formula_sum            'C63 H81 B2 Ge2 N6'
_chemical_formula_weight         1089.13
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-02-17 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.060(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.5261(14)
_cell_length_b                   13.2680(15)
_cell_length_c                   21.209(2)
_cell_measurement_reflns_used    50414
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      1
_cell_volume                     5874.8(10)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0759
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50365
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         1.819
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.067
_exptl_absorpt_correction_T_max  0.878
_exptl_absorpt_correction_T_min  0.762
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
Gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12445
_refine_ls_number_restraints     633
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0138P)^2^+11.6022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.1018
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8543
_reflns_number_total             12445
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01950e5.cif
_cod_data_source_block           3a
_cod_database_code               1546891