O,N-HETEROCYCLIC GERMYLENES AS EFFICIENT CATALYSTS FOR HYDROBORATION AND CYANOSILYLATION OF BENZALDEHYDE
Arsenyeva, Kseniya Vital'evna; Pashanova, Kira Igorevna; Trofimova, Olesya Yur'evna; Ershova, Irina V.; Chegerev, Maxim G.; Starikova, Alyona A.; Cherkasov, Anton Vladimirovich; Syroeshkin, Mikhail A.; Kozmenkova, Anna Ya.; Piskunov, Alexandr Vladimirovich; New Journal of Chemistry 45 (2021) 11758–11767; doi:10.1039/D1NJ01644J

data_7060725
_publ_section_title
;
 O,N-HETEROCYCLIC GERMYLENES AS EFFICIENT CATALYSTS FOR HYDROBORATION AND
 CYANOSILYLATION OF BENZALDEHYDE
;
_journal_issue                   26
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11758
_journal_page_last               11767
_journal_paper_doi               10.1039/D1NJ01644J
_journal_volume                  45
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H35 Ge N O'
_chemical_formula_sum            'C24 H35 Ge N O'
_chemical_formula_weight         426.12
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-03-31 deposited with the CCDC.	2021-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.2660(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4557(3)
_cell_length_b                   15.3711(4)
_cell_length_c                   13.4947(3)
_cell_measurement_reflns_used    9185
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.00
_cell_measurement_theta_min      2.65
_cell_volume                     2167.11(10)
_computing_cell_refinement       'Saint 8.38a'
_computing_data_collection       APEX3
_computing_data_reduction        'Saint 8.38a'
_computing_structure_refinement  'SHELXL 2018/3'
_computing_structure_solution    'SHELXT 2018/2'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 Quest (CMOS)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21207
_diffrn_reflns_point_group_measured_fraction_full 0.817
_diffrn_reflns_point_group_measured_fraction_max 0.818
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.052
_diffrn_reflns_theta_min         1.949
_diffrn_source                   'microfocus tube'
_exptl_absorpt_coefficient_mu    1.427
_exptl_absorpt_correction_T_max  0.639
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       prism
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.530
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.340
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.915
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.472(7)
_refine_ls_extinction_coef       0.0029(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         10388
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0386P)^2^+0.5066P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0701
_refine_ls_wR_factor_ref         0.0709
_reflns_Friedel_coverage         0.586
_reflns_Friedel_fraction_full    0.621
_reflns_Friedel_fraction_max     0.626
_reflns_number_gt                10100
_reflns_number_total             10388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj01644j2.cif
_cod_data_source_block           geapad
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7060725
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.518
_shelx_estimated_absorpt_t_max   0.643
_shelx_res_checksum              25329