Regiodiscriminating Reactivity of Isolable NHC-Coordinated Disilenyl Germylene and Its Cyclic Isomer.
Nieder, David; Huch, Volker; Yildiz, Cem B.; Scheschkewitz, David; Journal of the American Chemical Society 138 (2016) 13996–14005; doi:10.1021/jacs.6b07815

data_4130895
_publ_section_title
;
 Regiodiscriminating Reactivity of Isolable NHC-Coordinated Disilenyl
 Germylene and Its Cyclic Isomer.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13996
_journal_page_last               14005
_journal_paper_doi               10.1021/jacs.6b07815
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety         'C71 H103 Ge N3 Si2, 0.5(C7 H8)'
_chemical_formula_sum            'C74.5 H107 Ge N3 Si2'
_chemical_formula_weight         1173.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 94.490(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7844(8)
_cell_length_b                   22.7467(13)
_cell_length_c                   23.4180(11)
_cell_measurement_reflns_used    7372
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      24.47
_cell_measurement_theta_min      2.60
_cell_volume                     6789.1(7)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0829
_diffrn_reflns_av_unetI/netI     0.1008
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            50088
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.431
_diffrn_reflns_theta_min         1.250
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6187
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_description       needle
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.927
_exptl_crystal_size_mid          0.066
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     771
_refine_ls_number_reflns         13888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0523
_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^)+(0.0414P)^2^+0.4642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8922
_reflns_number_total             13888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07815_si_001.cif
_cod_data_source_block           sh3579
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C74.50 H107 Ge N3 Si2'
_cod_database_code               4130895
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2014/6
_shelx_res_checksum              63801