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_4130894
_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         'C70 H100 Ge N2 Si2, 1.25(C5 H12)'
_chemical_formula_sum            'C76.25 H115 Ge N2 Si2'
_chemical_formula_weight         1188.47
_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   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 101.5350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6352(3)
_cell_length_b                   23.8472(6)
_cell_length_c                   25.5287(7)
_cell_measurement_reflns_used    9942
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.24
_cell_volume                     7536.8(3)
_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 0.998
_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  0.0316
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            75564
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.596
_diffrn_reflns_theta_min         1.180
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/4'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.047
_exptl_crystal_description       block
_exptl_crystal_F_000             2586
_exptl_crystal_size_max          0.517
_exptl_crystal_size_mid          0.509
_exptl_crystal_size_min          0.378
_refine_diff_density_max         1.135
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     763
_refine_ls_number_reflns         19229
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0571
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0852P)^2^+7.3593P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1777
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14641
_reflns_number_total             19229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07815_si_001.cif
_cod_data_source_block           sh3607
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4130894
_shelx_estimated_absorpt_t_min   0.791
_shelx_estimated_absorpt_t_max   0.840
_shelxl_version_number           2014/6
_shelx_res_checksum              77087