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_4130891
_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         'C62 H94 Ge N2 Si2, C9 H12'
_chemical_formula_sum            'C71 H106 Ge N2 Si2'
_chemical_formula_weight         1116.34
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
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_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   37.7343(15)
_cell_length_b                   37.7343(15)
_cell_length_c                   25.323(3)
_cell_measurement_reflns_used    9623
_cell_measurement_temperature    122(2)
_cell_measurement_theta_max      23.06
_cell_measurement_theta_min      2.30
_cell_volume                     31226(4)
_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      122(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  0.0592
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            134431
_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         27.150
_diffrn_reflns_theta_min         1.017
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.069
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             10908
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.277
_exptl_crystal_size_min          0.172
_platon_squeeze_details
;
;
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         15353
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+26.1825P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1275
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_reflns_number_gt                10927
_reflns_number_total             15353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07815_si_001.cif
_cod_data_source_block           sh3676aa
_cod_database_code               4130891
_shelx_estimated_absorpt_t_min   0.848
_shelx_estimated_absorpt_t_max   0.917
_shelxl_version_number           2014/6
_shelx_res_checksum              93093