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_4130892
_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 H93 Ge N2 Si2, 3(C7 H8)'
_chemical_formula_sum            'C83 H117 Ge N2 Si2'
_chemical_formula_weight         1271.55
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                114.148(5)
_cell_angle_beta                 112.883(5)
_cell_angle_gamma                96.575(5)
_cell_formula_units_Z            2
_cell_length_a                   15.9617(17)
_cell_length_b                   16.6009(18)
_cell_length_c                   17.9948(19)
_cell_measurement_reflns_used    9693
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.38
_cell_measurement_theta_min      2.35
_cell_volume                     3790.4(8)
_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      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
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_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            81062
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.504
_diffrn_reflns_theta_min         1.414
_exptl_absorpt_coefficient_mu    0.478
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6433
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BrukerAXS 2014'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.114
_exptl_crystal_description       block
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_exptl_crystal_size_min          0.354
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_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         22760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0848P)^2^+2.0480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
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_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           sh3540
_cod_original_cell_volume        3790.4(7)
_cod_database_code               4130892
_shelx_estimated_absorpt_t_min   0.544
_shelx_estimated_absorpt_t_max   0.849
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_shelx_res_checksum              10952