Three-membered cyclic digermylenes stabilized by an N-heterocyclic carbene
Müller, Thomas; Dong, Zhaowen; Schmidtmann, Marc; Winkler, Jan Mathis; Chemical Science  (2021) –; doi:10.1039/D1SC00956G

data_1561177
_publ_section_title
;
 Three-membered cyclic digermylenes stabilized by an N-heterocyclic
 carbene
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D1SC00956G
_journal_year                    2021
_chemical_formula_structural
'SiC4(C6H5)2(Si(C2H5)3)2Ge2(C11H20N2)2 *0.5C7H8'
_chemical_formula_sum            'C53.5 H84 Ge2 N4 Si3'
_chemical_formula_weight         1012.69
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-01-27 deposited with the CCDC.	2021-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                92.7304(15)
_cell_angle_beta                 91.3450(16)
_cell_angle_gamma                111.8890(15)
_cell_formula_units_Z            2
_cell_length_a                   11.7931(5)
_cell_length_b                   14.4290(6)
_cell_length_c                   17.6548(6)
_cell_measurement_reflns_used    9831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.48
_cell_measurement_theta_min      2.23
_cell_volume                     2781.69(19)
_computing_cell_refinement       'Bruker SAINT V8.37A'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT V8.37A'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013/1 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0467
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            119718
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.031
_diffrn_reflns_theta_min         1.524
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.182
_exptl_absorpt_correction_T_max  0.9272
_exptl_absorpt_correction_T_min  0.7849
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS-2016/2 (Sheldrick)'
_exptl_crystal_colour            'metallic green red'
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             1078
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.080
_refine_diff_density_max         1.543
_refine_diff_density_min         -0.769
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     602
_refine_ls_number_reflns         19379
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+1.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0870
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14851
_reflns_number_total             19379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00956g3.cif
_cod_data_source_block           dzw130
_cod_original_formula_sum        'C53.50 H84 Ge2 N4 Si3'
_cod_database_code               1561177
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.911
_exptl_absorpt_special_details
;
 numerical absorption correction followed by correction based on
 symmetry-related measurements (multi-scan)
;
_shelx_res_checksum              82938
_shelx_hkl_checksum              29495