Carbene Stabilized Interconnected Bis-germylene and its Silicon Analogue with Small Methyl Substituents
Roesky, Herbert W.; Kundu, Subrata; Samuel, Prinson P.; Luebben, Anna; Andrada, Diego Marcelo; Frenking, G.; Dittrich, Birger; Dalton Trans.  (2017) –; doi:10.1039/C7DT01796K

data_7043141
_publ_section_title
;
 Carbene Stabilized Interconnected Bis-germylene and its Silicon Analogue
 with Small Methyl Substituents
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01796K
_journal_year                    2017
_chemical_formula_moiety         'C42 H68 N2 Si2'
_chemical_formula_sum            'C42 H68 N2 Si2'
_chemical_formula_weight         657.16
_chemical_name_common            'carbene stabilized bissilylene'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2017-02-21 deposited with the CCDC.
2017-05-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   39.475(17)
_cell_length_b                   39.475(17)
_cell_length_c                   10.222(8)
_cell_measurement_reflns_used    98804
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      0.949
_cell_volume                     15929(16)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'SHELXLE (Huebschle, 2011)'
_computing_publication_material  'enCIFer 1.5.1, CCDC, 2015'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Microdiffractometer at the SLS'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6538
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0228
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       -56
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            218622
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        23.096
_diffrn_reflns_theta_max         27.848
_diffrn_reflns_theta_min         0.949
_diffrn_source                   'monochromated X-rays beamline X10SA@SLS'
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6745
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS version 2016/1, multi-scan. (G. M. Sheldrick, 2016)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.096
_exptl_crystal_description       plate
_exptl_crystal_F_000             5792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: n-hexane'
_exptl_crystal_size_max          0.024
_exptl_crystal_size_mid          0.016
_exptl_crystal_size_min          0.011
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         12048
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0484P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1124
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10377
_reflns_number_total             12048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01796k2.cif
_cod_data_source_block           skr200
_cod_depositor_comments
;

2018-03-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        15928(18)
_cod_original_formula_moiety     'C84 H136 N4 Si4'
_cod_original_formula_sum        'C84 H136 N4 Si4'
_cod_original_formula_units_Z    8
_cod_original_formula_weight     1314.32
_cod_database_code               7043141
_shelxl_version_number           2014/6
_shelx_res_checksum              67355