Synthesis and isolation of a cyclic bis-vinyl germylene <i>via</i> a diazoolefin adduct of germylene dichloride.
Eisner, Teresa; Kostenko, Arseni; J Kiefer, Fiona; Inoue, Shigeyoshi; Chemical communications (Cambridge, England) 60 (2024) 558–561; doi:10.1039/d3cc05090d

data_7132451
_publ_section_title
;
 Synthesis and isolation of a cyclic bis-vinyl germylene <i>via</i> a
 diazoolefin adduct of germylene dichloride.
;
_journal_issue                   5
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              558
_journal_page_last               561
_journal_paper_doi               10.1039/d3cc05090d
_journal_volume                  60
_journal_year                    2024
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C56 H72 Ge N6'
_chemical_formula_sum            'C56 H72 Ge N6'
_chemical_formula_weight         901.78
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.047(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   39.420(2)
_cell_length_b                   12.4890(8)
_cell_length_c                   22.5821(13)
_cell_measurement_reflns_used    9253
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.36
_cell_volume                     10375.8(11)
_computing_cell_refinement       'SAINT (Bruker, 2017)'
_computing_data_collection       'APEX 4 Control Software (Bruker, 2021)'
_computing_data_reduction        'SAINT (Bruker, 2017)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2014)'
_computing_structure_refinement
'SHELXL (Sheldrick, 2017), SHELXLE (Huebschle, 2011)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 ' CMOS plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker Photon CMOS '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  'Helios optic'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'IMS microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            239774
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.78
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            'clear yellowish orange'
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3856
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.275
_exptl_crystal_size_min          0.188
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.785
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     584
_refine_ls_number_reflns         9922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0374P)^2^+18.3191P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                8872
_reflns_number_total             9922
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d3cc05090d2.cif
_cod_data_source_block           mo_eiste24_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7132449--7132451.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7132451
_shelx_res_checksum              60037
_shelx_hkl_checksum              5633