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_7132450
_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         '2(C28 H36 Cl2 N4 Sn), C4 H4 O, 2(C4 H8 O)'
_chemical_formula_sum            'C68 H92 Cl4 N8 O3 Sn2'
_chemical_formula_weight         1448.72
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2023-10-16 deposited with the CCDC.	2023-12-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.162(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.096(2)
_cell_length_b                   12.7331(8)
_cell_length_c                   18.1401(11)
_cell_measurement_reflns_used    9327
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.6966
_cell_measurement_theta_min      2.6270
_cell_volume                     7163.6(8)
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-201n (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon CMOS'
_diffrn_measurement_method       'phi- and omega-rotation'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'microfocus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            175354
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.895
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6200
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2, Bruker, 2016'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2992
_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.231
_refine_diff_density_max         0.427
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.367(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         13617
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0167
_refine_ls_R_factor_gt           0.0166
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'W=1/[\S^2^(FO^2^)+(0.0204P)^2^+4.7665P] WHERE P=(FO^2^+2FC^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.0438
_reflns_number_gt                13537
_reflns_number_total             13617
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            d3cc05090d2.cif
_cod_data_source_block           mo_eiste23_3_0m
_cod_depositor_comments
'Adding full bibliography for 7132449--7132451.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7132450
_publcif_datablock.id            {76fee9de-4176-4fd9-b8e7-8627a1549c8d}
_shelx_res_checksum              25186
_shelx_hkl_checksum              34357
_publcif_funding_html
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;