Bis(chlorogermyliumylidene) and its significant role in elusive reductive cyclization.
Majumdar, Moumita; Raut, Ravindra K.; Sahoo, Padmini; Kumar, Vikas; Chemical communications (Cambridge, England) 54 (2018) 10839–10842; doi:10.1039/c8cc06067c

data_7122274
_publ_section_title
;
 Bis(chlorogermyliumylidene) and its significant role in elusive reductive
 cyclization.
;
_journal_issue                   77
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              10839
_journal_page_last               10842
_journal_paper_doi               10.1039/c8cc06067c
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C16 H18 Cl2 Ge2 N4, C F3 O3 S, C F3 O3 S'
_chemical_formula_sum            'C18 H18 Cl2 F6 Ge2 N4 O6 S2'
_chemical_formula_weight         780.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-05-21 deposited with the CCDC.
2018-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                64.284(4)
_cell_angle_beta                 80.304(4)
_cell_angle_gamma                73.576(4)
_cell_formula_units_Z            2
_cell_length_a                   8.3092(11)
_cell_length_b                   13.8633(19)
_cell_length_c                   13.8680(19)
_cell_measurement_reflns_used    9782
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.81
_cell_measurement_theta_min      3.54
_cell_volume                     1378.6(3)
_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 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'CMOS-Photon 100'
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            14028
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.798
_diffrn_reflns_theta_min         3.542
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.664
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS;Universitat Gottingen,1997'
_exptl_crystal_colour            Pale-yellow
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0606P)^2^+2.7129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1117
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4776
_reflns_number_total             5238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc06067c2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7122274--7122277.cif.'
_cod_database_code               7122274
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              793