A stable free tetragermacyclobutadiene incorporating fused-ring bulky EMind groups.
Suzuki, Katsunori; Numata, Yasuyuki; Fujita, Naoko; Hayakawa, Naoki; Tanikawa, Tomoharu; Hashizume, Daisuke; Tamao, Kohei; Fueno, Hiroyuki; Tanaka, Kazuyoshi; Matsuo, Tsukasa; Chemical communications (Cambridge, England) 54 (2018) 2200–2203; doi:10.1039/c7cc09443d

data_7121143
_publ_section_title
;
 A stable free tetragermacyclobutadiene incorporating fused-ring bulky
 EMind groups.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2200
_journal_page_last               2203
_journal_paper_doi               10.1039/c7cc09443d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C48 H74 Cl2 Ge2'
_chemical_formula_sum            'C48 H74 Cl2 Ge2'
_chemical_formula_weight         867.15
_chemical_name_common            (EMind)ClGe=GeCl(EMind)
_chemical_name_systematic        dichlorodigermene
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive
_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-2017/1
_audit_update_record
;
2017-10-19 deposited with the CCDC.
2018-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                118.544(4)
_cell_angle_beta                 92.150(3)
_cell_angle_gamma                113.282(3)
_cell_formula_units_Z            1
_cell_length_a                   10.9924(4)
_cell_length_b                   11.3428(4)
_cell_length_c                   11.8084(5)
_cell_measurement_reflns_used    8311
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9590
_cell_measurement_theta_min      3.7020
_cell_volume                     1140.33(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    SIR2008
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18211
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         3.626
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78275
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       Block
_exptl_crystal_F_000             460
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: THF and pentane'
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.111
_refine_diff_density_max         0.783
_refine_diff_density_min         -0.468
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         5213
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0293P)^2^+2.1871P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4378
_reflns_number_total             5213
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc09443d2.cif
_cod_data_source_block           EMind2Ge2Cl2
_cod_depositor_comments
'Adding full bibliography for 7121142--7121143.cif.'
_cod_original_cell_volume        1140.33(9)
_cod_database_code               7121143
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.774
_shelx_estimated_absorpt_t_max   0.854
_shelx_res_checksum              3081