1,2-Dihalodigermenes bearing bulky Eind groups: synthesis, characterization, and conversion to halogermylenoids.
Hayakawa, Naoki; Sugahara, Tomohiro; Numata, Yasuyuki; Kawaai, Hotaka; Yamatani, Kenta; Nishimura, Shogo; Goda, Shun; Suzuki, Yuko; Tanikawa, Tomoharu; Nakai, Hidetaka; Hashizume, Daisuke; Sasamori, Takahiro; Tokitoh, Norihiro; Matsuo, Tsukasa; Dalton transactions (Cambridge, England : 2003) 47 (2018) 814–822; doi:10.1039/c7dt03819d

data_7044994
_publ_section_title
;
 1,2-Dihalodigermenes bearing bulky Eind groups: synthesis,
 characterization, and conversion to halogermylenoids.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              814
_journal_page_last               822
_journal_paper_doi               10.1039/c7dt03819d
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C64 H106 Br2 Li4 O2'
_chemical_formula_sum            'C64 H106 Br2 Li4 O2'
_chemical_formula_weight         1095.06
_chemical_name_common            (Eind)Li(THF)(LiBr)]2
_chemical_name_systematic        '(Eind)Li LiBr complex'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2017-04-11 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.486(5)
_cell_length_b                   19.226(5)
_cell_length_c                   17.324(4)
_cell_measurement_reflns_used    16172
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.57
_cell_measurement_theta_min      2.09
_cell_volume                     6490(3)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    SIR2002
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-10 with Saturn724'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            53484
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.423
_diffrn_reflns_theta_min         2.351
_diffrn_source                   'Fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    1.287
_exptl_absorpt_correction_T_max  0.689
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.521
_exptl_crystal_size_mid          0.368
_exptl_crystal_size_min          0.289
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         7388
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0762
_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^)+(0.0559P)^2^+7.8206P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1696
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5422
_reflns_number_total             7388
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03819d3.cif
_cod_data_source_block           Eind_Li_THF_LiBr2
_cod_depositor_comments
'Adding full bibliography for 7044992--7044997.cif.'
_cod_database_code               7044994
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.554
_shelx_estimated_absorpt_t_max   0.707
_shelx_res_checksum              17070