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_7044997
_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         'C56 H90 Br2 Ge'
_chemical_formula_sum            'C56 H90 Br2 Ge'
_chemical_formula_weight         995.68
_chemical_name_common            (Eind)2GeBr2
_chemical_name_systematic        dibromogermane
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-04-10 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.352(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6306(9)
_cell_length_b                   26.7797(16)
_cell_length_c                   18.0740(14)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.5770
_cell_measurement_theta_min      3.0260
_cell_volume                     5044.7(7)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    SIR2011
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.1967
_diffrn_reflns_av_unetI/netI     0.1486
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44270
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.757
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80918
_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            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             2112
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.111
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.047
_refine_diff_density_max         1.728
_refine_diff_density_min         -1.262
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 2182 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.033(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9587
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1166
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1808P)^2^+34.5014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2992
_refine_ls_wR_factor_ref         0.3219
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.938
_reflns_Friedel_fraction_max     0.934
_reflns_number_gt                7439
_reflns_number_total             9587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03819d3.cif
_cod_data_source_block           Eind2GeBr2
_cod_depositor_comments
'Adding full bibliography for 7044992--7044997.cif.'
_cod_database_code               7044997
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              45540