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_7044992
_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 Ge2'
_chemical_formula_sum            'C56 H90 Br2 Ge2'
_chemical_formula_weight         1068.32
_chemical_melting_point          424.0(10)
_chemical_name_common            (Eind)BrGe=GeBe(Eind)
_chemical_name_systematic        dibromodigermene
_chemical_properties_physical
', Air-sensitive,Moisture-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_update_record
;
2017-04-06 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                97.1732(10)
_cell_angle_beta                 93.3651(10)
_cell_angle_gamma                97.2483(11)
_cell_formula_units_Z            1
_cell_length_a                   10.43530(14)
_cell_length_b                   10.52080(14)
_cell_length_c                   12.12440(14)
_cell_measurement_reflns_used    35324
_cell_measurement_temperature    100
_cell_measurement_theta_max      32.79
_cell_measurement_theta_min      2.76
_cell_volume                     1306.38(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.3b (Rigaku OD, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2.1'
_computing_publication_material  'CrystalStructure 4.2.1 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      100
_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  'Rigaku XtaLAB P200'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            79445
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         3.037
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.816
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.3b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             560.00
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.112
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.51
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     279
_refine_ls_number_reflns         7611
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0290P)^2^+1.1579P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0616
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6867
_reflns_number_total             7611
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7dt03819d3.cif
_cod_data_source_block           Eind2Ge2Br2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '423-425' was changed to '424.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7044992--7044997.cif.
;
_cod_database_code               7044992
_shelxl_version_number           2013-4
_shelx_res_checksum              57946