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_7044995
_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 Cl2 Ge2'
_chemical_formula_sum            'C56 H90 Cl2 Ge2'
_chemical_formula_weight         979.35
_chemical_melting_point          405(2)
_chemical_name_common            (Eind)ClGe=GeCl(Eind)
_chemical_name_systematic        dichlorodigermene
_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_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-06 deposited with the CCDC.
2017-12-08 downloaded from the CCDC.
;
_cell_angle_alpha                97.829(2)
_cell_angle_beta                 93.325(2)
_cell_angle_gamma                97.830(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4792(3)
_cell_length_b                   10.5003(2)
_cell_length_c                   12.0496(3)
_cell_measurement_reflns_used    12419
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.5060
_cell_measurement_theta_min      3.6940
_cell_volume                     1297.30(6)
_computing_cell_refinement       CrysAlisPro
_computing_data_collection       CrysAlisPro
_computing_data_reduction        CrysAlisPro
_computing_molecular_graphics    SHELXLE
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR2011
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.811
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_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  0.0433
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_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       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            30745
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         3.657
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Empirical
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_description       Plate
_exptl_crystal_F_000             524
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.063
_refine_diff_density_max         0.953
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         7495
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0275P)^2^+1.6289P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1003
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6614
_reflns_number_total             7495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03819d3.cif
_cod_data_source_block           Eind2Ge2Cl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '403-407' was changed to '405(2)' -
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               7044995
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              62088