Synthesis and Characterization of a 1,2-Digermabenzene
Sasamori, Takahiro; Sugahara, Tomohiro; Agou, Tomohiro; Guo, Jing-Dong; Nagase, Shigeru; Streubel, Rainer; Tokitoh, Norihiro; Organometallics 34 (2015) 2106–; doi:10.1021/om501204u

data_4085307
_publ_section_title
;
 Synthesis and Characterization of a 1,2-Digermabenzene
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2106
_journal_paper_doi               10.1021/om501204u
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C48 H98 Br2 Ge2 Si8, C6 H6'
_chemical_formula_sum            'C54 H104 Br2 Ge2 Si8'
_chemical_formula_weight         1283.09
_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-97
_cell_angle_alpha                82.3768(19)
_cell_angle_beta                 86.935(2)
_cell_angle_gamma                75.4857(13)
_cell_formula_units_Z            2
_cell_length_a                   9.5903(2)
_cell_length_b                   12.1744(3)
_cell_length_c                   30.5707(9)
_cell_measurement_reflns_used    7744
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      30.2795
_cell_measurement_theta_min      1.7877
_cell_volume                     3424.10(15)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics
;
Yadokari-XG 2011 (Wakita, Nemoto et al., 2011)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR2004
_diffrn_ambient_temperature      103(2)
_diffrn_detector_area_resol_mean 14.7059
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0530
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            27891
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    2.215
_exptl_absorpt_correction_T_max  0.6783
_exptl_absorpt_correction_T_min  0.6534
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
MULABS - Empirical Correction for Absorption Anisotropy.
Blessing, R. H., Acta Crystallogr. 1995, A51, 33-38.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.841
_refine_diff_density_min         -1.098
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^2^+3.9609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1256
_reflns_number_gt                8726
_reflns_number_total             11871
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501204u_si_002.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 4085307--4085309.cif.'
_cod_database_code               4085307