Inorganic-Salt-Free Reduction in Main-Group Chemistry: Synthesis of a Dibismuthene and a Distibene
Majhi, Paresh Kumar; Ikeda, Hideaki; Sasamori, Takahiro; Tsurugi, Hayato; Mashima, Kazushi; Tokitoh, Norihiro; Organometallics 36 (2017) 1224–; doi:10.1021/acs.organomet.7b00147

data_4089280
_publ_section_title
;
 Inorganic-Salt-Free Reduction in Main-Group Chemistry: Synthesis of a
 Dibismuthene and a Distibene
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1224
_journal_paper_doi               10.1021/acs.organomet.7b00147
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C48 H98 Sb2 Si8'
_chemical_formula_sum            'C48 H98 Sb2 Si8'
_chemical_formula_weight         1143.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.0117(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.3034(3)
_cell_length_b                   9.2632(2)
_cell_length_c                   20.9519(6)
_cell_measurement_reflns_used    44777
_cell_measurement_temperature    103(2)
_cell_measurement_theta_max      26.0
_cell_measurement_theta_min      1.45
_cell_volume                     3094.91(13)
_computing_cell_refinement       HKL2000
_computing_data_collection       CrystalClear
_computing_data_reduction        HKL2000
_computing_molecular_graphics
'Yadokari-XG 2011 (Wakita Nemoto et al., 2011)'
_computing_publication_material
'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 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44777
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.9491
_exptl_absorpt_correction_T_min  0.9018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 MULABS - Empirical Correction for Absorption Anisotropy.
 Blessing, R. H., Acta Cryst., A51, 33-38 (1995).
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         6079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+1.9881P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0614
_refine_ls_wR_factor_ref         0.0659
_reflns_number_gt                5004
_reflns_number_total             6079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00147_si_002.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        3094.91(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4089280