Organobismuth(III) and Dibismuthine Complexes Bearing N,N′-Disubstituted 1,8-Diaminonaphthalene Ligand: Synthesis, Structure, and Reactivity
Nekoueishahraki, Bijan; Samuel, Prinson P.; Roesky, Herbert W.; Stern, Daniel; Matussek, Julia; Stalke, Dietmar; Organometallics 31 (2012) 6697–; doi:10.1021/om300758s

data_4079475
_publ_section_title
;
 Organobismuth(III) and Dibismuthine Complexes Bearing
 N,N&#x2032;-Disubstituted 1,8-Diaminonaphthalene Ligand: Synthesis,
 Structure, and Reactivity
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              6697
_journal_paper_doi               10.1021/om300758s
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C32 H48 Bi2 N4 S Si4'
_chemical_formula_sum            'C32 H48 Bi2 N4 S Si4'
_chemical_formula_weight         1051.12
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   '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                 114.8660(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.3481(14)
_cell_length_b                   12.9325(8)
_cell_length_c                   27.2352(16)
_cell_measurement_reflns_used    9135
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.754
_cell_measurement_theta_min      2.184
_cell_volume                     7780.8(8)
_computing_cell_refinement       'SAINT V7.46A (Bruker, 2008)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2008)'
_computing_data_reduction        'SAINT V7.46A (Bruker, 2008)'
_computing_molecular_graphics    'XSHELL v4.01 (Bruker, 2000)'
_computing_publication_material  'XSHELL v4.01 (Bruker, 2000)'
_computing_structure_refinement  'XL in SHELXTL v2008/2(Sheldrick, 2008)'
_computing_structure_solution    'XS in SHELXTL v2008/2(Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker TXS rotating Anode'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Helios multilayer mirror optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            109915
_diffrn_reflns_theta_full        26.76
_diffrn_reflns_theta_max         26.76
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    9.238
_exptl_absorpt_correction_T_max  0.5761
_exptl_absorpt_correction_T_min  0.4350
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/2 (Sheldrick, 2008)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.549
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         16556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0228
_refine_ls_R_factor_gt           0.0170
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0112P)^2^+8.4983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0331
_refine_ls_wR_factor_ref         0.0344
_reflns_number_gt                14660
_reflns_number_total             16556
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300758s_si_002.cif
_cod_data_source_block           9
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4079475