Synthesis and Structural Study of Organoantimony(III) and Organobismuth(III) Triflates and Cations Containing O,C,O-Pincer Type Ligands†
Dostál, Libor; Novák, Petr; Jambor, Roman; Růžička, Aleš; Císařová, Ivana; Jirásko, Robert; Holeček, Jaroslav; Organometallics 26 (2007) 2911–; doi:10.1021/om070186b

data_4083666
_publ_section_title
;
 Synthesis and Structural Study of Organoantimony(III) and
 Organobismuth(III) Triflates and Cations Containing O,C,O-Pincer Type
 Ligands&#x2020;
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2911
_journal_paper_doi               10.1021/om070186b
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         '(C17 H25 Bi1 F6 O8 S2)(C H2 Cl2)'
_chemical_formula_sum            'C19 H27 Bi Cl2 F6 O8 S2'
_chemical_formula_weight         841.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                97.763(5)
_cell_angle_beta                 111.887(4)
_cell_angle_gamma                114.022(5)
_cell_formula_units_Z            2
_cell_length_a                   10.3090(4)
_cell_length_b                   12.5560(9)
_cell_length_c                   13.5140(8)
_cell_measurement_reflns_used    21456
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     1395.10(18)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Nonius KappaCCD area detector'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1119
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21490
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    6.595
_exptl_absorpt_correction_T_max  0.596
_exptl_absorpt_correction_T_min  0.289
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             757
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.1
_refine_diff_density_max         4.553
_refine_diff_density_min         -4.312
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0869P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                5081
_reflns_number_total             6393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070186b.cif
_cod_data_source_block           LD061114Bi2
_cod_original_cell_volume        1395.10(14)
_cod_original_formula_sum        'C19 H27 Bi1 Cl2 F6 O8 S2'
_cod_database_code               4083666