Hybrid Dibismuthines and Distibines: Preparation and Properties of Antimony and Bismuth Oxygen, Sulfur, and Nitrogen Donor Ligands
Benjamin, Sophie L.; Karagiannidis, Louise; Levason, William; Reid, Gillian; Rogers, Michael C.; Organometallics 30 (2011) 895–; doi:10.1021/om1010148

data_4063902
_publ_section_title
;
 Hybrid Dibismuthines and Distibines: Preparation and Properties of
 Antimony and Bismuth Oxygen, Sulfur, and Nitrogen Donor Ligands
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              895
_journal_paper_doi               10.1021/om1010148
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C26 H22 Bi Fe O3 1+, B F4 1-, 0.9(C H2 Cl2)'
_chemical_formula_structural
'((CO)2 (C5 H5) (C19 H17 Bi O) Fe) (B F4) (C H2 Cl2)0.9'
_chemical_formula_sum            'C26.9 H23.8 B Bi Cl1.8 F4 Fe O3'
_chemical_formula_weight         810.51
_chemical_name_systematic
; 
 dicarbonyl(eta^5^-cyclopentadienyl)[(2-methoxyphenyl)(diphenyl)bismuthine]-
 iron(II) tetrafluoroborate dichloromethane solvate 
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_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_date             2009-12-24
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                88.091(10)
_cell_angle_beta                 66.197(10)
_cell_angle_gamma                82.102(10)
_cell_formula_units_Z            2
_cell_length_a                   10.481(2)
_cell_length_b                   12.3341(15)
_cell_length_c                   12.370(3)
_cell_measurement_reflns_used    46488
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     1448.8(5)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29158
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         3.37
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.784
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'G.M. Sheldrick, (2007). SADABS. Version 2007/2. Bruker AXS Inc.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             779.6
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.959
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         6634
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0438P)^2^+5.9024P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                5790
_reflns_number_total             6634
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om1010148_si_002.cif
_cod_data_source_block           09mcrlk11
_cod_original_cell_volume        1448.8(4)
_cod_original_formula_sum        'C26.90 H23.80 B Bi Cl1.80 F4 Fe O3'
_cod_database_code               4063902