Synthesis and Characterizations of Bismuth-Bridged Triiridium Carbonyl Complexes Containing Germyl/Germylene and Stannyl/Stannylene Ligands
Adams, Richard D.; Chen, Mingwei; Elpitiya, Gaya; Zhang, Qiang; Organometallics 31 (2012) 7264–; doi:10.1021/om300813t

data_4083253
_publ_section_title
;
 Synthesis and Characterizations of Bismuth-Bridged Triiridium Carbonyl
 Complexes Containing Germyl/Germylene and Stannyl/Stannylene Ligands
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              7264
_journal_paper_doi               10.1021/om300813t
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C14 H10 Bi0.33 Ir O2 Sn'
_chemical_formula_weight         590.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           159
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   12.4372(3)
_cell_length_b                   12.4372(3)
_cell_length_c                   38.7624(19)
_cell_measurement_reflns_used    8062
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.22
_cell_measurement_theta_min      2.16
_cell_volume                     5192.6(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0853
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            62262
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.05
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    12.489
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.569883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    2.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_platon_squeeze_details
'The unit cell contain solvent molecules(Total Potential Solvent Accessible Void Vol is 1020.0 Ang^3 and Electron Count/Cell is 373) which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON.'
_refine_diff_density_max         0.821
_refine_diff_density_min         -1.776
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         6166
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0450
_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^)+(0.0540P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1055
_refine_ls_wR_factor_ref         0.1095
_reflns_number_gt                5411
_reflns_number_total             6166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300813t_si_001.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P31c
_cod_database_code               4083253