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_4083251
_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            'C42.25 H30.5 Bi Cl0.5 Ge3 Ir3 O6'
_chemical_formula_weight         1655.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 98.623(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   33.584(17)
_cell_length_b                   14.609(6)
_cell_length_c                   37.282(16)
_cell_measurement_reflns_used    9287
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      26.40
_cell_measurement_theta_min      2.18
_cell_volume                     18085(14)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.1659
_diffrn_reflns_av_sigmaI/netI    0.0848
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            104130
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.10
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    14.712
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.375256
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            RED
_exptl_crystal_density_diffrn    2.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             12008
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.066
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     967
_refine_ls_number_reflns         15920
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0453P)^2^+355.6757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1345
_refine_ls_wR_factor_ref         0.1665
_reflns_number_gt                8714
_reflns_number_total             15920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300813t_si_001.cif
_cod_data_source_block           compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        18084(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C42.25 H30.50 Bi Cl0.50 Ge3 Ir3 O6'
_cod_database_code               4083251