α-Cleavage of Phenyl Groups from GePh3Ligands in Iridium Carbonyl Cluster Complexes. A Mechanism and Its Role in the Synthesis of Bridging Germylene Ligands
Adams, Richard D.; Fang, Fang; Zhang, Qiang; Hall, Michael B.; Trufan, Eszter; Organometallics 31 (2012) 2621–; doi:10.1021/om2007002

data_4077847
_publ_section_title
;
 \a-Cleavage of Phenyl Groups from GePh3Ligands in Iridium Carbonyl
 Cluster Complexes. A Mechanism and Its Role in the Synthesis of Bridging
 Germylene Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2621
_journal_paper_doi               10.1021/om2007002
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C96 H65 Ge5 Ir3 O7'
_chemical_formula_weight         2270.03
_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                86.979(2)
_cell_angle_beta                 85.865(2)
_cell_angle_gamma                80.614(2)
_cell_formula_units_Z            2
_cell_length_a                   10.3576(11)
_cell_length_b                   14.9377(16)
_cell_length_c                   29.463(3)
_cell_measurement_reflns_used    6466
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.21
_cell_measurement_theta_min      2.18
_cell_volume                     4481.9(8)
_computing_cell_refinement       'SAINT+  V6.45 (Bruker, 2003)'
_computing_data_collection       'SMART V5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT+  V6.45'
_computing_molecular_graphics    'SHELXTL V6.1 (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       '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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            54507
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    6.139
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS, Bruker, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.191
_refine_diff_density_min         -2.348
_refine_diff_density_rms         0.186
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.963
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     877
_refine_ls_number_reflns         15819
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.963
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0620
_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^)+(0.1491P)^2^+43.2381P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2019
_refine_ls_wR_factor_ref         0.2206
_reflns_number_gt                12155
_reflns_number_total             15819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om2007002_si_002.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        4481.8(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4077847