Rearrangement of Iridabenzvalenes to Iridabenzenes and/or η5-Cyclopentadienyliridium(I) Complexes: Experimental and Computational Analysis of the Influence of Silyl Ring Substituents and Phosphine Ligands§
Wu, He-Ping; Ess, Daniel H.; Lanza, Seren; Weakley, Timothy J. R.; Houk, K. N.; Baldridge, Kim K.; Haley, Michael M.; Organometallics 26 (2007) 3957–; doi:10.1021/om700336d

data_4073449
_publ_section_title
;
 Rearrangement of Iridabenzvalenes to Iridabenzenes and/or
 \h5-Cyclopentadienyliridium(I) Complexes:&#x00A0; Experimental and
 Computational Analysis of the Influence of Silyl Ring Substituents and
 Phosphine Ligands&#x00A7;
;
_journal_issue                   16
_journal_name_full               Organometallics
_journal_page_first              3957
_journal_paper_doi               10.1021/om700336d
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C48 H51 Ir O P2 Si2 '
_chemical_formula_sum            'C48 H51 Ir O P2 Si2'
_chemical_formula_weight         954.27
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_date             2002-04-06
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                95.282(17)
_cell_angle_beta                 102.43(2)
_cell_angle_gamma                95.649(13)
_cell_formula_units_Z            2
_cell_length_a                   11.958(3)
_cell_length_b                   13.1110(14)
_cell_length_c                   14.535(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      14.9
_cell_measurement_theta_min      14.0
_cell_volume                     2199.5(9)
_computing_cell_refinement       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'TEXSAN (Molecular Structure Corp., 1997)'
_computing_publication_material  'TEXSAN (Molecular Structure Corp., 1997)'
_computing_structure_refinement  'TEXSAN (Molecular Structure Corp., 1997)'
_computing_structure_solution    'TEXSAN (Molecular Structure Corp., 1997)'
_diffrn_ambient_temperature      296
_diffrn_measurement_device_type  'Nonius CAD-4 serial diffractometer'
_diffrn_orient_matrix_UB_11      0.08267
_diffrn_orient_matrix_UB_12      0.02820
_diffrn_orient_matrix_UB_13      0.02642
_diffrn_orient_matrix_UB_21      -0.01963
_diffrn_orient_matrix_UB_22      0.07138
_diffrn_orient_matrix_UB_23      -0.00888
_diffrn_orient_matrix_UB_31      -0.01492
_diffrn_orient_matrix_UB_32      0.00807
_diffrn_orient_matrix_UB_33      0.06523
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_av_sigmaI/netI    0.030
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8225
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        15.2
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.205
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            pale
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.87
_refine_diff_density_min         -1.44
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       '3.7(3) \\times 10^-7^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.58
_refine_ls_goodness_of_fit_ref   1.59
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7812
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.058
_refine_ls_R_factor_gt           0.033
_refine_ls_shift/su_max          0.0190
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I) + (0.025I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.078
_refine_ls_wR_factor_ref         0.038
_reflns_number_gt                7024
_reflns_number_total             7812
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            om700336d-file002.cif
_cod_data_source_block           HW0302
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2199.5(8)
_cod_original_sg_symbol_H-M      'P -1       '
_cod_original_formula_sum        'C48 H51 Ir O P2 Si2 '
_cod_database_code               4073449
_publ_section_exptl
;Crystals were epoxy-coated and mounted on glass fibres.  The first 
crystal decomposed in the middle of the shell 17.5-22 \% \q and the 
remainder of the data were collected from the second crystal.  The 
data sets were corrected for linear decay before they were merged.  
Absorption corrections based on azimuthal scans of the two crystals 
led to no decrease in standard deviations or residuals, and the results 
here are based on un-corrected data.  Structure solution: SIR92 E-map 
(Altomare et al., 1994).  Most hydrogen atoms, including those attached 
to the benzvalene unit, were located in a difference map.  All hydrogen 
atoms were included at calculated, updated positions [d(C-H) = 0.95 \%A; 
B(H) = 1.2B~eq~(C)].  The value of a secondary extinction parameter was 
also refined.
;