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_4073448
_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_sum            'C54 H51 Cl4 I Ir2 O2 P2 Si'
_chemical_formula_weight         1475.19
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             2003-01-16
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                90
_cell_angle_beta                 112.648(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.558(3)
_cell_length_b                   15.874(3)
_cell_length_c                   20.342(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      13.0
_cell_volume                     5530.4(16)
_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_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.00817
_diffrn_orient_matrix_UB_12      -0.02952
_diffrn_orient_matrix_UB_13      0.04000
_diffrn_orient_matrix_UB_21      -0.05124
_diffrn_orient_matrix_UB_22      -0.02195
_diffrn_orient_matrix_UB_23      -0.03415
_diffrn_orient_matrix_UB_31      0.02676
_diffrn_orient_matrix_UB_32      -0.05113
_diffrn_orient_matrix_UB_33      -0.00843
_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  0.023
_diffrn_reflns_av_sigmaI/netI    0.050
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6327
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         17.48
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        23.3
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.690
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews (1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2840
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.16
_refine_diff_density_min         -1.82
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       0.00000000
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.81
_refine_ls_goodness_of_fit_ref   1.92
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     541
_refine_ls_number_reflns         6119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.083
_refine_ls_R_factor_gt           0.046
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.0009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I) + (0.020I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.103
_refine_ls_wR_factor_ref         0.050
_reflns_number_gt                4573
_reflns_number_total             6119
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            om700336d-file001.cif
_cod_data_source_block           HW1101
_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        5530.4(15)
_cod_original_sg_symbol_H-M      'P 21/a     '
_cod_original_formula_sum        'C54 H51 Cl4 I Ir2 O2 P2 Si '
_cod_database_code               4073448