Metallabenzenes and Valence Isomers. 3. Unexpected Rearrangement of Two Regioisomeric Iridabenzenes to an (η5-Cyclopentadienyl)iridium(I) Complex
Wu, He-Ping; Lanza, Seren; Weakley, Timothy J. R.; Haley, Michael M.; Organometallics 21 (2002) 2824–; doi:10.1021/om0201563

data_4076860
_publ_section_title
;
 Metallabenzenes and Valence Isomers. 3. Unexpected Rearrangement of Two
 Regioisomeric Iridabenzenes to an (\h5-Cyclopentadienyl)iridium(I)
 Complex
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              2824
_journal_paper_doi               10.1021/om0201563
_journal_volume                  21
_journal_year                    2002
_chemical_formula_moiety         'C33 H32 Ir O P Si '
_chemical_formula_structural
'Ir ((C6 H5) C5 H3 (Si (C H3)3))(C O)(P (C6 H5)3 )'
_chemical_formula_sum            'C33 H32 Ir O P Si'
_chemical_formula_weight         695.89
_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             2001-11-05
_audit_creation_method           'by teXsan v1.7'
_cell_angle_alpha                90
_cell_angle_beta                 94.343(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1428(17)
_cell_length_b                   32.708(2)
_cell_length_c                   9.7927(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      15.9
_cell_measurement_theta_min      15.0
_cell_volume                     2920.0(6)
_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_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Nonius CAD-4 serial diffractometer'
_diffrn_measurement_method       \w
_diffrn_orient_matrix_UB_11      0.01539
_diffrn_orient_matrix_UB_12      -0.02914
_diffrn_orient_matrix_UB_13      -0.02622
_diffrn_orient_matrix_UB_21      -0.00922
_diffrn_orient_matrix_UB_22      -0.00857
_diffrn_orient_matrix_UB_23      0.09699
_diffrn_orient_matrix_UB_31      -0.10819
_diffrn_orient_matrix_UB_32      -0.00341
_diffrn_orient_matrix_UB_33      -0.01989
_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  0.012
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            5587
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.9
_diffrn_standards_decay_%        2.2
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.705
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.323
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North,Phillips & Matthews (1968)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.583
_exptl_crystal_density_meas      ?
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1376.00
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.74
_refine_diff_density_min         -0.62
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_coef       '2.6(0.9) \\times 10^-8^'
_refine_ls_extinction_expression 'equ(3) Acta Cryst.(1968) A24, p213.'
_refine_ls_extinction_method     'Zachariasen (1967)'
_refine_ls_goodness_of_fit_all   1.17
_refine_ls_goodness_of_fit_ref   1.19
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     463
_refine_ls_number_reflns         5114
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.032
_refine_ls_R_factor_gt           0.022
_refine_ls_shift/su_max          0.025
_refine_ls_shift/su_mean         0.001
_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         0.052
_refine_ls_wR_factor_ref         0.025
_reflns_number_gt                4292
_reflns_number_total             5114
_reflns_threshold_expression     I>1.00\s(I)
_cod_data_source_file            om0201563.cif
_cod_data_source_block           C33H32IrOPSi
_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        2920.0(5)
_cod_original_sg_symbol_H-M      'P 21/a     '
_cod_original_formula_sum        'C33 H32 Ir O P Si '
_cod_database_code               4076860