Direct Synthesis of an Iridabenzene from a Nucleophilic 3-Vinyl-1-cyclopropene
Robert D. Gilbertson; Timothy J. R. Weakley; Michael M. Haley; Journal of the American Chemical Society 121 (1999) 2597–2598; doi:10.1021/ja984420o

data_4116323
_publ_contact_author_address
;
Department of Chemistry,
University of Oregon,
Eugene, OR 97403-1253
USA
;
_publ_contact_author_email       tweakley@oregon.uoregon.edu
_publ_contact_author_fax         01(541)3464643
_publ_contact_author_name        'Dr Timothy J. R. Weakley'
_publ_contact_author_phone       01(541)3464620
_publ_section_title
;
 Direct Synthesis of an Iridabenzene from a Nucleophilic
 3-Vinyl-1-cyclopropene
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2597
_journal_page_last               2598
_journal_paper_doi               10.1021/ja984420o
_journal_volume                  121
_journal_year                    1999
_chemical_formula_moiety         'C54 H43 Ir O P2, C7 H8 '
_chemical_formula_sum            'C61 H51 Ir O P2'
_chemical_formula_weight         1054.24
_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             1998-11-11
_audit_creation_method           'by teXsan v1.8'
_cell_angle_alpha                107.841(17)
_cell_angle_beta                 101.989(20)
_cell_angle_gamma                93.318(16)
_cell_formula_units_Z            2
_cell_length_a                   10.417(2)
_cell_length_b                   13.4360(16)
_cell_length_c                   19.230(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      14.0
_cell_measurement_theta_min      13.0
_cell_volume                     2484.7(9)
_computing_cell_refinement       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_collection       'CAD4/PC (Enraf-Nonius, 1993)'
_computing_data_reduction        'TEXSAN (Molecular Structure Corp., 1989)'
_computing_publication_material  'TEXSAN (Molecular Structure Corp., 1989)'
_computing_structure_refinement  'TEXSAN (Molecular Structure Corp., 1989)'
_computing_structure_solution    'TEXSAN (Molecular Structure Corp., 1989)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_orient_matrix_UB_11      0.03418
_diffrn_orient_matrix_UB_12      -0.06682
_diffrn_orient_matrix_UB_13      0.00334
_diffrn_orient_matrix_UB_21      -0.06556
_diffrn_orient_matrix_UB_22      -0.04076
_diffrn_orient_matrix_UB_23      -0.04785
_diffrn_orient_matrix_UB_31      0.06580
_diffrn_orient_matrix_UB_32      0.00958
_diffrn_orient_matrix_UB_33      -0.02934
_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  0.015
_diffrn_reflns_av_sigmaI/netI    0.040
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9247
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         25.0
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        0.66
_diffrn_standards_interval_count 300
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.80
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.836
_exptl_absorpt_correction_type
;
\y scans (North,Phillips & Matthews, 1968)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       prism
_exptl_crystal_F_000             1064.00
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.23
_refine_diff_density_min         -2.65
_refine_ls_abs_structure_details 'not applicable'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   3.01
_refine_ls_goodness_of_fit_ref   3.17
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7797
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.060
_refine_ls_R_factor_gt           0.050
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4F~o~^2^/[\s^2^(I)+(0.02I)^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.067
_refine_ls_wR_factor_ref         0.066
_reflns_number_gt                7797
_reflns_number_total             8721
_reflns_threshold_expression     I>1.5\s(I)
_cod_data_source_file            ja984420o.cif
_cod_data_source_block           C54H43IrOP2,C7H8
_cod_original_cell_volume        2484.8(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C61 H51 Ir O P2 '
_cod_database_code               4116323