Competition between vinylidene rearrangement and 1,2-insertion of carbon-disubstituted internal alkynes at a Cp*Ir(iii) complex.
Ikeda, Yousuke; Kodama, Shintaro; Tsuchida, Noriko; Ishii, Youichi; Dalton transactions (Cambridge, England : 2003) 44 (2015) 17448–17452; doi:10.1039/c5dt02207j

data_7036233
_publ_section_title
;
 Competition between vinylidene rearrangement and 1,2-insertion of
 carbon-disubstituted internal alkynes at a Cp*Ir(iii) complex.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17448
_journal_page_last               17452
_journal_paper_doi               10.1039/c5dt02207j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C67 H39 B Cl2 F28 Ir N'
_chemical_formula_sum            'C67 H39 B Cl2 F28 Ir N'
_chemical_formula_weight         1663.94
_chemical_name_systematic        4c
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2015-03-06 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                88.498(4)
_cell_angle_beta                 73.243(4)
_cell_angle_gamma                79.690(3)
_cell_formula_units_Z            2
_cell_length_a                   13.6103(14)
_cell_length_b                   14.1674(17)
_cell_length_c                   17.5443(19)
_cell_measurement_reflns_used    11372
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.27
_cell_measurement_theta_min      2.77
_cell_volume                     3185.8(6)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF99-PATTY (Gould, et al., 1999)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26414
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.311
_exptl_absorpt_correction_T_max  0.707
_exptl_absorpt_correction_T_min  0.594
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1632.00
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/hexane'
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.150
_refine_diff_density_max         2.600
_refine_diff_density_min         -1.260
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     887
_refine_ls_number_reflns         14095
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0520P)^2^+5.3037P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                12349
_reflns_number_total             14095
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5dt02207j2.cif
_cod_data_source_block           4c
_cod_depositor_comments
'Adding full bibliography for 7036230--7036235.cif.'
_cod_original_cell_volume        3185.8(7)
_cod_database_code               7036233