Oxidative addition of an aromatic ortho C-H bond of tetraphosphine to asymmetric diiridium(i) centres.
Nakajima, Takayuki; Noda, Sayo; Sakamoto, Miyuki; Matsui, Aya; Nakamae, Kanako; Kure, Bunsho; Ura, Yasuyuki; Tanase, Tomoaki; Dalton transactions (Cambridge, England : 2003) 45 (2016) 4747–4761; doi:10.1039/c5dt04725k

data_7038200
_publ_section_title
;
 Oxidative addition of an aromatic ortho C-H bond of tetraphosphine to
 asymmetric diiridium(i) centres.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4747
_journal_page_last               4761
_journal_paper_doi               10.1039/c5dt04725k
_journal_volume                  45
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C63 H83 F12 Ir N2 O3 P6'
_chemical_formula_sum            'C63 H83 F12 Ir N2 O3 P6'
_chemical_formula_weight         1522.40
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2016-01-25 deposited with the CCDC.
2016-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.058(3)
_cell_length_b                   18.478(4)
_cell_length_c                   28.214(6)
_cell_measurement_reflns_used    18444
_cell_measurement_temperature    153
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.06
_cell_volume                     6808(3)
_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    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      153
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0719
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            79705
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.185
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3096.00
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.019
_refine_diff_density_max         4.350
_refine_diff_density_min         -1.760
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  7049 Friedel Pairs'
_refine_ls_abs_structure_Flack   -0.028(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     787
_refine_ls_number_reflns         15541
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0987P)^2^+3.8123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1803
_reflns_number_gt                13436
_reflns_number_total             15541
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c5dt04725k2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7038197--7038203.cif.'
_cod_database_code               7038200