Cyclometalated Iridium Complexes from Intramolecular C‒H Activation of [IrCp*Cl{═C(OMe)CH═C(CH3)R}L] (R = CH3, Ph; L = PPh2Me, PMe3)
Talavera, M.; Bolaño, S.; Bravo, J.; Castro, J.; Garc\?ía-Fontán, S.; Organometallics 32 (2013) 7241–; doi:10.1021/om4008778

data_4081996
_publ_section_title
;
 Cyclometalated Iridium Complexes from Intramolecular C--H Activation of
 [IrCp*Cl{&#x2550;C(OMe)CH&#x2550;C(CH3)R}L] (R = CH3, Ph; L = PPh2Me,
 PMe3)
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7241
_journal_paper_doi               10.1021/om4008778
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C29 H37 F6 Ir O P2'
_chemical_formula_weight         769.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.303(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.486(3)
_cell_length_b                   18.667(4)
_cell_length_c                   19.250(4)
_cell_measurement_reflns_used    8680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.96
_cell_measurement_theta_min      2.38
_cell_volume                     5914(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52415
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.52
_exptl_absorpt_coefficient_mu    4.683
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5619
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.615
_refine_diff_density_min         -1.572
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         14190
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0633
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+34.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1372
_reflns_number_gt                11230
_reflns_number_total             14190
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4008778_si_001.cif
_cod_data_source_block           2a_md
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

2026-05-15
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C58 H74 F12 Ir2 O2 P4'
_cod_original_formula_weight         1539.45
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               4081996