Iridium Compounds with κ-P,P,Si(biPSi) Pincer Ligands: Favoring Reactive Structures in Unsaturated Complexes
Eduardo Sola; Alba García-Camprubí; José L. Andrés; Marta Martín; Pablo Plou; Journal of the American Chemical Society 132 (2010) 9111–9121; doi:10.1021/ja102479h

data_4102624
_publ_contact_author_address
;
  Dr. Marta Mart\'in
  Departamento de Qu\'imica Inorg\'anica - I.C.M.A.
  Facultad de Ciencias
  Universidad de Zaragoza - C.S.I.C.
  50009 Zaragoza, Spain
;
_publ_contact_author_email       martam@unizar.es
_publ_contact_author_fax         '+34 956 761187'
_publ_contact_author_name        'Dr. Marta Mart\'in'
_publ_contact_author_phone       '+34 976 762026'
_publ_section_title
;
 Iridium Compounds with \k-P,P,Si(biPSi) Pincer Ligands: Favoring Reactive
 Structures in Unsaturated Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9111
_journal_page_last               9121
_journal_paper_doi               10.1021/ja102479h
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C33 H39 Cl Ir N P2 Si, C H2 Cl2'
_chemical_formula_sum            'C34 H41 Cl3 Ir N P2 Si'
_chemical_formula_weight         852.28
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6296(6)
_cell_length_b                   20.8340(16)
_cell_length_c                   21.0695(16)
_cell_measurement_reflns_used    4930
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.884
_cell_measurement_theta_min      2.750
_cell_volume                     3349.1(4)
_computing_cell_refinement       'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_data_collection       'SMART v. 5.611 (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT+ v. 6.01 (Bruker AXS, 2000)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'XCIF program, SHELXTLv6.10,BrukerAXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_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  0.0754
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40301
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    4.383
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  SADABS: Area-Detector Absorption Correction. (1996)  Bruker-AXS 
  within SAINT+ package, v. 6.01.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.693
_refine_diff_density_min         -1.395
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0097P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0461
_reflns_number_gt                3259
_reflns_number_total             4419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja102479h_si_002_6.cif
_cod_data_source_block           marta55s
_cod_database_code               4102624