Addition of Water Across Si-Ir Bonds in Iridium Complexes with κ-P,P,Si(biPSi) Pincer Ligands
Alba García-Camprubí; Marta Martín; Eduardo Sola; Inorganic Chemistry 49 (2010) 10649–10657; doi:10.1021/ic1016774

data_4317078
_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
;
 Addition of Water Across Si-Ir Bonds in Iridium Complexes with
 \k-P,P,Si(biPSi) Pincer Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10649
_journal_page_last               10657
_journal_paper_doi               10.1021/ic1016774
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C33 H42 Ir O P2 Si, 0.5(C4 O), 0.4(C Cl2), C F3 O3 S'
_chemical_formula_sum            'C36.4 H46.3 Cl0.8 F3 Ir O4.5 P2 S Si'
_chemical_formula_weight         955.48
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.914(2)
_cell_angle_beta                 80.057(2)
_cell_angle_gamma                87.371(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8088(12)
_cell_length_b                   12.3483(17)
_cell_length_c                   18.596(3)
_cell_measurement_reflns_used    3811
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      2.24
_cell_volume                     1972.1(5)
_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      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.907
_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  0.0512
_diffrn_reflns_av_sigmaI/netI    0.1089
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17650
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.656
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.701
_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    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             957
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.764
_refine_diff_density_min         -3.164
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         9277
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0538
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0375P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                7452
_reflns_number_total             9277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016774_si_001_3.cif
_cod_data_source_block           mar136as
_cod_original_formula_sum        'C36.40 H46.30 Cl0.80 F3 Ir O4.50 P2 S Si'
_cod_database_code               4317078