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_4317076
_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         'C35 H41 F Ir N2 P2 Si, B F4'
_chemical_formula_sum            'C35 H41 B F5 Ir N2 P2 Si'
_chemical_formula_weight         877.77
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 95.9480(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1805(8)
_cell_length_b                   9.5246(7)
_cell_length_c                   33.037(2)
_cell_measurement_reflns_used    4184
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      24.16
_cell_measurement_theta_min      2.23
_cell_volume                     3499.2(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      100.0(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.935
_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  0.0919
_diffrn_reflns_av_sigmaI/netI    0.1119
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            42818
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.05
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        'no decay'
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.661
_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    1.666
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1744
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.179
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         8723
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.883
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0447
_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^)+(0.0235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                5685
_reflns_number_total             8723
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1016774_si_001_1.cif
_cod_data_source_block           mar117as
_cod_original_cell_volume        3499.1(4)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4317076