Oxidative Addition of X−H (X = C, N, O) Bonds to [Ir(PMe3)4]Cl and Catalytic Hydration of Acetonitrile Using its Peroxo Derivative, [Ir(O2)(PMe3)4]Cl, as Catalyst Precursor
Crestani, Marco G.; Steffen, Andreas; Kenwright, Alan M.; Batsanov, Andrei S.; Howard, Judith A. K.; Marder, Todd B.; Organometallics 28 (2009) 2904–; doi:10.1021/om9000633

data_4069173
_publ_section_title
;
 Oxidative Addition of X&#x2212;H (X = C, N, O) Bonds to [Ir(PMe3)4]Cl and
 Catalytic Hydration of Acetonitrile Using its Peroxo Derivative,
 [Ir(O2)(PMe3)4]Cl, as Catalyst Precursor
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2904
_journal_paper_doi               10.1021/om9000633
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C12 H36 Ir O2 P4 1+,Cl 1-,3(C2 H3 N)'
_chemical_formula_sum            'C18 H45 Cl Ir N3 O2 P4'
_chemical_formula_weight         687.10
_chemical_name_systematic
;dioxygen-tetra(trimethylphosphine)iridium(I) chloride
 tri-acetonitrile solvate 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.681(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.792(2)
_cell_length_b                   12.8057(16)
_cell_length_c                   27.675(4)
_cell_measurement_reflns_used    9470
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.96
_cell_measurement_theta_min      2.27
_cell_volume                     5756.8(13)
_computing_cell_refinement       'SAINT version 6.45A (Bruker, 2003)'
_computing_data_collection       'SMART version 5.049 (Bruker, 1998)'
_computing_data_reduction        'SAINT version 6.45A (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL version 6.14 (Bruker, 2003)'
_computing_publication_material  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_refinement  'SHELXTL version 6.14 (Bruker, 2003)'
_computing_structure_solution    'SHELXTL version 6.14 (Bruker, 2003)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Siemens SMART 1K CCD area detector'
_diffrn_measurement_method       '\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  0.0261
_diffrn_reflns_av_sigmaI/netI    0.0196
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            39790
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.97
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.972
_exptl_absorpt_correction_T_max  0.2788
_exptl_absorpt_correction_T_min  0.0926
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
'SADABS-2006/1 (Bruker), R(int)=0.147 before correction'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.816
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.243
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         8110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.243
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0215
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0111P)^2^+14.1394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0467
_reflns_number_gt                7563
_reflns_number_total             8110
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om9000633_si_002.cif
_cod_data_source_block           9a
_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 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4069173