Structure and Reactivity of New Iridium Complexes with Bis(Oxazoline)-Phosphonito Ligands
Riccardo Peloso; Roberto Pattacini; Catherine S. J. Cazin; Pierre Braunstein; Inorganic Chemistry 48 (2009) 11415–11424; doi:10.1021/ic901579u

data_4303717
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
UMR 7177 CNRS
Universit\'e Louis Pasteur
Institut Le Bel 
4, rue Blaise Pascal 
F-67070 STRASBOURG 
FRANCE 
;
_publ_contact_author_email       braunstein@chimie.u-strasbg.fr
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_section_title
;
Structure and Reactivity of New Iridium Complexes with
Bis(Oxazoline)-Phosphonito Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11415
_journal_page_last               11424
_journal_paper_doi               10.1021/ic901579u
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety
'C30 H45 Ir N2 O4 P, C32 H12 B F24, 0.5(C6 H6)'
_chemical_formula_sum            'C65 H60 B F24 Ir N2 O4 P'
_chemical_formula_weight         1623.13
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 122.268(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7530(3)
_cell_length_b                   23.6740(7)
_cell_length_c                   24.5963(6)
_cell_measurement_reflns_used    25231
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     6771.5(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_sigmaI/netI    0.1057
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            35689
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.30
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  0.850
_exptl_absorpt_correction_T_min  0.751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'L. Spek, J. Appl.Cryst. 2003, 36, 7, B. Blessing, Acta Cryst, 1995, A51, 33'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3236
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.782
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     912
_refine_ls_number_reflns         13281
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0526
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1258
_reflns_number_gt                8171
_reflns_number_total             13281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901579u_si_002_2.cif
_cod_data_source_block           Compound3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4303717