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_4303718
_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       braunst@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
'C44 H70 Ir2 N4 O8 P2,2(C32 H12 B F24),4(C H2 Cl2)'
_chemical_formula_sum            'C112 H102 B2 Cl8 F48 Ir2 N4 O8 P2'
_chemical_formula_weight         3295.54
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                71.857(4)
_cell_angle_beta                 79.532(3)
_cell_angle_gamma                87.282(5)
_cell_formula_units_Z            1
_cell_length_a                   12.4044(11)
_cell_length_b                   14.6314(10)
_cell_length_c                   18.9398(17)
_cell_measurement_reflns_used    10210
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.42
_cell_measurement_theta_min      0.998
_cell_volume                     3212.0(5)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0948
_diffrn_reflns_av_sigmaI/netI    0.1268
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19854
_diffrn_reflns_theta_full        30.82
_diffrn_reflns_theta_max         30.82
_diffrn_reflns_theta_min         1.15
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.385
_exptl_absorpt_correction_T_max  0.834
_exptl_absorpt_correction_T_min  0.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1628
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.383
_refine_diff_density_min         -2.302
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     876
_refine_ls_number_reflns         19854
_refine_ls_number_restraints     284
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.1207
_refine_ls_R_factor_gt           0.0702
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0956P)^2^+3.1527P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1738
_reflns_number_gt                13784
_reflns_number_total             19854
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901579u_si_002_3.cif
_cod_data_source_block           compound4
_cod_database_code               4303718