Complexes with Hybrid Phosphorus-NHC Ligands: Pincer-Type Ir Hydrides, Dinuclear Ag and Ir and Tetranuclear Cu and Ag Complexes
Xianghao Liu; Pierre Braunstein; Inorganic Chemistry 52 (2013) 7367–7379; doi:10.1021/ic302854t

data_4335313
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
UMR 7177 CNRS
Universit\'e de Strasbourg
Institut Le Bel - 4 rue Blaise Pascal, 67081 Strasbourg Cedex - France
;
_publ_contact_author_email       braunstein@unistra.fr
_publ_contact_author_fax         '+33 (0)3 68 85 13 22'
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       '+33 (0)3 68 85 13 08'
_publ_section_title
;
 Complexes with Hybrid Phosphorus-NHC Ligands: Pincer-Type Ir Hydrides,
 Dinuclear Ag and Ir and Tetranuclear Cu and Ag Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7367
_journal_page_last               7379
_journal_paper_doi               10.1021/ic302854t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C64 H70 Ir2 N4 P2, C8 H16 O2, 2(F6 P)'
_chemical_formula_sum            'C72 H86 F12 Ir2 N4 O2 P4'
_chemical_formula_weight         1775.73
_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                62.225(3)
_cell_angle_beta                 72.114(3)
_cell_angle_gamma                85.688(3)
_cell_formula_units_Z            1
_cell_length_a                   10.0347(6)
_cell_length_b                   14.2909(6)
_cell_length_c                   14.4418(7)
_cell_measurement_reflns_used    5071
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.103
_cell_measurement_theta_min      0.998
_cell_volume                     1738.16(16)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10687
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.997
_exptl_absorpt_correction_T_max  0.675
_exptl_absorpt_correction_T_min  0.570
_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            red
_exptl_crystal_density_diffrn    1.696
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.421
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     422
_refine_ls_number_reflns         6819
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0583P)^2^+1.9670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                5227
_reflns_number_total             6819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302854t_si_001_2.cif
_cod_data_source_block           complex4_Liu12
_cod_original_cell_volume        1738.17(15)
_cod_database_code               4335313