Synthesis and Characterization of Iridium(I) and Iridium(III) Complexes Containing Dialkylbiphenylphosphines
O’Connor, Abby R.; Kaminsky, Werner; Chan, Benny C.; Heinekey, D. M.; Goldberg, Karen I.; Organometallics 32 (2013) 4016–; doi:10.1021/om400266d

data_4080958
_publ_section_title
;
 Synthesis and Characterization of Iridium(I) and Iridium(III) Complexes
 Containing Dialkylbiphenylphosphines
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4016
_journal_paper_doi               10.1021/om400266d
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety
'C32 H12 B F24, C24 H33 Ir P, 0.43(C6 H14), 0.14(C H2 Cl2) '
_chemical_formula_sum            'C58.71 H51.28 B Cl0.29 F24 Ir P'
_chemical_formula_weight         1456.95
_chemical_name_common            iiia0271
_chemical_name_systematic
;
 iiia0271
;
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-05-04T12:21:41-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                71.987(2)
_cell_angle_beta                 68.813(2)
_cell_angle_gamma                86.029(2)
_cell_formula_units_Z            4
_cell_length_a                   17.6548(6)
_cell_length_b                   18.0941(6)
_cell_length_c                   20.6767(7)
_cell_measurement_reflns_used    794
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     5850.1(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            206598
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         33.28
_diffrn_reflns_theta_min         1.67
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.438
_exptl_absorpt_correction_T_max  0.7112
_exptl_absorpt_correction_T_min  0.7112
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2886.3
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.002
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1690
_refine_ls_number_reflns         44898
_refine_ls_number_restraints     154
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0698
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+7.6525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0723
_refine_ls_wR_factor_ref         0.0841
_reflns_number_gt                31959
_reflns_number_total             44898
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400266d_si_002.cif
_cod_data_source_block           iiia0271_0m
_cod_original_cell_volume        5850.1(3)
_cod_database_code               4080958