Cyclometalated Iridium(III) Complexes Containing Hydroxide/Chloride Ligands: Isolation of Heterobridged Dinuclear Iridium(III) Compounds Containing μ-OH and μ-Pyrazole Ligands
Vadapalli Chandrasekhar; Bani Mahanti; Priyanka Bandipalli; Kotamarthi Bhanuprakash; Inorganic Chemistry 51 (2012) 10536–10547; doi:10.1021/ic300694m

data_4330550
_publ_contact_author_email       vc@iitk.ac.in
_publ_section_title
;
 Cyclometalated Iridium(III) Complexes Containing Hydroxide/Chloride
 Ligands: Isolation of Heterobridged Dinuclear Iridium(III) Compounds
 Containing \m-OH and \m-Pyrazole Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10536
_journal_page_last               10547
_journal_paper_doi               10.1021/ic300694m
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C32 H27 Ir N4 O'
_chemical_formula_weight         675.78
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   9.571(5)
_cell_length_b                   10.490(5)
_cell_length_c                   27.375(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2748(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            39277
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    4.889
_exptl_absorpt_correction_T_max  0.822
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.604
_refine_diff_density_min         -2.308
_refine_diff_density_rms         0.145
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         5121
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          2.286
_refine_ls_shift/su_mean         0.046
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+17.4767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1168
_reflns_number_gt                4980
_reflns_number_total             5121
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300694m_si_002_5.cif
_cod_data_source_block           complex5
_cod_database_code               4330550