Synthesis, Characterization, and Properties of Doubly Alkynyl Bridging Dinuclear Cyclometalated Iridium(III) Complexes
Fernández-Cestau, Julio; Giménez, Nora; Lalinde, Elena; Montaño, Patricia; Moreno, M. Teresa; Sánchez, Sergio; Organometallics 34 (2015) 1766–; doi:10.1021/acs.organomet.5b00111

data_4087428
_publ_section_title
;
 Synthesis, Characterization, and Properties of Doubly Alkynyl Bridging
 Dinuclear Cyclometalated Iridium(III) Complexes
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1766
_journal_paper_doi               10.1021/acs.organomet.5b00111
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C56 H50 Ir2 N4'
_chemical_formula_weight         1214.62
_chemical_name_common            pms193
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-01-15T17:35:20-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                86.160(2)
_cell_angle_beta                 89.497(2)
_cell_angle_gamma                85.358(3)
_cell_formula_units_Z            1
_cell_length_a                   8.7163(4)
_cell_length_b                   9.9747(5)
_cell_length_c                   13.0686(6)
_cell_measurement_reflns_used    2498
_cell_measurement_temperature    173(2)
_cell_volume                     1129.94(9)
_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_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0083511
_diffrn_orient_matrix_UB_12      0.065063
_diffrn_orient_matrix_UB_13      0.0551495
_diffrn_orient_matrix_UB_21      -0.1098847
_diffrn_orient_matrix_UB_22      0.025533
_diffrn_orient_matrix_UB_23      -0.0189843
_diffrn_orient_matrix_UB_31      -0.0332409
_diffrn_orient_matrix_UB_32      -0.0726418
_diffrn_orient_matrix_UB_33      0.0497973
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0448
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16135
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         3.125
_exptl_absorpt_coefficient_mu    6.102
_exptl_absorpt_correction_T_max  0.6513
_exptl_absorpt_correction_T_min  0.5544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             586
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.016
_refine_diff_density_min         -1.303
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     288
_refine_ls_number_reflns         4602
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+3.6431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                4261
_reflns_number_total             4602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00111_si_002.cif
_cod_data_source_block           6.1,5CH2Cl2
_cod_database_code               4087428
_shelx_estimated_absorpt_t_min   0.581
_shelx_estimated_absorpt_t_max   0.75