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_4087426
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C68 H58 Ir2 N4 O2'
_chemical_formula_sum            'C68 H58 Ir2 N4 O2'
_chemical_formula_weight         1347.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2013-10-22T09:58:34-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 98.4640(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1506(2)
_cell_length_b                   10.13610(10)
_cell_length_c                   41.1377(6)
_cell_measurement_reflns_used    34927
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     0.71073
_cell_volume                     5423.76(13)
_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-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 1.001
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.058059
_diffrn_orient_matrix_UB_12      -0.048922
_diffrn_orient_matrix_UB_13      0.013153
_diffrn_orient_matrix_UB_21      -0.047453
_diffrn_orient_matrix_UB_22      -0.031348
_diffrn_orient_matrix_UB_23      0.015264
_diffrn_orient_matrix_UB_31      -0.016967
_diffrn_orient_matrix_UB_32      -0.079732
_diffrn_orient_matrix_UB_33      -0.014072
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 1.001
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12336
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 1.001
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.071
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    4.943
_exptl_absorpt_correction_T_max  0.6538
_exptl_absorpt_correction_T_min  0.5383
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Linear fit to sin(theta)/lambda - 12 parameters
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.65
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2656
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.17
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.191
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.937
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     674
_refine_ls_number_reflns         10250
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+187.6400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1115
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                8977
_reflns_number_total             10250
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00111_si_002.cif
_cod_data_source_block           1.2(CH3)2CO
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087426
_exptl_absorpt_factor_mur        0.494
_exptl_absorpt_correction_t_ave  0.6098
_exptl_absorpt_rmerge_before     0.1011
_exptl_absorpt_rmerge_after      0.0983