Formation of Dinuclear Iridium Complexes by NHC-Supported C–H Bond Activation
Esteruelas, Miguel A.; López, Ana M.; Oñate, Enrique; San-Torcuato, Ainhoa; Tsai, Jui-Yi; Xia, Chuanjun; Organometallics 36 (2017) 699–; doi:10.1021/acs.organomet.6b00891

data_4086954
_publ_section_title
;
 Formation of Dinuclear Iridium Complexes by NHC-Supported C--H Bond
 Activation
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              699
_journal_paper_doi               10.1021/acs.organomet.6b00891
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         '2(C50 H100 Ir2 N4 P4), C7 H8'
_chemical_formula_sum            'C53.5 H104 Ir2 N4 P4'
_chemical_formula_weight         1311.69
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                107.101(3)
_cell_angle_beta                 94.717(3)
_cell_angle_gamma                113.622(2)
_cell_formula_units_Z            2
_cell_length_a                   12.671(2)
_cell_length_b                   13.823(2)
_cell_length_c                   19.540(5)
_cell_measurement_reflns_used    7761
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      2
_cell_volume                     2917.8(10)
_computing_cell_refinement       'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_data_collection       'apex2 v. 7.0 (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT+ v. 7.56a (Bruker AXS, 2008)'
_computing_molecular_graphics    'XP, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_publication_material  'XCIF, SHELXTL v. 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32370
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.62
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.702
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.659
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Absorption correction performed with SADABS program. This is based on the
method of Blessing: Blessing, R. H., Acta Crystallogr., Sect. A 1995, 51, 33.

SADABS: Area-Detector Absorption Correction. Bruker-AXS 
within SAINT+ package, v. 6.1 (2000).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.278
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         14710
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                10789
_reflns_number_total             14710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00891_si_002.cif
_cod_data_source_block           2-enriquen102
_cod_depositor_comments
'Adding full bibliography for 4086954--4086957.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C53.50 H104 Ir2 N4 P4'
_cod_database_code               4086954