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_4086956
_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         '4(C31 H54 Br Ir N2 P2), 2(CH40)'
_chemical_formula_sum            'C31.5 H56 Br Ir N2 O0.5 P2'
_chemical_formula_weight         804.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.522(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.222(4)
_cell_length_b                   15.518(5)
_cell_length_c                   17.539(5)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     3549.1(19)
_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      173(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.930
_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  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0435
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40542
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         29.66
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.001
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.563
_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    1.506
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.122
_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     365
_refine_ls_number_reflns         9344
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+0.4724P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                7447
_reflns_number_total             9344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00891_si_002.cif
_cod_data_source_block           6-enriquen90b
_cod_depositor_comments
'Adding full bibliography for 4086954--4086957.cif.'
_cod_original_cell_volume        3549.0(19)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C31.50 H56 Br Ir N2 O0.50 P2'
_cod_database_code               4086956