Catalytic Dehydrogenative C-C Coupling by a Pincer-Ligated Iridium Complex.
Wilklow-Marnell, Miles; Li, Bo; Zhou, Tian; Krogh-Jespersen, Karsten; Brennessel, William W.; Emge, Thomas J.; Goldman, Alan S.; Jones, William D.; Journal of the American Chemical Society 139 (2017) 8977–8989; doi:10.1021/jacs.7b03433

data_4126367
_publ_section_title
;
 Catalytic Dehydrogenative C-C Coupling by a Pincer-Ligated Iridium
 Complex.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8977
_journal_page_last               8989
_journal_paper_doi               10.1021/jacs.7b03433
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C36 H47 Ir P2'
_chemical_formula_weight         733.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                92.263(3)
_cell_angle_beta                 107.127(3)
_cell_angle_gamma                91.127(3)
_cell_formula_units_Z            2
_cell_length_a                   9.9152(12)
_cell_length_b                   11.9825(14)
_cell_length_c                   14.1511(17)
_cell_measurement_reflns_used    5863
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      2.33
_cell_volume                     1604.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1133
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18351
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.003
_diffrn_reflns_theta_min         1.507
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    4.283
_exptl_absorpt_correction_T_max  0.4322
_exptl_absorpt_correction_T_min  0.2821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT (SADABS)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_description       plate
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.03
_refine_diff_density_max         4.622
_refine_diff_density_min         -3.263
_refine_diff_density_rms         0.283
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         18351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0612
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0657P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1516
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15678
_reflns_number_total             18351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b03433_si_008.cif
_cod_data_source_block           twin4_P-1
_cod_depositor_comments
;

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C0.72 H0.94 Ir0.02 P0.04'
_cod_original_formula_weight         14.68
_cod_original_formula_units_Z            100
_cod_database_code               4126367
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              49794
_shelx_hkl_checksum              78593