Hydrogen Activation by an Iridium(III) Complex Bearing a Bidentate Protic NH,NR-NHC∧Phosphine Ligand
Cepa, Steffen; Schulte to Brinke, Christian; Roelfes, Florian; Hahn, F. Ekkehardt; Organometallics 34 (2015) 5454–; doi:10.1021/acs.organomet.5b00799

data_4088002
_publ_section_title
;
 Hydrogen Activation by an Iridium(III) Complex Bearing a Bidentate Protic
 NH,NR-NHC&#x2227;Phosphine Ligand
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5454
_journal_paper_doi               10.1021/acs.organomet.5b00799
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C33 H50 Cl2 Ir N2 P, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C33.5 H51 Cl3 Ir N2 P'
_chemical_formula_weight         811.28
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 95.786(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.6119(7)
_cell_length_b                   14.9729(6)
_cell_length_c                   27.5702(12)
_cell_measurement_reflns_used    42740
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.756
_cell_measurement_theta_min      2.9745
_cell_volume                     6822.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            124604
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         30.992
_diffrn_reflns_theta_min         2.438
_exptl_absorpt_coefficient_mu    4.221
_exptl_absorpt_correction_T_max  0.5520
_exptl_absorpt_correction_T_min  0.4174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2012)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       plate
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.051
_refine_diff_density_max         2.735
_refine_diff_density_min         -1.699
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         21556
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0270P)^2^+10.0556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0603
_refine_ls_wR_factor_ref         0.0635
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18558
_reflns_number_total             21556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00799_si_002.cif
_cod_data_source_block           '[3]'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C33.50 H51 Cl3 Ir N2 P'
_cod_database_code               4088002