Hydrogen Addition to (pincer)IrI(CO) Complexes: The Importance of Steric and Electronic Factors
Goldberg, Jonathan M.; Cherry, Sophia D. T.; Guard, Louise M.; Kaminsky, Werner; Goldberg, Karen I.; Heinekey, D. Michael; Organometallics 35 (2016) 3546–; doi:10.1021/acs.organomet.6b00598

data_4086746
_publ_section_title
;
 Hydrogen Addition to (pincer)IrI(CO) Complexes: The Importance of Steric
 and Electronic Factors
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              3546
_journal_paper_doi               10.1021/acs.organomet.6b00598
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C40 H70 Ir2 N2 P4'
_chemical_formula_sum            'C40 H70 Ir2 N2 P4'
_chemical_formula_weight         1087.26
_chemical_name_common            '[(iPr)4(PCP)Ir]2(?-N2)'
_chemical_name_systematic        '[(iPr)4(PCP)Ir]2(?-N2)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 111.938(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4680(15)
_cell_length_b                   10.9382(6)
_cell_length_c                   20.3858(14)
_cell_measurement_reflns_used    97720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.404
_cell_measurement_theta_min      2.045
_cell_volume                     4440.4(5)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            97720
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.404
_diffrn_reflns_theta_min         2.045
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.160
_exptl_absorpt_correction_T_max  0.9457
_exptl_absorpt_correction_T_min  0.8422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.279
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.103
_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     225
_refine_ls_number_reflns         5567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0286
_refine_ls_R_factor_gt           0.0190
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0157P)^2^+9.0550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0374
_refine_ls_wR_factor_ref         0.0404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4734
_reflns_number_total             5567
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00598_si_002.cif
_cod_data_source_block           '[(iPr)4(PCP)Ir]2(mu-N2)'
_cod_depositor_comments
'Adding full bibliography for 4086743--4086746.cif.'
_cod_database_code               4086746
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              54162
_shelx_hkl_checksum              96946