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_4086744
_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         'C24 H37 Ir N O3 P2, B F4'
_chemical_formula_sum            'C24 H37 B F4 Ir N O3 P2'
_chemical_formula_weight         728.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.427(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6974(7)
_cell_length_b                   14.1665(10)
_cell_length_c                   18.4112(11)
_cell_measurement_reflns_used    39743
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     2789.3(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-14 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.880
_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  0.0730
_diffrn_reflns_av_unetI/netI     0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39743
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.502
_diffrn_reflns_theta_min         1.437
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_transmission_factor_max   0.9452
_exptl_transmission_factor_min   0.7353
_refine_diff_density_max         4.485
_refine_diff_density_min         -4.630
_refine_diff_density_rms         0.589
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.328
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         4991
_refine_ls_number_restraints     216
_refine_ls_restrained_S_all      1.306
_refine_ls_R_factor_all          0.1413
_refine_ls_R_factor_gt           0.0999
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+187.6540P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2024
_refine_ls_wR_factor_ref         0.2244
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3653
_reflns_number_total             4991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00598_si_002.cif
_cod_data_source_block           complex_7_BF4
_cod_depositor_comments
'Adding full bibliography for 4086743--4086746.cif.'
_cod_database_code               4086744
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.524
_shelx_estimated_absorpt_t_max   0.866
_shelx_res_checksum              8278
_shelx_hkl_checksum              74848