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_4086743
_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         'C19 H33 Ir O3 P2'
_chemical_formula_sum            'C19 H33 Ir O3 P2'
_chemical_formula_weight         563.59
_chemical_name_common            complex_trans_5
_chemical_name_systematic        complex_trans_5
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                105.935(3)
_cell_angle_beta                 92.176(3)
_cell_angle_gamma                107.411(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8388(5)
_cell_length_b                   9.9117(7)
_cell_length_c                   15.1225(10)
_cell_measurement_reflns_used    46232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      2
_cell_volume                     1068.76(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.993
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0179
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46232
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_min         2.257
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.411
_exptl_absorpt_correction_T_max  0.567
_exptl_absorpt_correction_T_min  0.392
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       piece
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.558
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0143
_refine_ls_R_factor_gt           0.0132
_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^)+(0.0112P)^2^+0.4789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0268
_refine_ls_wR_factor_ref         0.0271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5144
_reflns_number_total             5353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00598_si_002.cif
_cod_data_source_block           complex_trans_5
_cod_depositor_comments
'Adding full bibliography for 4086743--4086746.cif.'
_cod_database_code               4086743
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.392
_shelx_estimated_absorpt_t_max   0.567
_shelx_res_checksum              9629
_shelx_hkl_checksum              501