Iridium Pincer Catalysts for Silane Dehydrocoupling: Ligand Effects on Selectivity and Activity
Mucha, Neil T.; Waterman, Rory; Organometallics 34 (2015) 3865–; doi:10.1021/acs.organomet.5b00486

data_4087672
_publ_section_title
;
 Iridium Pincer Catalysts for Silane Dehydrocoupling: Ligand Effects on
 Selectivity and Activity
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              3865
_journal_paper_doi               10.1021/acs.organomet.5b00486
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C24 H42 Cl Ir O4 P2'
_chemical_formula_sum            'C24 H42 Cl Ir O4 P2'
_chemical_formula_weight         684.16
_chemical_name_common            p-COOMetbu(POCOP)IrHCl
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 91.087(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.6097(14)
_cell_length_b                   26.515(4)
_cell_length_c                   20.822(3)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    135(2)
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.27
_cell_volume                     5856.5(14)
_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-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            58323
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.200
_diffrn_reflns_theta_min         1.244
_exptl_absorpt_coefficient_mu    4.785
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5566
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         10526
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0237P)^2^+10.8762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0657
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8600
_reflns_number_total             10526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00486_si_003.cif
_cod_data_source_block           NM87_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        5856.5(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087672
_shelx_estimated_absorpt_t_min   0.646
_shelx_estimated_absorpt_t_max   0.759
_shelxl_version_number           2014/6
_shelx_res_checksum              31284
_shelx_hkl_checksum              53087