H/D Exchange Under Mild Conditions in Arenes and Unactivated Alkanes with C6D6 and D2O Using Rigid, Electron-rich Iridium PCP Pincer Complexes
Smith, Joel; Durrant, George; Ess, Daniel H.; Gelfand, Benjamin Sidney; Piers, Warren; Chemical Science  (2020) –; doi:10.1039/D0SC02694H

data_1558326
_publ_section_title
;
 H/D Exchange Under Mild Conditions in Arenes and Unactivated Alkanes with
 C6D6 and D2O Using Rigid, Electron-rich Iridium PCP Pincer Complexes
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02694H
_journal_year                    2020
_chemical_formula_moiety         'C32 H55 Ir N2 P2'
_chemical_formula_sum            'C32 H55 Ir N2 P2'
_chemical_formula_weight         721.92
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-06-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-11 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                82.027(3)
_cell_angle_beta                 74.303(4)
_cell_angle_gamma                82.556(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1782(6)
_cell_length_b                   10.3488(5)
_cell_length_c                   16.3633(11)
_cell_measurement_reflns_used    8463
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.494
_cell_measurement_theta_min      2.697
_cell_volume                     1635.59(17)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.978
_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  0.0872
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17788
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.532
_diffrn_reflns_theta_min         2.157
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.202
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0978 before and 0.0516 after correction. The Ratio of minimum to maximum transmission is 0.6554. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.599
_refine_diff_density_min         -1.982
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         7379
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5973
_reflns_number_total             7379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02694h2.cif
_cod_data_source_block           181109_js_polyhydride_0m
_cod_database_code               1558326
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.487
_shelx_estimated_absorpt_t_min   0.487
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Ir1 \\sim H \\sim HA \\sim HB \\sim HC: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C1(H1), C21(H21), C24(H24), C27(H27), C30(H30)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C10(H10), C12(H12)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18B,H18C,
 H18A), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_res_checksum              31674
_shelx_hkl_checksum              51581
_olex2_submission_special_instructions 'No special instructions were received'