Modulation of H<sup>+</sup>/H<sup>-</sup> exchange in iridium-hydride 2-hydroxypyridine complexes by remote Lewis acids.
Shanahan, J. P.; Moore, C. M.; Kampf, Jeff W.; Szymczak, N. K.; Chemical communications (Cambridge, England) 57 (2021) 11705–11708; doi:10.1039/d1cc04778g

data_7129198
_publ_section_title
;
 Modulation of H<sup>+</sup>/H<sup>-</sup> exchange in iridium-hydride
 2-hydroxypyridine complexes by remote Lewis acids.
;
_journal_issue                   88
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11705
_journal_page_last               11708
_journal_paper_doi               10.1039/d1cc04778g
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
;
'(C114 H82 F10 Ir2 N6 O4 P4 Zn2), 1.5(C5 H12), (C H2 Cl2)'
;
_chemical_formula_sum            'C122.5 H102 Cl2 F10 Ir2 N6 O4 P4 Zn2'
_chemical_formula_weight         2622.01
_chemical_properties_physical    Moisture-sensitive
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-17 deposited with the CCDC.	2021-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                74.069(3)
_cell_angle_beta                 71.860(2)
_cell_angle_gamma                80.182(2)
_cell_formula_units_Z            2
_cell_length_a                   15.0726(4)
_cell_length_b                   19.6116(6)
_cell_length_c                   20.9592(6)
_cell_measurement_reflns_used    32621
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      69.3520
_cell_measurement_theta_min      2.2660
_cell_volume                     5636.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_temperature      85(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0929
_diffrn_reflns_av_unetI/netI     0.0593
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            84816
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.695
_diffrn_reflns_theta_min         2.283
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    6.518
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       block
_exptl_crystal_F_000             2618
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.060
_refine_diff_density_max         2.248
_refine_diff_density_min         -2.207
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1580
_refine_ls_number_reflns         20413
_refine_ls_number_restraints     538
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0559
_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^)+(0.1035P)^2^+9.5275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1529
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17789
_reflns_number_total             20413
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04778g2.cif
_cod_data_source_block           jps1089
_cod_original_formula_sum        'C122.50 H102 Cl2 F10 Ir2 N6 O4 P4 Zn2'
_cod_database_code               7129198
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.624
_shelx_estimated_absorpt_t_max   0.696
_shelx_res_checksum              94728
_shelx_hkl_checksum              80124