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_7129199
_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
;
	2(C51 H42 Ir N3 O2 P2), (C4 H10 O), 1.5(C H2 Cl2) [+ solvent]
;
_chemical_formula_sum            'C53.75 H48.5 Cl1.5 Ir N3 O2.5 P2'
_chemical_formula_weight         1083.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual-space
_atom_sites_solution_secondary   difmap
_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                90
_cell_angle_beta                 103.5510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.95100(10)
_cell_length_b                   27.4111(2)
_cell_length_c                   23.76380(10)
_cell_measurement_reflns_used    66886
_cell_measurement_temperature    85(2)
_cell_measurement_theta_max      73.2190
_cell_measurement_theta_min      2.4840
_cell_volume                     10101.10(11)
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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  0.1057
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            302176
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.135
_diffrn_reflns_theta_min         3.037
_diffrn_source                   'micro-focus rotating anode'
_exptl_absorpt_coefficient_mu    6.784
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58578
_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    1.425
_exptl_crystal_description       needle
_exptl_crystal_F_000             4356
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.045
_refine_diff_density_min         -1.941
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1194
_refine_ls_number_reflns         20398
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0747P)^2^+36.5240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1341
_refine_ls_wR_factor_ref         0.1406
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17811
_reflns_number_total             20398
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04778g2.cif
_cod_data_source_block           cm4119_sq
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C53.75 H48.50 Cl1.50 Ir N3 O2.50 P2'
_cod_database_code               7129199
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.686
_shelx_estimated_absorpt_t_max   0.876
_shelx_res_checksum              21654
_shelx_hkl_checksum              55970
_shelx_fab_checksum              11779