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_7129196
_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         'C52 H45 Ir N3 O2 P2, B F4, C H2 Cl2'
_chemical_formula_sum            'C53 H47 B Cl2 F4 Ir N3 O2 P2'
_chemical_formula_weight         1169.78
_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
_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
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_cell_angle_gamma                90
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_cell_length_c                   19.90960(10)
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_cell_measurement_temperature    85(2)
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_cell_measurement_theta_min      2.3050
_cell_volume                     4794.81(6)
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_computing_data_collection
'CrystalClear-SM Expert 2.0 r16 (Rigaku, 2014)'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
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_diffrn_measured_fraction_theta_max 0.994
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
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_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            71360
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.425
_diffrn_reflns_theta_min         3.018
_diffrn_source                   'micro-focus rotating anode'
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_exptl_absorpt_correction_T_max  1.00000
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_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    1.620
_exptl_crystal_description       plate
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.160
_refine_diff_density_max         2.988
_refine_diff_density_min         -2.130
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       0.00011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         8949
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0362
_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^)+(0.0542P)^2^+12.7248P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0970
_refine_ls_wR_factor_ref         0.0970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8941
_reflns_number_total             8949
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04778g2.cif
_cod_data_source_block           jps2254
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7129196
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.264
_shelx_estimated_absorpt_t_max   0.378
_shelx_res_checksum              25481
_shelx_hkl_checksum              57699