New, potentially chelating NHC ligands; synthesis, complexation studies, and preliminary catalytic evaluation.
Ou, Arnold; Wu, Linglin; Salvador, Alvaro; Sipos, Gellert; Zhao, Guangzhen; Skelton, Brian W.; Sobolev, Alexandre N.; Dorta, Reto; Dalton transactions (Cambridge, England : 2003) 46 (2017) 3631–3641; doi:10.1039/c6dt04534k

data_7042176
_publ_section_title
;
 New, potentially chelating NHC ligands; synthesis, complexation studies,
 and preliminary catalytic evaluation.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3631
_journal_page_last               3641
_journal_paper_doi               10.1039/c6dt04534k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety
'C33 H32 Cl Ir N4 O4, 0.75(C D2 Cl2), 0.25(H2 O)'
_chemical_formula_sum            'C33.75 H32.5 Cl2.5 D1.5 Ir N4 O4.25'
_chemical_formula_weight         845.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-24 deposited with the CCDC.
2017-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                74.248(2)
_cell_angle_beta                 88.409(2)
_cell_angle_gamma                80.650(2)
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_cell_length_b                   11.5132(3)
_cell_length_c                   15.6027(3)
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.943
_cell_measurement_theta_min      3.112
_cell_volume                     1673.47(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0009
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur-S, Sapphire3 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0473
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            60875
_diffrn_reflns_point_group_measured_fraction_full 0.996
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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 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       plate
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.120
_refine_diff_density_max         3.573
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         16783
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0350P)^2^+3.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0884
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15305
_reflns_number_total             16783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04534k2.cif
_cod_data_source_block           rda640
_cod_depositor_comments
'Adding full bibliography for 7042167--7042177.cif.'
_cod_original_formula_sum        'C33.75 H32.50 Cl2.50 D1.50 Ir N4 O4.25'
_cod_database_code               7042176
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.303
_shelx_estimated_absorpt_t_max   0.631
_shelx_res_checksum              60966