Challenges in cyclometalation: steric effects leading to competing pathways and η<sup>1</sup>,η<sup>2</sup>-cyclometalated iridium(iii) complexes.
Chen, Houguang Jeremy; Teo, Ronald Hong Xiang; Wong, Jonathan; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13046–13051; doi:10.1039/c8dt02639d

data_7047276
_publ_section_title
;
 Challenges in cyclometalation: steric effects leading to competing
 pathways and \h<sup>1</sup>,\h<sup>2</sup>-cyclometalated iridium(iii)
 complexes.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13046
_journal_page_last               13051
_journal_paper_doi               10.1039/c8dt02639d
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_sum            'C23 H29 Cl Ir N'
_chemical_formula_weight         547.12
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_update_record
;
2018-08-04 deposited with the CCDC.
2018-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.8309(9)
_cell_length_b                   18.449(2)
_cell_length_c                   28.858(3)
_cell_measurement_reflns_used    8791
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      29.2505
_cell_measurement_theta_min      5.0958
_cell_volume                     4169.2(8)
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2016)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'XP (Bruker AXS Inc., 2016)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Bruker AXS Inc., 2016)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            35193
_diffrn_reflns_theta_full        31.08
_diffrn_reflns_theta_max         31.08
_diffrn_reflns_theta_min         5.10
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker KappaCCD'
_exptl_absorpt_coefficient_mu    6.539
_exptl_absorpt_correction_T_max  0.28
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.260
_refine_diff_density_max         2.375
_refine_diff_density_min         -1.503
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.021(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         13198
_refine_ls_number_restraints     595
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0378
_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^)+(0.0117P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0623
_refine_ls_wR_factor_ref         0.0646
_reflns_number_gt                11509
_reflns_number_total             13198
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02639d2.cif
_cod_data_source_block           leung788
_cod_depositor_comments
'Adding full bibliography for 7047276--7047278.cif.'
_cod_database_code               7047276
_shelx_res_checksum              11102