Syntheses and crystal structures of 4-benzyl-1-ethyl-1,2,4-triazolium bromide and its corresponding NHC complexes of rhodium and iridium.
Lerch, Timothy G.; Albert, Daniel R.; Gau, Michael; Rajaseelan, Edward; Acta crystallographica. Section E, Crystallographic communications 81 (2025) 350–357; doi:10.1107/S2056989025002671

data_2023460
_publ_section_title
;
 Syntheses and crystal structures of 4-benzyl-1-ethyl-1,2,4-triazolium
 bromide and its corresponding NHC complexes of rhodium and iridium.
;
_journal_issue                   'Pt 4'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              350
_journal_page_last               357
_journal_paper_doi               10.1107/S2056989025002671
_journal_volume                  81
_journal_year                    2025
_chemical_formula_iupac          '[Ir (C8 H12) (C11 H13 N3) (C18 H15 P)] B F4'
_chemical_formula_moiety         'C37 H40 Ir N3 P +, B F4 -'
_chemical_formula_sum            'C37 H40 B F4 Ir N3 P'
_chemical_formula_weight         836.70
_chemical_name_systematic
'(4-Benzyl-1-ethyl-1,2,4-triazol-5-ylidene)[(1,2,5,6-\h)-cycloocta-1,5-diene](triphenylphosphane)iridium(I) tetrafluoridoborate'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_cell_angle_alpha                79.8203(14)
_cell_angle_beta                 86.1222(13)
_cell_angle_gamma                89.3859(13)
_cell_formula_units_Z            2
_cell_length_a                   9.47197(15)
_cell_length_b                   9.50712(15)
_cell_length_c                   18.7104(3)
_cell_measurement_reflns_used    35729
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.3180
_cell_measurement_theta_min      2.1550
_cell_volume                     1654.57(5)
_computing_cell_refinement
;
CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)
;
_computing_data_collection
'CrysAlisPro system (CCD 43.142a 64-bit (release 17-10-2024))'
_computing_data_reduction
;
CrysAlisPro 1.171.43.142a (Rigaku OD, 2024)
;
_computing_molecular_graphics
;
Olex2 1.3 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018/3 (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0452
_diffrn_reflns_av_unetI/netI     0.0448
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            50908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.155
_exptl_absorpt_coefficient_mu    4.138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SCALE3 ABSPACK; Rigaku OD, 2024)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_description       block
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         3.377
_refine_diff_density_min         -1.118
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 6303 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons <i>et al.</i>,  2013)
;
_refine_ls_abs_structure_Flack   -0.008(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         15249
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0302P)^2^+0.5824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0617
_reflns_number_gt                14450
_reflns_number_total             15249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hb8128.cif
_cod_data_source_block           5
_cod_depositor_comments
'Adding full bibliography for 2023458--2023461.cif.'
_cod_database_code               2023460
_shelx_estimated_absorpt_t_min   0.360
_shelx_estimated_absorpt_t_max   0.450
_shelx_hkl_checksum              9513
_shelx_res_checksum              36101