Crystal structures of the (η2:η2-cycloocta-1,5-diene)(η6-toluene)iridium(I) cation and μ-chlorido-iridium(III) complexes of 2-(phosphinito)- and 2-(phosphinomethyl)anthraquinone ligands
Thackeray, Sachin; Mahoney, James; Arrington, Ashleigh; Wilklow-Marnell, Miles; Brennessel, William W.; Acta Crystallographica Section E Crystallographic Communications 80 (2024) 1101–1109; doi:10.1107/S2056989024008922

data_2023272
_publ_section_title
;
 Crystal structures of the
 (\h2:\h2-cycloocta-1,5-diene)(\h6-toluene)iridium(I) cation and
 \m-chlorido-iridium(III) complexes of 2-(phosphinito)- and
 2-(phosphinomethyl)anthraquinone ligands
;
_journal_coeditor_code           JY2049
_journal_issue                   10
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              1101
_journal_page_last               1109
_journal_paper_doi               10.1107/S2056989024008922
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac
'[Ir (C7 H8) (C8 H12)], [Ir2 H2 (C22 H24 O3 P1)2 Cl3], C7 H8'
_chemical_formula_moiety         'C15 H20 Ir1 +, C44 H50 Cl3 Ir2 O6 P2 -, C7 H8'
_chemical_formula_sum            'C66 H78 Cl3 Ir3 O6 P2'
_chemical_formula_weight         1712.17
_chemical_name_systematic
;(\h^2^:\h^2^-Cycloocta-1,5-diene)(\h^6^-toluene)iridium(I)
tri-\m-chlorido-bis({3-[(di-<i>tert</i>-butylphosphanyl)oxy]-9,10-dioxoanthracen-2-yl}hydridoiridium(III)) toluene monosolvate,
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.5-ac6-015
(compiled 2023.12.04 svn.r209d9fb2 for Rigaku Oxford Diffraction, GUI svn.r6873)
;
_cell_angle_alpha                88.5722(12)
_cell_angle_beta                 87.0030(12)
_cell_angle_gamma                79.7149(11)
_cell_formula_units_Z            2
_cell_length_a                   13.15698(17)
_cell_length_b                   13.58360(18)
_cell_length_c                   17.5470(3)
_cell_measurement_reflns_used    23439
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.5950
_cell_measurement_theta_min      2.5490
_cell_volume                     3080.99(8)
_computing_cell_refinement
;
CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)
;
_computing_data_collection
;
CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)
;
_computing_data_reduction
;
CrysAlisPro 1.171.42.101a (Rigaku OD, 2023)
;
_computing_molecular_graphics
;
Olex2 1.5-ac6-015 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
Olex2 1.5-ac6-015 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
<i>SHELXL2019/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/2</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            51464
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         78.197
_diffrn_reflns_theta_min         2.522
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    14.378
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64287
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Rigaku OD, 2023)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       plate
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.011
_refine_diff_density_max         1.521
_refine_diff_density_min         -1.718
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     881
_refine_ls_number_reflns         12864
_refine_ls_number_restraints     395
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0514P)^2^+3.1792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0919
_reflns_number_gt                11114
_reflns_number_total             12864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jy2049.cif
_cod_data_source_block           1
_cod_database_code               2023272
_shelx_estimated_absorpt_t_min   0.342
_shelx_estimated_absorpt_t_max   0.858
_shelx_hkl_checksum              46952
_shelx_res_checksum              32912