Cyclometalated iridium complexes based on monodentate aminophosphanes
Palmese, Marco; Pérez-Torrente, Jesús J.; Passarelli, Vincenzo; Dalton Transactions  (2022) –; doi:10.1039/D2DT02081E

data_7710795
_publ_section_title
;
 Cyclometalated iridium complexes based on monodentate aminophosphanes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02081E
_journal_year                    2022
_chemical_formula_moiety
'C59 H57 Ir N4 P3, P F6, 1.5(C2 H3 N), 0.5(C4 H10 O)'
_chemical_formula_sum            'C64 H66.5 F6 Ir N5.5 O0.5 P4'
_chemical_formula_weight         1350.80
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-06-13 deposited with the CCDC.	2022-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.556(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8378(10)
_cell_length_b                   23.4102(8)
_cell_length_c                   20.6295(8)
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.282
_cell_measurement_theta_min      2.290
_cell_volume                     11990.8(8)
_computing_cell_refinement       'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_data_collection       'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2016) in APEX4'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            337915
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.975
_diffrn_source                   'Mo microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.399
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.7473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       prism
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.415
_refine_diff_density_min         -0.872
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1504
_refine_ls_number_reflns         22758
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0425P)^2^+27.7541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19821
_reflns_number_total             22758
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02081e3.cif
_cod_data_source_block           cmpd_12PF6_VPX396v_MP1195a
_cod_depositor_comments
;

2024-09-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C128 H133 F12 Ir2 N11 O P8'
_cod_original_formula_weight         2701.61
_cod_original_formula_moiety
'2 (C59 H57 Ir N4 P3), 2 (P F6), 3 (C2 H3 N), C4 H10 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7710795
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.659
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              46571
_shelx_hkl_checksum              517