Synthesis and reactivity of an iridium complex based on a tridentate aminophosphano ligand
Palmese, Marco; Pérez-Torrente, Jesús J.; Passarelli, Vincenzo; Dalton Transactions  (2022) –; doi:10.1039/D2DT00794K

data_7710107
_publ_section_title
;
 Synthesis and reactivity of an iridium complex based on a tridentate
 aminophosphano ligand
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00794K
_journal_year                    2022
_chemical_formula_moiety
'4 (C50 H57 Cl Ir N4 P2 Si), 3 (C4 H8 O), 4 (P F6)'
_chemical_formula_sum            'C212 H252 Cl4 F24 Ir4 N16 O3 P12 Si4'
_chemical_formula_weight         4922.88
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2022-03-01 deposited with the CCDC.	2022-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.1930(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   46.824(5)
_cell_length_b                   10.9773(11)
_cell_length_c                   25.668(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.245
_cell_measurement_theta_min      2.253
_cell_volume                     11286(2)
_computing_cell_refinement       'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_data_collection       'SMART in APEX2 (Bruker AXS,2008)'
_computing_data_reduction        'SAINT+ in APEX2 (Bruker AXS,2008)'
_computing_molecular_graphics    'XP program, SHELXTL v6.12, Bruker2000'
_computing_publication_material  'XCIF program, PLATON(Spek, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX DUO system'
_diffrn_measurement_method       '\w and \f rotations with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       60
_diffrn_reflns_limit_h_min       -60
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58271
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_min         1.915
_exptl_absorpt_coefficient_mu    2.579
_exptl_absorpt_correction_T_max  0.6846
_exptl_absorpt_correction_T_min  0.5347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       prism
_exptl_crystal_F_000             4976
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.175
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.485
_refine_diff_density_min         -1.093
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         12421
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0273P)^2^+35.0598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10134
_reflns_number_total             12421
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00794k2.cif
_cod_data_source_block           4PF6
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7710107
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              72559