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_7710106
_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
'2(C50 H58 Ir N4 P2 Si), 2 (P F6), C H2 Cl2, C6 H14'
_chemical_formula_sum            'C107 H132 Cl2 F12 Ir2 N8 P6 Si2'
_chemical_formula_weight         2455.50
_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     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                86.1880(10)
_cell_angle_beta                 77.4030(10)
_cell_angle_gamma                85.9510(10)
_cell_formula_units_Z            1
_cell_length_a                   10.9615(7)
_cell_length_b                   12.7205(8)
_cell_length_c                   20.4705(12)
_cell_measurement_reflns_used    9807
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.436
_cell_measurement_theta_min      2.422
_cell_volume                     2774.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       '\w rotations with narrow frames'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0280
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34093
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.858
_exptl_absorpt_coefficient_mu    2.621
_exptl_absorpt_correction_T_max  0.5792
_exptl_absorpt_correction_T_min  0.4326
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Multi-scan correction included in APEX2 package (Bruker AXS, 2008)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       prism
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     630
_refine_ls_number_reflns         11291
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0293
_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^)+(0.0400P)^2^+4.4671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10499
_reflns_number_total             11291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00794k2.cif
_cod_data_source_block           1PF6
_cod_database_code               7710106
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_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.
;
_shelx_res_checksum              82622