Iridium complexes of an <i>ortho</i>-trifluoromethylphenyl substituted PONOP pincer ligand.
Poole, Ethan W.; Bustos, Itxaso; Hood, Thomas M.; Smart, Jennifer E.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 52 (2023) 1096–1104; doi:10.1039/d2dt03608h

data_7712058
_publ_section_title
;
 Iridium complexes of an <i>ortho</i>-trifluoromethylphenyl substituted
 PONOP pincer ligand.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1096
_journal_page_last               1104
_journal_paper_doi               10.1039/d2dt03608h
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety
'C45 H27 F12 Ir N O2 P2, C32 H12 B F24, C H2 Cl2'
_chemical_formula_sum            'C78 H41 B Cl2 F36 Ir N O2 P2'
_chemical_formula_weight         2043.97
_chemical_melting_point          ?
_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   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-03-03
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-11-02 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                83.9191(10)
_cell_angle_beta                 81.3532(10)
_cell_angle_gamma                79.1239(10)
_cell_formula_units_Z            2
_cell_length_a                   13.84188(16)
_cell_length_b                   16.00726(18)
_cell_length_c                   18.2641(2)
_cell_measurement_reflns_used    54128
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6870
_cell_measurement_theta_min      3.2300
_cell_volume                     3916.37(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6093
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -92.00  -2.00   1.00    1.00    -  -42.07 125.00 150.00   90
  2  \w   -117.00 -18.00   1.00    1.00    -  -42.07 -37.00 -90.00   99
  3  \w    -66.00  32.00   1.00    1.00    -  -42.07  37.00  90.00   98
  4  \w    -70.00  31.00   1.00    1.00    -  -42.07  57.00  30.00  101
  5  \w      1.00  83.00   1.00    1.00    -   42.07 -99.00 150.00   82
  6  \w     27.00 100.00   1.00    1.00    -   42.07-130.00  40.00   73
  7  \w     81.00 178.00   1.00    4.00    -  107.00  45.00  90.00   97
  8  \w     34.00 133.00   1.00    4.00    -  107.00 -45.00 -90.00   99
  9  \w     81.00 178.00   1.00    4.00    -  107.00  45.00 150.00   97
 10  \w     94.00 178.00   1.00    4.00    -  107.00 125.00   0.00   84
 11  \w     34.00 118.00   1.00    4.00    -  107.00-125.00-150.00   84
 12  \w     24.00 110.00   1.00    4.00    -  107.00 -94.00  60.00   86
 13  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 -30.00   84
 14  \w     34.00 118.00   1.00    4.00    -  107.00-125.00  60.00   84
 15  \w     81.00 178.00   1.00    4.00    -  107.00  45.00 120.00   97
 16  \w     34.00 118.00   1.00    4.00    -  107.00-125.00  30.00   84
 17  \w     81.00 178.00   1.00    4.00    -  107.00  45.00-150.00   97
 18  \w     81.00 178.00   1.00    4.00    -  107.00  45.00  30.00   97
 19  \w     34.00 118.00   1.00    4.00    -  107.00-125.00-120.00   84
 20  \w     34.00 118.00   1.00    4.00    -  107.00-125.00   0.00   84
 21  \w     34.00 118.00   1.00    4.00    -  107.00-125.00-180.00   84
 22  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 -60.00   84
 23  \w     34.00 118.00   1.00    4.00    -  107.00-125.00  90.00   84
 24  \w     81.00 178.00   1.00    4.00    -  107.00  45.00   0.00   97
 25  \w     34.00 133.00   1.00    4.00    -  107.00 -45.00 120.00   99
 26  \w     94.00 178.00   1.00    4.00    -  107.00 125.00 -30.00   84
 27  \w     35.00 136.00   1.00    4.00    -  107.00 -61.00  30.00  101
 28  \w     94.00 178.00   1.00    4.00    -  107.00 125.00  90.00   84
 29  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 120.00   84
 30  \w     94.00 178.00   1.00    4.00    -  107.00 125.00  30.00   84
 31  \w   -114.00 -14.00   1.00    1.00    -  -42.07 -57.00 120.00  100
 32  \w   -114.00 -14.00   1.00    1.00    -  -42.07 -57.00-180.00  100
 33  \w   -118.00  -9.00   1.00    1.00    -  -42.07 -77.00  90.00  109
 34  \w    -66.00  32.00   1.00    1.00    -  -42.07  37.00 -60.00   98
 35  \w   -118.00  -9.00   1.00    1.00    -  -42.07 -77.00   0.00  109
 36  \w   -118.00  -9.00   1.00    1.00    -  -42.07 -77.00-180.00  109
 37  \w   -118.00  -9.00   1.00    1.00    -  -42.07 -77.00 -90.00  109
 38  \w     74.00 114.00   1.00    4.00    -  107.00  77.00 150.00   40
 39  \w     74.00 178.00   1.00    4.00    -  107.00  77.00  30.00  104
 40  \w     74.00 178.00   1.00    4.00    -  107.00  77.00-150.00  104
 41  \w     78.00 178.00   1.00    4.00    -  107.00  61.00 -60.00  100
 42  \w     81.00 178.00   1.00    4.00    -  107.00  45.00 -90.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1051400000
_diffrn_orient_matrix_UB_12      -0.0036872000
_diffrn_orient_matrix_UB_13      0.0197885000
_diffrn_orient_matrix_UB_21      -0.0399648000
_diffrn_orient_matrix_UB_22      -0.0106905000
_diffrn_orient_matrix_UB_23      0.0832205000
_diffrn_orient_matrix_UB_31      0.0206355000
_diffrn_orient_matrix_UB_32      -0.0976634000
_diffrn_orient_matrix_UB_33      -0.0029729000
_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  0.0343
_diffrn_reflns_av_unetI/netI     0.0190
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            91834
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.074
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         6.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.537
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.314
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2/hexane at 293 K'
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.101
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1325
_refine_ls_number_reflns         14854
_refine_ls_number_restraints     1460
_refine_ls_restrained_S_all      1.210
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0558P)^2^+7.3234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14349
_reflns_number_total             14854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03608h2.cif
_cod_data_source_block           0477abc19s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7712055--7712059.cif.
;
_cod_original_cell_volume        3916.38(8)
_cod_database_code               7712058
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 P2-C38 \\sim P2-C38A
 with sigma of 0.01
 F45A-C44A \\sim F47A-C44A \\sim F46A-C44A \\sim F47-C44 \\sim F46-C44 \\sim
F45-C44
 with sigma of 0.01
 F45-F46 \\sim F46-F47 \\sim F47-F45 \\sim F45A-F46A \\sim F46A-F47A \\sim
F47A-F45A
 with sigma of 0.01
 F45A-C39A \\sim F47A-C39A \\sim F46A-C39A \\sim F47-C39 \\sim F46-C39 \\sim
F45-C39
 with sigma of 0.01
 C44A-C39A \\sim C44-C39
 with sigma of 0.01
 Cl2A-C90A \\sim Cl2-C90 \\sim Cl1A-C90A \\sim Cl1-C90
 with sigma of 0.01
 C207-F1 \\sim C207-F2 \\sim C207-F3 \\sim C207-F1A \\sim C207-F2A \\sim
C207-F3A
 with sigma of 0.01
 F1-F2 \\sim F2-F3 \\sim F3-F1 \\sim F1A-F2A \\sim F2A-F3A \\sim F3A-F1A
 with sigma of 0.01
 C203-F1 \\sim C203-F2 \\sim C203-F3 \\sim C203-F1A \\sim C203-F2A \\sim
C203-F3A
 with sigma of 0.01
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim
C216-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim
C213-F12A
 with sigma of 0.01
 C224-F16 \\sim C224-F17 \\sim C224-F18 \\sim C224-F16A \\sim C224-F17A \\sim
C224-F18A
 with sigma of 0.01
 F16-F17 \\sim F17-F18 \\sim F18-F16 \\sim F16A-F17A \\sim F17A-F18A \\sim
F18A-F16A
 with sigma of 0.01
 C221-F16 \\sim C221-F17 \\sim C221-F18 \\sim C221-F16A \\sim C221-F17A \\sim
C221-F18A
 with sigma of 0.01
 C208-F4 \\sim C208-F5 \\sim C208-F6 \\sim C208-F4A \\sim C208-F5A \\sim
C208-F6A
 with sigma of 0.01
 F4-F5 \\sim F5-F6 \\sim F6-F4 \\sim F4A-F5A \\sim F5A-F6A \\sim F6A-F4A
 with sigma of 0.01
 C205-F4 \\sim C205-F5 \\sim C205-F6 \\sim C205-F4A \\sim C205-F5A \\sim
C205-F6A
 with sigma of 0.01
 C223-F13 \\sim C223-F14 \\sim C223-F15 \\sim C223-F13A \\sim C223-F14A \\sim
C223-F15A
 with sigma of 0.01
 F13-F14 \\sim F14-F15 \\sim F15-F13 \\sim F13A-F14A \\sim F14A-F15A \\sim
F15A-F13A
 with sigma of 0.01
 C219-F13 \\sim C219-F14 \\sim C219-F15 \\sim C219-F13A \\sim C219-F14A \\sim
C219-F15A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F35 \\sim F36 \\sim F37 \\sim F55 \\sim F56 \\sim F57 \\sim F65 \\sim F66 \\sim
F67 \\sim F45 \\sim F46 \\sim F47 \\sim F45A \\sim F46A \\sim F47A \\sim F7
\\sim F8 \\sim F9 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24
\\sim F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F10 \\sim F11 \\sim
F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F1A \\sim
F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A \\sim F10A \\sim F11A \\sim F12A
\\sim F13A \\sim F14A \\sim F15A \\sim F16A \\sim F17A \\sim F18A \\sim C38
\\sim C39 \\sim C44 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44A \\sim
C39A \\sim C38A \\sim C43A \\sim C42A \\sim C41A \\sim C40A \\sim C90 \\sim
C90A \\sim Cl1 \\sim Cl2 \\sim Cl1A \\sim Cl2A \\sim C224 \\sim C207 \\sim C216
\\sim C208 \\sim C223: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
Uanis(F35) \\sim Ueq, Uanis(F36) \\sim Ueq, Uanis(F37) \\sim Ueq, Uanis(F55)
\\sim Ueq, Uanis(F56) \\sim Ueq, Uanis(F57) \\sim Ueq, Uanis(F65) \\sim Ueq,
Uanis(F66) \\sim Ueq, Uanis(F67) \\sim Ueq, Uanis(F45) \\sim Ueq, Uanis(F46)
\\sim Ueq, Uanis(F47) \\sim Ueq, Uanis(F45A) \\sim Ueq, Uanis(F46A) \\sim Ueq,
Uanis(F47A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq,
Uanis(F22) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F1)
\\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq,
Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11)
\\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq,
Uanis(F15) \\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F10A)
\\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F13A) \\sim Ueq,
Uanis(F14A) \\sim Ueq, Uanis(F15A) \\sim Ueq, Uanis(F16A) \\sim Ueq,
Uanis(F17A) \\sim Ueq, Uanis(F18A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41) \\sim Ueq,
Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44A) \\sim Ueq, Uanis(C39A)
\\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C43A) \\sim Ueq, Uanis(C42A) \\sim Ueq,
Uanis(C41A) \\sim Ueq, Uanis(C40A) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C90A)
\\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl1A) \\sim Ueq,
Uanis(Cl2A) \\sim Ueq, Uanis(C224) \\sim Ueq, Uanis(C207) \\sim Ueq,
Uanis(C216) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(C223) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl1A) = Uanis(Cl1)
Uanis(C90A) = Uanis(C90)
Uanis(Cl2A) = Uanis(Cl2)
4. Others
 Sof(Cl1A)=Sof(Cl2A)=Sof(C90A)=Sof(H90C)=Sof(H90D)=1-FVAR(1)
 Sof(Cl1)=Sof(Cl2)=Sof(C90)=Sof(H90A)=Sof(H90B)=FVAR(1)
 Sof(F45A)=Sof(F46A)=Sof(F47A)=Sof(C39A)=Sof(C40A)=Sof(H40A)=Sof(C41A)=
 Sof(H41A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C38A)=Sof(C44A)=1-FVAR(2)
 Sof(F45)=Sof(F46)=Sof(F47)=Sof(C39)=Sof(C38)=Sof(C43)=Sof(H43)=Sof(C42)=
 Sof(H42)=Sof(C41)=Sof(H41)=Sof(C40)=Sof(H40)=Sof(C44)=FVAR(2)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(3)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(3)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(4)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(4)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(5)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(5)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(6)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(6)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(7)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(7)
5.a Secondary CH2 refined with riding coordinates:
 C90(H90A,H90B), C90A(H90C,H90D)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C22(H22), C23(H23), C24(H24), C30(H30), C31(H31), C32(H32), C33(H33), C50(H50),
  C51(H51), C52(H52), C53(H53), C60(H60), C61(H61), C62(H62), C63(H63),
 C43(H43), C42(H42), C41(H41), C40(H40), C40A(H40A), C41A(H41A), C42A(H42A),
 C43A(H43A), C202(H202), C204(H204), C206(H206), C210(H210), C212(H212),
 C214(H214), C218(H218), C220(H220), C222(H222), C226(H226), C228(H228),
 C230(H230)
5.c Fitted hexagon refined as free rotating group:
 C39(C38,C43,C42,C41,C40), C39A(C40A,C41A,C42A,C43A,C38A)
;
_shelx_res_checksum              85501
_shelx_hkl_checksum              64171
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.072
_oxdiff_exptl_absorpt_empirical_full_min 0.740