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_7712059
_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
'C46 H27 F12 Ir N O3 P2, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C79 H41 B Cl2 F36 Ir N O3 P2'
_chemical_formula_weight         2071.98
_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                78.4747(8)
_cell_angle_beta                 78.8231(8)
_cell_angle_gamma                75.6702(8)
_cell_formula_units_Z            2
_cell_length_a                   13.31679(12)
_cell_length_b                   16.58920(16)
_cell_length_c                   18.86855(17)
_cell_measurement_reflns_used    55982
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5530
_cell_measurement_theta_min      2.7190
_cell_volume                     3911.19(7)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_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   -114.00 -14.00   1.00    1.00    -  -41.82 -57.00 150.00  100
  2  \w    -66.00  33.00   1.00    1.00    -  -41.82  37.00  60.00   99
  3  \w    -87.00  -6.00   1.00    1.00    -  -41.82 125.00  60.00   81
  4  \w   -116.00 -17.00   1.00    1.00    -  -41.82 -37.00-120.00   99
  5  \w     10.00  36.00   1.00    1.00    -   41.82  74.00  13.64   26
  6  \w      8.00  42.00   1.00    1.00    -   41.82  81.00 -82.07   34
  7  \w      7.00  33.00   1.00    1.00    -   41.82  84.00-119.42   26
  8  \w     34.00 133.00   1.00    3.50    -  107.00 -45.00  30.00   99
  9  \w     24.00 107.00   1.00    3.50    -  107.00 -94.00-150.00   83
 10  \w     24.00 107.00   1.00    3.50    -  107.00 -94.00 120.00   83
 11  \w     78.00 178.00   1.00    3.50    -  107.00  61.00 -60.00  100
 12  \w     81.00 178.00   1.00    3.50    -  107.00  45.00-120.00   97
 13  \w     34.00 112.00   1.00    3.50    -  107.00-125.00  60.00   78
 14  \w     78.00 178.00   1.00    3.50    -  107.00  61.00-180.00  100
 15  \w     81.00 178.00   1.00    3.50    -  107.00  45.00   0.00   97
 16  \w     97.00 178.00   1.00    3.50    -  107.00 125.00-180.00   81
 17  \w     31.00 140.00   1.00    3.50    -  107.00 -77.00 120.00  109
 18  \w     24.00 107.00   1.00    3.50    -  107.00 -94.00 -90.00   83
 19  \w     81.00 178.00   1.00    3.50    -  107.00  45.00 -90.00   97
 20  \w     31.00 109.00   1.00    3.50    -  107.00-111.00 112.22   78
 21  \w     81.00 178.00   1.00    3.50    -  107.00  45.00 -30.00   97
 22  \w     34.00 112.00   1.00    3.50    -  107.00-125.00  90.00   78
 23  \w     34.00 112.00   1.00    3.50    -  107.00-125.00  30.00   78
 24  \w    103.00 178.00   1.00    3.50    -  107.00  77.00 -90.00   75
 25  \w     34.00 112.00   1.00    3.50    -  107.00-125.00 -60.00   78
 26  \w     81.00 178.00   1.00    3.50    -  107.00  45.00  60.00   97
 27  \w     34.00 112.00   1.00    3.50    -  107.00-125.00 -30.00   78
 28  \w     24.00 107.00   1.00    3.50    -  107.00 -94.00 -30.00   83
 29  \w     24.00 107.00   1.00    3.50    -  107.00 -94.00   0.00   83
 30  \w     28.00 108.00   1.00    3.50    -  107.00-104.00-156.99   80
 31  \w   -116.00 -17.00   1.00    1.00    -  -41.82 -37.00 -30.00   99
 32  \w    -87.00  -6.00   1.00    1.00    -  -41.82 125.00-180.00   81
 33  \w   -116.00 -17.00   1.00    1.00    -  -41.82 -37.00  30.00   99
 34  \w    -87.00  -6.00   1.00    1.00    -  -41.82 125.00 -90.00   81
 35  \w      8.00  34.00   1.00    1.00    -   41.82  83.00 177.56   26
 36  \w     10.00  36.00   1.00    1.00    -   41.82  73.00  37.19   26
 37  \w      8.00  42.00   1.00    1.00    -   41.82  82.00  79.46   34
 38  \w     79.00 178.00   1.00    3.50    -  107.00  54.00  15.61   99
 39  \w     78.00 178.00   1.00    3.50    -  107.00  61.00 150.00  100
 40  \w     81.00 178.00   1.00    3.50    -  107.00  45.00  90.00   97
 41  \w     81.00 178.00   1.00    3.50    -  107.00  45.00 120.00   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      -0.0025102000
_diffrn_orient_matrix_UB_12      0.0430627000
_diffrn_orient_matrix_UB_13      0.0656830000
_diffrn_orient_matrix_UB_21      0.0923442000
_diffrn_orient_matrix_UB_22      -0.0700003000
_diffrn_orient_matrix_UB_23      0.0244946000
_diffrn_orient_matrix_UB_31      0.0778481000
_diffrn_orient_matrix_UB_32      0.0516993000
_diffrn_orient_matrix_UB_33      -0.0468359000
_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  0.0307
_diffrn_reflns_av_unetI/netI     0.0217
_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       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            76080
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.075
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         6.374
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.565
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.246
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.759
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2/hexane at 293 K'
_exptl_crystal_size_max          0.292
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.263
_refine_diff_density_min         -0.916
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1237
_refine_ls_number_reflns         14844
_refine_ls_number_restraints     840
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0314P)^2^+8.1332P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14483
_reflns_number_total             14844
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03608h2.cif
_cod_data_source_block           0671abc22s
_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        3911.18(7)
_cod_database_code               7712059
_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
 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
 with sigma of 0.01
 F16-F17 \\sim F17-F18 \\sim F18-F16
 with sigma of 0.01
 C221-F16 \\sim C221-F17 \\sim C221-F18
 with sigma of 0.01
 C215-F7 \\sim C215-F8 \\sim C215-F9 \\sim C215-F7A \\sim C215-F8A \\sim
C215-F9A
 with sigma of 0.01
 F7-F8 \\sim F8-F9 \\sim F9-F7 \\sim F7A-F8A \\sim F8A-F9A \\sim F9A-F7A
 with sigma of 0.01
 C211-F7 \\sim C211-F8 \\sim C211-F9 \\sim C211-F7A \\sim C211-F8A \\sim
C211-F9A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F11 \\sim F12 \\sim F13 \\sim F14 \\sim F15 \\sim F16 \\sim F17
\\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim F35
\\sim F36 \\sim F37 \\sim F45 \\sim F46 \\sim F47 \\sim F55 \\sim F56 \\sim F57
\\sim F65 \\sim F66 \\sim F67 \\sim F10A \\sim F11A \\sim F12A \\sim F1A \\sim
F2A \\sim F3A \\sim F9A \\sim F8A \\sim F7A \\sim C216 \\sim C207 \\sim C218
\\sim C219 \\sim C220 \\sim C221 \\sim C223 \\sim C224 \\sim C217 \\sim C222
\\sim C215 \\sim C91 \\sim Cl4 \\sim Cl3 \\sim Cl1 \\sim C90 \\sim Cl2: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
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(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\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(F19) \\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22)
\\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F35) \\sim Ueq,
Uanis(F36) \\sim Ueq, Uanis(F37) \\sim Ueq, Uanis(F45) \\sim Ueq, Uanis(F46)
\\sim Ueq, Uanis(F47) \\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(F10A) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12A) \\sim Ueq,
Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq, Uanis(F9A)
\\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(C216) \\sim Ueq,
Uanis(C207) \\sim Ueq, Uanis(C218) \\sim Ueq, Uanis(C219) \\sim Ueq,
Uanis(C220) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C223) \\sim Ueq,
Uanis(C224) \\sim Ueq, Uanis(C217) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C215) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(Cl4) \\sim Ueq, Uanis(Cl3)
\\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(Cl2) \\sim Ueq:
with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(2)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(2)
 Sof(F9A)=Sof(F8A)=Sof(F7A)=1-FVAR(3)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(3)
 Fixed Sof: Cl2(0.5) Cl1(0.5) C90(0.5) H90A(0.5) H90B(0.5) Cl4(0.5) Cl3(0.5)
 C91(0.5) H91A(0.5) H91B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C90(H90A,H90B), C91(H91A,H91B)
5.b Aromatic/amide H refined with riding coordinates:
 C202(H202), C204(H204), C206(H206), C210(H210), C212(H212), C214(H214),
 C218(H218), C220(H220), C222(H222), C226(H226), C228(H228), C230(H230), 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), C40(H40), C41(H41),
  C42(H42), C43(H43), C50(H50), C51(H51), C52(H52), C53(H53), C60(H60),
 C61(H61), C62(H62), C63(H63)
;
_shelx_res_checksum              83565
_shelx_hkl_checksum              29267
_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 1.596
_oxdiff_exptl_absorpt_empirical_full_min 0.802