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_7712057
_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
'C39 H31 F12 Ir N O2 P2, C32 H12 B F24, 0.5[C5H12]'
_chemical_formula_sum            'C73.5 H49 B F36 Ir N O2 P2'
_chemical_formula_weight         1927.08
_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             2022-12-12
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-12-12 deposited with the CCDC.	2022-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                70.0356(13)
_cell_angle_beta                 85.5560(11)
_cell_angle_gamma                67.5931(13)
_cell_formula_units_Z            2
_cell_length_a                   13.06139(17)
_cell_length_b                   16.8397(2)
_cell_length_c                   20.1252(3)
_cell_measurement_reflns_used    36175
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4550
_cell_measurement_theta_min      2.9800
_cell_volume                     3839.33(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.40a (Rigaku OD, 2019)'
_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 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   -117.00 -18.00   1.00    1.00    -  -42.07 -37.00 -30.00   99
  2  \w   -117.00 -18.00   1.00    1.00    -  -42.07 -37.00-120.00   99
  3  \w   -117.00 -18.00   1.00    1.00    -  -42.07 -37.00 150.00   99
  4  \w     23.00  98.00   1.00    1.00    -   42.07-125.00   0.00   75
  5  \w      1.00  83.00   1.00    1.00    -   42.07 -99.00 120.00   82
  6  \w     81.00 178.00   1.00    4.00    -  107.00  45.00-150.00   97
  7  \w     78.00 178.00   1.00    4.00    -  107.00  61.00 150.00  100
  8  \w     94.00 178.00   1.00    4.00    -  107.00 125.00  60.00   84
  9  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 -60.00   84
 10  \w     94.00 178.00   1.00    4.00    -  107.00 125.00 150.00   84
 11  \w     35.00 136.00   1.00    4.00    -  107.00 -61.00 120.00  101
 12  \w     24.00 110.00   1.00    4.00    -  107.00 -94.00  60.00   86
 13  \w     34.00 133.00   1.00    4.00    -  107.00 -45.00-120.00   99
 14  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 -30.00   84
 15  \w     81.00 178.00   1.00    4.00    -  107.00  45.00-120.00   97
 16  \w     24.00 110.00   1.00    4.00    -  107.00 -94.00 120.00   86
 17  \w     24.00 110.00   1.00    4.00    -  107.00 -94.00 150.00   86
 18  \w     34.00 118.00   1.00    4.00    -  107.00-125.00   0.00   84
 19  \w     81.00 178.00   1.00    4.00    -  107.00  45.00  90.00   97
 20  \w     24.00 110.00   1.00    4.00    -  107.00 -94.00-150.00   86
 21  \w     94.00 178.00   1.00    4.00    -  107.00 125.00-150.00   84
 22  \w     78.00 178.00   1.00    4.00    -  107.00  61.00 120.00  100
 23  \w     34.00 118.00   1.00    4.00    -  107.00-125.00-180.00   84
 24  \w     34.00 133.00   1.00    4.00    -  107.00 -45.00 120.00   99
 25  \w     31.00 113.00   1.00    4.00    -  107.00-111.00  27.45   82
 26  \w   -118.00  -9.00   1.00    1.00    -  -42.07 -77.00 -60.00  109
 27  \w   -114.00 -14.00   1.00    1.00    -  -42.07 -57.00  90.00  100
;
_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      0.0495512000
_diffrn_orient_matrix_UB_12      -0.0606276000
_diffrn_orient_matrix_UB_13      -0.0461270000
_diffrn_orient_matrix_UB_21      -0.0358829000
_diffrn_orient_matrix_UB_22      0.0854746000
_diffrn_orient_matrix_UB_23      -0.0671510000
_diffrn_orient_matrix_UB_31      0.1122220000
_diffrn_orient_matrix_UB_32      0.0087619000
_diffrn_orient_matrix_UB_33      0.0045280000
_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  0.0883
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57249
_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         6.379
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.297
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.40a (Rigaku Oxford Diffraction, 2019)
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    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             1898
_exptl_crystal_recrystallization_method
'Crystals grown from Mesitylene/pentane/tert-butylethylene at 293 K'
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.075
_refine_diff_density_max         2.576
_refine_diff_density_min         -3.054
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1224
_refine_ls_number_reflns         14565
_refine_ls_number_restraints     1269
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1288P)^2^+4.1358P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1739
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13639
_reflns_number_total             14565
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03608h2.cif
_cod_data_source_block           0491abc19s_CCDC1
_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_formula_sum        'C73.50 H49 B F36 Ir N O2 P2'
_cod_database_code               7712057
_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
 At 1.5 times of:
  All C(H,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
 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
 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
 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
 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
 C231-F19 \\sim C231-F20 \\sim C231-F21 \\sim C231-F19A \\sim C231-F20A \\sim
C231-F21A
 with sigma of 0.01
 F19-F20 \\sim F20-F21 \\sim F21-F19 \\sim F19A-F20A \\sim F20A-F21A \\sim
F21A-F19A
 with sigma of 0.01
 C227-F19 \\sim C227-F20 \\sim C227-F21 \\sim C227-F19A \\sim C227-F20A \\sim
C227-F21A
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim
C232-F24A
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim
F24A-F22A
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim
C229-F24A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F36 \\sim F37 \\sim F38 \\sim F46 \\sim F47 \\sim F48 \\sim F56 \\sim F57 \\sim
F58 \\sim F66 \\sim F67 \\sim F68 \\sim F10 \\sim F11 \\sim F12 \\sim F1 \\sim
F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9 \\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 F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A
\\sim F6A \\sim F7A \\sim F8A \\sim F9A \\sim F13A \\sim F14A \\sim F15A \\sim
F16A \\sim F17A \\sim F18A \\sim F19A \\sim F20A \\sim F21A \\sim F22A \\sim
F23A \\sim F24A \\sim C207 \\sim C231 \\sim C232 \\sim C224 \\sim C223 \\sim
C215 \\sim C208 \\sim C4 \\sim C5 \\sim C7 \\sim C6 \\sim C9 \\sim C8: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(F36) \\sim Ueq, Uanis(F37) \\sim Ueq, Uanis(F38) \\sim Ueq, Uanis(F46)
\\sim Ueq, Uanis(F47) \\sim Ueq, Uanis(F48) \\sim Ueq, Uanis(F56) \\sim Ueq,
Uanis(F57) \\sim Ueq, Uanis(F58) \\sim Ueq, Uanis(F66) \\sim Ueq, Uanis(F67)
\\sim Ueq, Uanis(F68) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq,
Uanis(F12) \\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(F7)
\\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\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(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7A)
\\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9A) \\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(F19A) \\sim Ueq,
Uanis(F20A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22A) \\sim Ueq,
Uanis(F23A) \\sim Ueq, Uanis(F24A) \\sim Ueq, Uanis(C207) \\sim Ueq,
Uanis(C231) \\sim Ueq, Uanis(C232) \\sim Ueq, Uanis(C224) \\sim Ueq,
Uanis(C223) \\sim Ueq, Uanis(C215) \\sim Ueq, Uanis(C208) \\sim Ueq, Uanis(C4)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq,
Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.006 and sigma for
terminal atoms of 0.012
4. Others
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(2)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(4)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(4)
 Sof(F13A)=Sof(F14A)=Sof(F15A)=1-FVAR(5)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(5)
 Fixed Sof: F7(0.5) F8(0.5) F9(0.5) F16(0.5) F17(0.5) F18(0.5) F7A(0.5)
 F8A(0.5) F9A(0.5) F16A(0.5) F17A(0.5) F18A(0.5)
5.a Ternary CH refined with riding coordinates:
 C5(H5)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B)
5.c Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C30(H30), C31(H31), C32(H32), C33(H33),
 C41(H41), C42(H42), C43(H43), C44(H44), C51(H51), C52(H52), C53(H53), C54(H54),
  C61(H61), C62(H62), C63(H63), C64(H64), 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.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 40 electrons were 
found in a volume of 307\%A^3^ in 3 voids per unit cell. 
This is consistent with the presence of 
0.5[C5H12] per Asymmetric Unit 
which account for 42 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              11639
_shelx_hkl_checksum              26657
_shelx_fab_checksum              94756
_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 2.359
_oxdiff_exptl_absorpt_empirical_full_min 0.488