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_7712055
_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 Cl F12 Ir N O2 P2, 2(C H2 Cl2)'
_chemical_formula_sum            'C47 H31 Cl5 F12 Ir N O2 P2'
_chemical_formula_weight         1301.12
_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                105.4598(16)
_cell_angle_beta                 96.9097(19)
_cell_angle_gamma                95.2546(18)
_cell_formula_units_Z            2
_cell_length_a                   11.7656(3)
_cell_length_b                   12.2782(2)
_cell_length_c                   17.0512(3)
_cell_measurement_reflns_used    25055
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4110
_cell_measurement_theta_min      3.7330
_cell_volume                     2337.09(9)
_computing_cell_refinement       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.39a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.39a (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   -118.00  -9.00   1.00    1.00    -  -41.82 -77.00 -60.00  109
  2  \w   -116.00 -17.00   1.00    1.00    -  -41.82 -37.00-180.00   99
  3  \w      1.00  83.00   1.00    1.00    -   41.82 -99.00  60.00   82
  4  \w    -33.00  66.00   1.00    1.00    -   41.82 -37.00  90.00   99
  5  \w     23.00  98.00   1.00    1.00    -   41.82-125.00-180.00   75
  6  \w     81.00 178.00   1.00    4.00    -  107.00  45.00 120.00   97
  7  \w     34.00 118.00   1.00    4.00    -  107.00-125.00-180.00   84
  8  \w     31.00 140.00   1.00    4.00    -  107.00 -77.00   0.00  109
  9  \w     34.00 118.00   1.00    4.00    -  107.00-125.00   0.00   84
 10  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 -90.00   84
 11  \w     94.00 178.00   1.00    4.00    -  107.00 125.00   0.00   84
 12  \w     94.00 178.00   1.00    4.00    -  107.00 125.00  90.00   84
 13  \w     35.00 136.00   1.00    4.00    -  107.00 -61.00  60.00  101
 14  \w     34.00 118.00   1.00    4.00    -  107.00-125.00-120.00   84
 15  \w     94.00 178.00   1.00    4.00    -  107.00 125.00  60.00   84
 16  \w     34.00 118.00   1.00    4.00    -  107.00-125.00  60.00   84
 17  \w     34.00 118.00   1.00    4.00    -  107.00-125.00 -60.00   84
 18  \w     81.00 178.00   1.00    4.00    -  107.00  45.00   0.00   97
 19  \w     24.00 110.00   1.00    4.00    -  107.00 -94.00  60.00   86
 20  \w     81.00 178.00   1.00    4.00    -  107.00  45.00 -60.00   97
 21  \w     78.00 178.00   1.00    4.00    -  107.00  61.00  60.00  100
 22  \w     81.00 178.00   1.00    4.00    -  107.00  45.00  90.00   97
 23  \w     34.00 133.00   1.00    4.00    -  107.00 -45.00   0.00   99
 24  \w     81.00 178.00   1.00    4.00    -  107.00  45.00-180.00   97
 25  \w     34.00 133.00   1.00    4.00    -  107.00 -45.00-180.00   99
 26  \w     94.00 178.00   1.00    4.00    -  107.00 125.00  30.00   84
 27  \w   -118.00  -9.00   1.00    1.00    -  -41.82 -77.00-180.00  109
 28  \w   -118.00  -9.00   1.00    1.00    -  -41.82 -77.00-120.00  109
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1297320000
_diffrn_orient_matrix_UB_12      -0.0053617000
_diffrn_orient_matrix_UB_13      0.0226385000
_diffrn_orient_matrix_UB_21      -0.0142131000
_diffrn_orient_matrix_UB_22      0.0249867000
_diffrn_orient_matrix_UB_23      0.0915015000
_diffrn_orient_matrix_UB_31      -0.0256840000
_diffrn_orient_matrix_UB_32      -0.1287715000
_diffrn_orient_matrix_UB_33      -0.0103330000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.058
_diffrn_reflns_theta_max         70.058
_diffrn_reflns_theta_min         6.667
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.616
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.39a (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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.849
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2/hexane at 293 K'
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.073
_refine_diff_density_max         2.053
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8851
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.4688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.0941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8621
_reflns_number_total             8851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03608h2.cif
_cod_data_source_block           0475abc19s
_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        2337.08(9)
_cod_database_code               7712055
_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. Uiso/Uaniso restraints and constraints
Uanis(Cl2) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C91(H91A,H91B), C90(H90A,H90B)
3.b Aromatic/amide H refined with riding coordinates:
 C50(H50), C22(H22), C13(H13), C33(H33), C60(H60), C30(H30), C14(H14),
 C23(H23), C63(H63), C12(H12), C24(H24), C11(H11), C62(H62), C43(H43), C42(H42),
  C7(H7), C5(H5), C51(H51), C32(H32), C8(H8), C6(H6), C31(H31), C61(H61),
 C52(H52), C40(H40), C41(H41), C53(H53)
;
_shelx_res_checksum              88175
_shelx_hkl_checksum              2857
_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 909.082
_oxdiff_exptl_absorpt_empirical_full_min 0.535