Chiral CNN pincer Ir(III)-H complexes. Transient ligand and counterion influences in the asymmetric hydrogenation of imines and quinolines.
Wen, Yisong; Cabré, Albert; Benet-Buchholz, Jordi; Riera, Antoni; Verdaguer, Xavier; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10246–10253; doi:10.1039/d5dt00667h

data_7718838
_publ_section_title
;
 Chiral CNN pincer Ir(III)-H complexes. Transient ligand and counterion
 influences in the asymmetric hydrogenation of imines and quinolines.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10246
_journal_page_last               10253
_journal_paper_doi               10.1039/d5dt00667h
_journal_volume                  54
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety
'3(C40 H56 Ir N3 O P), 3(C32 H12 B F24), 0.5(C4 H10 O)'
_chemical_formula_sum            'C218 H209 B3 F72 Ir3 N9 O3.5 P3'
_chemical_formula_weight         5080.87
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2025-05-16
_audit_creation_method
;
Olex2 1.5-ac7-014
(compiled 2025.02.27 svn.r6f4c0eaf for Rigaku Oxford Diffraction, GUI svn.r7171)
;
_audit_update_record
;
2025-05-20 deposited with the CCDC.	2025-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                99.8450(10)
_cell_angle_beta                 90.5121(10)
_cell_angle_gamma                93.7691(10)
_cell_formula_units_Z            1
_cell_length_a                   13.52384(16)
_cell_length_b                   14.17502(16)
_cell_length_c                   28.9261(3)
_cell_measurement_reflns_used    92749
_cell_measurement_temperature    100
_cell_measurement_theta_max      34.2050
_cell_measurement_theta_min      1.8210
_cell_volume                     5450.53(11)
_computing_cell_refinement       'CrysAlisPro 1.171.44.110a (Rigaku OD, 2025)'
_computing_data_collection
'CrysAlisPro system (CCD 39.12b (release 24-11-2016))'
_computing_data_reduction        'CrysAlisPro 1.171.44.110a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac7-014 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_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    -50.00  57.10   0.30   15.00    --  -29.90  39.00-131.00  357
  2  \w   -118.00 -82.00   0.30   15.00    --  -29.90  39.00-131.00  120
  3  \w     56.00  81.50   0.30   15.00    --    5.00  39.00-131.00   85
  4  \w    -74.00 -45.20   0.30   15.00    --    5.00  39.00-131.00   96
  5  \w   -119.00  56.20   0.30   15.00    --  -29.90  55.00 -30.00  584
  6  \w   -119.00  58.00   0.30   15.00    --  -29.90  55.00  60.00  590
  7  \w   -119.00 -93.20   0.30   15.00    --  -29.90  55.00-150.00   86
  8  \w    -66.00  54.00   0.30   15.00    --  -29.90  55.00-150.00  400
  9  \w   -119.00  57.10   0.30   15.00    --  -29.90  55.00  30.00  587
 10  \w   -118.00  57.20   0.30   15.00    --  -29.90  55.00 -60.00  584
 11  \w   -118.00  58.10   0.30   15.00    --  -29.90  55.00 150.00  587
 12  \w   -118.00 -58.00   0.30   15.00    --  -29.90  55.00-120.00  200
 13  \w     33.00  57.90   0.30   15.00    --  -29.90  55.00-120.00   83
 14  \w   -119.00  58.00   0.30   15.00    --  -29.90  55.00 120.00  590
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0106012000
_diffrn_orient_matrix_UB_12      0.0382748000
_diffrn_orient_matrix_UB_13      -0.0117677000
_diffrn_orient_matrix_UB_21      0.0431673000
_diffrn_orient_matrix_UB_22      0.0268005000
_diffrn_orient_matrix_UB_23      0.0103294000
_diffrn_orient_matrix_UB_31      0.0281066000
_diffrn_orient_matrix_UB_32      -0.0202334000
_diffrn_orient_matrix_UB_33      -0.0193550000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            202831
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.333
_diffrn_reflns_theta_min         1.657
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.967
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.44.110a (Rigaku Oxford Diffraction, 2025)
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    1.548
_exptl_crystal_description       block
_exptl_crystal_F_000             2547
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.172
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 30432 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0132(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3400
_refine_ls_number_reflns         85423
_refine_ls_number_restraints     1924
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0632P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1134
_reflns_Friedel_coverage         0.958
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                72512
_reflns_number_total             85423
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00667h2.cif
_cod_data_source_block           acm_m96clt_jbb62
_cod_depositor_comments
'Adding full bibliography for 7718837--7718838.cif.'
_cod_original_cell_volume        5450.54(11)
_cod_original_formula_sum        'C218 H209 B3 F72 Ir3 N9 O3.50 P3'
_cod_database_code               7718838
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C72H66B1F24Ir1N3O1P1
_chemical_oxdiff_usercomment     'colourless plate'
_diffrn_oxdiff_digest_od_ed
;

;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4HA,H4HB,H4HC} of C4H, All C(H,H) groups
 At 1.5 times of:
  All Ir(H) groups, {H5CA,H5CB,H5CC} of C5C, {H6CA,H6CB,H6CC} of C6C, {H1IA,
  H1IB,H1IC} of C1I, {H4IA,H4IB,H4IC} of C4I, {H1HA,H1HB,H1HC} of C1H, {H6AA,
  H6AB,H6AC} of C6A, {H5AA,H5AB,H5AC} of C5A, {H6BA,H6BB,H6BC} of C6B, {H5BA,
  H5BB,H5BC} of C5B
2. Restrained distances
 C13S-C16S
 1.5 with sigma of 0.01
 C13S-C16W
 1.5 with sigma of 0.01
 C16S-F10S
 1.36 with sigma of 0.01
 C16S-F11S
 1.36 with sigma of 0.01
 C16S-F12S
 1.36 with sigma of 0.01
 F10S-F11S
 -2.13 with sigma of 0.02
 F11S-F12S
 -2.13 with sigma of 0.02
 F12S-F10S
 -2.13 with sigma of 0.02
 C16W-F10W
 1.36 with sigma of 0.01
 C16W-F11W
 1.36 with sigma of 0.01
 C16W-F12W
 1.36 with sigma of 0.01
 F10W-F11W
 -2.13 with sigma of 0.02
 F11W-F12W
 -2.13 with sigma of 0.02
 F12W-F10W
 -2.13 with sigma of 0.02
 C24S-F16S
 1.36 with sigma of 0.01
 C24S-F17S
 1.36 with sigma of 0.01
 C24S-F18S
 1.36 with sigma of 0.01
 F16S-F17S
 -2.13 with sigma of 0.02
 F17S-F18S
 -2.13 with sigma of 0.02
 F18S-F16S
 -2.13 with sigma of 0.02
 C24S-F16W
 1.36 with sigma of 0.01
 C24S-F17W
 1.36 with sigma of 0.01
 C24S-F18W
 1.36 with sigma of 0.01
 F16W-F17W
 -2.13 with sigma of 0.02
 F17W-F18W
 -2.13 with sigma of 0.02
 F18W-F16W
 -2.13 with sigma of 0.02
 C8U-F4U
 1.36 with sigma of 0.01
 C8U-F5U
 1.36 with sigma of 0.01
 C8U-F6U
 1.36 with sigma of 0.01
 C8U-F4V
 1.36 with sigma of 0.01
 C8U-F5V
 1.36 with sigma of 0.01
 C8U-F6V
 1.36 with sigma of 0.01
 C32U-F22U
 1.36 with sigma of 0.01
 C32U-F23U
 1.36 with sigma of 0.01
 C32U-F24U
 1.36 with sigma of 0.01
 F22U-F23U
 -2.13 with sigma of 0.02
 F23U-F24U
 -2.13 with sigma of 0.02
 F24U-F22U
 -2.13 with sigma of 0.02
 C32V-F22V
 1.36 with sigma of 0.01
 C32V-F23V
 1.36 with sigma of 0.01
 C32V-F24V
 1.36 with sigma of 0.01
 F22V-F23V
 -2.13 with sigma of 0.02
 F23V-F24V
 -2.13 with sigma of 0.02
 F24V-F22V
 -2.13 with sigma of 0.02
 C1I-C2I
 1.54 with sigma of 0.02
 C2I-O1I
 1.43 with sigma of 0.02
 O1I-C3I
 1.43 with sigma of 0.02
 C3I-C4I
 1.54 with sigma of 0.02
 C1H-C2H
 1.54 with sigma of 0.02
 C2H-O1H
 1.43 with sigma of 0.02
 O1H-C3H
 1.43 with sigma of 0.02
 C3H-C4H
 1.54 with sigma of 0.02
3. Rigid bond restraints
 F4S, F5S, F6S, F4W, F5W, F6W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F10S, F11S, F12S, C16W, F10W, F11W, F12W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16S, F10S, F11S, F12S, C16W, F10W, F11W, F12W, C13S, F13S, C14S, F14S, C15S,
 F15S, C17S, C18S, F16S, F17S, F18S, F16W, F17W, F18W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F19S, F20S, F21S, F19W, F20W, F21W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F22S, F23S, F24S, F22W, F23W, F24W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1T, F2T, F3T, F1W, F2W, F3W
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F4T, F5T, F6T, F4X, F5X, F6X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7T, F8T, F9T, F7X, F8X, F9X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F10T, F11T, F12T, F10X, F11X, F12X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F19T, F20T, F21T, F19X, F20X, F21X
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F1U, F2U, F3U, F1V, F2V, F3V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F4U, F5U, F6U, F4V, F5V, F6V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F7U, F8U, F9U, F7V, F8V, F9V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F13U, F14U, F15U, F13V, F14V, F15V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C16U, F10U, F11U, F12U, F10V, F11V, F12V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F16U, F17U, F18U, F16V, F17V, F18V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 F19U, F20U, F21U, F19V, F20V, F21V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C32U, F22U, F23U, F24U, C32V, F22V, F23V, F24V
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1I, C2I, O1I, C3I, C4I, C1H, C2H, O1H, C3H, C4H
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F4S \\sim F5S \\sim F6S \\sim F4W \\sim F5W \\sim F6W: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F10S \\sim F11S \\sim F12S \\sim C16W \\sim F10W \\sim F11W \\sim F12W: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C16S \\sim F10S \\sim F11S \\sim F12S \\sim C16W \\sim F10W \\sim F11W \\sim
F12W \\sim C13S \\sim F13S \\sim C14S \\sim F14S \\sim C15S \\sim F15S \\sim
C17S \\sim C18S \\sim F16S \\sim F17S \\sim F18S \\sim F16W \\sim F17W \\sim
F18W: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
F19S \\sim F20S \\sim F21S \\sim F19W \\sim F20W \\sim F21W: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F22S \\sim F23S \\sim F24S \\sim F22W \\sim F23W \\sim F24W: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F1T \\sim F2T \\sim F3T \\sim F1W \\sim F2W \\sim F3W: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F4T \\sim F5T \\sim F6T \\sim F4X \\sim F5X \\sim F6X: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F7T \\sim F8T \\sim F9T \\sim F7X \\sim F8X \\sim F9X: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F10T \\sim F11T \\sim F12T \\sim F10X \\sim F11X \\sim F12X: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F19T \\sim F20T \\sim F21T \\sim F19X \\sim F20X \\sim F21X: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F1U \\sim F2U \\sim F3U \\sim F1V \\sim F2V \\sim F3V: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F4U \\sim F5U \\sim F6U \\sim F4V \\sim F5V \\sim F6V: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F7U \\sim F8U \\sim F9U \\sim F7V \\sim F8V \\sim F9V: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
F13U \\sim F14U \\sim F15U \\sim F13V \\sim F14V \\sim F15V: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C16U \\sim F10U \\sim F11U \\sim F12U \\sim F10V \\sim F11V \\sim F12V: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F16U \\sim F17U \\sim F18U \\sim F16V \\sim F17V \\sim F18V: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
F19U \\sim F20U \\sim F21U \\sim F19V \\sim F20V \\sim F21V: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C32U \\sim F22U \\sim F23U \\sim F24U \\sim C32V \\sim F22V \\sim F23V \\sim
F24V: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
2A
C1I \\sim C2I \\sim O1I \\sim C3I \\sim C4I \\sim C1H \\sim C2H \\sim O1H \\sim
C3H \\sim C4H: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Uanis(F4S) \\sim Ueq, Uanis(F5S) \\sim Ueq, Uanis(F6S) \\sim Ueq, Uanis(F4W)
\\sim Ueq, Uanis(F5W) \\sim Ueq, Uanis(F6W) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F10S) \\sim Ueq, Uanis(F11S) \\sim Ueq, Uanis(F12S) \\sim Ueq,
Uanis(C16W) \\sim Ueq, Uanis(F10W) \\sim Ueq, Uanis(F11W) \\sim Ueq,
Uanis(F12W) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C16S) \\sim Ueq, Uanis(F10S) \\sim Ueq, Uanis(F11S) \\sim Ueq,
Uanis(F12S) \\sim Ueq, Uanis(C16W) \\sim Ueq, Uanis(F10W) \\sim Ueq,
Uanis(F11W) \\sim Ueq, Uanis(F12W) \\sim Ueq, Uanis(C13S) \\sim Ueq,
Uanis(F13S) \\sim Ueq, Uanis(C14S) \\sim Ueq, Uanis(F14S) \\sim Ueq,
Uanis(C15S) \\sim Ueq, Uanis(F15S) \\sim Ueq, Uanis(C17S) \\sim Ueq,
Uanis(C18S) \\sim Ueq, Uanis(F16S) \\sim Ueq, Uanis(F17S) \\sim Ueq,
Uanis(F18S) \\sim Ueq, Uanis(F16W) \\sim Ueq, Uanis(F17W) \\sim Ueq,
Uanis(F18W) \\sim Ueq: with sigma of 0.003 and sigma for terminal atoms of 0.006
Uanis(F19S) \\sim Ueq, Uanis(F20S) \\sim Ueq, Uanis(F21S) \\sim Ueq,
Uanis(F19W) \\sim Ueq, Uanis(F20W) \\sim Ueq, Uanis(F21W) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F22S) \\sim Ueq, Uanis(F23S) \\sim Ueq, Uanis(F24S) \\sim Ueq,
Uanis(F22W) \\sim Ueq, Uanis(F23W) \\sim Ueq, Uanis(F24W) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1T) \\sim Ueq, Uanis(F2T) \\sim Ueq, Uanis(F3T) \\sim Ueq, Uanis(F1W)
\\sim Ueq, Uanis(F2W) \\sim Ueq, Uanis(F3W) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F4T) \\sim Ueq, Uanis(F5T) \\sim Ueq, Uanis(F6T) \\sim Ueq, Uanis(F4X)
\\sim Ueq, Uanis(F5X) \\sim Ueq, Uanis(F6X) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F7T) \\sim Ueq, Uanis(F8T) \\sim Ueq, Uanis(F9T) \\sim Ueq, Uanis(F7X)
\\sim Ueq, Uanis(F8X) \\sim Ueq, Uanis(F9X) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F10T) \\sim Ueq, Uanis(F11T) \\sim Ueq, Uanis(F12T) \\sim Ueq,
Uanis(F10X) \\sim Ueq, Uanis(F11X) \\sim Ueq, Uanis(F12X) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F19T) \\sim Ueq, Uanis(F20T) \\sim Ueq, Uanis(F21T) \\sim Ueq,
Uanis(F19X) \\sim Ueq, Uanis(F20X) \\sim Ueq, Uanis(F21X) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(F1U) \\sim Ueq, Uanis(F2U) \\sim Ueq, Uanis(F3U) \\sim Ueq, Uanis(F1V)
\\sim Ueq, Uanis(F2V) \\sim Ueq, Uanis(F3V) \\sim Ueq: with sigma of 0.003 and
sigma for terminal atoms of 0.006
Uanis(F4U) \\sim Ueq, Uanis(F5U) \\sim Ueq, Uanis(F6U) \\sim Ueq, Uanis(F4V)
\\sim Ueq, Uanis(F5V) \\sim Ueq, Uanis(F6V) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F7U) \\sim Ueq, Uanis(F8U) \\sim Ueq, Uanis(F9U) \\sim Ueq, Uanis(F7V)
\\sim Ueq, Uanis(F8V) \\sim Ueq, Uanis(F9V) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(F13U) \\sim Ueq, Uanis(F14U) \\sim Ueq, Uanis(F15U) \\sim Ueq,
Uanis(F13V) \\sim Ueq, Uanis(F14V) \\sim Ueq, Uanis(F15V) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C16U) \\sim Ueq, Uanis(F10U) \\sim Ueq, Uanis(F11U) \\sim Ueq,
Uanis(F12U) \\sim Ueq, Uanis(F10V) \\sim Ueq, Uanis(F11V) \\sim Ueq,
Uanis(F12V) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(F16U) \\sim Ueq, Uanis(F17U) \\sim Ueq, Uanis(F18U) \\sim Ueq,
Uanis(F16V) \\sim Ueq, Uanis(F17V) \\sim Ueq, Uanis(F18V) \\sim Ueq: with sigma
of 0.003 and sigma for terminal atoms of 0.006
Uanis(F19U) \\sim Ueq, Uanis(F20U) \\sim Ueq, Uanis(F21U) \\sim Ueq,
Uanis(F19V) \\sim Ueq, Uanis(F20V) \\sim Ueq, Uanis(F21V) \\sim Ueq: with sigma
of 0.005 and sigma for terminal atoms of 0.01
Uanis(C32U) \\sim Ueq, Uanis(F22U) \\sim Ueq, Uanis(F23U) \\sim Ueq,
Uanis(F24U) \\sim Ueq, Uanis(C32V) \\sim Ueq, Uanis(F22V) \\sim Ueq,
Uanis(F23V) \\sim Ueq, Uanis(F24V) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
Uanis(C1I) \\sim Ueq, Uanis(C2I) \\sim Ueq, Uanis(O1I) \\sim Ueq, Uanis(C3I)
\\sim Ueq, Uanis(C4I) \\sim Ueq, Uanis(C1H) \\sim Ueq, Uanis(C2H) \\sim Ueq,
Uanis(O1H) \\sim Ueq, Uanis(C3H) \\sim Ueq, Uanis(C4H) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
5. Same fragment restrains
{F4S, F5S, F6S} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F4W, F5W, F6W}
{F7T, F8T, F9T} sigma for 1-2: 0.01, 1-3: 0.04
as in
{F7X, F8X, F9X}
{F4T, F5T, F6T} sigma for 1-2: 0.01, 1-3: 0.04
as in
{F4X, F5X, F6X}
{F19S, F20S, F21S} sigma for 1-2: 0.01, 1-3: 0.04
as in
{F19W, F20W, F21W}
{F19T, F20T, F21T} sigma for 1-2: 0.01, 1-3: 0.04
as in
{F19X, F20X, F21X}
{F22S, F23S, F24S} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F22W, F23W, F24W}
{F1U, F2U, F3U} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F1V, F2V, F3V}
{F16U, F17U, F18U} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F16V, F17V, F18V}
{F10U, F11U, F12U} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F10V, F11V, F12V}
{F4U, F5U, F6U} sigma for 1-2: 0.001, 1-3: 0.04
as in
{F4V, F5V, F6V}
{F19U, F20U, F21U} sigma for 1-2: 0.01, 1-3: 0.04
as in
{F19V, F20V, F21V}
{F7U, F8U, F9U} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F7V, F8V, F9V}
{F13U, F14U, F15U} sigma for 1-2: 0.02, 1-3: 0.04
as in
{F13V, F14V, F15V}
6. Others
 Sof(C32V)=Sof(F22V)=Sof(F23V)=Sof(F24V)=1-FVAR(1)
 Sof(C32U)=Sof(F22U)=Sof(F23U)=Sof(F24U)=FVAR(1)
 Sof(F16V)=Sof(F17V)=Sof(F18V)=1-FVAR(2)
 Sof(F16U)=Sof(F17U)=Sof(F18U)=FVAR(2)
 Sof(F10V)=Sof(F11V)=Sof(F12V)=1-FVAR(3)
 Sof(F10U)=Sof(F11U)=Sof(F12U)=FVAR(3)
 Sof(F1V)=Sof(F2V)=Sof(F3V)=1-FVAR(4)
 Sof(F1U)=Sof(F2U)=Sof(F3U)=FVAR(4)
 Sof(F1W)=Sof(F2W)=Sof(F3W)=1-FVAR(5)
 Sof(F1T)=Sof(F2T)=Sof(F3T)=FVAR(5)
 Sof(F4W)=Sof(F5W)=Sof(F6W)=1-FVAR(6)
 Sof(F4S)=Sof(F5S)=Sof(F6S)=FVAR(6)
 Sof(F16W)=Sof(F17W)=Sof(F18W)=1-FVAR(7)
 Sof(F16S)=Sof(F17S)=Sof(F18S)=FVAR(7)
 Sof(F19W)=Sof(F20W)=Sof(F21W)=1-FVAR(8)
 Sof(F19S)=Sof(F20S)=Sof(F21S)=FVAR(8)
 Sof(F4V)=Sof(F5V)=Sof(F6V)=1-FVAR(9)
 Sof(F4U)=Sof(F5U)=Sof(F6U)=FVAR(9)
 Sof(F7V)=Sof(F8V)=Sof(F9V)=1-FVAR(10)
 Sof(F7U)=Sof(F8U)=Sof(F9U)=FVAR(10)
 Sof(F4X)=Sof(F5X)=Sof(F6X)=1-FVAR(11)
 Sof(F4T)=Sof(F5T)=Sof(F6T)=FVAR(11)
 Sof(F19X)=Sof(F20X)=Sof(F21X)=1-FVAR(12)
 Sof(F19T)=Sof(F20T)=Sof(F21T)=FVAR(12)
 Sof(F19V)=Sof(F20V)=Sof(F21V)=1-FVAR(13)
 Sof(F19U)=Sof(F20U)=Sof(F21U)=FVAR(13)
 Sof(F22W)=Sof(F23W)=Sof(F24W)=1-FVAR(14)
 Sof(F22S)=Sof(F23S)=Sof(F24S)=FVAR(14)
 Sof(C16W)=Sof(F10W)=Sof(F11W)=Sof(F12W)=1-FVAR(15)
 Sof(C16S)=Sof(F10S)=Sof(F11S)=Sof(F12S)=FVAR(15)
 Sof(F7X)=Sof(F8X)=Sof(F9X)=1-FVAR(16)
 Sof(F7T)=Sof(F8T)=Sof(F9T)=FVAR(16)
 Sof(F10X)=Sof(F11X)=Sof(F12X)=1-FVAR(17)
 Sof(F10T)=Sof(F11T)=Sof(F12T)=FVAR(17)
 Sof(F13V)=Sof(F14V)=Sof(F15V)=1-FVAR(18)
 Sof(F13U)=Sof(F14U)=Sof(F15U)=FVAR(18)
 Fixed Sof: C1I(0.25) H1IA(0.25) H1IB(0.25) H1IC(0.25) C2I(0.25) H2IA(0.25)
 H2IB(0.25) O1I(0.25) C3I(0.25) H3IA(0.25) H3IB(0.25) C4I(0.25) H4IA(0.25)
 H4IB(0.25) H4IC(0.25) C1H(0.25) H1HA(0.25) H1HB(0.25) H1HC(0.25) C2H(0.25)
 H2HA(0.25) H2HB(0.25) O1H(0.25) C3H(0.25) H3HA(0.25) H3HB(0.25) C4H(0.25)
 H4HA(0.25) H4HB(0.25) H4HC(0.25)
7.a Riding coordinates:
 Ir1A(H), Ir1B(HA), Ir1C(HB)
7.b Ternary CH refined with riding coordinates:
 C1A(H1A), C4A(H4A), C18A(H18A), C24A(H24A), C30A(H30A), C1B(H1B), C4B(H4B),
 C18B(H18B), C24B(H24B), C30B(H30B), C1C(H1C), C4C(H4C), C18C(H18C), C24C(H24C),
  C30C(H30C)
7.c Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C19A(H19A,H19B), C20A(H20A,H20B), C21A(H21A,H21B), C22A(H22A,
 H22B), C23A(H23A,H23B), C25A(H25A,H25B), C26A(H26A,H26B), C27A(H27A,H27B),
 C28A(H28A,H28B), C29A(H29A,H29B), C31A(H31A,H31B), C32A(H32A,H32B), C33A(H33A,
 H33B), C34A(H34A,H34B), C35A(H35A,H35B), C2B(H2BA,H2BB), C19B(H19E,H19F),
 C20B(H20E,H20F), C21B(H21E,H21F), C22B(H22E,H22F), C23B(H23E,H23F), C25B(H25E,
 H25F), C26B(H26E,H26F), C27B(H27E,H27F), C28B(H28E,H28F), C29B(H29E,H29F),
 C31B(H31E,H31F), C32B(H32E,H32F), C33B(H33E,H33F), C34B(H34E,H34F), C35B(H35E,
 H35F), C2C(H2CA,H2CB), C19C(H19C,H19D), C20C(H20C,H20D), C21C(H21C,H21D),
 C22C(H22C,H22D), C23C(H23C,H23D), C25C(H25C,H25D), C26C(H26C,H26D), C27C(H27C,
 H27D), C28C(H28C,H28D), C29C(H29C,H29D), C31C(H31C,H31D), C32C(H32C,H32D),
 C33C(H33C,H33D), C34C(H34C,H34D), C35C(H35C,H35D), C2I(H2IA,H2IB), C3I(H3IA,
 H3IB), C2H(H2HA,H2HB), C3H(H3HA,H3HB)
7.d Me refined with riding coordinates:
 C1I(H1IA,H1IB,H1IC), C4I(H4IA,H4IB,H4IC), C1H(H1HA,H1HB,H1HC), C4H(H4HA,H4HB,
 H4HC)
7.e Aromatic/amide H refined with riding coordinates:
 C40C(H40C), C8A(H8A), C9A(H9A), C10A(H10A), C13A(H13A), C14A(H14A),
 C15A(H15A), C16A(H16A), C36A(H36A), C37A(H37A), C38A(H38A), C39A(H39A),
 C40A(H40A), C8B(H8B), C9B(H9B), C10B(H10B), C13B(H13B), C14B(H14B), C15B(H15B),
  C16B(H16B), C36B(H36B), C37B(H37B), C38B(H38B), C39B(H39B), C40B(H40B),
 C8C(H8C), C9C(H9C), C10C(H10C), C13C(H13C), C14C(H14C), C15C(H15C), C16C(H16C),
  C36C(H36C), C37C(H37C), C38C(H38C), C39C(H39C), C2S(H2S), C4S(H4S), C6S(H6S),
 C10S(H10S), C12S(H12S), C14S(H14S), C18S(H18S), C20S(H20S), C22S(H22S),
 C26S(H26S), C28S(H28S), C30S(H30S), C2T(H2T), C4T(H4T), C6T(H6T), C10T(H10T),
 C12T(H12T), C14T(H14T), C18T(H18T), C20T(H20T), C22T(H22T), C26T(H26T),
 C28T(H28T), C30T(H30T), C2U(H2U), C4U(H4U), C6U(H6U), C10U(H10U), C12U(H12U),
 C14U(H14U), C18U(H18U), C20U(H20U), C22U(H22U), C26U(H26U), C28U(H28U),
 C30U(H30U)
7.f Idealised Me refined as rotating group:
 C5A(H5AA,H5AB,H5AC), C6A(H6AA,H6AB,H6AC), C5B(H5BA,H5BB,H5BC), C6B(H6BA,H6BB,
 H6BC), C5C(H5CA,H5CB,H5CC), C6C(H6CA,H6CB,H6CC)
;
_shelx_res_checksum              33171
_shelx_hkl_checksum              15055
_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 1.340
_oxdiff_exptl_absorpt_empirical_full_min 0.714