Low-coordinate iridium NHC complexes derived from selective and reversible C-H bond activation of fluoroarenes
Simone A. Hauser; Ivan Prokes; Adrian B. Chaplin; Chem.Commun. 51 (2015) 4425–; doi:10.1039/C5cc00529A

data_7116654
_publ_section_title
;
 Low-coordinate iridium NHC complexes derived from selective and
 reversible C-H bond activation of fluoroarenes
;
_journal_name_full               Chem.Commun.
_journal_page_first              4425
_journal_paper_doi               10.1039/C5cc00529A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'1(C39 H51 F2 Ir N6 O6), 0.5(C6 H4 F2), 1(C32 H12 B F24)'
_chemical_formula_sum            'C74 H66 B F27 Ir N6 O6'
_chemical_formula_weight         1851.33
_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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-12-04 deposited with the CCDC.
2015-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                96.4495(9)
_cell_angle_beta                 91.4551(9)
_cell_angle_gamma                106.0089(9)
_cell_formula_units_Z            4
_cell_length_a                   14.29260(15)
_cell_length_b                   17.57617(19)
_cell_length_c                   30.9787(4)
_cell_measurement_reflns_used    59707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.6200
_cell_measurement_theta_min      2.9690
_cell_volume                     7420.04(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -60.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593  -77.0000 -120.0000 109

  2 omega   81.00  107.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593  178.0000 -120.0000 26

  3 omega  -13.00   55.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593  -99.0000   90.0000 68

  4 omega  -59.00   44.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593  -38.0000  120.0000 103

  5 omega   27.00   55.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0968   57.0000  -60.0000 28

  6 omega  -14.00   23.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0968  -99.0000 -150.0000 37

  7 omega -106.00  -53.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0968  178.0000 -120.0000 53

  8 omega   -4.00   22.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.0968   57.0000  -60.0000 26

  9 omega   -9.00   93.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593   38.0000 -120.0000 102

 10 omega   -9.00   93.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593   38.0000  150.0000 102

 11 omega  -12.00   91.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593   57.0000    0.0000 103

 12 omega  -57.00   47.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1593  -57.0000   90.0000 104
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction: Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0159166000
_diffrn_orient_matrix_UB_12      0.0178771000
_diffrn_orient_matrix_UB_13      -0.0189297000
_diffrn_orient_matrix_UB_21      0.0229682000
_diffrn_orient_matrix_UB_22      0.0365189000
_diffrn_orient_matrix_UB_23      0.0131084000
_diffrn_orient_matrix_UB_31      0.0435204000
_diffrn_orient_matrix_UB_32      -0.0117067000
_diffrn_orient_matrix_UB_33      0.0016240000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            140009
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.681
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         2.947
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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    1.657
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3700
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.414
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2493
_refine_ls_number_reflns         28177
_refine_ls_number_restraints     2984
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0319P)^2^+22.8987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0897
_reflns_Friedel_coverage         0.000
_reflns_number_gt                24431
_reflns_number_total             28177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc00529a2.cif
_cod_data_source_block           0047abc13
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_cell_volume        7420.03(14)
_cod_database_code               7116654
_shelxl_version_number           2013-4
_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
 C507-F1A \\sim C507-F2A \\sim C507-F3A \\sim C307-F3 \\sim C307-F1 \\sim
C307-F2
 with sigma of 0.01
 F1A-F2A \\sim F2A-F3A \\sim F3A-F1A \\sim F3-F1 \\sim F1-F2 \\sim F2-F3
 with sigma of 0.01
 C407-F101 \\sim C407-F102 \\sim C407-F103 \\sim C407-F201 \\sim C407-F202
\\sim C407-F203
 with sigma of 0.01
 F101-F102 \\sim F102-F103 \\sim F103-F101 \\sim F201-F202 \\sim F202-F203
\\sim F203-F201
 with sigma of 0.01
 C403-F101 \\sim C403-F102 \\sim C403-F103 \\sim C403-F201 \\sim C403-F202
\\sim C403-F203
 with sigma of 0.01
 C415-F107 \\sim C415-F308 \\sim C415-F309 \\sim C415-F207 \\sim C415-F408
\\sim C415-F409
 with sigma of 0.01
 F107-F308 \\sim F308-F309 \\sim F309-F107 \\sim F207-F408 \\sim F408-F409
\\sim F409-F207
 with sigma of 0.01
 C411-F107 \\sim C411-F308 \\sim C411-F309 \\sim C411-F207 \\sim C411-F408
\\sim C411-F409
 with sigma of 0.01
 C423-F113 \\sim C423-F114 \\sim C423-F115 \\sim C423-F213 \\sim C423-F214
\\sim C423-F215
 with sigma of 0.01
 F113-F114 \\sim F114-F115 \\sim F115-F113 \\sim F213-F214 \\sim F214-F215
\\sim F215-F213
 with sigma of 0.01
 C419-F113 \\sim C419-F114 \\sim C419-F115 \\sim C419-F213 \\sim C419-F214
\\sim C419-F215
 with sigma of 0.01
 C432-F122 \\sim C432-F123 \\sim C432-F124 \\sim C432-F222 \\sim C432-F223
\\sim C432-F224
 with sigma of 0.01
 F122-F123 \\sim F123-F124 \\sim F124-F122 \\sim F222-F223 \\sim F223-F224
\\sim F224-F222
 with sigma of 0.01
 C429-F122 \\sim C429-F123 \\sim C429-F124 \\sim C429-F222 \\sim C429-F223
\\sim C429-F224
 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
 C215-F7 \\sim C215-F8B \\sim C215-F9B \\sim C215-F7A \\sim C215-F8C \\sim
C215-F9C
 with sigma of 0.01
 F7-F8B \\sim F8B-F9B \\sim F9B-F7 \\sim F7A-F8C \\sim F8C-F9C \\sim F9C-F7A
 with sigma of 0.01
 C211-F7 \\sim C211-F8B \\sim C211-F9B \\sim C211-F7A \\sim C211-F8C \\sim
C211-F9C
 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
 C508-F4A \\sim C508-F5A \\sim C508-F6A \\sim C308-F5 \\sim C308-F4 \\sim
C308-F6
 with sigma of 0.01
 F4A-F5A \\sim F5A-F6A \\sim F6A-F4A \\sim F5-F4 \\sim F4-F6 \\sim F6-F5
 with sigma of 0.01
 C503-C507 \\sim C303-C307
 with sigma of 0.01
 C505-C508 \\sim C305-C308
 with sigma of 0.01
 C501-B200 \\sim C301-B200
 with sigma of 0.01
 C503-F1A \\sim C503-F2A \\sim C503-F3A \\sim C303-F3 \\sim C303-F1 \\sim
C303-F2
 with sigma of 0.01
 C505-F4A \\sim C505-F5A \\sim C505-F6A \\sim C305-F5 \\sim C305-F4 \\sim
C305-F6
 with sigma of 0.01
 F8A-C6A \\sim F9A-C7A \\sim F9-C7 \\sim F8-C6 \\sim F108-C106 \\sim F109-C107
\\sim F209-C207 \\sim F208-
 C206
 with sigma of 0.01
 C2-F9 \\sim F9-C6 \\sim C7-F8 \\sim F8-C5 \\sim C2-F9A \\sim F9A-C6A \\sim
C7A-F8A \\sim F8A-C5A \\sim C102-
 F109 \\sim F109-C106 \\sim C107-F108 \\sim F108-C105 \\sim C102-F209 \\sim
F209-C206 \\sim C207-F208 ~
 F208-C205
 with sigma of 0.01
 O36-C35A \\sim O36-C35 \\sim O148-C147 \\sim O148-C247
 with sigma of 0.01
 C35A-C34 \\sim C35-C34 \\sim C147-C146 \\sim C146-C247
 with sigma of 0.01
 C40-C34 \\sim C40A-C34 \\sim C39A-C34 \\sim C39-C34 \\sim C146-C252 \\sim
C152-C146 \\sim C153-C146 ~
 C146-C253
 with sigma of 0.01
 C35-C39 \\sim C35-C40 \\sim C35A-C39A \\sim C35A-C40A \\sim C147-C152 \\sim
C147-C153 \\sim C247-C252
 \\sim C247-C253
 with sigma of 0.01
 F92-C902 \\sim F82-C802 \\sim F91-C901 \\sim F81-C801
 with sigma of 0.01
 C806-F81 \\sim F81-C802 \\sim C801-F82 \\sim F82-C803 \\sim C906-F91 \\sim
F91-C902 \\sim C901-F92 ~
 F92-C903
 with sigma of 0.01
3. Restrained planarity
 C801, C802, C803, C804, C805, C806, F81, F82
 with sigma of 0.01
 C901, C902, C903, C904, C905, C906, F91, F92
 with sigma of 0.01
 C301, C302, C303, C304, C305, C306, C307, C308
 with sigma of 0.01
 C508, C505, C506, C502, C501, C503, C504, C507
 with sigma of 0.01
 C2, C3, C4, C5, C6, C7, F8, F9
 with sigma of 0.01
 C2, C3A, C7A, C6A, C5A, C4A, F8A, F9A
 with sigma of 0.01
 C102, C103, C104, C105, C106, C107, F108, F109
 with sigma of 0.01
 C102, C203, C204, C205, C206, C207, F208, F209
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
F8 \\sim F8A \\sim F9 \\sim F9A \\sim F108 \\sim F109 \\sim F208 \\sim F209
\\sim F91 \\sim F92 \\sim F81 \\sim F82 \\sim F1 \\sim F1A \\sim F2 \\sim F2A
\\sim F3 \\sim F3A \\sim F4 \\sim F4A \\sim F5 \\sim F5A \\sim F6 \\sim F6A
\\sim F7 \\sim F7A \\sim F8B \\sim F8C \\sim F9B \\sim F9C \\sim F10 \\sim F10A
\\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim F14 \\sim F15 \\sim
F16 \\sim F16A \\sim F17 \\sim F17A \\sim F18 \\sim F18A \\sim F19 \\sim F20
\\sim F21 \\sim F22 \\sim F23 \\sim F24 \\sim F101 \\sim F102 \\sim F103 \\sim
F104 \\sim F105 \\sim F106 \\sim F107 \\sim F110 \\sim F111 \\sim F112 \\sim
F113 \\sim F114 \\sim F115 \\sim F116 \\sim F117 \\sim F118 \\sim F119 \\sim
F120 \\sim F121 \\sim F122 \\sim F123 \\sim F124 \\sim F201 \\sim F202 \\sim
F203 \\sim F207 \\sim F213 \\sim F214 \\sim F215 \\sim F222 \\sim F223 \\sim
F224 \\sim F308 \\sim F309 \\sim F408 \\sim F409 \\sim C432 \\sim C407 \\sim
C408 \\sim C415 \\sim C423 \\sim C308 \\sim C508 \\sim C305 \\sim C505 \\sim
C306 \\sim C506 \\sim C301 \\sim C501 \\sim B200 \\sim C302 \\sim C502 \\sim
C503 \\sim C303 \\sim C504 \\sim C304 \\sim C307 \\sim C507 \\sim C224 \\sim
C216 \\sim C215 \\sim C2 \\sim C7A \\sim C3 \\sim C4 \\sim C6A \\sim C5 \\sim
C5A \\sim C4A \\sim C6 \\sim C3A \\sim C7 \\sim O36 \\sim C35 \\sim C35A \\sim
C34 \\sim C39 \\sim C39A \\sim C40 \\sim C40A \\sim O148 \\sim C147 \\sim C247
\\sim C146 \\sim C252 \\sim C152 \\sim C253 \\sim C153 \\sim C102 \\sim C103
\\sim C104 \\sim C105 \\sim C106 \\sim C107 \\sim F108 \\sim F109 \\sim C203
\\sim C204 \\sim C205 \\sim C206 \\sim C207 \\sim F208 \\sim F209: within 1.7A
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F9A)
\\sim Ueq, Uanis(F108) \\sim Ueq, Uanis(F109) \\sim Ueq, Uanis(F208) \\sim Ueq,
Uanis(F209) \\sim Ueq, Uanis(F91) \\sim Ueq, Uanis(F92) \\sim Ueq, Uanis(F81)
\\sim Ueq, Uanis(F82) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F1A) \\sim Ueq,
Uanis(F2) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F3A)
\\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F5) \\sim Ueq,
Uanis(F5A) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F8B) \\sim Ueq, Uanis(F8C) \\sim Ueq,
Uanis(F9B) \\sim Ueq, Uanis(F9C) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A)
\\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq,
Uanis(F12A) \\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15)
\\sim Ueq, Uanis(F16) \\sim Ueq, Uanis(F16A) \\sim Ueq, Uanis(F17) \\sim Ueq,
Uanis(F17A) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F18A) \\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(F101) \\sim Ueq, Uanis(F102)
\\sim Ueq, Uanis(F103) \\sim Ueq, Uanis(F104) \\sim Ueq, Uanis(F105) \\sim Ueq,
Uanis(F106) \\sim Ueq, Uanis(F107) \\sim Ueq, Uanis(F110) \\sim Ueq,
Uanis(F111) \\sim Ueq, Uanis(F112) \\sim Ueq, Uanis(F113) \\sim Ueq,
Uanis(F114) \\sim Ueq, Uanis(F115) \\sim Ueq, Uanis(F116) \\sim Ueq,
Uanis(F117) \\sim Ueq, Uanis(F118) \\sim Ueq, Uanis(F119) \\sim Ueq,
Uanis(F120) \\sim Ueq, Uanis(F121) \\sim Ueq, Uanis(F122) \\sim Ueq,
Uanis(F123) \\sim Ueq, Uanis(F124) \\sim Ueq, Uanis(F201) \\sim Ueq,
Uanis(F202) \\sim Ueq, Uanis(F203) \\sim Ueq, Uanis(F207) \\sim Ueq,
Uanis(F213) \\sim Ueq, Uanis(F214) \\sim Ueq, Uanis(F215) \\sim Ueq,
Uanis(F222) \\sim Ueq, Uanis(F223) \\sim Ueq, Uanis(F224) \\sim Ueq,
Uanis(F308) \\sim Ueq, Uanis(F309) \\sim Ueq, Uanis(F408) \\sim Ueq,
Uanis(F409) \\sim Ueq, Uanis(C432) \\sim Ueq, Uanis(C407) \\sim Ueq,
Uanis(C408) \\sim Ueq, Uanis(C415) \\sim Ueq, Uanis(C423) \\sim Ueq,
Uanis(C308) \\sim Ueq, Uanis(C508) \\sim Ueq, Uanis(C305) \\sim Ueq,
Uanis(C505) \\sim Ueq, Uanis(C306) \\sim Ueq, Uanis(C506) \\sim Ueq,
Uanis(C301) \\sim Ueq, Uanis(C501) \\sim Ueq, Uanis(B200) \\sim Ueq,
Uanis(C302) \\sim Ueq, Uanis(C502) \\sim Ueq, Uanis(C503) \\sim Ueq,
Uanis(C303) \\sim Ueq, Uanis(C504) \\sim Ueq, Uanis(C304) \\sim Ueq,
Uanis(C307) \\sim Ueq, Uanis(C507) \\sim Ueq, Uanis(C224) \\sim Ueq,
Uanis(C216) \\sim Ueq, Uanis(C215) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6A) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C6)
\\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O36) \\sim Ueq,
Uanis(C35) \\sim Ueq, Uanis(C35A) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C39)
\\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C40A) \\sim Ueq,
Uanis(O148) \\sim Ueq, Uanis(C147) \\sim Ueq, Uanis(C247) \\sim Ueq,
Uanis(C146) \\sim Ueq, Uanis(C252) \\sim Ueq, Uanis(C152) \\sim Ueq,
Uanis(C253) \\sim Ueq, Uanis(C153) \\sim Ueq, Uanis(C102) \\sim Ueq,
Uanis(C103) \\sim Ueq, Uanis(C104) \\sim Ueq, Uanis(C105) \\sim Ueq,
Uanis(C106) \\sim Ueq, Uanis(C107) \\sim Ueq, Uanis(F108) \\sim Ueq,
Uanis(F109) \\sim Ueq, Uanis(C203) \\sim Ueq, Uanis(C204) \\sim Ueq,
Uanis(C205) \\sim Ueq, Uanis(C206) \\sim Ueq, Uanis(C207) \\sim Ueq,
Uanis(F208) \\sim Ueq, Uanis(F209) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C35A) = Uanis(C35)
Uanis(C40) = Uanis(C40A)
Uanis(C39A) = Uanis(C39)
Uanis(F6A) = Uanis(F6)
Uanis(F81) = Uanis(F82) = Uanis(C806) = Uanis(C805) = Uanis(C804) = Uanis(C803)
= Uanis(C802) = Uanis(C801) = Uanis(F91) = Uanis(F92) = Uanis(C902) =
Uanis(C901) = Uanis(C906) = Uanis(C905) = Uanis(C904) = Uanis(C903)
5. Others
 Sof(F208)=Sof(F209)=Sof(C203)=Sof(H203)=Sof(C204)=Sof(H204)=Sof(C205)=
 Sof(H205)=Sof(C206)=Sof(C207)=1-FVAR(1)
 Sof(F108)=Sof(F109)=Sof(C103)=Sof(H103)=Sof(C104)=Sof(H104)=Sof(C105)=
 Sof(H105)=Sof(C106)=Sof(C107)=FVAR(1)
 Sof(F8A)=Sof(F9A)=Sof(C7A)=Sof(C6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=
 Sof(C3A)=Sof(H3A)=1-FVAR(2)
 Sof(F8)=Sof(F9)=Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=Sof(C6)=
 Sof(C7)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=Sof(C501)=Sof(C506)=
 Sof(H506)=Sof(C505)=Sof(C504)=Sof(H504)=Sof(C503)=Sof(C502)=Sof(H502)=
 Sof(C507)=Sof(C508)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=Sof(C301)=Sof(C302)=Sof(H302)=
 Sof(C303)=Sof(C304)=Sof(H304)=Sof(C305)=Sof(C306)=Sof(H306)=Sof(C307)=
 Sof(C308)=FVAR(3)
 Sof(F207)=Sof(F408)=Sof(F409)=1-FVAR(4)
 Sof(F107)=Sof(F308)=Sof(F309)=FVAR(4)
 Sof(F213)=Sof(F214)=Sof(F215)=1-FVAR(5)
 Sof(F113)=Sof(F114)=Sof(F115)=FVAR(5)
 Sof(F201)=Sof(F202)=Sof(F203)=1-FVAR(6)
 Sof(F101)=Sof(F102)=Sof(F103)=FVAR(6)
 Sof(F222)=Sof(F223)=Sof(F224)=1-FVAR(7)
 Sof(F122)=Sof(F123)=Sof(F124)=FVAR(7)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(8)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(8)
 Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(9)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(9)
 Sof(F7A)=Sof(F8C)=Sof(F9C)=1-FVAR(10)
 Sof(F7)=Sof(F8B)=Sof(F9B)=FVAR(10)
 Sof(C35A)=Sof(H35C)=Sof(H35D)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=
 Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(11)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(11)
 Sof(C247)=Sof(H24D)=Sof(H24E)=Sof(C252)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C253)=Sof(H25G)=Sof(H25H)=Sof(H25I)=1-FVAR(12)
 Sof(C147)=Sof(H14D)=Sof(H14E)=Sof(C152)=Sof(H15C)=Sof(H15D)=Sof(H15E)=
 Sof(C153)=Sof(H15F)=Sof(H15G)=Sof(H15H)=FVAR(12)
 Sof(F91)=Sof(F92)=Sof(C902)=Sof(C901)=Sof(C906)=Sof(H906)=Sof(C905)=Sof(H905)=
 Sof(C904)=Sof(H904)=Sof(C903)=Sof(H903)=1-FVAR(13)
 Sof(F81)=Sof(F82)=Sof(C806)=Sof(H806)=Sof(C805)=Sof(H805)=Sof(C804)=Sof(H804)=
 Sof(C803)=Sof(H803)=Sof(C802)=Sof(C801)=FVAR(13)
6.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C20(H20A,H20B), C32(H32A,H32B), C35(H35A,H35B), C35A(H35C,
 H35D), C47(H47A,H47B), C50(H50A,H50B), C117(H11A,H11B), C120(H12A,H12B),
 C132(H13A,H13B), C135(H13C,H13D), C147(H14D,H14E), C150(H15A,H15B), C247(H24D,
 H24E)
6.b Aromatic/amide H refined with riding coordinates:
 C5A(H5A), C4A(H4A), C3A(H3A), C3(H3), C4(H4), C5(H5), C203(H203), C204(H204),
 C205(H205), C103(H103), C104(H104), C105(H105), C906(H906), C905(H905),
 C904(H904), C903(H903), C806(H806), C805(H805), C804(H804), C803(H803),
 C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222),
 C226(H226), C228(H228), C230(H230), C302(H302), C304(H304), C306(H306),
 C506(H506), C504(H504), C502(H502), C402(H402), C404(H404), C406(H406),
 C410(H410), C412(H412), C414(H414), C418(H418), C420(H420), C422(H422),
 C426(H426), C428(H428), C430(H430)
6.c Fitted hexagon refined as free rotating group:
 C2(C7A,C6A,C5A,C4A,C3A), C102(C203,C204,C205,C206,C207), C902(C901,C906,C905,
 C904,C903), C806(C805,C804,C803,C802,C801), C301(C302,C303,C304,C305,C306),
 C501(C506,C505,C504,C503,C502)
6.d Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C39A(H39D,H39E,H39F), C40(H40A,H40B,H40C), C40A(H40D,H40E,H40F), C52(H52A,H52B,
 H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C),
 C122(H12C,H12D,H12E), C123(H12F,H12G,H12H), C124(H12I,H12J,H12K), C125(H12L,
 H12M,H12N), C137(H13E,H13F,H13G), C138(H13H,H13I,H13J), C139(H13K,H13L,H13M),
 C140(H14A,H14B,H14C), C152(H15C,H15D,H15E), C153(H15F,H15G,H15H), C154(H15I,
 H15J,H15K), C155(H15L,H15M,H15N), C252(H25D,H25E,H25F), C253(H25G,H25H,H25I)
;
_olex2_submission_special_instructions 'No special instructions were received'