Enhancing the nucleophilicity of aluminyl anions: targeting selective C–H activation
Kallmeier, Fabian; Nelmes, Gareth R.; McMullin, Claire L.; Edwards, Alison J.; Hicks, Jamie; Chemical Science 16 (2025) 10750–10758; doi:10.1039/D5SC02682B

data_1574622
_publ_section_title
;
 Enhancing the nucleophilicity of aluminyl anions: targeting selective
 C--H activation
;
_journal_issue                   24
_journal_name_full               'Chemical Science'
_journal_page_first              10750
_journal_page_last               10758
_journal_paper_doi               10.1039/D5SC02682B
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety
'C12 H24 K O6, C41 H70 Al N2 O Si2, 1.5(C5 H12)'
_chemical_formula_sum            'C60.5 H112 Al K N2 O7 Si2'
_chemical_formula_weight         1101.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.06 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-03-20 deposited with the CCDC.	2025-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.317(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8565(3)
_cell_length_b                   22.3423(5)
_cell_length_c                   19.5531(5)
_cell_measurement_reflns_used    11603
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.3820
_cell_measurement_theta_min      3.0410
_cell_volume                     6767.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_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    -76.00  26.00   0.50    2.00    --  -46.57  92.00 168.00  204
  2  \w     13.00  59.00   0.50    2.00    --   46.57 -92.00  55.00   92
  3  \w     -8.00  24.00   0.50    2.00    --  -46.57  19.00 -60.00   64
  4  \w     -8.00  26.00   0.50    2.00    --  -46.57  19.00 -90.00   68
  5  \w      1.00  27.00   0.50    2.00    --  -46.57  19.00-120.00   52
  6  \w     -3.00  29.00   0.50    2.00    --  -46.57  19.00 -30.00   64
  7  \w     -7.00  20.00   0.50    2.00    --  -46.57  38.00 -30.00   54
  8  \w     16.00  41.00   0.50    2.00    --   46.57  91.00 -62.59   50
  9  \w     56.00 105.00   0.50    8.00    --  107.75 -92.00  55.00   98
 10  \w    102.00 166.00   0.50    8.00    --  107.75  92.00 168.00  128
 11  \w     36.00  65.00   0.50    8.00    --  107.75 -45.00 150.00   58
 12  \w     32.00  58.00   0.50    8.00    --  107.75 -30.00 -90.00   52
 13  \w     33.00  59.00   0.50    8.00    --  107.75 -30.00  30.00   52
 14  \w     32.00  58.00   0.50    8.00    --  107.75 -30.00  90.00   52
 15  \w     35.00  64.00   0.50    8.00    --  107.75 -45.00  30.00   58
 16  \w     36.00  71.00   0.50    8.00    --  107.75 -45.00  60.00   70
 17  \w     33.00  58.00   0.50    8.00    --  107.75 -30.00  60.00   50
 18  \w     52.00  92.00   0.50    8.00    --  107.75 -61.00  90.00   80
 19  \w     40.00  65.00   0.50    8.00    --  107.75 -45.00 -60.00   50
 20  \w     33.00  58.00   0.50    8.00    --  107.75 -30.00 -60.00   50
 21  \w     35.00  71.00   0.50    8.00    --  107.75 -45.00-120.00   72
 22  \w     32.00  59.00   0.50    8.00    --  107.75 -30.00-120.00   54
 23  \w     38.00  73.00   0.50    8.00    --  107.75 -45.00-180.00   70
 24  \w     34.00  59.00   0.50    8.00    --  107.75 -30.00   0.00   50
 25  \w     38.00  73.00   0.50    8.00    --  107.75 -45.00 120.00   70
 26  \w     33.00  58.00   0.50    8.00    --  107.75 -30.00-180.00   50
 27  \w     55.00  95.00   0.50    8.00    --  107.75 -95.00 150.00   80
 28  \w     62.00  90.00   0.50    8.00    --  107.75 -95.00 -60.00   56
 29  \w     40.00  69.00   0.50    8.00    --  107.75 -45.00-150.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0170863000
_diffrn_orient_matrix_UB_12      0.0235601000
_diffrn_orient_matrix_UB_13      0.0698633000
_diffrn_orient_matrix_UB_21      0.0355668000
_diffrn_orient_matrix_UB_22      -0.0587623000
_diffrn_orient_matrix_UB_23      0.0361877000
_diffrn_orient_matrix_UB_31      0.0912686000
_diffrn_orient_matrix_UB_32      0.0273297000
_diffrn_orient_matrix_UB_33      0.0177482000
_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  0.0395
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            43199
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.494
_diffrn_reflns_theta_max         66.494
_diffrn_reflns_theta_min         3.044
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.510
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_description       block
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1103
_refine_ls_number_reflns         11922
_refine_ls_number_restraints     756
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1625P)^2^+2.6926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2492
_refine_ls_wR_factor_ref         0.2762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8299
_reflns_number_total             11922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc02682b2.cif
_cod_data_source_block           compound-4
_cod_depositor_comments
'Adding full bibliography for 1574617--1574626.cif.'
_cod_original_formula_sum        'C60.50 H112 Al K N2 O7 Si2'
_cod_database_code               1574622
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         C52H74AlKN2O7Si2
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.704
_diffrn_oxdiff_ac3_digest_hkl    01a8e72081a8a799d770c24bac098716c05552
_diffrn_oxdiff_digest_hkl
;
014722cfc2dfdb309dc6f09750b4e6fa5d7ec4
;
_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
 C43-C42 = C45-C44 = C47-C46 = C49-C48 = C51-C50 = C53-C52
 1.53 with sigma of 0.008
 O2-C53 = O2-C42 = O3-C43 = O3-C44 = O4-C45 = O4-C46 = O5-C47 = O5-C48 = O6-
 C49 = O6-C50 = O7-C51 = O7-C52
 1.4 with sigma of 0.008
 C43A-C42A = C53A-C52A = C51A-C50A = C49A-C48A = C47A-C46A = C45A-C44A
 1.53 with sigma of 0.008
 O3A-C43A = O3A-C44A = O4A-C45A = O4A-C46A = O5A-C47A = O5A-C48A = O6A-C49A =
 O6A-C50A = O7A-C51A = O7A-C52A = O2A-C53A = O2A-C42A
 1.4 with sigma of 0.008
 C14-C15 = C14-C16 = C14-C17 = C14A-C15A = C14A-C16A = C14A-C17A
 1.53 with sigma of 0.008
 C23A-C20 = C23-C20 = C21A-C20 = C21-C20 = C22A-C20 = C22-C20
 1.53 with sigma of 0.008
 Si1-C24 = Si1-C27 = Si1-C30 = Si2-C36 = Si2-C39 = Si2-C33
 1.87 with sigma of 0.008
 C25-C24 = C26-C24 = C28-C27 = C29-C27 = C32-C30 = C31-C30 = C35-C33 = C34-C33
 = C37-C36 = C38-C36 = C40-C39 = C41-C39
 1.53 with sigma of 0.008
 Si1A-C24A = Si1A-C27A = Si1A-C30A = Si2A-C36A = Si2A-C39A = Si2A-C33A
 1.87 with sigma of 0.008
 C25A-C24A = C26A-C24A = C28A-C27A = C32A-C30A = C31A-C30A = C37A-C36A = C38A-
 C36A = C40A-C39A = C41A-C39A = C35A-C33A = C34A-C33A
 1.53 with sigma of 0.008
 C27A-C29A
 1.53 with sigma of 0.008
 C54-C55 = C55-C56 = C56-C57 = C57-C58
 1.53 with sigma of 0.008
 C54A-C55A = C55A-C56A = C56A-C57A = C57A-C58A
 1.53 with sigma of 0.008
 C59-C60 = C60-C61 = C61-C62 = C62-C63
 1.53 with sigma of 0.008
 C15-C16 = C16-C17 = C17-C15 = C15A-C16A = C16A-C17A = C17A-C15A
 2.5 with sigma of 0.008
 C21-C22 = C22-C23 = C23-C21 = C21A-C22A = C22A-C23A = C23A-C21A
 2.5 with sigma of 0.008
 C40-C41
 2.5 with sigma of 0.008
 Si2-C40 = Si2-C41
 2.9 with sigma of 0.008
 C35A-C34A
 2.5 with sigma of 0.008
 Si2A-C34A = Si2A-C35A
 2.9 with sigma of 0.008
 C54-C56 = C55-C57 = C56-C58
 2.5 with sigma of 0.008
 C54A-C56A = C55A-C57A = C56A-C58A
 2.5 with sigma of 0.008
 C59-C61 = C60-C62 = C61-C63
 2.5 with sigma of 0.008
 C29A-C28A
 2.5 with sigma of 0.008
 C29A-Si1A = C28A-Si1A
 2.9 with sigma of 0.008
3. Uiso/Uaniso restraints and constraints
C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A \\sim C17 \\sim C17A:
within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
C20 \\sim C21 \\sim C21A \\sim C22 \\sim C22A \\sim C23 \\sim C23A: within 2A
with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A
Si1 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim
C31 \\sim C32: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Si2 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim
C40 \\sim C41: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01 within 2A
Si1A \\sim C24A \\sim C25A \\sim C26A \\sim C27A \\sim C28A \\sim C29A \\sim
C30A \\sim C31A \\sim C32A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
Si2A \\sim C33A \\sim C34A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim
C39A \\sim C40A \\sim C41A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
C54A \\sim C55A \\sim C56A \\sim C57A \\sim C58A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.01 within 2A
C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01 within 2A
O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim C42 \\sim C43 \\sim C44
\\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52
\\sim C53: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01
within 2A
O2A \\sim O3A \\sim O4A \\sim O5A \\sim O6A \\sim O7A \\sim C42A \\sim C43A
\\sim C44A \\sim C45A \\sim C46A \\sim C47A \\sim C48A \\sim C49A \\sim C50A
\\sim C51A \\sim C52A \\sim C53A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01 within 2A
Uanis(C11) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4. Others
 Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(C42A)=Sof(H42C)=
 Sof(H42D)=Sof(C43A)=Sof(H43C)=Sof(H43D)=Sof(C44A)=Sof(H44C)=Sof(H44D)=
 Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46C)=Sof(H46D)=Sof(C47A)=
 Sof(H47C)=Sof(H47D)=Sof(C48A)=Sof(H48C)=Sof(H48D)=Sof(C49A)=Sof(H49C)=
 Sof(H49D)=Sof(C50A)=Sof(H50C)=Sof(H50D)=Sof(C51A)=Sof(H51C)=Sof(H51D)=
 Sof(C52A)=Sof(H52C)=Sof(H52D)=Sof(C53A)=Sof(H53C)=Sof(H53D)=1-FVAR(1)
 Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(C42)=Sof(H42A)=Sof(H42B)=
 Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C50)=Sof(H50A)=Sof(H50B)=
 Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(C53)=Sof(H53A)=
 Sof(H53B)=FVAR(1)
 Sof(C14A)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16A)=Sof(H16D)=
 Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(C22A)=Sof(H22D)=Sof(H22E)=
 Sof(H22F)=Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(3)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(3)
 Sof(Si1A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27A)=Sof(C28A)=
 Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30A)=Sof(H30A)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C32A)=
 Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(4)
 Sof(Si1)=Sof(C24)=Sof(H24)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=
 Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28A)=Sof(H28B)=
 Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(4)
 Sof(Si2A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34D)=Sof(H34E)=Sof(H34F)=
 Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36A)=Sof(C37A)=
 Sof(H37D)=Sof(H37E)=Sof(H37F)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=
 Sof(C39A)=Sof(H39A)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=Sof(C41A)=
 Sof(H41D)=Sof(H41E)=Sof(H41F)=1-FVAR(5)
 Sof(Si2)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=
 Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37A)=Sof(H37B)=
 Sof(H37C)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39)=Sof(C40)=
 Sof(H40A)=Sof(H40B)=Sof(H40C)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(5)
 Fixed Sof: C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C54A(0.5) H54D(0.5)
 H54E(0.5) H54F(0.5) C55(0.5) H55A(0.5) H55B(0.5) C55A(0.5) H55C(0.5) H55D(0.5)
 C56(0.5) H56A(0.5) H56B(0.5) C56A(0.5) H56C(0.5) H56D(0.5) C57(0.5) H57A(0.5)
 H57B(0.5) C57A(0.5) H57C(0.5) H57D(0.5) C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5)
 C58A(0.5) H58D(0.5) H58E(0.5) H58F(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 C60(0.5) H60A(0.5) H60B(0.5) C61(0.5) H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5)
 H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
5.a Ternary CH refined with riding coordinates:
 C24(H24), C24A(H24A), C27(H27), C27A(H27A), C30(H30), C30A(H30A), C33(H33),
 C33A(H33A), C36(H36), C36A(H36A), C39(H39), C39A(H39A)
5.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C42A(H42C,H42D), C43(H43A,H43B), C43A(H43C,H43D), C44(H44A,
 H44B), C44A(H44C,H44D), C45(H45A,H45B), C45A(H45C,H45D), C46(H46A,H46B),
 C46A(H46C,H46D), C47(H47A,H47B), C47A(H47C,H47D), C48(H48A,H48B), C48A(H48C,
 H48D), C49(H49A,H49B), C49A(H49C,H49D), C50(H50A,H50B), C50A(H50C,H50D),
 C51(H51A,H51B), C51A(H51C,H51D), C52(H52A,H52B), C52A(H52C,H52D), C53(H53A,
 H53B), C53A(H53C,H53D), C55(H55A,H55B), C55A(H55C,H55D), C56(H56A,H56B),
 C56A(H56C,H56D), C57(H57A,H57B), C57A(H57C,H57D), C60(H60A,H60B), C61(H61A,
 H61B), C62(H62A,H62B)
5.c Me refined with riding coordinates:
 C54(H54A,H54B,H54C), C54A(H54D,H54E,H54F), C58(H58A,H58B,H58C), C58A(H58D,
 H58E,H58F), C59(H59A,H59B,H59C), C63(H63A,H63B,H63C)
5.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C11(H11)
5.e Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C15A(H15D,H15E,H15F), C16(H16A,H16B,H16C), C16A(H16D,
 H16E,H16F), C17(H17A,H17B,H17C), C17A(H17D,H17E,H17F), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C21A(H21D,H21E,H21F), C22(H22A,H22B,
 H22C), C22A(H22D,H22E,H22F), C23(H23A,H23B,H23C), C23A(H23D,H23E,H23F),
 C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C26(H26A,H26B,H26C), C26A(H26D,H26E,
 H26F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C29(H29A,H29B,H29C),
 C29A(H29D,H29E,H29F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F), C32(H32A,H32B,
 H32C), C32A(H32D,H32E,H32F), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F),
 C35(H35A,H35B,H35C), C35A(H35D,H35E,H35F), C37(H37A,H37B,H37C), C37A(H37D,H37E,
 H37F), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F), C40(H40A,H40B,H40C),
 C40A(H40D,H40E,H40F), C41(H41A,H41B,H41C), C41A(H41D,H41E,H41F)
;
_shelx_res_checksum              18917
_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 1.759
_oxdiff_exptl_absorpt_empirical_full_min 0.622