Inside or outside the box? Effect of substrate location on coordination-cage based catalysis
Solea, Atena B.; Sudittapong, Burin; Taylor, Christopher G. P.; Ward, Michael D.; Dalton Transactions  (2022) –; doi:10.1039/D2DT01713J

data_7710648
_publ_section_title
;
 Inside or outside the box? Effect of substrate location on
 coordination-cage based catalysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01713J
_journal_year                    2022
_chemical_formula_moiety
'2(C168 H132 N36 Ni4), 9.6(B F4), 2.3(C8 H7 N O4), 6.4[BF4], 13[CH3OH]'
_chemical_formula_sum            'C367.4 H332.1 B16 F64 N74.3 Ni8 O22.2'
_chemical_formula_weight         8001.99
_chemical_properties_physical    Efflorescent
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-13
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-05-27 deposited with the CCDC.	2022-06-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.927(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.4788(5)
_cell_length_b                   30.5879(5)
_cell_length_c                   39.9794(7)
_cell_measurement_reflns_used    19357
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      58.1760
_cell_measurement_theta_min      2.7780
_cell_volume                     37797.0(11)
_computing_cell_refinement       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.80a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6093
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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    -74.00  31.00   0.30   20.00    --  -41.82  77.00-180.00  350
  2  \w     14.00  99.20   0.30   20.00    --   41.82  57.00  90.00  284
  3  \w     86.00 126.20   0.30   20.00    --   41.82-178.00  30.00  134
  4  \w     44.00 134.00   0.30  117.50    --  105.98 -61.00  30.00  300
  5  \w    104.00 165.20   0.30  117.50    --  105.98  77.00  30.00  204
  6  \w     79.00 177.10   0.30  117.50    --  105.98  61.00-180.00  327
  7  \w     30.00 131.10   0.30  117.50    --  105.98 -77.00 -90.00  337
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  '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      0.0119307000
_diffrn_orient_matrix_UB_12      0.0411494000
_diffrn_orient_matrix_UB_13      -0.0184075000
_diffrn_orient_matrix_UB_21      0.0318808000
_diffrn_orient_matrix_UB_22      -0.0271344000
_diffrn_orient_matrix_UB_23      -0.0163736000
_diffrn_orient_matrix_UB_31      -0.0364256000
_diffrn_orient_matrix_UB_32      -0.0102946000
_diffrn_orient_matrix_UB_33      -0.0305499000
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0693
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            119936
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        65.088
_diffrn_reflns_theta_max         65.088
_diffrn_reflns_theta_min         2.675
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.80a (Rigaku Oxford Diffraction, 2020)
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            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             16457
_exptl_crystal_preparation
'Crystal of the nickel cage were grown in methanol solvothermally contained within a glass via. Crystal was soaked in a solution of 4-Nitrophenyl acetate in methanolic mother liquor (from the solvothermal crystals growth) for 24 hours. Crystals were transferred to Fomblin oil before being mounted on a MiteGen Microloop.'
_exptl_crystal_recrystallization_method
'crystal grown from solvothermal slow rolling, then immersed in solution of guest'
_exptl_crystal_size_max          0.177
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.112
_refine_diff_density_max         1.170
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     4633
_refine_ls_number_reflns         63718
_refine_ls_number_restraints     21834
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.2009
_refine_ls_R_factor_gt           0.1191
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3261
_refine_ls_wR_factor_ref         0.4049
_reflns_Friedel_coverage         0.000
_reflns_number_gt                28449
_reflns_number_total             63718
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01713j2.cif
_cod_data_source_block           bs02_2
_cod_original_formula_sum        'C367.40 H332.10 B16 F64 N74.30 Ni8 O22.20'
_cod_database_code               7710648
_smtbx_masks_special_details
;
A solvent mask was calculated and 1968 electrons were 
found in a volume of 7504\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
6.4[BF4], 13[CH3OH] per Formula Unit 
which account for 1986 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C300 H300 N72 Ni8 B16 F64'
_chemical_oxdiff_usercomment
'4NPA Ni 15np Bf4 cube soaked 4nitrophenylacetate'
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.802
_reflns_odcompleteness_completeness 98.48
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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
 C11G-O21G = C11H-O21H = C11I-O21I
 1.407 with sigma of 0.02
 O21G-C22G = O21H-C22H = O21I-C22I
 1.355 with sigma of 0.02
 C22G-O23G = C22H-O23H = C22I-O23I
 1.205 with sigma of 0.02
 C22G-C24G = C22H-C24H = C22I-C24I
 1.491 with sigma of 0.02
 C11G-C22G = C11H-C22H = C11I-C22I
 2.37 with sigma of 0.04
 O21G-O23G = O21H-O23H = O21I-O23I
 2.245 with sigma of 0.04
 O21G-C24G = O21H-C24H = O21I-C24I
 2.346 with sigma of 0.04
 O23G-C24G = O23H-C24H = O23I-C24I
 2.393 with sigma of 0.04
 N31I-C14I = N31H-C14H = N31G-C14G
 1.461 with sigma of 0.02
 N31G-O32G = N31G-O33G = N31H-O32H = N31H-O33H = N31I-O32I = N31I-O33I
 1.225 with sigma of 0.02
 O32G-O33G = O33H-O32H = O33I-O32I
 2.144 with sigma of 0.04
 C14G-O32G = C14G-O33G = C14H-O32H = C14H-O33H = C14I-O32I = C14I-O33I
 2.311 with sigma of 0.04
3. Restrained planarity
 O21G, C22G, O23G, C24G
 with sigma of 0.1
 C14G, N31G, O32G, O33G
 with sigma of 0.1
 O21H, C22H, O23H, C24H
 with sigma of 0.1
 C14H, N31H, O32H, O33H
 with sigma of 0.1
 O21I, C22I, O23I, C24I
 with sigma of 0.1
 C14I, N31I, O32I, O33I
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2.5A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2.5A
Uanis(B45) = Uanis(B45A)
Uanis(B55) = Uanis(B55A)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Same fragment restrains
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31A, C32A, C33A, C34A, C35A, C36A}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41A, N42A, C43A, C44A, C45A, C46A}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11B, C12B, C13B, C14B, C15B, C16B}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21B, N22B, C23B, C24B, C25B, C26B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31B, C32B, C33B, C34B, C35B, C36B}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41B, N42B, C43B, C44B, C45B, C46B}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50B, C51B, C52B, C53B, C54B, C55B, C56B, C57B, C58B, C59B}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11C, C12C, C13C, C14C, C15C, C16C}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21C, N22C, C23C, C24C, C25C, C26C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31C, C32C, C33C, C34C, C35C, C36C}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41C, N42C, C43C, C44C, C45C, C46C}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50C, C51C, C52C, C53C, C54C, C55C, C56C, C57C, C58C, C59C}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11D, C12D, C13D, C14D, C15D, C16D}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21D, N22D, C23D, C24D, C25D, C26D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31D, C32D, C33D, C34D, C35D, C36D}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41D, N42D, C43D, C44D, C45D, C46D}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50D, C51D, C52D, C53D, C54D, C55D, C56D, C57D, C58D, C59D}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11E, C12E, C13E, C14E, C15E, C16E}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21E, N22E, C23E, C24E, C25E, C26E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31E, C32E, C33E, C34E, C35E, C36E}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41E, N42E, C43E, C44E, C45E, C46E}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50E, C51E, C52E, C53E, C54E, C55E, C56E, C57E, C58E, C59E}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11F, C12F, C13F, C14F, C15F, C16F}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21F, N22F, C23F, C24F, C25F, C26F}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31F, C32F, C33F, C34F, C35F, C36F}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41F, N42F, C43F, C44F, C45F, C46F}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50F, C51F, C52F, C53F, C54F, C55F, C56F, C57F, C58F, C59F}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11J, C12J, C13J, C14J, C15J, C16J}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21J, N22J, C23J, C24J, C25J, C26J}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31J, C32J, C33J, C34J, C35J, C36J}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41J, N42J, C43J, C44J, C45J, C46J}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50J, C51J, C52J, C53J, C54J, C55J, C56J, C57J, C58J, C59J}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11K, C12K, C13K, C14K, C15K, C16K}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21K, N22K, C23K, C24K, C25K, C26K}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31K, C32K, C33K, C34K, C35K, C36K}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41K, N42K, C43K, C44K, C45K, C46K}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50K, C51K, C52K, C53K, C54K, C55K, C56K, C57K, C58K, C59K}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11L, C12L, C13L, C14L, C15L, C16L}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21L, N22L, C23L, C24L, C25L, C26L}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31L, C32L, C33L, C34L, C35L, C36L}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41L, N42L, C43L, C44L, C45L, C46L}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50L, C51L, C52L, C53L, C54L, C55L, C56L, C57L, C58L, C59L}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11M, C12M, C13M, C14M, C15M, C16M}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21M, N22M, C23M, C24M, C25M, C26M}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31M, C32M, C33M, C34M, C35M, C36M}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41M, N42M, C43M, C44M, C45M, C46M}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50M, C51M, C52M, C53M, C54M, C55M, C56M, C57M, C58M, C59M}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11N, C12N, C13N, C14N, C15N, C16N}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21N, N22N, C23N, C24N, C25N, C26N}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31N, C32N, C33N, C34N, C35N, C36N}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41N, N42N, C43N, C44N, C45N, C46N}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50N, C51N, C52N, C53N, C54N, C55N, C56N, C57N, C58N, C59N}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N11P, C12P, C13P, C14P, C15P, C16P}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N21P, N22P, C23P, C24P, C25P, C26P}
{N11A, C12A, C13A, C14A, C15A, C16A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N31P, C32P, C33P, C34P, C35P, C36P}
{N21A, N22A, C23A, C24A, C25A, C26A} sigma for 1-2: 0.02, 1-3: 0.04
as in
{N41P, N42P, C43P, C44P, C45P, C46P}
{C50A, C51A, C52A, C53A, C54A, C55A, C56A, C57A, C58A, C59A} sigma for 1-2:
0.02, 1-3: 0.04
as in
{C50P, C51P, C52P, C53P, C54P, C55P, C56P, C57P, C58P, C59P}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B15, F16, F17, F18, F19}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B20, F21, F22, F23, F24}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B25, F26, F27, F28, F29}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B30, F31, F32, F33, F34}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B35, F36, F37, F38, F39}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B40, F41, F42, F43, F44}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B45, F46, F47, F48, F49}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B45A, F46A, F47A, F48A, F49A}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B50, F51, F52, F53, F54}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B55, F56, F57, F58, F59}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B55A, F56A, F57A, F58A, F59A}
{B10, F11, F12, F13, F14} sigma for 1-2: 0.02, 1-3: 0.04
as in
{B60, F61, F62, F63, F64}
7. Others
 Fixed Sof: B35(0.75) F36(0.75) F37(0.75) F38(0.75) F39(0.75) B40(0.5)
 F41(0.5) F42(0.5) F43(0.5) F44(0.5) B45(0.5) F46(0.5) F47(0.5) F48(0.5)
 F49(0.5) B45A(0.5) F46A(0.5) F47A(0.5) F48A(0.5) F49A(0.5) B50(0.7) F51(0.7)
 F52(0.7) F53(0.7) F54(0.7) B55(0.5) F56(0.5) F57(0.5) F58(0.5) F59(0.5)
 B55A(0.5) F56A(0.5) F57A(0.5) F58A(0.5) F59A(0.5) B60(0.65) F61(0.65)
 F62(0.65) F63(0.65) F64(0.65) C11I(0.3) C12I(0.3) H12I(0.3) C13I(0.3)
 H13I(0.3) C14I(0.3) C15I(0.3) H15I(0.3) C16I(0.3) H16I(0.3) O21I(0.3)
 C22I(0.3) O23I(0.3) C24I(0.3) H24S(0.3) H24T(0.3) H24U(0.3) N31I(0.3)
 O32I(0.3) O33I(0.3)
8.a Secondary CH2 refined with riding coordinates:
 C26A(H26A,H26B), C46A(H46A,H46B), C26B(H26C,H26D), C46B(H46C,H46D), C26C(H26E,
 H26F), C46C(H46E,H46F), C26D(H26G,H26H), C46D(H46G,H46H), C26E(H26I,H26J),
 C46E(H46I,H46J), C26F(H26K,H26L), C46F(H46K,H46L), C26J(H26M,H26N), C46J(H46M,
 H46N), C26K(H26O,H26P), C46K(H46O,H46P), C26L(H26Q,H26R), C46L(H46Q,H46R),
 C26M(H26S,H26T), C46M(H46S,H46T), C26N(H26U,H26V), C46N(H46U,H46V), C26P(H26W,
 H26X), C46P(H46W,H46X)
8.b Me refined with riding coordinates:
 C24G(H24G,H24H,H24I), C24H(H24O,H24Q,H24R), C24I(H24S,H24T,H24U)
8.c Aromatic/amide H refined with riding coordinates:
 C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C23A(H23A), C24A(H24A),
 C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C43A(H43A), C44A(H44A),
 C51A(H51A), C52A(H52A), C53A(H53A), C56A(H56A), C57A(H57A), C58A(H58A),
 C13B(H13B), C14B(H14B), C15B(H15B), C16B(H16B), C23B(H23B), C24B(H24B),
 C33B(H33B), C34B(H34B), C35B(H35B), C36B(H36B), C43B(H43B), C44B(H44B),
 C51B(H51B), C52B(H52B), C53B(H53B), C56B(H56B), C57B(H57B), C58B(H58B),
 C13C(H13C), C14C(H14C), C15C(H15C), C16C(H16C), C23C(H23C), C24C(H24C),
 C33C(H33C), C34C(H34C), C35C(H35C), C36C(H36C), C43C(H43C), C44C(H44C),
 C51C(H51C), C52C(H52C), C53C(H53C), C56C(H56C), C57C(H57C), C58C(H58C),
 C13D(H13D), C14D(H14D), C15D(H15D), C16D(H16D), C23D(H23D), C24D(H24D),
 C33D(H33D), C34D(H34D), C35D(H35D), C36D(H36D), C43D(H43D), C44D(H44D),
 C51D(H51D), C52D(H52D), C53D(H53D), C56D(H56D), C57D(H57D), C58D(H58D),
 C13E(H13E), C14E(H14E), C15E(H15E), C16E(H16E), C23E(H23E), C24E(H24E),
 C33E(H33E), C34E(H34E), C35E(H35E), C36E(H36E), C43E(H43E), C44E(H44E),
 C51E(H51E), C52E(H52E), C53E(H53E), C56E(H56E), C57E(H57E), C58E(H58E),
 C13F(H13F), C14F(H14F), C15F(H15F), C16F(H16F), C23F(H23F), C24F(H24F),
 C33F(H33F), C34F(H34F), C35F(H35F), C36F(H36F), C43F(H43F), C44F(H44F),
 C51F(H51F), C52F(H52F), C53F(H53F), C56F(H56F), C57F(H57F), C58F(H58F),
 C13J(H13J), C14J(H14J), C15J(H15J), C16J(H16J), C23J(H23J), C24J(H24J),
 C33J(H33J), C34J(H34J), C35J(H35J), C36J(H36J), C43J(H43J), C44J(H44J),
 C51J(H51J), C52J(H52J), C53J(H53J), C56J(H56J), C57J(H57J), C58J(H58J),
 C13K(H13K), C14K(H14K), C15K(H15K), C16K(H16K), C23K(H23K), C24K(H24K),
 C33K(H33K), C34K(H34K), C35K(H35K), C36K(H36K), C43K(H43K), C44K(H44K),
 C51K(H51K), C52K(H52K), C53K(H53K), C56K(H56K), C57K(H57K), C58K(H58K),
 C13L(H13L), C14L(H14L), C15L(H15L), C16L(H16L), C23L(H23L), C24L(H24L),
 C33L(H33L), C34L(H34L), C35L(H35L), C36L(H36L), C43L(H43L), C44L(H44L),
 C51L(H51L), C52L(H52L), C53L(H53L), C56L(H56L), C57L(H57L), C58L(H58L),
 C13M(H13M), C14M(H14M), C15M(H15M), C16M(H16M), C23M(H23M), C24M(H24M),
 C33M(H33M), C34M(H34M), C35M(H35M), C36M(H36M), C43M(H43M), C44M(H44M),
 C51M(H51M), C52M(H52M), C53M(H53M), C56M(H56M), C57M(H57M), C58M(H58M),
 C13N(H13N), C14N(H14N), C15N(H15N), C16N(H16N), C23N(H23N), C24N(H24N),
 C33N(H33N), C34N(H34N), C35N(H35N), C36N(H36N), C43N(H43N), C44N(H44N),
 C51N(H51N), C52N(H52N), C53N(H53N), C56N(H56N), C57N(H57N), C58N(H58N),
 C13P(H13P), C14P(H14P), C15P(H15P), C16P(H16P), C23P(H23P), C24P(H24P),
 C33P(H33P), C34P(H34P), C35P(H35P), C36P(H36P), C43P(H43P), C44P(H44P),
 C51P(H51P), C52P(H52P), C53P(H53P), C56P(H56P), C57P(H57P), C58P(H58P),
 C12G(H12G), C13G(H13G), C15G(H15G), C16G(H16G), C12H(H12H), C13H(H13H),
 C15H(H15H), C16H(H16H), C12I(H12I), C13I(H13I), C15I(H15I), C16I(H16I)
8.d Fitted hexagon refined as free rotating group:
 C11G(C12G,C13G,C14G,C15G,C16G), C11H(C12H,C13H,C14H,C15H,C16H), C11I(C12I,
 C13I,C14I,C15I,C16I)
;
_shelx_res_checksum              26261
_shelx_hkl_checksum              2271
_shelx_fab_checksum              45050
_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 1.921
_oxdiff_exptl_absorpt_empirical_full_min 0.716