Self-Sorting Assembly of Molecular Trefoil Knots of Single Handedness.
Zhong, Jiankang; Zhang, Liang; August, David P.; Whitehead, George F. S.; Leigh, David A.; Journal of the American Chemical Society 141 (2019) 14249–14256; doi:10.1021/jacs.9b06127

data_4128815
_publ_section_title
;
 Self-Sorting Assembly of Molecular Trefoil Knots of Single Handedness.
;
_journal_issue                   36
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14249
_journal_page_last               14256
_journal_paper_doi               10.1021/jacs.9b06127
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C90 H102 Co3 N18 O12, 3(B F4), 4(C2 H3 N)'
_chemical_formula_sum            'C98 H114 B3 Co3 F12 N22 O12'
_chemical_formula_weight         2229.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.308(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.4608(10)
_cell_length_b                   20.0262(6)
_cell_length_c                   17.6570(12)
_cell_measurement_reflns_used    8961
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      70.4640
_cell_measurement_theta_min      5.1700
_cell_volume                     5670.3(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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    -45.00 -20.00   1.00    1.00    --    5.00 -45.00  -1.00   25
  2  \w   -132.00 -50.00   1.00    1.00    --  -45.10 -45.00  -1.00   82
  3  \w     -5.00  21.00   1.00    1.00    --  -45.10  45.00 148.00   26
  4  \w   -156.00-130.00   1.00   20.00    -- -110.00 -45.00  -1.00   26
  5  \w    -48.00 -21.00   1.00   20.00    -- -110.00  45.00 148.00   27
  6  \w   -135.00 -77.00   1.00   20.00    -- -110.00  45.00 148.00   58
  7  \w      0.00  26.00   1.00    1.00    --    5.00  45.00 148.00   26
  8  \w    -50.00 -11.00   1.00    1.00    --  -45.10 -52.00-179.77   39
  9  \w   -133.00 -99.00   1.00    1.00    --  -45.10 -52.00-179.77   34
 10  \w   -132.00 -11.00   1.00    1.00    --  -45.10 -52.00  55.31  121
 11  \w    -69.00 -44.00   1.00    1.00    --  -45.10  50.00 -91.22   25
 12  \w   -133.00 -13.00   1.00    1.00    --  -45.10 -57.00 -60.00  120
 13  \w    -39.00  44.00   1.00    1.00    --  -45.10  50.00 -91.22   83
 14  \w   -184.00-135.00   1.00   20.00    -- -110.00 -75.00-115.22   49
 15  \w   -142.00 -21.00   1.00   20.00    -- -110.00  57.00   0.00  121
 16  \w   -187.00-156.00   1.00   20.00    -- -110.00 -36.00 -98.94   31
 17  \w   -199.00 -87.00   1.00   20.00    -- -110.00 -19.00 150.00  112
 18  \w    -59.00 -21.00   1.00   20.00    -- -110.00 -19.00 150.00   38
 19  \w    -98.00 -72.00   1.00   20.00    -- -110.00 -41.00-101.71   26
 20  \w    -98.00 -70.00   1.00   20.00    -- -110.00 -75.00-115.22   28
 21  \w    -96.00 -70.00   1.00   20.00    -- -110.00 -76.00 -60.00   26
 22  \w   -199.00-108.00   1.00   20.00    -- -110.00 -76.00 -60.00   91
 23  \w   -199.00 -70.00   1.00   20.00    -- -110.00 -76.00 -30.00  129
 24  \w   -169.00-143.00   1.00   20.00    -- -110.00 -38.00-180.00   26
 25  \w   -107.00 -69.00   1.00   20.00    -- -110.00 -38.00-180.00   38
 26  \w   -198.00-173.00   1.00   20.00    -- -110.00 -53.00-113.72   25
 27  \w   -113.00 -76.00   1.00   20.00    -- -110.00 -53.00-113.72   37
 28  \w    -97.00 -72.00   1.00   20.00    -- -110.00 -73.00-103.88   25
 29  \w   -146.00-120.00   1.00   20.00    -- -110.00 -38.00-120.00   26
 30  \w   -108.00 -74.00   1.00   20.00    -- -110.00 -38.00-120.00   34
 31  \w   -185.00-160.00   1.00   20.00    -- -110.00   0.00   0.00   25
 32  \w    -98.00 -73.00   1.00   20.00    -- -110.00 -42.00-119.15   25
 33  \w   -198.00-168.00   1.00   20.00    -- -110.00 -19.00 120.00   30
 34  \w   -102.00 -77.00   1.00   20.00    -- -110.00 -47.00-115.47   25
 35  \w   -166.00-127.00   1.00   20.00    -- -110.00 -41.00 -93.29   39
 36  \w    -96.00 -71.00   1.00   20.00    -- -110.00 -41.00 -93.29   25
 37  \w   -175.00-134.00   1.00   20.00    -- -110.00 -57.00  90.00   41
 38  \w    -96.00 -71.00   1.00   20.00    -- -110.00 -76.00 -90.00   25
 39  \w   -194.00-106.00   1.00   20.00    -- -110.00 -43.00-153.55   88
 40  \w   -135.00-107.00   1.00   20.00    -- -110.00 -19.00 120.00   28
 41  \w    -97.00 -72.00   1.00   20.00    -- -110.00 -74.00 -75.65   25
 42  \w    -93.00 -68.00   1.00   20.00    -- -110.00 -36.00 -98.94   25
 43  \w    -68.00 -25.00   1.00   20.00    -- -110.00   0.00   0.00   43
 44  \w    -47.00 -22.00   1.00   20.00    -- -110.00 -19.00-150.00   25
 45  \w   -182.00-156.00   1.00   20.00    -- -110.00 -57.00 -30.00   26
 46  \w    -98.00 -73.00   1.00   20.00    -- -110.00 -45.00-140.25   25
 47  \w    -97.00 -72.00   1.00   20.00    -- -110.00 -39.00-143.26   25
 48  \w   -151.00 -41.00   1.00   20.00    -- -110.00  38.00   0.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0453442000
_diffrn_orient_matrix_UB_12      -0.0117924000
_diffrn_orient_matrix_UB_13      -0.0934993000
_diffrn_orient_matrix_UB_21      -0.0671613000
_diffrn_orient_matrix_UB_22      -0.0411835000
_diffrn_orient_matrix_UB_23      0.0151078000
_diffrn_orient_matrix_UB_31      -0.0516472000
_diffrn_orient_matrix_UB_32      0.0638684000
_diffrn_orient_matrix_UB_33      -0.0075314000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27996
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        56.915
_diffrn_reflns_theta_max         56.915
_diffrn_reflns_theta_min         5.192
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    4.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.12b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.573
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.014
_refine_diff_density_max         0.642
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 2086 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.453
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         7547
_refine_ls_number_restraints     922
_refine_ls_restrained_S_all      1.450
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1200
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3169
_refine_ls_wR_factor_ref         0.3485
_reflns_Friedel_coverage         0.920
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                5947
_reflns_number_total             7547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b06127_si_004.cif
_cod_data_source_block           rdl25
_cod_database_code               4128815
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.201
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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
 C44-C45 = C29-C30 = C1-C2
 1.35 with sigma of 0.02
 N13-C49
 1.15 with sigma of 0.02
 C49-C48
 1.54 with sigma of 0.01
 C48-N13
 2.69 with sigma of 0.02
 C42-C44 = C4-C2 = C27-C29
 2.4 with sigma of 0.02
 C42-C43 = C44-C43 = C3-C4 = C3-C2 = C27-C28 = C29-C28
 1.54 with sigma of 0.02
 N12-C47
 1.15 with sigma of 0.02
 C47-C46
 1.54 with sigma of 0.02
 H45B-C6A_$1
 -2 with sigma of 0.02
 N12-N12_$2
 -3 with sigma of 0.02
 O6-C42 \\sim O6-C40 \\sim O1-C4 \\sim O1-C6 \\sim O4-C25 \\sim O4-C27
 with sigma of 0.02
 C28-C30 \\sim C3-C1 \\sim C45-C43
 with sigma of 0.02
 O1-C7 \\sim O1-C5 \\sim O6-C39 \\sim O6-C41 \\sim O4-C26 \\sim O4-C24
 with sigma of 0.02
 Co1-N4 \\sim Co1-N4A
 with sigma of 0.02
 Co1-N3 \\sim Co1-N3A
 with sigma of 0.02
 O2-C13 \\sim O2A-C13A
 with sigma of 0.02
 C14-C13 \\sim C14-C13A
 with sigma of 0.02
 N4-C13 \\sim N4A-C13A
 with sigma of 0.02
 N4-C11 \\sim N4A-C11A
 with sigma of 0.02
 N3-C5 \\sim N3A-C5A
 with sigma of 0.02
 N3-C9 \\sim N3A-C9A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C6-O1 \\sim C6A-O1A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 O1-C4 \\sim O1A-C4A
 with sigma of 0.02
 C10-C11 \\sim C10A-C11A
 with sigma of 0.02
 C12-C11 \\sim C12A-C11A
 with sigma of 0.02
 C4-C3 \\sim C4A-C3A
 with sigma of 0.02
 C3-C2 \\sim C3A-C2A
 with sigma of 0.02
 C2-C1 \\sim C2A-C1A
 with sigma of 0.02
 Co1-C5 \\sim Co1-C5A
 with sigma of 0.04
 Co1-C9 \\sim Co1-C9A
 with sigma of 0.04
 Co1-C13 \\sim Co1-C13A
 with sigma of 0.04
 Co1-C11 \\sim Co1-C11A
 with sigma of 0.04
 O2-C14 \\sim O2A-C14
 with sigma of 0.04
 O2-N4 \\sim O2A-N4A
 with sigma of 0.04
 C14-N4 \\sim C14-N4A
 with sigma of 0.04
 N4-C10 \\sim N4A-C10A
 with sigma of 0.04
 N4-C12 \\sim N4A-C12A
 with sigma of 0.04
 N3-C6 \\sim N3A-C6A
 with sigma of 0.04
 N3-C8 \\sim N3A-C8A
 with sigma of 0.04
 N3-C10 \\sim N3A-C10A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 C5-C9 \\sim C5A-C9A
 with sigma of 0.04
 C5-O1 \\sim C5A-O1A
 with sigma of 0.04
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C6-C4 \\sim C6A-C4A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C7-O1 \\sim C7A-O1A
 with sigma of 0.04
 C8-C10 \\sim C8A-C10A
 with sigma of 0.04
 C9-C11 \\sim C9A-C11A
 with sigma of 0.04
 O1-C3 \\sim O1A-C3A
 with sigma of 0.04
 C13-C11 \\sim C13A-C11A
 with sigma of 0.04
 C10-C12 \\sim C10A-C12A
 with sigma of 0.04
 C4-C2 \\sim C4A-C2A
 with sigma of 0.04
 C3-C1 \\sim C3A-C1A
 with sigma of 0.04
 Co1-N10 \\sim Co1-N10A
 with sigma of 0.02
 Co1-N11 \\sim Co1-N11A
 with sigma of 0.02
 C34-C35 \\sim C34A-C35A
 with sigma of 0.02
 N10-C33 \\sim N10A-C33
 with sigma of 0.02
 N10-C35 \\sim N10A-C35A
 with sigma of 0.02
 O6-C40 \\sim O6A-C40A
 with sigma of 0.02
 O6-C42 \\sim O6A-C42A
 with sigma of 0.02
 N11-C37 \\sim N11A-C37A
 with sigma of 0.02
 N11-C41 \\sim N11A-C41A
 with sigma of 0.02
 C37-C38 \\sim C37A-C38A
 with sigma of 0.02
 C37-C36 \\sim C37A-C36A
 with sigma of 0.02
 C39-C38 \\sim C39A-C38A
 with sigma of 0.02
 C39-C40 \\sim C39A-C40A
 with sigma of 0.02
 C41-C40 \\sim C41A-C40A
 with sigma of 0.02
 C36-C35 \\sim C36A-C35A
 with sigma of 0.02
 C45-C44 \\sim C45A-C44A
 with sigma of 0.02
 C44-C43 \\sim C44A-C43A
 with sigma of 0.02
 C42-C43 \\sim C42A-C43A
 with sigma of 0.02
 Co1-C37 \\sim Co1-C37A
 with sigma of 0.04
 Co1-C41 \\sim Co1-C41A
 with sigma of 0.04
 Co1-C35 \\sim Co1-C35A
 with sigma of 0.04
 C34-N10 \\sim C34A-N10A
 with sigma of 0.04
 C34-C36 \\sim C34A-C36A
 with sigma of 0.04
 N10-C36 \\sim N10A-C36A
 with sigma of 0.04
 O6-C39 \\sim O6A-C39A
 with sigma of 0.04
 O6-C41 \\sim O6A-C41A
 with sigma of 0.04
 O6-C43 \\sim O6A-C43A
 with sigma of 0.04
 N11-C38 \\sim N11A-C38A
 with sigma of 0.04
 N11-C36 \\sim N11A-C36A
 with sigma of 0.04
 N11-C40 \\sim N11A-C40A
 with sigma of 0.04
 C33-C35 \\sim C33-C35A
 with sigma of 0.04
 C37-C39 \\sim C37A-C39A
 with sigma of 0.04
 C37-C41 \\sim C37A-C41A
 with sigma of 0.04
 C37-C35 \\sim C37A-C35A
 with sigma of 0.04
 C39-C41 \\sim C39A-C41A
 with sigma of 0.04
 C38-C36 \\sim C38A-C36A
 with sigma of 0.04
 C38-C40 \\sim C38A-C40A
 with sigma of 0.04
 C40-C42 \\sim C40A-C42A
 with sigma of 0.04
 C45-C43 \\sim C45A-C43A
 with sigma of 0.04
 C44-C42 \\sim C44A-C42A
 with sigma of 0.04
 O4-C25 \\sim O4A-C25
 with sigma of 0.02
 O4-C27 \\sim O4A-C27A
 with sigma of 0.02
 C27-C28 \\sim C27A-C28A
 with sigma of 0.02
 C29-C28 \\sim C29A-C28A
 with sigma of 0.02
 C29-C30 \\sim C29A-C30A
 with sigma of 0.02
 O4-C28 \\sim O4A-C28A
 with sigma of 0.04
 C25-C27 \\sim C25-C27A
 with sigma of 0.04
 C27-C29 \\sim C27A-C29A
 with sigma of 0.04
 C28-C30 \\sim C28A-C30A
 with sigma of 0.04
 Co1-N4 \\sim Co1-N4A \\sim Co1-N3A \\sim Co1-N3 \\sim Co1-N10 \\sim Co1-N10A
\\sim Co1-N11A \\sim Co1-N11
 \\sim Co1-N5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. 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
5. Others
 Fixed Sof: O2(0.5) N4(0.5) N3(0.5) C5(0.5) H5(0.5) C6(0.5) C7(0.5) H7(0.5)
 C8(0.5) H8(0.5) C9(0.5) O1(0.5) C34(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
 N10(0.5) O4(0.5) C13(0.5) O6(0.5) N11(0.5) C37(0.5) C10(0.5) H10A(0.5)
 H10B(0.5) C39(0.5) H39(0.5) C38(0.5) H38(0.5) C41(0.5) H41(0.5) C12(0.5)
 H12A(0.5) H12B(0.5) H12C(0.5) C36(0.5) H36A(0.5) H36B(0.5) C40(0.5) C11(0.5)
 H11(0.5) C35(0.5) H35(0.5) C27(0.5) H27A(0.5) H27B(0.5) C45(0.5) H45A(0.5)
 H45B(0.5) C44(0.5) H44(0.5) C4(0.5) H4A(0.5) H4B(0.5) C42(0.5) H42A(0.5)
 H42B(0.5) C29(0.5) H29(0.5) C28(0.5) H28A(0.5) H28B(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) C43(0.5) H43A(0.5) H43B(0.5) C3(0.5) H3A(0.5) H3B(0.5) C2(0.5)
 H2(0.5) C1(0.5) H1A(0.5) H1B(0.5) C12A(0.5) H12D(0.5) H12E(0.5) H12F(0.5)
 C11A(0.5) H11A(0.5) C10A(0.5) H10C(0.5) H10D(0.5) N4A(0.5) C13A(0.5) O2A(0.5)
 C9A(0.5) N3A(0.5) C5A(0.5) H5A(0.5) C8A(0.5) H8AA(0.5) H8AB(0.5) C6A(0.5)
 C7A(0.5) H7A(0.5) O1A(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) C3A(0.5) H3AA(0.5)
 H3AB(0.5) C2A(0.5) H2A(0.5) C1A(0.5) H1AA(0.5) H1AB(0.5) C34A(0.5) H34D(0.5)
 H34E(0.5) H34F(0.5) C35A(0.5) H35A(0.5) N10A(0.5) C36A(0.5) H36C(0.5)
 C37A(0.5) N11A(0.5) C41A(0.5) H41A(0.5) C38A(0.5) H38A(0.5) C39A(0.5)
 H39A(0.5) C40A(0.5) O6A(0.5) C42A(0.5) H42C(0.5) H42D(0.5) C43A(0.5) H43C(0.5)
 H43D(0.5) C44A(0.5) H44A(0.5) C45A(0.5) H45C(0.5) H45D(0.5) O4A(0.5) C27A(0.5)
 H27C(0.5) H27D(0.5) C29A(0.5) H29A(0.5) C28A(0.5) H28C(0.5) H28D(0.5)
 C30A(0.5) H30C(0.5) H30D(0.5)
6.a Ternary CH refined with riding coordinates:
 C20(H20), C11(H11), C35(H35), C11A(H11A), C35A(H35A)
6.b Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C10(H10A,H10B), C36(H36A,H36B), C27(H27A,H27B), C4(H4A,H4B),
 C42(H42A,H42B), C28(H28A,H28B), C43(H43A,H43B), C3(H3A,H3B), C10A(H10C,H10D),
 C8A(H8AA,H8AB), C4A(H4AA,H4AB), C3A(H3AA,H3AB), C42A(H42C,H42D), C43A(H43C,
 H43D), C27A(H27C,H27D), C28A(H28C,H28D)
6.c Me refined with riding coordinates:
 C34(H34A,H34B,H34C), C12(H12A,H12B,H12C), C12A(H12D,H12E,H12F), C34A(H34D,
 H34E,H34F)
6.d Aromatic/amide H refined with riding coordinates:
 C16(H16), C31(H31), C5(H5), C7(H7), C8(H8), C15(H15), C26(H26), C39(H39),
 C38(H38), C41(H41), C23(H23), C24(H24), C44(H44), C29(H29), C2(H2), C5A(H5A),
 C7A(H7A), C2A(H2A), C36A(H36C), C41A(H41A), C38A(H38A), C39A(H39A), C44A(H44A),
  C29A(H29A)
6.e X=CH2 refined with riding coordinates:
 C45(H45A,H45B), C30(H30A,H30B), C1(H1A,H1B), C1A(H1AA,H1AB), C45A(H45C,H45D),
 C30A(H30C,H30D)
6.f Idealised Me refined with riding coordinates:
 C48(H48A,H48B,H48C), C46(H46A,H46B,H46C)
6.g Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C)
;
_shelx_res_checksum              75565
_shelx_hkl_checksum              61698
_shelx_fab_checksum              80910
_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 1.817
_oxdiff_exptl_absorpt_empirical_full_min 0.568