Lanthanide Template Synthesis of Trefoil Knots of Single Handedness.
Zhang, Gen; Gil-Ramírez, Guzmán; Markevicius, Augustinas; Browne, Colm; Vitorica-Yrezabal, Iñigo J; Leigh, David A.; Journal of the American Chemical Society 137 (2015) 10437–10442; doi:10.1021/jacs.5b07069

data_4124245
_publ_section_title
;
 Lanthanide Template Synthesis of Trefoil Knots of Single Handedness.
;
_journal_issue                   32
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10437
_journal_page_last               10442
_journal_paper_doi               10.1021/jacs.5b07069
_journal_volume                  137
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C117.36 H116.64 F1.09 Lu N9 O13.09 S0.36, 2.64(C F3 O3 S), C4 H10 O, 0.64(C H4 O)'
_chemical_formula_sum            'C124.63 H129.15 F9 Lu N9 O22.63 S3'
_chemical_formula_weight         2557.31
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7797(4)
_cell_length_b                   22.7717(4)
_cell_length_c                   31.2128(7)
_cell_measurement_reflns_used    25362
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.5210
_cell_measurement_theta_min      2.4020
_cell_volume                     12637.3(5)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega   78.82  260.32   1.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      107.8559   73.8672   42.6420 121

  2 omega   79.77  261.27   1.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      108.8140   73.8672 -143.5789 121

  3 phi   -187.53  170.82   1.4994    7.5000
omega____ theta____ kappa____ phi______ frames
 -50.7813  -39.9910   73.8672     -     239

  4 omega -106.71   73.29   1.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -77.6710   73.8672   81.0288 120

  5 omega   80.61  262.11   1.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      109.6490   73.8672  -17.2547 121

  6 omega   83.20  264.70   1.5000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      112.2409   73.8672   58.2247 121
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_orient_matrix_UB_11      -0.0650744000
_diffrn_orient_matrix_UB_12      -0.0293076000
_diffrn_orient_matrix_UB_13      -0.0245595000
_diffrn_orient_matrix_UB_21      -0.0430385000
_diffrn_orient_matrix_UB_22      -0.0084919000
_diffrn_orient_matrix_UB_23      0.0423463000
_diffrn_orient_matrix_UB_31      -0.0377330000
_diffrn_orient_matrix_UB_32      0.0604203000
_diffrn_orient_matrix_UB_33      -0.0060155000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            71305
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.402
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.663
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61676
_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.
;
_exptl_crystal_colour            'clear brownish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_description       block
_exptl_crystal_F_000             5284
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.797
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 7267 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.002(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1442
_refine_ls_number_reflns         22915
_refine_ls_number_restraints     1623
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0704
_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^)+(0.1486P)^2^+5.0658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1965
_refine_ls_wR_factor_ref         0.2147
_reflns_Friedel_coverage         0.839
_reflns_friedel_fraction_full    0.984
_reflns_friedel_fraction_max     0.982
_reflns_number_gt                18244
_reflns_number_total             22915
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b07069_si_003.cif
_cod_data_source_block           xdl21
_cod_depositor_comments
'Adding full bibliography for 4124245--4124246.cif.'
_cod_database_code               4124245
_shelxl_version_number           2014/6
_reflns_odcompleteness_completeness 97.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.25
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O1D-C2N
 1.45 with sigma of 0.02
 C3B-C3C
 1.54 with sigma of 0.02
 C3B-O1D
 2.4 with sigma of 0.02
 C3B-C2V
 2.4 with sigma of 0.02
 C3C-C2V
 1.54 with sigma of 0.02
 C2V-C31
 1.3 with sigma of 0.02
 C3C-C31
 2.4 with sigma of 0.02
 C3U-O3Q
 2.4 with sigma of 0.02
 O3Q-C2F
 1.45 with sigma of 0.02
 O1D-C3J
 1.45 with sigma of 0.02
 C3J-C2N
 2.4 with sigma of 0.02
 C3J-C3B
 1.54 with sigma of 0.02
 C3J-C2N
 2.4 with sigma of 0.02
 C3J-C3B
 1.54 with sigma of 0.02
 C3C-C3J
 2.4 with sigma of 0.02
 C3E-C1R
 2.4 with sigma of 0.02
 O3G-C28
 1.4 with sigma of 0.02
 C2S-O13A
 2.55 with sigma of 0.02
 O11A-C2S
 2.55 with sigma of 0.02
 O10A-C2S
 2.55 with sigma of 0.02
 O10A-O11A
 2.45 with sigma of 0.02
 O11A-O13A
 2.45 with sigma of 0.02
 O10A-O13A
 2.45 with sigma of 0.02
 F15A-S1A
 2.6 with sigma of 0.02
 F7A-S1A
 2.6 with sigma of 0.02
 F7A-O13A
 3 with sigma of 0.02
 O10A-F7A
 3 with sigma of 0.02
 F15A-O13A
 3 with sigma of 0.02
 F15A-O11A
 3 with sigma of 0.02
 C3U-C4C
 1.54 with sigma of 0.02
 C4C-O3Q
 1.45 with sigma of 0.02
 C2V-C30
 2.4 with sigma of 0.02
 C31-C30
 1.54 with sigma of 0.02
 C30-C4C
 2.4 with sigma of 0.02
 C1W-C3I
 1.54 with sigma of 0.02
 C30-C3U
 1.54 with sigma of 0.02
 C4A-C3W
 1.33 with sigma of 0.02
 O3L-C1D
 2.4 with sigma of 0.02
 O3L-C3R
 2.4 with sigma of 0.02
 O3L-C3N
 1.45 with sigma of 0.02
 C28-C1T
 1.54 with sigma of 0.02
 C4A-C20
 1.54 with sigma of 0.02
 C20-C3W
 2.4 with sigma of 0.02
 C28-C1T
 1.54 with sigma of 0.02
 C1T-O3G
 2.4 with sigma of 0.02
 C1T-C20
 2.4 with sigma of 0.02
 C20-C4A
 1.3 with sigma of 0.02
 C3Y-C1R
 1.54 with sigma of 0.02
 C3Y-C1R
 1.54 with sigma of 0.02
 F12B-F15B
 2.35 with sigma of 0.02
 C4K-F12B
 1.35 with sigma of 0.02
 F15B-C4K
 1.35 with sigma of 0.02
 O10B-C4K
 2.6 with sigma of 0.02
 O11B-C4K
 2.6 with sigma of 0.02
 O11B-O10B
 2.4 with sigma of 0.02
 O13B-C4K
 2.6 with sigma of 0.02
 O13B-O10B
 2.4 with sigma of 0.02
 O13B-O11B
 2.4 with sigma of 0.02
 O13B-C4K
 2.6 with sigma of 0.02
 S1B-F15B
 2.6 with sigma of 0.02
 S1B-F12B
 2.6 with sigma of 0.02
 S1B-F7B
 2.6 with sigma of 0.02
 F7B-F12B
 2.35 with sigma of 0.02
 F7B-F15B
 2.35 with sigma of 0.02
 F7B-C4K
 1.35 with sigma of 0.02
 S1B-C4K
 1.9 with sigma of 0.02
 O3R-C4H
 1.45 with sigma of 0.02
 C16X-O3R
 1.45 with sigma of 0.02
 C16X-C4H
 2.4 with sigma of 0.02
 C4D-C16X
 2.4 with sigma of 0.02
 C30X-C16X
 1.54 with sigma of 0.02
 C30X-O3R
 2.4 with sigma of 0.02
 C13X-C4D
 1.54 with sigma of 0.02
 C13X-C30X
 2.4 with sigma of 0.02
 C35-C13X
 1.3 with sigma of 0.02
 C35-C4D
 2.4 with sigma of 0.02
 C21X-C35
 1.54 with sigma of 0.02
 C21X-C13X
 2.4 with sigma of 0.02
 C32X-C21X
 1.54 with sigma of 0.02
 C32X-C35
 2.4 with sigma of 0.02
 C1VV-C6VV
 1.54 with sigma of 0.02
 C6VV-O4VV
 2.4 with sigma of 0.02
 C1VV-C15V
 2.4 with sigma of 0.02
 O4VV-C15V
 1.45 with sigma of 0.02
 O4VV-C1VV
 1.45 with sigma of 0.02
 C45V-C15V
 1.54 with sigma of 0.02
 C45V-O4VV
 2.4 with sigma of 0.02
 C4D-C30
 1.54 with sigma of 0.02
 C3Q-C3R
 1.54 with sigma of 0.02
 C3Q-O3L
 1.54 with sigma of 0.02
 C3Q-C3N
 2.4 with sigma of 0.02
 C1T-C10E
 1.54 with sigma of 0.02
 C28-C10E
 2.4 with sigma of 0.02
 C20-C10E
 1.54 with sigma of 0.02
 C22-C28
 2.4 with sigma of 0.02
 C3M-C1W
 2.4 with sigma of 0.02
 C1W-C5
 1.54 with sigma of 0.02
 C3M-C3Y
 2.4 with sigma of 0.02
 C1R-C5
 2.4 with sigma of 0.02
 C3M-C3Y
 2.4 with sigma of 0.02
 C3M-C3Y
 2.4 with sigma of 0.02
 C1R-C5
 2.4 with sigma of 0.02
 C3M-C1R
 1.33 with sigma of 0.02
 C5-C3I
 2.4 with sigma of 0.02
 C5-C3M
 1.54 with sigma of 0.02
 C5-C1R
 2.4 with sigma of 0.02
 F12A-S1A
 2.6 with sigma of 0.02
 F12A-O10A
 3 with sigma of 0.02
 F12A-O11A
 3 with sigma of 0.02
 S4-O24 \\sim S4-O40 \\sim S4-O36 \\sim S2-O9 \\sim S2-O3 \\sim S2-O8
 with sigma of 0.02
 O13A-O11A \\sim O11A-O10A \\sim O10A-O13A
 with sigma of 0.02
 C3N-C1D \\sim C1A-C1 \\sim C1Z-C1E \\sim C50-C39 \\sim C1O-C1B \\sim C21-C1P
\\sim C2Z-C15
 with sigma of 0.02
 S1A-O10A \\sim S1A-O13A \\sim S1A-O11A \\sim S1B-O13B \\sim S1B-O10B \\sim
S1B-O11B
 with sigma of 0.02
 F7A-F12A \\sim F12A-F15A \\sim F15A-F7A
 with sigma of 0.02
 S1A-F7A \\sim S1A-F15A \\sim S1A-F12A
 with sigma of 0.02
 F1T-C2A \\sim F1X-C2A \\sim F28-C2A \\sim F3L-C2P \\sim F37-C2P \\sim F2-C2P
 with sigma of 0.02
 S2-C2A \\sim S4-C2P
 with sigma of 0.02
 S1A-C2S \\sim S4-C2P \\sim S2-C2A
 with sigma of 0.02
 S1A-O11A \\sim S1A-O10A \\sim S1A-O13A \\sim S4-O24 \\sim S4-O40 \\sim S4-O36
\\sim S2-O8 \\sim S2-O9 ~
 S2-O3
 with sigma of 0.02
 S1B-C4K \\sim S1A-C2S \\sim S4-C2P \\sim S2-C2A
 with sigma of 0.02
 F15A-C2S \\sim F7A-C2S \\sim F12A-C2S \\sim F37-C2P \\sim F3L-C2P \\sim F2-C2P
\\sim F1X-C2A \\sim F1T-
 C2A \\sim F28-C2A
 with sigma of 0.02
 C3A-C27 \\sim C27-C13 \\sim C2C-C13 \\sim C3A-C2Y \\sim C2Y-C2K \\sim C2K-C2C
\\sim C3D-C2C \\sim C47-C3D
 \\sim C47-C2X \\sim C2X-C2W \\sim C2W-C2K
 with sigma of 0.02
3. Restrained planarity
 C45V, C15V, O4VV, C6VV, C1VV
 with sigma of 0.1
 C1D, C3N, O3L, C3Q, C3R
 with sigma of 0.1
 C30, C31, C2V, C3C
 with sigma of 0.1
 C4D, C13X, C35, C21X
 with sigma of 0.1
 C5, C3M, C1R, C3Y
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O1D \\sim C2V \\sim C3B \\sim C3C \\sim C31 \\sim C3J \\sim C3U \\sim C4C \\sim
C30 \\sim O3Q \\sim O3R: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C28 \\sim C1T \\sim C20 \\sim C4A \\sim C3W \\sim C2T \\sim C4 \\sim C3I \\sim
C1W \\sim C5 \\sim C3M \\sim C1R \\sim C3Y \\sim C3E \\sim C1V \\sim C4C \\sim
C16X \\sim C3U \\sim C30X \\sim C30 \\sim C4D \\sim C31 \\sim C13X \\sim C35
\\sim C2V \\sim C3C \\sim C21X \\sim C32X \\sim C3B \\sim C3J: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C2S \\sim O10A \\sim S1A \\sim O11A \\sim O13A \\sim F12A \\sim F7A \\sim F15A
\\sim C4K \\sim F15B \\sim F12B \\sim F7B \\sim S1B \\sim O11B \\sim O13B \\sim
O10B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C3P \\sim C4H \\sim C4I \\sim C4B \\sim C4E \\sim C4G \\sim C4F \\sim C3L \\sim
C3T \\sim C42: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C2D \\sim C3L \\sim C2U \\sim C3T \\sim C42 \\sim C2L \\sim C4B \\sim C2J \\sim
C4E \\sim C2O \\sim C4F \\sim C2R \\sim C3X \\sim C4G \\sim C3O \\sim C3P \\sim
C4H \\sim C4I \\sim C3S: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C2Y \\sim C3A \\sim C27 \\sim C13 \\sim C2C \\sim C2K: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uiso(C45V) = Uiso(C1VV) = Uiso(O4VV) = Uiso(C6VV) = Uiso(C15V) = Uiso(C3R) =
Uiso(C1D) = Uiso(C3N) = Uiso(O3L) = Uiso(C3Q)
Uanis(O13B) = Uanis(O10B) = Uanis(O11B)
5. Rigid body (RIGU) restrains
 C1D, C3N, O3L, C3R
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 O2A, O3G, C4, C2T, C3W, C4A, C20, C1T, C28
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C29, C33, C3F, C1N, C45, C3H, C3G, C3Z, C22, C3V, O3G, C28, C1T, C20, C4A,
 C3W, C2T, C4, O2A, C2E, C40, C26, C2G, C24, C2Q, C1U, C48, C1Y, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C4K, F15B, F12B, S1B, O11B, O13B, O10B, F7B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15V, O4VV, C1VV, C6VV
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O30, C1V, O2T, C3E, C3I, C1R, C3Y, C5, C3M, C1W
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, O10A, O11A, C2S, O13A, F12A, F7A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F7A, C2S, F15A, F12A, S1A, O10A, O11A, O13A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2A, S2, O8, O9, O3, F28, F1T, F1X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C3L, C4F, C4E, C4B, C42, C3T, C4I, C4H, C3P, C4G, O3R, C16X, C30X, C4D, C13X,
 C35, C21X, C32X, C3J
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C28, C1T, C10E, C20, C4A, C2T, C3W, C4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(C1D)=Sof(H1DA)=Sof(H1DB)=Sof(H1DC)=Sof(O3L)=Sof(C3N)=Sof(H3NA)=Sof(H3NB)=
 Sof(C3R)=Sof(H3RA)=Sof(H3RB)=Sof(H3RC)=Sof(C3Q)=Sof(H3QA)=Sof(H3QB)=1-FVAR(1)
 Sof(C1VV)=Sof(H1VC)=Sof(H1VD)=Sof(O4VV)=Sof(C6VV)=Sof(H6VA)=Sof(H6VB)=
 Sof(H6VC)=Sof(C15V)=Sof(H15B)=Sof(H15C)=Sof(C45V)=Sof(H45A)=Sof(H45B)=
 Sof(H45C)=FVAR(1)
 Sof(H15A)=Sof(H3JC)=Sof(H3JD)=Sof(C42)=Sof(H42A)=Sof(C3T)=Sof(H3T)=Sof(C3L)=
 Sof(C4F)=Sof(H4F)=Sof(C4E)=Sof(C4B)=Sof(C4I)=Sof(H4I)=Sof(C4H)=Sof(C3P)=
 Sof(H3P)=Sof(C4G)=Sof(H4G)=Sof(O3R)=Sof(C16X)=Sof(H16A)=Sof(H16B)=Sof(C30X)=
 Sof(H30C)=Sof(H30D)=Sof(C4D)=Sof(H4DA)=Sof(H4DB)=Sof(C13X)=Sof(H13X)=Sof(C35)=
 Sof(H35)=Sof(C21X)=Sof(H21A)=Sof(H21B)=Sof(C32X)=Sof(H32A)=Sof(H32B)=1-FVAR(2)
 Sof(H15)=Sof(C3S)=Sof(H3S)=Sof(C2F)=Sof(C3O)=Sof(H3O)=Sof(C3X)=Sof(H3X)=
 Sof(C2O)=Sof(C2J)=Sof(C2L)=Sof(H2L)=Sof(C2U)=Sof(H2U)=Sof(C2D)=Sof(C2R)=
 Sof(H2R)=Sof(C2V)=Sof(H2V)=Sof(C3B)=Sof(H3BA)=Sof(H3BB)=Sof(C3C)=Sof(H3CA)=
 Sof(H3CB)=Sof(C31)=Sof(H31A)=Sof(H3JA)=Sof(H3JB)=Sof(O3Q)=Sof(C3U)=Sof(H3UA)=
 Sof(H3UB)=Sof(C4C)=Sof(H4CA)=Sof(H4CB)=Sof(C30)=Sof(H30A)=Sof(H30B)=FVAR(2)
 Sof(H3A)=Sof(O10)=Sof(H10C)=Sof(C3)=Sof(H3B)=Sof(H3C)=Sof(H3E)=Sof(F15B)=
 Sof(C4K)=Sof(F12B)=Sof(F7B)=Sof(S1B)=Sof(O10B)=Sof(O13B)=Sof(O11B)=1-FVAR(3)
 Sof(O10A)=Sof(S1A)=Sof(O11A)=Sof(C2S)=Sof(O13A)=Sof(F12A)=Sof(F7A)=Sof(F15A)=
 FVAR(3)
7.a :
 C3S(C2F,C3O,C3X,C2O,C2J,C2L,C2U,C2D,C2R,O2T,C2V,C2W,C2X,C2Y,C2Z,C37,C3A,C3B,
 C3C,C3D,C3E,O3G,C3I,F3L,C1,C4,C1P,C1R,C2T,C31,C3J,O3Q,C3U,C3V,C22,C3Z,C3G,C3H,
 C45,C1N,C3F,C33,C29,C3W,C3Y,C4A,C4C,C20,C2A,C1D,C5,C3M,C1W,C30,C1T,C28,O3L,C3N,
 C3R,O10A,S1A,O11A,C2S,O13A,F12A,F7A,F15A,O10,C3,C42,C3T,C3L,C4F,C4E,C4B,C4I,
 C4H,C3P,C4G,O3R,C3Q,F15B,C4K,F12B,F7B,S1B,O10B,O13B,O11B,C16X,C30X,C4D,C13X,
 C35,C21X,C32X,C1VV,O4VV,C6VV,C15V,C45V,C10E)
7.b Ternary CH refined with riding coordinates:
 C15(H15), C15(H15A), C1A(H1A), C21(H21), C1O(H1O), C39(H39), C1Z(H1Z)
7.c Secondary CH2 refined with riding coordinates:
 C1V(H1VA,H1VB), C3B(H3BA,H3BB), C3C(H3CA,H3CB), C3E(H3EA,H3EB), C3I(H3IA,
 H3IB), C4(H4A,H4B), C2T(H2TA,H2TB), C3J(H3JA,H3JB), C3J(H3JC,H3JD), C3U(H3UA,
 H3UB), C3W(H3WA,H3WB), C3Y(H3YA,H3YB), C4C(H4CA,H4CB), C5(H5A,H5B), C1W(H1WA,
 H1WB), C30(H30A,H30B), C1T(H1TA,H1TB), C28(H28A,H28B), C3N(H3NA,H3NB),
 C3Q(H3QA,H3QB), C16X(H16A,H16B), C30X(H30C,H30D), C4D(H4DA,H4DB), C21X(H21A,
 H21B), C32X(H32A,H32B), C1VV(H1VC,H1VD), C15V(H15B,H15C), C10E(H10A,H10B)
7.d Me refined with riding coordinates:
 C1B(H1BA,H1BB,H1BC), C1E(H1EA,H1EB,H1EC), C50(H50A,H50B,H50C), C2Z(H2ZA,H2ZB,
 H2ZC), C1(H1B,H1D,H1E), C1P(H1PA,H1PB,H1PC), C1D(H1DA,H1DB,H1DC), C3R(H3RA,
 H3RB,H3RC), C6VV(H6VA,H6VB,H6VC), C45V(H45A,H45B,H45C)
7.e Aromatic/amide H refined with riding coordinates:
 C19(H19), N22(H22), N31(H31), C38(H38), C41(H41), N42(H42), C43(H43),
 C46(H46), N1(H1), N5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C13(H13), C17(H17), C1C(H1C), C1F(H1F), C1G(H1G), C1H(H1H), C26(H26), N1P(H1P),
  C1S(H1S), C40(H40), C1U(H1U), C47(H47), C48(H48), C49(H49), C2H(H2H),
 C2I(H2I), C2M(H2M), C2Q(H2Q), C3S(H3S), C3O(H3O), C3X(H3X), C2L(H2L), C2U(H2U),
  C2R(H2R), C2V(H2V), C2W(H2W), C2Y(H2Y), C37(H37), C3A(H3A), C3D(H3D),
 C1R(H1R), C31(H31A), C3V(H3V), C3Z(H3Z), C3G(H3G), C1N(H1N), C3F(H3F),
 C29(H29), C4A(H4AA), C20(H20), C3M(H3M), C42(H42A), C3T(H3T), C4F(H4F),
 C4I(H4I), C3P(H3P), C4G(H4G), C13X(H13X), C35(H35)
7.f Idealised Me refined as rotating group:
 C3(H3B,H3C,H3E)
7.g Idealised tetrahedral OH refined as rotating group:
 O10(H10C)
;
_shelx_res_checksum              31793
_shelx_hkl_checksum              56862
_olex2_submission_special_instructions 'No special instructions were received'