Statistical optimization of guest uptake in crystalline sponges: grading structural outcomes.
Carroll, Robert C.; Coles, Simon J.; IUCrJ 11 (2024) –; doi:10.1107/S2052252524004871

data_1571878
_publ_section_title
;
 Statistical optimization of guest uptake in crystalline sponges: grading
 structural outcomes.
;
_journal_coeditor_code           LT5068
_journal_issue                   4
_journal_name_full               IUCrJ
_journal_paper_doi               10.1107/S2052252524004871
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety
'C72 H48 I12 N24 Zn6, 1.09(C15 H16 O3), 1.217(C6 H12)'
_chemical_formula_sum            'C95.66 H80.05 I12.01 N24 O3.27 Zn6.01'
_chemical_formula_weight         3534.43
_chemical_name_systematic
; (2',6'-dimethoxy-[1,1'-biphenyl]-2-yl)methanol
 (absorbed in crystalline sponge)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-26
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2024.01.24 svn.r2f8d729c for OlexSys, GUI svn.r6923)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.192(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6222(19)
_cell_length_b                   14.9929(6)
_cell_length_c                   34.405(2)
_cell_measurement_reflns_used    15706
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.0660
_cell_measurement_theta_min      2.6290
_cell_volume                     15943.8(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'hybrid pixel array detector'
_diffrn_detector_area_resol_mean 10
_diffrn_detector_dtime           0.000
_diffrn_detector_type            'Rigaku, HyPix 6000HE'
_diffrn_measured_fraction_theta_full 0.991
_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   -116.00 -91.00   0.50    4.00    -- -103.00 -27.00 174.00   50
  2  \w    -65.00 -34.00   0.50    4.00    -- -103.00  61.00-150.00   62
  3  \w    -55.00 -30.00   0.50    4.00    -- -103.00  77.00  90.00   50
  4  \w   -103.00 -62.00   0.50    4.00    -- -103.00  77.00  90.00   82
  5  \w    -65.00 -38.00   0.50    4.00    -- -103.00  61.00 -60.00   54
  6  \w    -67.00 -32.00   0.50    4.00    -- -103.00  61.00 -90.00   70
  7  \w    -55.00 -30.00   0.50    4.00    -- -103.00  61.00-120.00   50
  8  \w    -55.00 -30.00   0.50    4.00    -- -103.00  61.00 120.00   50
  9  \w    -58.00 -33.00   0.50    4.00    -- -103.00  61.00 -30.00   50
 10  \w    -66.00 -33.00   0.50    4.00    -- -103.00  61.00-180.00   66
 11  \w    -58.00 -33.00   0.50    4.00    -- -103.00  61.00  90.00   50
 12  \w    -55.00 -30.00   0.50    4.00    -- -103.00  61.00 150.00   50
 13  \w     91.00 174.00   0.50    4.00    --  101.75  27.00 -23.00  166
 14  \w     40.00  68.00   0.50    4.00    --  101.75 -61.00-150.00   56
 15  \w     35.00  62.00   0.50    4.00    --  101.75 -94.00   0.00   54
 16  \w     29.00  73.00   0.50    4.00    --  101.75 -61.00 -90.00   88
 17  \w     34.00  73.00   0.50    4.00    --  101.75 -61.00 120.00   78
 18  \w     36.00  71.00   0.50    4.00    --  101.75 -61.00   0.00   70
 19  \w     38.00  72.00   0.50    4.00    --  101.75 -61.00-180.00   68
 20  \w     32.00  70.00   0.50    4.00    --  101.75 -61.00-120.00   76
 21  \w     32.00  67.00   0.50    4.00    --  101.75 -61.00  90.00   70
 22  \w     74.00 100.00   0.50    4.00    --  101.75 -94.00   0.00   52
 23  \w     38.00  73.00   0.50    4.00    --  101.75 -61.00  30.00   70
 24  \w    -30.00  16.00   0.50    0.50    --  -46.26  27.00 -23.00   92
 25  \w   -120.00 -41.00   0.50    0.50    --  -46.26 -27.00 174.00  158
 26  \w     34.00 121.00   0.50    0.50    --   46.26  27.00 -23.00  174
 27  \w      2.00  28.00   0.50    0.50    --   46.26 -27.00 174.00   52
 28  \w    -12.00  13.00   0.50    0.50    --  -46.26  19.00-120.00   50
 29  \w    -40.00  20.00   0.50    0.50    --  -46.26  37.00 120.00  120
 30  \w    -27.00  17.00   0.50    0.50    --   46.26 -19.00  30.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_details
'Rigaku Oxford Difffraction, UG2 \k goniometer'
_diffrn_measurement_device_type
; Rigaku 007HF equipped with Varimax confocal mirrors and a UG2 goniometer
 and HyPix 6000HE detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen loops'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0385409000
_diffrn_orient_matrix_UB_12      0.0087287000
_diffrn_orient_matrix_UB_13      -0.0355384000
_diffrn_orient_matrix_UB_21      -0.0285395000
_diffrn_orient_matrix_UB_22      0.0348423000
_diffrn_orient_matrix_UB_23      0.0280847000
_diffrn_orient_matrix_UB_31      0.0137596000
_diffrn_orient_matrix_UB_32      0.0961433000
_diffrn_orient_matrix_UB_33      -0.0067936000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  'Varimax focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            100270
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.136
_diffrn_source                   'Rotating anode'
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_target            Cu
_diffrn_source_type              'Rigaku 007 HF'
_diffrn_source_voltage           40.0
_exptl_absorpt_coefficient_mu    19.580
_exptl_absorpt_correction_T_max  0.232
_exptl_absorpt_correction_T_min  0.070
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.72a (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       block
_exptl_crystal_F_000             6659
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.415
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1609
_refine_ls_number_reflns         28894
_refine_ls_number_restraints     823
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.1687
_refine_ls_R_factor_gt           0.1477
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0905P)^2^+673.4932P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3505
_refine_ls_wR_factor_ref         0.3623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21921
_reflns_number_total             28894
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_10_96c
_cod_original_cell_volume        15943.7(16)
_cod_database_code               1571878
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     9300-04
_shelx_estimated_absorpt_t_max   0.202
_shelx_estimated_absorpt_t_min   0.077
_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, All O(H) groups
2. Restrained distances
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 C4B-C7B = C5B-C13B
 1.51 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C4A-C7A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O2A-C14A = O3A-C15A = O1A-C13A
 1.43 with sigma of 0.02
 C12A-O3A = C8A-O2A
 1.37 with sigma of 0.02
 C809-C808 = C809-C810 = C808-C807 = C807-C812 = C812-C811 = C811-C810
 1.54 with sigma of 0.02
 C806-C805 = C806-C801 = C805-C804 = C804-C803 = C803-C802 = C802-C801
 1.54 with sigma of 0.02
 C816-C815 = C816-C817 = C815-C814 = C814-C813 = C813-C818 = C818-C817
 1.54 with sigma of 0.02
 O1B-C5B
 2.4 with sigma of 0.04
 C7B-O2B
 2.35 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.02
 C12A-C15A
 2.4 with sigma of 0.02
 C8A-C14A
 2.4 with sigma of 0.04
 C809-C807 = C809-C811 = C808-C812 = C807-C811 = C812-C810
 2.54 with sigma of 0.04
 C806-C804 = C806-C802 = C805-C803 = C804-C802 = C803-C801
 2.54 with sigma of 0.04
 C816-C814 = C816-C818 = C815-C813 = C814-C818 = C813-C817
 2.54 with sigma of 0.04
 C2A-C1A \\sim C3A-C2A \\sim C4A-C3A \\sim C5A-C4A \\sim C6A-C5A \\sim C6A-C1A
 with sigma of 0.02
 C8A-C7A \\sim C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim
C7A-C12A
 with sigma of 0.02
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C3B-C7B \\sim C7B-C5B
 with sigma of 0.04
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C1A \\sim C6A-C2A
 with sigma of 0.02
 C8A-C10A \\sim C9A-C11A \\sim C10A-C12A
 with sigma of 0.02
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 Zn35-N318 \\sim Zn45-N318
 with sigma of 0.02
 Zn35-N319 \\sim Zn45-N319
 with sigma of 0.02
 I309-I310 \\sim I409-I410
 with sigma of 0.04
 I309-N318 \\sim I409-N318
 with sigma of 0.04
 I309-N319 \\sim I409-N319
 with sigma of 0.04
 I310-N318 \\sim I410-N318
 with sigma of 0.04
 I310-N319 \\sim I410-N319
 with sigma of 0.04
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 Zn33-N307 \\sim Zn43-N307
 with sigma of 0.02
 I305-I306 \\sim I405-I406
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I401-Zn41 \\sim I301-Zn31
 with sigma of 0.02
 I402-Zn41 \\sim I302-Zn31
 with sigma of 0.02
 Zn41-N301 \\sim Zn31-N301
 with sigma of 0.02
 I401-I402 \\sim I301-I302
 with sigma of 0.04
 I401-N301 \\sim I301-N301
 with sigma of 0.04
 I402-N301 \\sim I302-N301
 with sigma of 0.04
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 Zn36-N324 \\sim Zn46-N324
 with sigma of 0.02
 I312-I311 \\sim I412-I411
 with sigma of 0.04
 I312-N324 \\sim I412-N324
 with sigma of 0.04
 I311-N324 \\sim I411-N324
 with sigma of 0.04
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 Zn32-N305 \\sim Zn42-N305
 with sigma of 0.02
 I304-I303 \\sim I404-I403
 with sigma of 0.04
 I304-N305 \\sim I404-N305
 with sigma of 0.04
 I303-N305 \\sim I403-N305
 with sigma of 0.04
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 Zn34-N313 \\sim Zn44-N313
 with sigma of 0.02
 Zn34-N312 \\sim Zn44-N312
 with sigma of 0.02
 I307-I308 \\sim I407-I408
 with sigma of 0.04
 I307-N313 \\sim I407-N313
 with sigma of 0.04
 I307-N312 \\sim I407-N312
 with sigma of 0.04
 I308-N313 \\sim I408-N313
 with sigma of 0.04
 I308-N312 \\sim I408-N312
 with sigma of 0.04
 Zn53-N307 \\sim Zn53-N306
 with sigma of 0.02
 C809-C808 \\sim C808-C807 \\sim C807-C812 \\sim C812-C811 \\sim C811-C810
\\sim C810-C809
 with sigma of 0.02
 C809-C811 \\sim C807-C811 \\sim C808-C810 \\sim C808-C812 \\sim C812-C810
\\sim C809-C807
 with sigma of 0.04
 C806-C805 \\sim C805-C804 \\sim C804-C803 \\sim C803-C802 \\sim C802-C801
\\sim C801-C806
 with sigma of 0.02
 C806-C802 \\sim C804-C802 \\sim C805-C801 \\sim C805-C803 \\sim C803-C801
\\sim C806-C804
 with sigma of 0.04
 C816-C815 \\sim C815-C814 \\sim C814-C813 \\sim C813-C818 \\sim C818-C817
\\sim C817-C816
 with sigma of 0.02
 C816-C818 \\sim C814-C818 \\sim C815-C817 \\sim C815-C813 \\sim C813-C817
\\sim C816-C814
 with sigma of 0.04
3. Restrained planarity
 C6B, C5B, C4B, C13B
 with sigma of 0.1
 C4A, C5A, C6A, C13A
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7B \\sim C4B \\sim C3B \\sim C5B \\sim C2B \\sim C6B \\sim C13B \\sim C12B
\\sim C8B \\sim C1B \\sim O1B \\sim O3B \\sim C11B \\sim O2B \\sim C9B \\sim
C15B \\sim C10B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim O1A
\\sim O2A \\sim O3A: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08 within 2A
C370 \\sim C369 \\sim C368 \\sim N324 \\sim C372 \\sim C371: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C303 \\sim C302 \\sim C301 \\sim C305 \\sim C304: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C809 \\sim C808 \\sim C807 \\sim C812 \\sim C811 \\sim C810: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C806 \\sim C805 \\sim C804 \\sim C803 \\sim C802 \\sim C801: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C816 \\sim C815 \\sim C814 \\sim C813 \\sim C818 \\sim C817: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
N301 \\sim C303 \\sim C305 \\sim C304 \\sim C302 \\sim C301: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn45) = Uanis(Zn35)
Uanis(I409) = Uanis(I309)
Uanis(Zn44) = Uanis(Zn34)
5. Rigid body (RIGU) restrains
 C7B, C4B, C3B, C5B, C2B, C6B, C13B, C12B, C8B, C1B, O1B, O3B, C11B, O2B, C9B,
 C15B, C10B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C809, C808, C807, C812, C811, C810
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C806, C805, C804, C803, C802, C801
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C816, C815, C814, C813, C818, C817
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I404)=Sof(Zn42)=Sof(I403)=1-FVAR(1)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(1)
 Sof(I301)=Sof(Zn31)=Sof(I302)=1-FVAR(2)
 Sof(I401)=Sof(I402)=Sof(Zn41)=FVAR(2)
 Sof(I409)=Sof(Zn45)=Sof(I410)=1-FVAR(3)
 Sof(I309)=Sof(I310)=Sof(Zn35)=FVAR(3)
 Fixed Sof: I305(0.48092) I306(0.48092) I307(0.56431) I308(0.56431)
 I312(0.61352) I311(0.61352) Zn33(0.48092) Zn34(0.56431) Zn36(0.61352)
 O2A(0.84241) O3A(0.84241) C3A(0.84241) H3A(0.84241) O1A(0.84241) H1AA(0.84241)
 C4A(0.84241) C2A(0.84241) H2A(0.84241) C7A(0.84241) C1A(0.84241) H1A(0.84241)
 C12A(0.84241) C8A(0.84241) C5A(0.84241) C10A(0.84241) H10A(0.84241)
 C9A(0.84241) H9A(0.84241) C15A(0.84241) H15A(0.84241) H15B(0.84241)
 H15C(0.84241) C13A(0.84241) H13A(0.84241) H13B(0.84241) C6A(0.84241)
 H6A(0.84241) C11A(0.84241) H11A(0.84241) C14A(0.84241) H14A(0.84241)
 H14B(0.84241) H14C(0.84241) I406(0.45329) Zn43(0.45329) I405(0.45329)
 I411(0.38647) Zn46(0.38647) I412(0.38647) I506(0.06579) I505(0.06579)
 Zn53(0.06579) Zn44(0.43569) I407(0.43569) I408(0.43569) C809(0.48053)
 H80A(0.48053) H80B(0.48053) C808(0.48053) H80C(0.48053) H80D(0.48053)
 C807(0.48053) H80E(0.48053) H80F(0.48053) C812(0.48053) H81A(0.48053)
 H81B(0.48053) C811(0.48053) H81C(0.48053) H81D(0.48053) C810(0.48053)
 H81E(0.48053) H81F(0.48053) C806(0.42028) H80G(0.42028) H80H(0.42028)
 C805(0.42028) H80I(0.42028) H80J(0.42028) C804(0.42028) H80K(0.42028)
 H80L(0.42028) C803(0.42028) H80M(0.42028) H80N(0.42028) C802(0.42028)
 H80O(0.42028) H80P(0.42028) C801(0.42028) H80Q(0.42028) H80R(0.42028)
 C816(0.3159) H81G(0.3159) H81H(0.3159) C815(0.3159) H81I(0.3159) H81J(0.3159)
 C814(0.3159) H81K(0.3159) H81L(0.3159) C813(0.3159) H81M(0.3159) H81N(0.3159)
 C818(0.3159) H81O(0.3159) H81P(0.3159) C817(0.3159) H81Q(0.3159) H81R(0.3159)
 C4B(0.24801) C3B(0.24801) H3B(0.24801) C2B(0.24801) H2B(0.24801) C1B(0.24801)
 H1B(0.24801) C6B(0.24801) H6B(0.24801) C5B(0.24801) O2B(0.24801) O3B(0.24801)
 C7B(0.24801) C12B(0.24801) C11B(0.24801) H11B(0.24801) C10B(0.24801)
 H10B(0.24801) C9B(0.24801) H9B(0.24801) C8B(0.24801) C13B(0.24801)
 H13C(0.24801) H13D(0.24801) O1B(0.24801) H1BA(0.24801) C15B(0.24801)
 H15D(0.24801) H15E(0.24801) H15F(0.24801) C14B(0.24801) H14D(0.24801)
 H14E(0.24801) H14F(0.24801)
 Fixed Uiso: I506(0.08) I505(0.08) Zn53(0.08) C809(0.08) C808(0.08) C807(0.08)
 C812(0.08) C811(0.08) C810(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C809(H80A,H80B), C808(H80C,H80D), C807(H80E,H80F), C812(H81A,
 H81B), C811(H81C,H81D), C810(H81E,H81F), C806(H80G,H80H), C805(H80I,H80J),
 C804(H80K,H80L), C803(H80M,H80N), C802(H80O,H80P), C801(H80Q,H80R), C816(H81G,
 H81H), C815(H81I,H81J), C814(H81K,H81L), C813(H81M,H81N), C818(H81O,H81P),
 C817(H81Q,H81R), C13B(H13C,H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C315(H315), C332(H332), C351(H351), C320(H320), C329(H329), C319(H319),
 C340(H340), C314(H314), C331(H331), C322(H322), C336(H336), C333(H333),
 C330(H330), C317(H317), C372(H372), C353(H353), C354(H354), C348(H348),
 C371(H371), C369(H369), C349(H349), C358(H358), C368(H368), C323(H323),
 C364(H364), C3A(H3A), C365(H365), C350(H350), C337(H337), C367(H367),
 C328(H328), C312(H312), C305(H305), C356(H356), C304(H304), C366(H366),
 C355(H355), C347(H347), C359(H359), C2A(H2A), C313(H313), C1A(H1A), C338(H338),
  C341(H341), C318(H318), C10A(H10A), C311(H311), C335(H335), C310(H310),
 C9A(H9A), C302(H302), C6A(H6A), C11A(H11A), C346(H346), C301(H301), C3B(H3B),
 C2B(H2B), C1B(H1B), C6B(H6B), C11B(H11B), C10B(H10B), C9B(H9B)
7.c Fitted hexagon refined as free rotating group:
 C4B(C3B,C2B,C1B,C6B,C5B), C7B(C12B,C11B,C10B,C9B,C8B)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1AA), O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C15A(H15A,H15B,H15C), C14A(H14A,H14B,H14C), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F)
;
_shelx_res_checksum              87362
_shelx_hkl_checksum              74059
_olex2_date_sample_data_collection 2023-02-27
_olex2_date_sample_submission    2022-02-27
_olex2_submission_original_sample_id 50_10_96c
_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
- Detector area scaling
- B-factor correction
;
_oxdiff_exptl_absorpt_empirical_full_max 3.937
_oxdiff_exptl_absorpt_empirical_full_min 0.382