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_1571874
_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, 0.896(C15 H16 O3), 0.789(C6 H12)'
_chemical_formula_sum            'C90.17 H71.8 I12 N24 O2.69 Zn6'
_chemical_formula_weight         3449.54
_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             2024-01-22
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.955(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.5685(8)
_cell_length_b                   15.0410(3)
_cell_length_c                   34.3133(9)
_cell_measurement_reflns_used    16519
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.5620
_cell_measurement_theta_min      2.8340
_cell_volume                     15939.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_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 0.990
_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   -147.00 -90.00   0.38    3.50    -- -103.00 -14.00 162.00  150
  2  \w   -132.00-104.64   0.38    3.50    -- -103.00 -15.00-120.00   72
  3  \w    -68.00 -38.74   0.38    3.50    -- -103.00  61.00   0.00   77
  4  \w   -171.00-135.28   0.38    3.50    -- -103.00 -15.00-120.00   94
  5  \w    -69.00 -34.80   0.38    3.50    -- -103.00  61.00-180.00   90
  6  \w   -159.00 -99.72   0.38    3.50    -- -103.00 -30.00  90.00  156
  7  \w    -68.00 -34.94   0.38    3.50    -- -103.00  61.00 -30.00   87
  8  \w    -62.00 -30.08   0.38    3.50    -- -103.00  61.00  30.00   84
  9  \w   -157.00 -95.06   0.38    3.50    -- -103.00 -45.00  60.00  163
 10  \w    -57.00 -32.30   0.38    3.50    -- -103.00  61.00 -90.00   65
 11  \w    -61.00 -33.64   0.38    3.50    -- -103.00  61.00  60.00   72
 12  \w     89.00 158.16   0.38    3.50    --  101.75  14.00 -26.00  182
 13  \w     58.00 104.36   0.38    3.50    --  101.75-125.00  90.00  122
 14  \w     35.00  96.94   0.38    3.50    --  101.75 -94.00 120.00  163
 15  \w     33.00  58.46   0.38    3.50    --  101.75-125.00  60.00   67
 16  \w     43.00  68.08   0.38    3.50    --  101.75 -61.00   0.00   66
 17  \w     40.00 103.08   0.38    3.50    --  101.75 -94.00 -90.00  166
 18  \w    -22.00  19.04   0.38    0.40    --  -46.11  14.00 -26.00  108
 19  \w   -119.00 -40.72   0.38    0.40    --  -46.11 -14.00 162.00  206
 20  \w    -26.00  -0.92   0.38    0.40    --   46.11 -14.00 162.00   66
 21  \w     33.00 113.18   0.38    0.40    --   46.11  14.00 -26.00  211
 22  \w    -24.00  12.10   0.38    0.40    --  -46.11  19.00 120.00   95
 23  \w     36.00  90.72   0.38    0.40    --   46.11-125.00   0.00  144
;
_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      0.0497535000
_diffrn_orient_matrix_UB_12      -0.0072441000
_diffrn_orient_matrix_UB_13      0.0102662000
_diffrn_orient_matrix_UB_21      -0.0015171000
_diffrn_orient_matrix_UB_22      -0.0176209000
_diffrn_orient_matrix_UB_23      0.0439335000
_diffrn_orient_matrix_UB_31      -0.0033184000
_diffrn_orient_matrix_UB_32      -0.1005962000
_diffrn_orient_matrix_UB_33      -0.0084100000
_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  0.0498
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            96418
_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         68.249
_diffrn_reflns_theta_min         2.135
_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    19.556
_exptl_absorpt_correction_T_max  0.359
_exptl_absorpt_correction_T_min  0.104
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.122a (Rigaku Oxford Diffraction, 2021)
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    1.437
_exptl_crystal_description       block
_exptl_crystal_F_000             6473
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.420
_refine_diff_density_min         -1.243
_refine_diff_density_rms         0.222
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1713
_refine_ls_number_reflns         28902
_refine_ls_number_restraints     903
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.1219
_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^)+(0.1298P)^2^+275.2107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3322
_refine_ls_wR_factor_ref         0.3445
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22231
_reflns_number_total             28902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_10_48b
_cod_original_formula_sum        'C90.17 H71.80 I12 N24 O2.69 Zn6'
_cod_database_code               1571874
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)2'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.341
_shelx_estimated_absorpt_t_min   0.094
_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
 C13B-O1B = C15B-O3B = C14B-O2B
 1.43 with sigma of 0.02
 O3A-C12A
 1.37 with sigma of 0.02
 C13B-C5B
 1.51 with sigma of 0.02
 C7B-C4B
 1.5 with sigma of 0.02
 O1A-C13A = O2A-C14A = O3A-C15A
 1.43 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 C801-C806 = C801-C802 = C806-C805 = C805-C804 = C804-C803 = C803-C802
 1.54 with sigma of 0.02
 C811-C810 = C811-C812 = C810-C809 = C809-C808 = C808-C807 = C807-C812
 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
 C15B-C12B
 2.4 with sigma of 0.04
 C5A-O1A
 2.4 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.04
 C5B-O1B
 2.4 with sigma of 0.04
 C801-C805 = C801-C803 = C806-C804 = C805-C803 = C804-C802
 2.54 with sigma of 0.04
 C811-C809 = C811-C807 = C810-C808 = C809-C807 = C808-C812
 2.54 with sigma of 0.04
 C816-C814 = C816-C818 = C815-C813 = C814-C818 = C813-C817
 2.54 with sigma of 0.04
 C6A-C5A \\sim C5A-C4A \\sim C4A-C3A \\sim C3A-C2A \\sim C2A-C1A \\sim C6A-C1A
 with sigma of 0.02
 C7B-C8B \\sim C12B-C7B \\sim C12B-C11B \\sim C10B-C11B \\sim C10B-C9B \\sim
C9B-C8B
 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
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C1A \\sim C6A-C2A
 with sigma of 0.04
 C12B-C4B \\sim C4B-C8B
 with sigma of 0.04
 C7A-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7A \\sim
C12A-C8A
 with sigma of 0.04
 C5B-C7B \\sim C7B-C3B
 with sigma of 0.04
 C1A-C4A \\sim C2A-C5A \\sim C3A-C6A
 with sigma of 0.04
 C11A-O3A \\sim O3A-C7A
 with sigma of 0.02
 C9B-O2B \\sim O2B-C7B
 with sigma of 0.04
 C6B-C13B \\sim C13B-C4B
 with sigma of 0.04
 I303-Zn32 \\sim I403-Zn42
 with sigma of 0.02
 I304-Zn32 \\sim I404-Zn42
 with sigma of 0.02
 Zn32-N311 \\sim Zn42-N311
 with sigma of 0.02
 I303-I304 \\sim I403-I404
 with sigma of 0.04
 I303-N311 \\sim I403-N311
 with sigma of 0.04
 I304-N311 \\sim I404-N311
 with sigma of 0.04
 I409-Zn45 \\sim I309-Zn35
 with sigma of 0.02
 I410-Zn45 \\sim I310-Zn35
 with sigma of 0.02
 Zn45-N319 \\sim Zn35-N319
 with sigma of 0.02
 Zn45-N318 \\sim Zn35-N318
 with sigma of 0.02
 I409-I410 \\sim I309-I310
 with sigma of 0.04
 I409-N319 \\sim I309-N319
 with sigma of 0.04
 I409-N318 \\sim I309-N318
 with sigma of 0.04
 I410-N319 \\sim I310-N319
 with sigma of 0.04
 I410-N318 \\sim I310-N318
 with sigma of 0.04
 I306-Zn33 \\sim I406-Zn43
 with sigma of 0.02
 I305-Zn33 \\sim I405-Zn43
 with sigma of 0.02
 Zn33-N312 \\sim Zn43-N312
 with sigma of 0.02
 Zn33-N313 \\sim Zn43-N313
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N312 \\sim I406-N312
 with sigma of 0.04
 I306-N313 \\sim I406-N313
 with sigma of 0.04
 I305-N312 \\sim I405-N312
 with sigma of 0.04
 I305-N313 \\sim I405-N313
 with sigma of 0.04
 I308-Zn34 \\sim I408-Zn44
 with sigma of 0.02
 I307-Zn34 \\sim I407-Zn44
 with sigma of 0.02
 Zn34-N317 \\sim Zn44-N317
 with sigma of 0.02
 I308-I307 \\sim I408-I407
 with sigma of 0.04
 I308-N317 \\sim I408-N317
 with sigma of 0.04
 I307-N317 \\sim I407-N317
 with sigma of 0.04
 I302-Zn31 \\sim I402-Zn41
 with sigma of 0.02
 I301-Zn31 \\sim I401-Zn41
 with sigma of 0.02
 Zn31-N306 \\sim Zn41-N306
 with sigma of 0.02
 Zn31-N307 \\sim Zn41-N307
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N306 \\sim I402-N306
 with sigma of 0.04
 I302-N307 \\sim I402-N307
 with sigma of 0.04
 I301-N306 \\sim I401-N306
 with sigma of 0.04
 I301-N307 \\sim I401-N307
 with sigma of 0.04
 I411-Zn46 \\sim I311-Zn36
 with sigma of 0.02
 I412-Zn46 \\sim I312-Zn36
 with sigma of 0.02
 Zn46-N324 \\sim Zn36-N324
 with sigma of 0.02
 I411-I412 \\sim I311-I312
 with sigma of 0.04
 I411-N324 \\sim I311-N324
 with sigma of 0.04
 I412-N324 \\sim I312-N324
 with sigma of 0.04
 I504-Zn52 \\sim I404-Zn42
 with sigma of 0.02
 I503-Zn52 \\sim I403-Zn42
 with sigma of 0.02
 N318-C450 \\sim N318-C350
 with sigma of 0.02
 C352-C451 \\sim C352-C351
 with sigma of 0.02
 C450-C451 \\sim C350-C351
 with sigma of 0.02
 N318-C451 \\sim N318-C351
 with sigma of 0.04
 C352-C450 \\sim C352-C350
 with sigma of 0.04
 Zn53-N313 \\sim Zn43-N313
 with sigma of 0.02
 I302-Zn31 \\sim I502-Zn51
 with sigma of 0.02
 I501-Zn51 \\sim I301-Zn31
 with sigma of 0.02
 Zn51-N306 \\sim Zn31-N306
 with sigma of 0.02
 Zn51-N307 \\sim Zn31-N307
 with sigma of 0.02
 C801-C806 \\sim C806-C805 \\sim C805-C804 \\sim C804-C803 \\sim C803-C802
\\sim C802-C801
 with sigma of 0.02
 C801-C803 \\sim C805-C803 \\sim C806-C802 \\sim C806-C804 \\sim C804-C802
\\sim C801-C805
 with sigma of 0.04
 C811-C810 \\sim C810-C809 \\sim C809-C808 \\sim C808-C807 \\sim C807-C812
\\sim C812-C811
 with sigma of 0.02
 C811-C807 \\sim C809-C807 \\sim C810-C812 \\sim C810-C808 \\sim C808-C812
\\sim C811-C809
 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
 C3B, C4B, C5B, C13B
 with sigma of 0.1
 O2B, C8B, C12B, O3B, C7B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O2A \\sim C8A \\sim C14A \\sim C9A \\sim C10A \\sim C4A \\sim C12A
\\sim C11A \\sim C3A \\sim C5A \\sim O3A \\sim C2A \\sim C6A \\sim C13A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C4B \\sim C3B \\sim C5B \\sim C7B \\sim C2B \\sim C6B \\sim C13B \\sim C12B
\\sim C8B \\sim C1B \\sim O1B \\sim C11B \\sim O3B \\sim C9B \\sim O2B \\sim
C10B \\sim C15B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C801 \\sim C806 \\sim C805 \\sim C804 \\sim C803 \\sim C802: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C811 \\sim C810 \\sim C809 \\sim C808 \\sim C807 \\sim C812: 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
C330 \\sim N311 \\sim C329 \\sim C328 \\sim C327 \\sim C331: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn46) = Uanis(Zn36)
Uanis(C351) = Uanis(C451) = Uanis(C450) = Uanis(C350)
5. Rigid body (RIGU) restrains
 C7B, C4B, C3B, C5B, C2B, C6B, C13B, C12B, C8B, C1B, O1B, C11B, O3B, C9B, O2B,
 C10B, C15B, C14B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C801, C806, C805, C804, C803, C802
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C811, C810, C809, C808, C807, C812
 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
 1*[Sof(I306)+Sof(I305)+Sof(Zn33)]+1*[Sof(I406)+Sof(Zn43)+Sof(I405)]+1*
 [Sof(I506)+Sof(I505)+Sof(Zn53)]=1 with esd of 0.00001
 Sof(I312)=Sof(Zn36)=Sof(I311)=1-FVAR(1)
 Sof(I411)=Sof(I412)=Sof(Zn46)=FVAR(1)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(2)
 Sof(I406)=Sof(Zn43)=Sof(I405)=FVAR(3)
 Sof(I506)=Sof(I505)=Sof(Zn53)=FVAR(4)
 Sof(C350)=Sof(H350)=Sof(C351)=Sof(H351)=1-FVAR(5)
 Sof(C450)=Sof(H450)=Sof(C451)=Sof(H451)=FVAR(5)
 Fixed Sof: I308(0.47908) I303(0.48393) I307(0.47908) I409(0.39202)
 I410(0.39202) I302(0.47328) I304(0.48393) I301(0.47328) Zn34(0.47908)
 Zn45(0.39202) Zn32(0.48393) Zn31(0.47328) O2A(0.70328) O3A(0.70328)
 O1A(0.70328) H1A(0.70328) C7A(0.70328) C4A(0.70328) C8A(0.70328) C3A(0.70328)
 H3A(0.70328) C5A(0.70328) C1A(0.70328) H1AA(0.70328) C12A(0.70328)
 C11A(0.70328) H11A(0.70328) C10A(0.70328) H10A(0.70328) C2A(0.70328)
 H2A(0.70328) C6A(0.70328) H6A(0.70328) C9A(0.70328) H9A(0.70328) C14A(0.70328)
 H14A(0.70328) H14B(0.70328) H14C(0.70328) C13A(0.70328) H13A(0.70328)
 H13B(0.70328) C15A(0.70328) H15A(0.70328) H15B(0.70328) H15C(0.70328)
 I403(0.46688) Zn42(0.46688) I404(0.46688) I309(0.43675) Zn35(0.43675)
 I310(0.43675) I408(0.47381) Zn44(0.47381) I407(0.47381) I401(0.49347)
 Zn41(0.49347) I402(0.49347) I509(0.17123) Zn55(0.17123) I510(0.17123)
 I507(0.04711) I508(0.04711) Zn54(0.04711) I503(0.04919) Zn52(0.04919)
 I504(0.04919) I501(0.03324) I502(0.03324) Zn51(0.03324) C801(0.34338)
 H80A(0.34338) H80B(0.34338) C806(0.34338) H80C(0.34338) H80D(0.34338)
 C805(0.34338) H80E(0.34338) H80F(0.34338) C804(0.34338) H80G(0.34338)
 H80H(0.34338) C803(0.34338) H80I(0.34338) H80J(0.34338) C802(0.34338)
 H80K(0.34338) H80L(0.34338) C811(0.18785) H81A(0.18785) H81B(0.18785)
 C810(0.18785) H81C(0.18785) H81D(0.18785) C809(0.18785) H80M(0.18785)
 H80N(0.18785) C808(0.18785) H80O(0.18785) H80P(0.18785) C807(0.18785)
 H80Q(0.18785) H80R(0.18785) C812(0.18785) H81E(0.18785) H81F(0.18785)
 C4B(0.19248) C3B(0.19248) H3B(0.19248) C2B(0.19248) H2B(0.19248) C1B(0.19248)
 H1B(0.19248) C6B(0.19248) H6B(0.19248) C5B(0.19248) C7B(0.19248) C12B(0.19248)
 C11B(0.19248) H11B(0.19248) C10B(0.19248) H10B(0.19248) C9B(0.19248)
 H9B(0.19248) C8B(0.19248) O3B(0.19248) O2B(0.19248) C816(0.25749)
 H81G(0.25749) H81H(0.25749) C815(0.25749) H81I(0.25749) H81J(0.25749)
 C814(0.25749) H81K(0.25749) H81L(0.25749) C813(0.25749) H81M(0.25749)
 H81N(0.25749) C818(0.25749) H81O(0.25749) H81P(0.25749) C817(0.25749)
 H81Q(0.25749) H81R(0.25749) C14B(0.19248) H14D(0.19248) H14E(0.19248)
 H14F(0.19248) C15B(0.19248) H15D(0.19248) H15E(0.19248) H15F(0.19248)
 C13B(0.19248) H13C(0.19248) H13D(0.19248) O1B(0.19248) H1BA(0.19248)
 Fixed Uiso: I506(0.08) I505(0.08) Zn53(0.08) I507(0.08) I508(0.08) Zn54(0.08)
 I503(0.08) Zn52(0.08) I504(0.08) I501(0.08) I502(0.08) Zn51(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C801(H80A,H80B), C806(H80C,H80D), C805(H80E,H80F), C804(H80G,
 H80H), C803(H80I,H80J), C802(H80K,H80L), C811(H81A,H81B), C810(H81C,H81D),
 C809(H80M,H80N), C808(H80O,H80P), C807(H80Q,H80R), C812(H81E,H81F), 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:
 C301(H301), C372(H372), C302(H302), C355(H355), C348(H348), C367(H367),
 C358(H358), C371(H371), C349(H349), C315(H315), C356(H356), C365(H365),
 C368(H368), C314(H314), C304(H304), C366(H366), C346(H346), C320(H320),
 C328(H328), C330(H330), C353(H353), C336(H336), C364(H364), C310(H310),
 C311(H311), C332(H332), C305(H305), C369(H369), C333(H333), C313(H313),
 C331(H331), C319(H319), C359(H359), C318(H318), C335(H335), C337(H337),
 C329(H329), C322(H322), C347(H347), C312(H312), C323(H323), C3A(H3A),
 C1A(H1AA), C338(H338), C341(H341), C317(H317), C354(H354), C11A(H11A),
 C10A(H10A), C2A(H2A), C6A(H6A), C340(H340), C9A(H9A), C450(H450), C451(H451),
 C350(H350), C351(H351), 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(H1A), O1B(H1BA)
7.e Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F)
;
_shelx_res_checksum              55728
_shelx_hkl_checksum              60914
_olex2_date_sample_data_collection 2022-07-28
_olex2_date_sample_submission    2022-07-28
_olex2_submission_original_sample_id 50_10_48b
_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 2.862
_oxdiff_exptl_absorpt_empirical_full_min 0.284