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_1571857
_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
'C108 H72 I18 N36 Zn9, 1.245(C15 H16 O3), 2.722(C6 H12)'
_chemical_formula_sum            'C143 H124.58 I18 N36 O3.73 Zn9'
_chemical_formula_weight         5279.69
_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           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-31
_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                 100.198(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   78.834(3)
_cell_length_b                   14.9690(3)
_cell_length_c                   41.7028(12)
_cell_measurement_reflns_used    13450
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.9910
_cell_measurement_theta_min      2.2640
_cell_volume                     48435(3)
_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_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 0.994
_diffrn_measured_fraction_theta_max 0.993
_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   -146.00 -85.20   0.38    2.00    -- -103.00-115.00-135.00  160
  2  \w   -108.00 -52.90   0.38    2.00    -- -103.00 115.00 -46.00  145
  3  \w   -112.00 -86.92   0.38    2.00    -- -103.00 165.00 100.00   66
  4  \w   -115.00 -64.84   0.38    2.00    -- -103.00-165.00  77.00  132
  5  \w    -95.00 -43.70   0.38    2.00    -- -103.00  77.00 -60.00  135
  6  \w   -129.00-101.64   0.38    2.00    -- -103.00 -15.00 120.00   72
  7  \w    -60.00 -33.78   0.38    2.00    -- -103.00  61.00 150.00   69
  8  \w   -130.00 -89.72   0.38    2.00    -- -103.00 -30.00 120.00  106
  9  \w    -60.00 -29.98   0.38    2.00    -- -103.00  61.00 -30.00   79
 10  \w   -173.00-135.00   0.38    2.00    -- -103.00 -30.00 120.00  100
 11  \w   -174.00-113.20   0.38    2.00    -- -103.00 -45.00 -90.00  160
 12  \w     62.00 107.22   0.38    2.00    --  101.75-115.00-135.00  119
 13  \w     30.00  63.06   0.38    2.00    --  101.75 -61.00   0.00   87
 14  \w     29.00  54.46   0.38    2.00    --  101.75 -61.00-120.00   67
 15  \w     45.00  71.22   0.38    2.00    --  101.75 -94.00-120.00   69
 16  \w     46.00  72.22   0.38    2.00    --  101.75 -61.00 -90.00   69
 17  \w     33.00  71.76   0.38    2.00    --  101.75 -61.00  30.00  102
 18  \w     74.00 103.64   0.38    2.00    --  101.75 -94.00-120.00   78
 19  \w     30.00  72.56   0.38    2.00    --  101.75 -61.00-150.00  112
 20  \w    -77.00 -50.78   0.38    0.50    --  -46.26-165.00  77.00   69
 21  \w   -102.00 -75.78   0.38    0.50    --  -46.26 165.00 100.00   69
 22  \w     56.00  81.08   0.38    0.50    --   46.26-165.00  77.00   66
 23  \w     48.00  81.82   0.38    0.50    --   46.26-115.00-135.00   89
 24  \w     63.00 116.20   0.38    0.50    --   46.26 165.00 100.00  140
 25  \w    -24.00  17.04   0.38    0.50    --  -46.26  19.00-120.00  108
 26  \w   -118.00 -32.12   0.38    0.50    --  -46.26 -57.00-120.00  226
 27  \w    -22.00   4.22   0.38    0.50    --  -46.26  19.00-150.00   69
 28  \w    -27.00  26.20   0.38    0.50    --   46.26 -19.00-120.00  140
;
_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      -0.0132821000
_diffrn_orient_matrix_UB_12      -0.0014844000
_diffrn_orient_matrix_UB_13      0.0230324000
_diffrn_orient_matrix_UB_21      -0.0021640000
_diffrn_orient_matrix_UB_22      -0.1015879000
_diffrn_orient_matrix_UB_23      -0.0050492000
_diffrn_orient_matrix_UB_31      0.0146031000
_diffrn_orient_matrix_UB_32      -0.0164627000
_diffrn_orient_matrix_UB_33      0.0291795000
_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  0.0696
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       94
_diffrn_reflns_limit_h_min       -93
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            166422
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.250
_diffrn_reflns_theta_min         2.153
_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    19.317
_exptl_absorpt_correction_T_max  0.448
_exptl_absorpt_correction_T_min  0.047
_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    1.448
_exptl_crystal_description       block
_exptl_crystal_F_000             19908
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.204
_refine_diff_density_min         -1.767
_refine_diff_density_rms         0.298
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2502
_refine_ls_number_reflns         44038
_refine_ls_number_restraints     1335
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1488
_refine_ls_R_factor_gt           0.1201
_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^)+(0.1403P)^2^+2693.1392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3400
_refine_ls_wR_factor_ref         0.3586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                31061
_reflns_number_total             44038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           25_10_48c
_cod_original_cell_volume        48435(2)
_cod_database_code               1571857
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         '(Zn3 I6 N12 H24 C36) (C15 H16 O3)2 (C6 H12)3'
_chemical_oxdiff_usercomment     JP-9300-04
_shelx_estimated_absorpt_t_max   0.445
_shelx_estimated_absorpt_t_min   0.101
_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
 C2B-C1B = C3B-C2B = C4B-C3B = C5B-C4B = C6B-C5B = C6B-C1B
 1.39 with sigma of 0.02
 C2A-C1A = C3A-C2A = C4A-C3A = C5A-C4A = C6A-C5A = C6A-C1A
 1.39 with sigma of 0.02
 C8B-C7B = C9B-C8B = C9B-C10B = C11B-C10B = C12B-C11B = C7B-C12B
 1.39 with sigma of 0.02
 C7A-C4A
 1.5 with sigma of 0.02
 C7B-C4B
 1.5 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 C5A-C13A
 1.51 with sigma of 0.02
 O2A-C8A
 1.37 with sigma of 0.02
 O3B-C15B = O1B-C13B = O2B-C14B
 1.43 with sigma of 0.02
 O2B-C8B = O3B-C12B
 1.37 with sigma of 0.02
 C833-C1O = C833-C834 = C1O-C832 = C832-C831 = C831-C835 = C835-C834
 1.54 with sigma of 0.02
 C821-C820 = C821-C822 = C820-C819 = C819-C824 = C824-C823 = C823-C822
 1.54 with sigma of 0.02
 C802-C801 = C802-C803 = C801-C806 = C806-C805 = C805-C804 = C804-C803
 1.54 with sigma of 0.02
 C829-C828 = C829-C830 = C828-C827 = C827-C826 = C826-C825 = C825-C830
 1.54 with sigma of 0.02
 C808-C807 = C808-C809 = C807-C812 = C812-C811 = C811-C810 = C810-C809
 1.54 with sigma of 0.02
 C815-C814 = C815-C816 = C814-C813 = C813-C818 = C818-C817 = C817-C816
 1.54 with sigma of 0.02
 C840-C839 = C840-C841 = C839-C838 = C838-C837 = C837-C836 = C836-C841
 1.54 with sigma of 0.02
 C1B-C3B = C2B-C4B = C3B-C5B = C4B-C6B = C5B-C1B = C6B-C2B
 2.4 with sigma of 0.04
 C1A-C3A = C2A-C4A = C3A-C5A = C4A-C6A = C5A-C1A = C6A-C2A
 2.4 with sigma of 0.04
 C7B-C9B = C8B-C10B = C9B-C11B = C10B-C12B = C11B-C7B = C12B-C8B
 2.4 with sigma of 0.04
 O1A-C5A
 2.4 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.02
 C5B-O1B
 2.4 with sigma of 0.04
 C833-C832 = C833-C835 = C1O-C831 = C832-C835 = C831-C834
 2.54 with sigma of 0.04
 C821-C819 = C821-C823 = C820-C824 = C819-C823 = C824-C822
 2.54 with sigma of 0.04
 C802-C806 = C802-C804 = C801-C805 = C806-C804 = C805-C803
 2.54 with sigma of 0.04
 C829-C827 = C829-C825 = C828-C826 = C827-C825 = C826-C830
 2.54 with sigma of 0.04
 C808-C812 = C808-C810 = C807-C811 = C812-C810 = C811-C809
 2.54 with sigma of 0.04
 C815-C813 = C815-C817 = C814-C818 = C813-C817 = C818-C816
 2.54 with sigma of 0.04
 C840-C838 = C840-C836 = C839-C837 = C838-C836 = C837-C841
 2.54 with sigma of 0.04
 C8A-C7A \\sim C9A-C8A \\sim C9A-C10A \\sim C11A-C10A \\sim C12A-C11A \\sim
C7A-C12A
 with sigma of 0.02
 C8A-C10A \\sim C9A-C11A \\sim C11A-C7A
 with sigma of 0.04
 C7B-C10B \\sim C8B-C11B \\sim C9B-C12B
 with sigma of 0.04
 C1A-C4A \\sim C2A-C5A \\sim C3A-C6A
 with sigma of 0.04
 O2A-C14A \\sim O3A-C15A \\sim O1A-C13A
 with sigma of 0.02
 C7B-O2B \\sim O2B-C9B
 with sigma of 0.04
 C4B-C13B \\sim C13B-C6B
 with sigma of 0.04
 C7B-O3B \\sim O3B-C11B
 with sigma of 0.02
 C833-C1O \\sim C1O-C832 \\sim C832-C831 \\sim C831-C835 \\sim C835-C834 \\sim
C834-C833
 with sigma of 0.02
 C833-C835 \\sim C832-C835 \\sim C1O-C834 \\sim C1O-C831 \\sim C831-C834 \\sim
C833-C832
 with sigma of 0.04
 I309-Zn35 \\sim I409-Zn45
 with sigma of 0.02
 I310-Zn35 \\sim I410-Zn45
 with sigma of 0.02
 Zn35-N317 \\sim Zn45-N317
 with sigma of 0.02
 I309-I310 \\sim I409-I410
 with sigma of 0.04
 I309-N317 \\sim I409-N317
 with sigma of 0.04
 I310-N317 \\sim I410-N317
 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-N307 \\sim Zn43-N307
 with sigma of 0.02
 Zn33-N306 \\sim Zn43-N306
 with sigma of 0.02
 I306-I305 \\sim I406-I405
 with sigma of 0.04
 I306-N307 \\sim I406-N307
 with sigma of 0.04
 I306-N306 \\sim I406-N306
 with sigma of 0.04
 I305-N307 \\sim I405-N307
 with sigma of 0.04
 I305-N306 \\sim I405-N306
 with sigma of 0.04
 I314-Zn37 \\sim I414-Zn47
 with sigma of 0.02
 I313-Zn37 \\sim I413-Zn47
 with sigma of 0.02
 Zn37-N325 \\sim Zn47-N325
 with sigma of 0.02
 Zn37-N324 \\sim Zn47-N324
 with sigma of 0.02
 I314-I313 \\sim I414-I413
 with sigma of 0.04
 I314-N325 \\sim I414-N325
 with sigma of 0.04
 I314-N324 \\sim I414-N324
 with sigma of 0.04
 I313-N325 \\sim I413-N325
 with sigma of 0.04
 I313-N324 \\sim I413-N324
 with sigma of 0.04
 I403-Zn42 \\sim I303-Zn32
 with sigma of 0.02
 I404-Zn42 \\sim I304-Zn32
 with sigma of 0.02
 Zn42-N305 \\sim Zn32-N305
 with sigma of 0.02
 I403-I404 \\sim I303-I304
 with sigma of 0.04
 I403-N305 \\sim I303-N305
 with sigma of 0.04
 I404-N305 \\sim I304-N305
 with sigma of 0.04
 I317-Zn39 \\sim I417-Zn49
 with sigma of 0.02
 I318-Zn39 \\sim I418-Zn49
 with sigma of 0.02
 Zn39-N330 \\sim Zn49-N330
 with sigma of 0.02
 Zn39-N331 \\sim Zn49-N331
 with sigma of 0.02
 I317-I318 \\sim I417-I418
 with sigma of 0.04
 I317-N330 \\sim I417-N330
 with sigma of 0.04
 I317-N331 \\sim I417-N331
 with sigma of 0.04
 I318-N330 \\sim I418-N330
 with sigma of 0.04
 I318-N331 \\sim I418-N331
 with sigma of 0.04
 I315-Zn38 \\sim I415-Zn48
 with sigma of 0.02
 I316-Zn38 \\sim I416-Zn48
 with sigma of 0.02
 Zn38-N329 \\sim Zn48-N329
 with sigma of 0.02
 I315-I316 \\sim I415-I416
 with sigma of 0.04
 I315-N329 \\sim I415-N329
 with sigma of 0.04
 I316-N329 \\sim I416-N329
 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-N301 \\sim Zn41-N301
 with sigma of 0.02
 I302-I301 \\sim I402-I401
 with sigma of 0.04
 I302-N301 \\sim I402-N301
 with sigma of 0.04
 I301-N301 \\sim I401-N301
 with sigma of 0.04
 I516-Zn58 \\sim I416-Zn48
 with sigma of 0.02
 I515-Zn58 \\sim I415-Zn48
 with sigma of 0.02
 I312-Zn36 \\sim I412-Zn46
 with sigma of 0.02
 I311-Zn36 \\sim I411-Zn46
 with sigma of 0.02
 Zn36-N319 \\sim Zn46-N319
 with sigma of 0.02
 Zn36-N318 \\sim Zn46-N318
 with sigma of 0.02
 I312-I311 \\sim I412-I411
 with sigma of 0.04
 I312-N319 \\sim I412-N319
 with sigma of 0.04
 I312-N318 \\sim I412-N318
 with sigma of 0.04
 I311-N319 \\sim I411-N319
 with sigma of 0.04
 I311-N318 \\sim I411-N318
 with sigma of 0.04
 I512-Zn56 \\sim I412-Zn46
 with sigma of 0.02
 I511-Zn56 \\sim I411-Zn46
 with sigma of 0.02
 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
 C821-C820 \\sim C820-C819 \\sim C819-C824 \\sim C824-C823 \\sim C823-C822
\\sim C822-C821
 with sigma of 0.02
 C821-C823 \\sim C819-C823 \\sim C820-C822 \\sim C820-C824 \\sim C824-C822
\\sim C821-C819
 with sigma of 0.04
 C802-C801 \\sim C801-C806 \\sim C806-C805 \\sim C805-C804 \\sim C804-C803
\\sim C803-C802
 with sigma of 0.02
 C802-C804 \\sim C806-C804 \\sim C801-C803 \\sim C801-C805 \\sim C805-C803
\\sim C802-C806
 with sigma of 0.04
 C829-C828 \\sim C828-C827 \\sim C827-C826 \\sim C826-C825 \\sim C825-C830
\\sim C830-C829
 with sigma of 0.02
 C829-C825 \\sim C827-C825 \\sim C828-C830 \\sim C828-C826 \\sim C826-C830
\\sim C829-C827
 with sigma of 0.04
 C808-C807 \\sim C807-C812 \\sim C812-C811 \\sim C811-C810 \\sim C810-C809
\\sim C809-C808
 with sigma of 0.02
 C808-C810 \\sim C812-C810 \\sim C807-C809 \\sim C807-C811 \\sim C811-C809
\\sim C808-C812
 with sigma of 0.04
 C815-C814 \\sim C814-C813 \\sim C813-C818 \\sim C818-C817 \\sim C817-C816
\\sim C816-C815
 with sigma of 0.02
 C815-C817 \\sim C813-C817 \\sim C814-C816 \\sim C814-C818 \\sim C818-C816
\\sim C815-C813
 with sigma of 0.04
 C840-C839 \\sim C839-C838 \\sim C838-C837 \\sim C837-C836 \\sim C836-C841
\\sim C841-C840
 with sigma of 0.02
 C840-C836 \\sim C838-C836 \\sim C839-C841 \\sim C839-C837 \\sim C837-C841
\\sim C840-C838
 with sigma of 0.04
3. Restrained planarity
 C7B, C8B, C9B, C10B, C11B, C12B
 with sigma of 0.1
 C4B, C5B, C6B, C13B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C7A \\sim O2A \\sim C8A \\sim C14A \\sim C9A \\sim C4A \\sim C12A \\sim C10A
\\sim C3A \\sim C5A \\sim C11A \\sim O3A \\sim C2A \\sim C13A \\sim C6A \\sim
C15A \\sim C1A \\sim O1A: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C9B \\sim C4B \\sim C5B \\sim C3B \\sim C7B \\sim C6B \\sim C13B \\sim C2B
\\sim C12B \\sim C8B \\sim C1B \\sim O1B \\sim O3B \\sim C11B \\sim O2B \\sim
C15B \\sim C10B \\sim C14B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C833 \\sim C1O \\sim C832 \\sim C831 \\sim C835 \\sim C834: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
I407 \\sim I307 \\sim Zn44 \\sim Zn34 \\sim I308 \\sim I408: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C821 \\sim C820 \\sim C819 \\sim C824 \\sim C823 \\sim C822: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C802 \\sim C801 \\sim C806 \\sim C805 \\sim C804 \\sim C803: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C829 \\sim C828 \\sim C827 \\sim C826 \\sim C825 \\sim C830: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C808 \\sim C807 \\sim C812 \\sim C811 \\sim C810 \\sim C809: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C815 \\sim C814 \\sim C813 \\sim C818 \\sim C817 \\sim C816: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C840 \\sim C839 \\sim C838 \\sim C837 \\sim C836 \\sim C841: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(Zn35) = Uanis(Zn45)
5. Rigid body (RIGU) restrains
 C2B, C4B, C5B, C3B, C7B, 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
 C833, C1O, C832, C831, C835, C834
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I407, I307, Zn44, Zn34, I308, I408
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C821, C820, C819, C824, C823, C822
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C802, C801, C806, C805, C804, C803
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C829, C828, C827, C826, C825, C830
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C808, C807, C812, C811, C810, C809
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C815, C814, C813, C818, C817, C816
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C840, C839, C838, C837, C836, C841
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 I312, Zn36, Zn46, I511, I311, I411, I412
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N336, C399, C403, C402, C401, C400
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(1)
 Sof(I306)=Sof(I305)=Sof(Zn33)=FVAR(1)
 Sof(I418)=Sof(Zn49)=Sof(I417)=1-FVAR(2)
 Sof(I317)=Sof(I318)=Sof(Zn39)=FVAR(2)
 Sof(I410)=Sof(Zn45)=Sof(I409)=1-FVAR(3)
 Sof(I309)=Sof(I310)=Sof(Zn35)=FVAR(3)
 Sof(I304)=Sof(Zn32)=Sof(I303)=1-FVAR(4)
 Sof(I403)=Sof(I404)=Sof(Zn42)=FVAR(4)
 Sof(Zn44)=Sof(I408)=Sof(I407)=1-FVAR(5)
 Sof(I307)=Sof(I308)=Sof(Zn34)=FVAR(5)
 Fixed Sof: I302(0.48775) I301(0.48775) I312(0.45641) I311(0.45641)
 I314(0.48782) I313(0.48782) I315(0.69263) I316(0.69263) Zn36(0.45641)
 Zn31(0.48775) Zn37(0.48782) Zn38(0.69263) O2A(0.85819) O3A(0.85819)
 O1A(0.85819) H1A(0.85819) C7A(0.85819) C3A(0.85819) H3A(0.85819) C1A(0.85819)
 H1AA(0.85819) C4A(0.85819) C6A(0.85819) H6A(0.85819) C5A(0.85819) C2A(0.85819)
 H2A(0.85819) C8A(0.85819) C12A(0.85819) C11A(0.85819) H11A(0.85819)
 C13A(0.85819) H13A(0.85819) H13B(0.85819) C10A(0.85819) H10A(0.85819)
 C9A(0.85819) H9A(0.85819) C14A(0.85819) H14A(0.85819) H14B(0.85819)
 H14C(0.85819) C15A(0.85819) H15A(0.85819) H15B(0.85819) H15C(0.85819)
 I414(0.41004) Zn47(0.41004) I413(0.41004) I416(0.25839) Zn48(0.25839)
 I415(0.25839) I402(0.35696) Zn41(0.35696) I401(0.35696) I514(0.10212)
 I513(0.10212) Zn57(0.10212) I502(0.1553) I501(0.1553) Zn51(0.1553)
 I515(0.04897) I516(0.04897) Zn58(0.04897) I412(0.50082) Zn46(0.50082)
 I411(0.50082) I512(0.04278) I511(0.04278) Zn56(0.04278) C4B(0.38664)
 O3B(0.38664) C6B(0.38664) H6B(0.38664) C2B(0.38664) H2B(0.38664) C5B(0.38664)
 C3B(0.38664) H3B(0.38664) C12B(0.38664) C11B(0.38664) H11B(0.38664)
 C1B(0.38664) H1B(0.38664) C7B(0.38664) C15B(0.38664) H15D(0.38664)
 H15E(0.38664) H15F(0.38664) C821(0.40836) H82A(0.40836) H82B(0.40836)
 C820(0.40836) H82C(0.40836) H82D(0.40836) C819(0.40836) H81A(0.40836)
 H81B(0.40836) C824(0.40836) H82E(0.40836) H82F(0.40836) C823(0.40836)
 H82G(0.40836) H82H(0.40836) C822(0.40836) H82I(0.40836) H82J(0.40836)
 C802(0.47319) H80A(0.47319) H80B(0.47319) C801(0.47319) H80C(0.47319)
 H80D(0.47319) C806(0.47319) H80E(0.47319) H80F(0.47319) C805(0.47319)
 H80G(0.47319) H80H(0.47319) C804(0.47319) H80I(0.47319) H80J(0.47319)
 C803(0.47319) H80K(0.47319) H80L(0.47319) C829(0.37592) H82K(0.37592)
 H82L(0.37592) C828(0.37592) H82M(0.37592) H82N(0.37592) C827(0.37592)
 H82O(0.37592) H82P(0.37592) C826(0.37592) H82Q(0.37592) H82R(0.37592)
 C825(0.37592) H82S(0.37592) H82T(0.37592) C830(0.37592) H83A(0.37592)
 H83B(0.37592) C808(0.45898) H80M(0.45898) H80N(0.45898) C807(0.45898)
 H80O(0.45898) H80P(0.45898) C812(0.45898) H81C(0.45898) H81D(0.45898)
 C811(0.45898) H81E(0.45898) H81F(0.45898) C810(0.45898) H81G(0.45898)
 H81H(0.45898) C809(0.45898) H80Q(0.45898) H80R(0.45898) C833(0.32277)
 H83C(0.32277) H83D(0.32277) C1O(0.32277) H1OA(0.32277) H1OB(0.32277)
 C832(0.32277) H83E(0.32277) H83F(0.32277) C831(0.32277) H83G(0.32277)
 H83H(0.32277) C835(0.32277) H83I(0.32277) H83J(0.32277) C834(0.32277)
 H83K(0.32277) H83L(0.32277) C815(0.44738) H81I(0.44738) H81J(0.44738)
 C814(0.44738) H81K(0.44738) H81L(0.44738) C813(0.44738) H81M(0.44738)
 H81N(0.44738) C818(0.44738) H81O(0.44738) H81P(0.44738) C817(0.44738)
 H81Q(0.44738) H81R(0.44738) C816(0.44738) H81S(0.44738) H81T(0.44738)
 C10B(0.38664) H10B(0.38664) C13B(0.38664) H13C(0.38664) H13D(0.38664)
 O2B(0.38664) C9B(0.38664) H9B(0.38664) O1B(0.38664) H1BA(0.38664) C8B(0.38664)
 C14B(0.38664) H14D(0.38664) H14E(0.38664) H14F(0.38664) C840(0.23534)
 H84A(0.23534) H84B(0.23534) C839(0.23534) H83M(0.23534) H83N(0.23534)
 C838(0.23534) H83O(0.23534) H83P(0.23534) C837(0.23534) H83Q(0.23534)
 H83R(0.23534) C836(0.23534) H83S(0.23534) H83T(0.23534) C841(0.23534)
 H84C(0.23534) H84D(0.23534)
 Fixed Uiso: I514(0.08) I513(0.08) Zn57(0.08) I515(0.08) I516(0.08) Zn58(0.08)
 I512(0.08) I511(0.08) Zn56(0.08) C840(0.08) C839(0.08) C838(0.08) C837(0.08)
 C836(0.08) C841(0.08)
7.a Secondary CH2 refined with riding coordinates:
 C13A(H13A,H13B), C821(H82A,H82B), C820(H82C,H82D), C819(H81A,H81B), C824(H82E,
 H82F), C823(H82G,H82H), C822(H82I,H82J), C802(H80A,H80B), C801(H80C,H80D),
 C806(H80E,H80F), C805(H80G,H80H), C804(H80I,H80J), C803(H80K,H80L), C829(H82K,
 H82L), C828(H82M,H82N), C827(H82O,H82P), C826(H82Q,H82R), C825(H82S,H82T),
 C830(H83A,H83B), C808(H80M,H80N), C807(H80O,H80P), C812(H81C,H81D), C811(H81E,
 H81F), C810(H81G,H81H), C809(H80Q,H80R), C833(H83C,H83D), C1O(H1OA,H1OB),
 C832(H83E,H83F), C831(H83G,H83H), C835(H83I,H83J), C834(H83K,H83L), C815(H81I,
 H81J), C814(H81K,H81L), C813(H81M,H81N), C818(H81O,H81P), C817(H81Q,H81R),
 C816(H81S,H81T), C13B(H13C,H13D), C840(H84A,H84B), C839(H83M,H83N), C838(H83O,
 H83P), C837(H83Q,H83R), C836(H83S,H83T), C841(H84C,H84D)
7.b Aromatic/amide H refined with riding coordinates:
 C347(H347), C338(H338), C367(H367), C364(H364), C348(H348), C355(H355),
 C323(H323), C349(H349), C340(H340), C341(H341), C356(H356), C365(H365),
 C301(H301), C353(H353), C354(H354), C313(H313), C322(H322), C335(H335),
 C337(H337), C336(H336), C351(H351), C315(H315), C3A(H3A), C346(H346),
 C318(H318), C1A(H1AA), C314(H314), C328(H328), C333(H333), C319(H319),
 C332(H332), C6A(H6A), C385(H385), C304(H304), C329(H329), C366(H366),
 C387(H387), C2A(H2A), C350(H350), C320(H320), C390(H390), C305(H305),
 C384(H384), C312(H312), C395(H395), C317(H317), C302(H302), C374(H374),
 C377(H377), C311(H311), C11A(H11A), C376(H376), C405(H405), C394(H394),
 C331(H331), C386(H386), C10A(H10A), C310(H310), C373(H373), C372(H372),
 C389(H389), C9A(H9A), C383(H383), C403(H403), C404(H404), C368(H368),
 C371(H371), C359(H359), C402(H402), C382(H382), C330(H330), C358(H358),
 C401(H401), C408(H408), C369(H369), C407(H407), C391(H391), C400(H400),
 C392(H392), C6B(H6B), C2B(H2B), C3B(H3B), C11B(H11B), C1B(H1B), C10B(H10B),
 C9B(H9B)
7.c Tetrahedral OH refined with riding coordinates:
 O1A(H1A), O1B(H1BA)
7.d Idealised Me refined with everything fixed:
 C14A(H14A,H14B,H14C), C15A(H15A,H15B,H15C), C15B(H15D,H15E,H15F), C14B(H14D,
 H14E,H14F)
;
_shelx_res_checksum              3956
_shelx_hkl_checksum              75044
_olex2_date_sample_data_collection 2023-03-10
_olex2_date_sample_submission    2023-03-10
_olex2_submission_original_sample_id 25_10_48c
_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 2.445
_oxdiff_exptl_absorpt_empirical_full_min 0.442