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_1571876
_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, 0.915(C15 H16 O3), 1.065(C6 H12)'
_chemical_formula_sum            'C92.12 H75.43 I12 N24 O2.75 Zn6'
_chemical_formula_weight         3477.60
_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             2024-01-23
_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                 102.171(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.6878(7)
_cell_length_b                   14.9984(3)
_cell_length_c                   34.4068(8)
_cell_measurement_reflns_used    25249
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.6560
_cell_measurement_theta_min      2.6200
_cell_volume                     15984.8(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_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 2018/2 (Sheldrick, 2018)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -174.00 -90.00   0.50    3.00    -- -103.00 -24.00 176.00  168
  2  \w    -69.00 -30.00   0.50    3.00    -- -103.00  61.00 -30.00   78
  3  \w   -174.00 -89.00   0.50    3.00    -- -103.00 -15.00-120.00  170
  4  \w    -69.00 -30.00   0.50    3.00    -- -103.00  61.00   0.00   78
  5  \w     89.00 175.00   0.50    3.00    --  101.75  24.00 -18.00  172
  6  \w     29.00 108.00   0.50    3.00    --  101.75 -77.00  60.00  158
  7  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00-120.00   88
  8  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00-150.00   88
  9  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00  90.00   88
 10  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00   0.00   88
 11  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00  60.00   88
 12  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00 -90.00   88
 13  \w     29.00 108.00   0.50    3.00    --  101.75 -77.00 -30.00  158
 14  \w     29.00 108.00   0.50    3.00    --  101.75 -77.00  30.00  158
 15  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00 -30.00   88
 16  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00 150.00   88
 17  \w     29.00  73.00   0.50    3.00    --  101.75 -61.00-180.00   88
 18  \w    -28.00  28.00   0.50    0.50    --  -46.36  24.00 -18.00  112
 19  \w   -120.00 -34.00   0.50    0.50    --  -46.36 -24.00 176.00  172
 20  \w     34.00 121.00   0.50    0.50    --   46.36  24.00 -18.00  174
 21  \w    -28.00  32.00   0.50    0.50    --   46.36 -24.00 176.00  120
 22  \w     23.00  94.00   0.50    0.50    --   46.36-125.00-120.00  142
 23  \w    -28.00  28.00   0.50    0.50    --   46.36 -19.00  30.00  112
;
_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      0.0496691000
_diffrn_orient_matrix_UB_12      0.0059855000
_diffrn_orient_matrix_UB_13      0.0098652000
_diffrn_orient_matrix_UB_21      -0.0006929000
_diffrn_orient_matrix_UB_22      0.0320285000
_diffrn_orient_matrix_UB_23      -0.0427064000
_diffrn_orient_matrix_UB_31      -0.0028692000
_diffrn_orient_matrix_UB_32      0.0972998000
_diffrn_orient_matrix_UB_33      0.0133871000
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            136060
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.251
_diffrn_reflns_theta_min         2.133
_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    19.505
_exptl_absorpt_correction_T_max  0.341
_exptl_absorpt_correction_T_min  0.096
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
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    1.445
_exptl_crystal_description       block
_exptl_crystal_F_000             6536
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.508
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1640
_refine_ls_number_reflns         29217
_refine_ls_number_restraints     803
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0874
_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^)+(0.1174P)^2^+120.3981P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2576
_refine_ls_wR_factor_ref         0.2691
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22340
_reflns_number_total             29217
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lt5068.cif
_cod_data_source_block           50_10_96a
_cod_database_code               1571876
_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   0.342
_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
 C7B-C4B
 1.5 with sigma of 0.02
 C5B-C13B
 1.51 with sigma of 0.02
 O1B-C13B = O2B-C14B = O3B-C15B
 1.43 with sigma of 0.02
 O2A-C8A = O3A-C12A
 1.37 with sigma of 0.02
 O2B-C8B = O3B-C12B
 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
 C816-C815 = C816-C817 = C815-C814 = C814-C813 = C813-C818 = C818-C817
 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
 C822-C821 = C822-C823 = C821-C820 = C820-C819 = C819-C824 = C824-C823
 1.54 with sigma of 0.02
 C5B-O1B
 2.4 with sigma of 0.04
 C12A-C15A
 2.4 with sigma of 0.02
 O1A-C5A
 2.4 with sigma of 0.04
 C8B-C14B
 2.4 with sigma of 0.02
 C809-C807 = C809-C811 = C808-C812 = C807-C811 = C812-C810
 2.54 with sigma of 0.04
 C816-C814 = C816-C818 = C815-C813 = C814-C818 = C813-C817
 2.54 with sigma of 0.04
 C802-C806 = C802-C804 = C801-C805 = C806-C804 = C805-C803
 2.54 with sigma of 0.04
 C822-C820 = C822-C824 = C821-C819 = C820-C824 = C819-C823
 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
 C1A-C3A \\sim C2A-C4A \\sim C3A-C5A \\sim C4A-C6A \\sim C5A-C1A \\sim C6A-C2A
 with sigma of 0.04
 C3B-C7B \\sim C7B-C5B
 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
 C8B-C4B \\sim C4B-C12B
 with sigma of 0.04
 O1A-C13A \\sim O2A-C14A \\sim O3A-C15A
 with sigma of 0.02
 C5A-C13A \\sim C7A-C4A
 with sigma of 0.02
 N306-C314 \\sim N306-C414
 with sigma of 0.02
 C316-C315 \\sim C316-C415
 with sigma of 0.02
 C315-C314 \\sim C415-C414
 with sigma of 0.02
 N306-C315 \\sim N306-C415
 with sigma of 0.04
 C316-C314 \\sim C316-C414
 with sigma of 0.04
 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
 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
 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
 C822-C821 \\sim C821-C820 \\sim C820-C819 \\sim C819-C824 \\sim C824-C823
\\sim C823-C822
 with sigma of 0.02
 C822-C824 \\sim C820-C824 \\sim C821-C823 \\sim C821-C819 \\sim C819-C823
\\sim C822-C820
 with sigma of 0.04
3. Restrained planarity
 O2B, C8B, C7B, C12B, O3B
 with sigma of 0.1
 C6B, C5B, C4B, C13B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
I308 \\sim I408 \\sim Zn34 \\sim Zn44 \\sim I307 \\sim I407: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
O2A \\sim O3A \\sim C12A \\sim C15A \\sim C7A \\sim C11A \\sim C4A \\sim C8A
\\sim C10A \\sim C3A \\sim C5A \\sim C9A \\sim C2A \\sim C6A \\sim C13A \\sim
C14A \\sim C1A \\sim O1A: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
C12B \\sim C4B \\sim C3B \\sim C5B \\sim C7B \\sim C2B \\sim C6B \\sim C13B
\\sim C8B \\sim C1B \\sim O1B \\sim O2B \\sim C9B \\sim C11B \\sim O3B \\sim
C14B \\sim C10B \\sim C15B: 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
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
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
C822 \\sim C821 \\sim C820 \\sim C819 \\sim C824 \\sim C823: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
Uanis(C414) = Uanis(C415) = Uanis(C315) = Uanis(C314)
5. Rigid body (RIGU) restrains
 I407, I408, Zn44, Zn34, I308, I307
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C12B, C4B, C3B, C5B, C7B, C2B, C6B, C13B, C8B, C1B, O1B, O2B, C9B, C11B, O3B,
 C14B, C10B, C15B
 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
 C816, C815, C814, C813, C818, C817
 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
 C822, C821, C820, C819, C824, C823
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Sof(I311)=Sof(Zn36)=Sof(I312)=1-FVAR(1)
 Sof(I411)=Sof(I412)=Sof(Zn46)=FVAR(1)
 Sof(I406)=Sof(Zn43)=Sof(I405)=1-FVAR(2)
 Sof(I305)=Sof(I306)=Sof(Zn33)=FVAR(2)
 Sof(Zn35)=Sof(I310)=Sof(I309)=1-FVAR(3)
 Sof(I409)=Sof(I410)=Sof(Zn45)=FVAR(3)
 Sof(I402)=Sof(Zn41)=Sof(I401)=1-FVAR(4)
 Sof(I302)=Sof(I301)=Sof(Zn31)=FVAR(4)
 Sof(Zn42)=Sof(I403)=Sof(I404)=1-FVAR(5)
 Sof(I304)=Sof(I303)=Sof(Zn32)=FVAR(5)
 Sof(Zn34)=Sof(I308)=Sof(I307)=1-FVAR(6)
 Sof(I407)=Sof(I408)=Sof(Zn44)=FVAR(6)
 Sof(C415)=Sof(H415)=Sof(C414)=Sof(H414)=1-FVAR(7)
 Sof(C315)=Sof(H315)=Sof(C314)=Sof(H314)=FVAR(7)
 Fixed Sof: O3A(0.74122) O2A(0.74122) O1A(0.74122) H1AA(0.74122) C4A(0.74122)
 C3A(0.74122) H3A(0.74122) C7A(0.74122) C5A(0.74122) C1A(0.74122) H1A(0.74122)
 C2A(0.74122) H2A(0.74122) C8A(0.74122) C6A(0.74122) H6A(0.74122) C12A(0.74122)
 C10A(0.74122) H10A(0.74122) C11A(0.74122) H11A(0.74122) C14A(0.74122)
 H14A(0.74122) H14B(0.74122) H14C(0.74122) C13A(0.74122) H13A(0.74122)
 H13B(0.74122) C9A(0.74122) H9A(0.74122) C15A(0.74122) H15A(0.74122)
 H15B(0.74122) H15C(0.74122) C4B(0.17405) C3B(0.17405) H3B(0.17405)
 C2B(0.17405) H2B(0.17405) C1B(0.17405) H1B(0.17405) C6B(0.17405) H6B(0.17405)
 C5B(0.17405) O2B(0.17405) C7B(0.17405) C8B(0.17405) C9B(0.17405) H9B(0.17405)
 C10B(0.17405) H10B(0.17405) C11B(0.17405) H11B(0.17405) C12B(0.17405)
 O3B(0.17405) C809(0.27802) H80A(0.27802) H80B(0.27802) C808(0.27802)
 H80C(0.27802) H80D(0.27802) C807(0.27802) H80E(0.27802) H80F(0.27802)
 C812(0.27802) H81A(0.27802) H81B(0.27802) C811(0.27802) H81C(0.27802)
 H81D(0.27802) C810(0.27802) H81E(0.27802) H81F(0.27802) C816(0.28464)
 H81G(0.28464) H81H(0.28464) C815(0.28464) H81I(0.28464) H81J(0.28464)
 C814(0.28464) H81K(0.28464) H81L(0.28464) C813(0.28464) H81M(0.28464)
 H81N(0.28464) C818(0.28464) H81O(0.28464) H81P(0.28464) C817(0.28464)
 H81Q(0.28464) H81R(0.28464) C802(0.29178) H80G(0.29178) H80H(0.29178)
 C801(0.29178) H80I(0.29178) H80J(0.29178) C806(0.29178) H80K(0.29178)
 H80L(0.29178) C805(0.29178) H80M(0.29178) H80N(0.29178) C804(0.29178)
 H80O(0.29178) H80P(0.29178) C803(0.29178) H80Q(0.29178) H80R(0.29178)
 C822(0.21088) H82A(0.21088) H82B(0.21088) C821(0.21088) H82C(0.21088)
 H82D(0.21088) C820(0.21088) H82E(0.21088) H82F(0.21088) C819(0.21088)
 H81S(0.21088) H81T(0.21088) C824(0.21088) H82G(0.21088) H82H(0.21088)
 C823(0.21088) H82I(0.21088) H82J(0.21088) O1B(0.17405) H1BA(0.17405)
 C13B(0.17405) H13C(0.17405) H13D(0.17405) C15B(0.17405) H15D(0.17405)
 H15E(0.17405) H15F(0.17405) C14B(0.17405) H14D(0.17405) H14E(0.17405)
 H14F(0.17405)
 Fixed Uiso: C802(0.08) C801(0.08) C806(0.08) C805(0.08) C804(0.08) C803(0.08)
 C822(0.08) C821(0.08) C820(0.08) C819(0.08) C824(0.08) C823(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), C816(H81G,H81H), C815(H81I,H81J),
 C814(H81K,H81L), C813(H81M,H81N), C818(H81O,H81P), C817(H81Q,H81R), C802(H80G,
 H80H), C801(H80I,H80J), C806(H80K,H80L), C805(H80M,H80N), C804(H80O,H80P),
 C803(H80Q,H80R), C822(H82A,H82B), C821(H82C,H82D), C820(H82E,H82F), C819(H81S,
 H81T), C824(H82G,H82H), C823(H82I,H82J), C13B(H13C,H13D)
7.b Aromatic/amide H refined with riding coordinates:
 C320(H320), C313(H313), C351(H351), C335(H335), C331(H331), C328(H328),
 C349(H349), C350(H350), C336(H336), C333(H333), C329(H329), C319(H319),
 C348(H348), C353(H353), C312(H312), C358(H358), C369(H369), C317(H317),
 C330(H330), C332(H332), C322(H322), C340(H340), C310(H310), C367(H367),
 C3A(H3A), C354(H354), C356(H356), C355(H355), C359(H359), C337(H337),
 C323(H323), C311(H311), C364(H364), C365(H365), C338(H338), C366(H366),
 C368(H368), C318(H318), C341(H341), C1A(H1A), C302(H302), C346(H346), C2A(H2A),
  C301(H301), C372(H372), C6A(H6A), C371(H371), C347(H347), C305(H305),
 C304(H304), C10A(H10A), C11A(H11A), C9A(H9A), C315(H315), C314(H314),
 C415(H415), C414(H414), C3B(H3B), C2B(H2B), C1B(H1B), C6B(H6B), C9B(H9B),
 C10B(H10B), C11B(H11B)
7.c Fitted hexagon refined as free rotating group:
 C4B(C3B,C2B,C1B,C6B,C5B), C7B(C8B,C9B,C10B,C11B,C12B)
7.d Tetrahedral OH refined with riding coordinates:
 O1A(H1AA), O1B(H1BA)
7.e 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              38100
_shelx_hkl_checksum              11249
_olex2_date_sample_data_collection 2022-05-30
_olex2_date_sample_submission    2022-05-30
_olex2_submission_original_sample_id 50_10_96a
_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 2.689
_oxdiff_exptl_absorpt_empirical_full_min 0.350