Keto-Adamantane-Based Macrocycle Crystalline Supramolecular Assemblies Showing Selective Vapochromism to Tetrahydrofuran.
Li, Zunhua; Tan, Yingzi; Ding, Manhua; Tang, Linli; Zeng, Fei; Molecules (Basel, Switzerland) 29 (2024) 719–; doi:10.3390/molecules29030719

data_1571126
_publ_section_title
;
 Keto-Adamantane-Based Macrocycle Crystalline Supramolecular Assemblies
 Showing Selective Vapochromism to Tetrahydrofuran.
;
_journal_issue                   3
_journal_name_full               'Molecules (Basel, Switzerland)'
_journal_page_first              719
_journal_paper_doi               10.3390/molecules29030719
_journal_volume                  29
_journal_year                    2024
_chemical_absolute_configuration na
_chemical_formula_moiety         'C54 H64 O8'
_chemical_formula_sum            'C54 H64 O8'
_chemical_formula_weight         841.05
_chemical_name_systematic        Mac
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   21.174(3)
_cell_length_b                   21.174(3)
_cell_length_c                   13.5099(19)
_cell_measurement_reflns_used    5334
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      19.76
_cell_measurement_theta_min      2.22
_cell_volume                     5245.5(13)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0550
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            53176
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_reflns_theta_min         2.444
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.053
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6749
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0784 before and 0.0486 after correction.
The Ratio of minimum to maximum transmission is 0.9052.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.799
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details
;
 Flack x determined using 1456 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         7981
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0874P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1418
_refine_ls_wR_factor_ref         0.1670
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                4161
_reflns_number_total             7981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2204281_0m.cif
_cod_data_source_block           2204281_0m
_cod_original_cell_volume        5245.7(17)
_cod_database_code               1571126
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.994
_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
2. Uiso/Uaniso restraints and constraints
C008 \\sim C009 \\sim C00G \\sim C00E \\sim C00H \\sim C00J: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C00G) \\sim Ueq, Uanis(C009) \\sim Ueq, Uanis(C008) \\sim Ueq,
Uanis(C00J) \\sim Ueq, Uanis(C00H) \\sim Ueq, Uanis(C00E) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C009) \\sim Ueq, Uanis(C008) \\sim Ueq, Uanis(C00G) \\sim Ueq,
Uanis(C00E) \\sim Ueq, Uanis(C00H) \\sim Ueq, Uanis(C00J) \\sim Ueq: with sigma
of 0.001 and sigma for terminal atoms of 0.002
3.a Ternary CH refined with riding coordinates:
 C00D(H00E), C00Q(H00R)
3.b Secondary CH2 refined with riding coordinates:
 C006(H00A,H00B), C00B(H00C,H00D), C00I(H00H,H00I), C00K(H00K,H00L), C00L(H00M,
 H00N), C00N(H00O,H00P), C00R(H00S,H00T)
3.c Aromatic/amide H refined with riding coordinates:
 C00F(H00F), C00G(H00G), C00J(H00J), C00O(H00Q)
3.d Idealised Me refined as rotating group:
 C00S(H00U,H00V,H00W), C00T(H00X,H00Y,H), C00U(H00Z,HA,HB), C00V(H00,HC,HD)
;
_shelx_res_checksum              4279
_shelx_hkl_checksum              55597
_shelx_fab_checksum              55769
_olex2_submission_special_instructions 'No special instructions were received'