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_1571125
_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_formula_moiety         '2(C54 H60 O10), C2 H4 Cl4, C16 Cl4 N4 O4'
_chemical_formula_sum            'C126 H124 Cl8 N4 O24'
_chemical_formula_weight         2361.88
_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             2022-12-08
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.022(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.227(5)
_cell_length_b                   18.218(5)
_cell_length_c                   19.010(5)
_cell_measurement_reflns_used    6295
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.49
_cell_measurement_theta_min      2.23
_cell_volume                     5892(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_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  0.0311
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32617
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         1.638
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7035
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             2472
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6693
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1149
_refine_ls_R_factor_gt           0.0801
_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^)+(0.1710P)^2^+1.7670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2302
_refine_ls_wR_factor_ref         0.2671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4222
_reflns_number_total             6693
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            11.cif
_cod_data_source_block           11
_cod_database_code               1571125
_shelx_shelxl_version_number     2018/3
_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. Restrained distances
 Cl-C1_$2 \\sim Cl1_$2-C1_$2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl3A \\sim C2A \\sim C3A \\sim C2 \\sim O2A \\sim C4A \\sim C4 \\sim
C3 \\sim C6A \\sim O1 \\sim C5 \\sim N1A \\sim N1 \\sim O1 \\sim Cl3A \\sim C2A
\\sim C3A \\sim C2 \\sim O2A \\sim C4A \\sim Cl2 \\sim C4 \\sim C3 \\sim C6A
\\sim C5 \\sim N1A \\sim N1: within -1.8A with sigma of 0.015 and sigma for
terminal atoms of 0.03 within -1.8A
4. Others
 Fixed Sof: Cl1(0.5) Cl(0.5) C1(0.5) H1A(0.5) H1B(0.5) Cl3A(0.5) O2A(0.5)
 C3(0.5) C4(0.5) C2(0.5) C2A(0.5) C3A(0.5) C4A(0.5) C6A(0.5) Cl2(0.5) C5(0.5)
 N1A(0.5) O1(0.5) N1(0.5)
5.a Ternary CH refined with riding coordinates:
 C00R(H00R), C00U(H00U)
5.b Secondary CH2 refined with riding coordinates:
 C009(H00A,H00B), C00K(H00D,H00E), C00O(H00F,H00G), C00Q(H00H,H00I), C00S(H00J,
 H00K), C00V(H00L,H00M), C1(H1A,H1B)
5.c Aromatic/amide H refined with riding coordinates:
 C008(H008), C00B(H00C), C00P(H00P), C00T(H00T)
5.d Fitted hexagon refined as free rotating group:
 C3(C4,C2,C2A,C3A,C4A)
5.e Idealised Me refined as rotating group:
 C00W(H00N,H00O,H00Q), C00X(H00S,H00V,H00W), C00Y(H00X,H00Y,H), C00Z(H00Z,HA,HB)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'