Insights into molecular recognition from the crystal structures of <i>p-tert</i>-butylcalix[6]arene complexed with different solvents
Malinska, Maura; IUCrJ 9 (2022) 55–64; doi:10.1107/S2052252521010678

data_1565858
_publ_section_title
;
 Insights into molecular recognition from the crystal structures of
 <i>p-tert</i>-butylcalix[6]arene complexed with different solvents
;
_journal_coeditor_code           ED5024
_journal_issue                   1
_journal_name_full               IUCrJ
_journal_page_first              55
_journal_page_last               64
_journal_paper_doi               10.1107/S2052252521010678
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         '3(C H2 Cl2), C66 H84 O6'
_chemical_formula_sum            'C69 H90 Cl6 O6'
_chemical_formula_weight         1228.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 96.732(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8792(10)
_cell_length_b                   19.6559(15)
_cell_length_c                   18.9669(10)
_cell_measurement_reflns_used    5262
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.8270
_cell_measurement_theta_min      2.0120
_cell_volume                     6619.6(7)
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1195
_diffrn_reflns_av_unetI/netI     0.1489
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            42665
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.497
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       plate
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.357
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.742
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     781
_refine_ls_number_reflns         13520
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1896
_refine_ls_R_factor_gt           0.1189
_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^)+(0.1277P)^2^+19.9101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2900
_refine_ls_wR_factor_ref         0.3347
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7355
_reflns_number_total             13520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ed5024.cif
_cod_data_source_block           x6_DCM_13_3
_cod_database_code               1565858
_shelx_estimated_absorpt_t_max   0.984
_shelx_estimated_absorpt_t_min   0.898
_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
 C69A-Cl5A
 1.76 with sigma of 0.02
 C69-Cl6
 1.76 with sigma of 0.005
 C69A-Cl6A
 1.76 with sigma of 0.02
 C69-Cl5
 1.76 with sigma of 0.02
 C7-C8 = C7-C9 = C7-C10
 1.54 with sigma of 0.005
 C62-C64 = C62-C63 = C62-C65 = C62-C58
 1.54 with sigma of 0.01
 C18-C21 = C18-C19 = C18-C20 = C18-C14
 1.54 with sigma of 0.02
 C29-C30
 1.54 with sigma of 0.02
 C18-C20
 1.54 with sigma of 0.02
 Cl6-Cl5
 2.93 with sigma of 0.04
 Cl6A-Cl5A
 2.93 with sigma of 0.04
 C10-C8
 2.51 with sigma of 0.04
 C9-C8
 2.51 with sigma of 0.04
 C4-C8
 2.51 with sigma of 0.04
 C10-C9
 2.51 with sigma of 0.04
 C10-C4
 2.51 with sigma of 0.04
 C4-C9
 2.51 with sigma of 0.04
3. Rigid bond restraints
 C69, Cl5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C69A, Cl6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C69A, Cl5A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C69, Cl6
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C69 \\sim Cl5 \\sim Cl6: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08
C69A \\sim Cl6A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C69A \\sim Cl5A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(C69A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C69A)=Sof(H69C)=Sof(H69D)=Sof(Cl6A)=Sof(Cl5A)=1-FVAR(1)
 Sof(Cl6)=Sof(Cl5)=Sof(C69)=Sof(H69A)=Sof(H69B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C55(H55A,H55B), C66(H66A,H66B), C44(H44A,H44B), C33(H33A,H33B), C11(H11A,
 H11B), C22(H22A,H22B), C68(H68A,H68B), C67(H67A,H67B), C69(H69A,H69B),
 C69A(H69C,H69D)
6.b Aromatic/amide H refined with riding coordinates:
 C59(H59), C48(H48), C46(H46), C35(H35), C13(H13), C37(H37), C24(H24),
 C57(H57), C3(H3A), C26(H26), C15(H15), C5(H5A)
6.c Tetrahedral OH refined with riding coordinates:
 O1(H1)
6.d Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C65(H65A,H65B,H65C), C54(H54A,H54B,
 H54C), C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C41(H41A,H41B,H41C), C31(H31A,
 H31B,H31C), C52(H52A,H52B,H52C), C21(H21A,H21B,H21C), C53(H53A,H53B,H53C),
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C64(H64A,H64B,H64C), C19(H19A,H19B,H19C),
 C10(H10A,H10B,H10C), C20(H20A,H20B,H20C), C63(H63A,H63B,H63C)
6.e Idealised tetrahedral OH refined as rotating group:
 O5(H5), O3(H3), O6(H6), O2(H2), O4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'