Influence of H-bond competitors on the solvent-dependent structures of an octaurea-calix[4]tube
Milone, Marco; Pisagatti, Ilenia; Gattuso, Giuseppe; Notti, Anna; Parisi, Melchiorre F.; Brancatelli, Giovanna; Hickey, Neal; Geremia, Silvano; RSC Advances 14 (2024) 4448–4455; doi:10.1039/D3RA08764F

data_7248093
_publ_section_title
;
 Influence of H-bond competitors on the solvent-dependent structures of an
 octaurea-calix[4]tube
;
_journal_issue                   7
_journal_name_full               'RSC Advances'
_journal_page_first              4448
_journal_page_last               4455
_journal_paper_doi               10.1039/D3RA08764F
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C128  H120  N16  O16, 9.2 (C2 H6 O1 S1)'
_chemical_formula_sum            'C146.4 H175.2 N16 O25.2 S9.2'
_chemical_formula_weight         2857.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-06 deposited with the CCDC.	2024-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                91.255(5)
_cell_angle_beta                 91.14(3)
_cell_angle_gamma                103.68(3)
_cell_formula_units_Z            1
_cell_length_a                   12.729(9)
_cell_length_b                   15.650(3)
_cell_length_c                   19.849(5)
_cell_measurement_reflns_used    20735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.940
_cell_measurement_theta_min      1.011
_cell_volume                     3840(3)
_computing_cell_refinement       'XDS, Kabsch 2010'
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        XDS
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Dectris Pilatus 2M'
_diffrn_measurement_method       'Rotating Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            81832
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         25.940
_diffrn_reflns_theta_min         1.011
_diffrn_source                   Elettra
_exptl_absorpt_coefficient_mu    0.193
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1514
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.720
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0027(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1019
_refine_ls_number_reflns         15039
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.1571
_refine_ls_R_factor_gt           0.1229
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3308
_refine_ls_wR_factor_ref         0.3694
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9391
_reflns_number_total             15039
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra08764f2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C146.40 H175.20 N16 O25.20 S9.20'
_cod_database_code               7248093
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.996
_shelx_res_checksum              35400
_shelx_hkl_checksum              11101