Size-dependent compression of threaded alkyldiphosphate in head to head cyclodextrin [3]pseudorotaxanes
Scelle, Jérémy; Vervoitte, Hugo; Bouteiller, Laurent; Chamoreau, Lise-Marie; Sollogoub, Matthieu; Vives, Guillaume; Hasenknopf, Bernold; Chemical Science 13 (2022) 2218–2225; doi:10.1039/D1SC05697B

data_1565995
_publ_section_title
;
 Size-dependent compression of threaded alkyldiphosphate in head to head
 cyclodextrin [3]pseudorotaxanes
;
_journal_issue                   8
_journal_name_full               'Chemical Science'
_journal_page_first              2218
_journal_page_last               2225
_journal_paper_doi               10.1039/D1SC05697B
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety
'2(C36 H60 O30), (C10 H20 O8 P2),4 K, 30.8 (H2 O)  '
_chemical_formula_sum            'C82 H201.75 K4 O98.88 P2'
_chemical_formula_weight         2988.51
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-11 deposited with the CCDC.	2022-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.3244(10)
_cell_length_b                   23.3244(10)
_cell_length_c                   48.784(3)
_cell_measurement_reflns_used    9979
_cell_measurement_temperature    120
_cell_measurement_theta_max      68.18
_cell_measurement_theta_min      2.83
_cell_volume                     26540(2)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER APEX 2'
_computing_data_reduction        'BRUKER SAINT'
_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, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            181579
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.725
_diffrn_reflns_theta_min         3.313
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.500
_exptl_absorpt_correction_T_max  0.6614
_exptl_absorpt_correction_T_min  0.5370
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0644 before and 0.0461 after correction. The Ratio of minimum to maximum transmission is 0.8119. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       prism
_exptl_crystal_F_000             12726
_exptl_crystal_recrystallization_method 'recrystalisation from solvent'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         2.024
_refine_diff_density_min         -1.048
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1822
_refine_ls_number_reflns         24318
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0842
_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^)+(0.1659P)^2^+41.1737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2352
_refine_ls_wR_factor_ref         0.2406
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                22712
_reflns_number_total             24318
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05697b2.cif
_cod_data_source_block           jsc340c_f_0m
_cod_depositor_comments
'Adding full bibliography for 1565992--1565995.cif.'
_cod_original_cell_volume        26540(3)
_cod_database_code               1565995
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.806
_shelx_estimated_absorpt_t_min   0.706
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.94(2)
 0.06(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(O50W) \\sim Ueq, Uanis(O41W) \\sim Ueq, Uanis(O46W) \\sim Ueq: with sigma
of 0.1 and sigma for terminal atoms of 0.2
Uanis(O40W) \\sim Ueq, Uanis(O205) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
4. Others
 Fixed Sof: O203(0.5) O201(0.25) O202(0.25) O205(0.5) O206(0.33333) K1(0.5)
 K3A(0.33333) K4(0.25) K5A(0.33333) O2W(0.5) O2WB(0.5) O3W(0.5) O3WB(0.5)
 O4W(0.5) O7W(0.75) O8W(0.5) O11W(0.5) K12W(0.5) O13W(0.5) K14W(0.5) O15W(0.75)
 O18W(0.5) O20W(0.5) O30W(0.5) O40W(0.5) O41W(0.5) O42W(0.5) O45W(0.5)
 O46W(0.5) O48W(0.25) O49W(0.5) O50W(0.25) K101(0.16667) K102(0.33333)
 O51W(0.5) K106(0.33333) O52W(0.5) K0AA(0.5) O53W(0.5)
5.a Ternary CH refined with riding coordinates:
 C1A1(H1A1), C2A1(H2A1), C3A1(H3A1), C4A1(H4A1), C5A1(H5A1), C1B1(H1B1),
 C2B1(H2B1), C3B1(H3B1), C4B1(H4B1), C5B1(H5B1), C1C1(H1C1), C2C1(H2C1),
 C3C1(H3C1), C4C1(H4C1), C5C1(H5C1), C1D1(H1D1), C2D1(H2D1), C3D1(H3D1),
 C4D1(H4D1), C5D1(H5D1), C1E1(H1E1), C2E1(H2E1), C3E1(H3E1), C4E1(H4E1),
 C5E1(H5E1), C1F1(H1F1), C2F1(H2F1), C3F1(H3F1), C4F1(H4F1), C5F1(H5F1),
 C1A2(H1A2), C3A2(H3A2), C4A2(H4A2), C5A2(H5A2), C1B2(H1B2), C2B2(H2B2),
 C3B2(H3B2), C4B2(H4B2), C5B2(H5B2), C1C2(H1C2), C3C2(H3C2), C4C2(H4C2),
 C5C2(H5C2), C1D2(H1D2), C2D2(H2D2), C3D2(H3D2), C4D2(H4D2), C5D2(H5D2),
 C1E2(H1E2), C2E2(H2E2), C3E2(H3E2), C4E2(H4E2), C5E2(H5E2), C1F2(H1F2),
 C2F2(H2F2), C3F2(H3F2), C4F2(H4F2), C5F2(H5F2)
5.b Secondary CH2 refined with riding coordinates:
 C6A1(H6AA,H6AB), C6B1(H6BA,H6BB), C6C1(H6CA,H6CB), C6D1(H6DA,H6DB), C6E1(H6EA,
 H6EB), C6F1(H6FA,H6FB), C6A2(H6AC,H6AD), C6B2(H6BC,H6BD), C6C2(H6CC,H6CD),
 C6D2(H6DC,H6DD), C6E2(H6EC,H6ED), C6F2(H6FC,H6FD), C1(H1A,H1B), C2(H2A,H2B),
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B)
;
_shelx_res_checksum              5812
_shelx_hkl_checksum              99446
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'