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_1565993
_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         'C9 O8 P2, 2 (C36 H60 O30), 28.5 (H2 O), 4K '
_chemical_formula_sum            'C81 H195 K4 O96.5 P2'
_chemical_formula_weight         2931.70
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-10-07
_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            4
_cell_length_a                   23.5333(18)
_cell_length_b                   23.5333(18)
_cell_length_c                   24.406(3)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    150
_cell_measurement_theta_max      64.24
_cell_measurement_theta_min      3.75
_cell_volume                     13516(2)
_computing_cell_refinement       'Bruker APEX3'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker APX3'
_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      150
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0775
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            83464
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        58.931
_diffrn_reflns_theta_max         58.930
_diffrn_reflns_theta_min         2.608
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.430
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0530 before and 0.0446 after correction. The Ratio of minimum to maximum transmission is 0.8623. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       block
_exptl_crystal_F_000             6236
_exptl_crystal_recrystallization_method 'recystallization from solvent'
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.148
_refine_diff_density_min         -0.719
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.02(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.210
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         9712
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0906
_refine_ls_R_factor_gt           0.0870
_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^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2450
_refine_ls_wR_factor_ref         0.2548
_reflns_Friedel_coverage         0.783
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9071
_reflns_number_total             9712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05697b2.cif
_cod_data_source_block           hv300620_c9_0m
_cod_depositor_comments
'Adding full bibliography for 1565992--1565995.cif.'
_cod_original_formula_sum        'C81 H195 K4 O96.50 P2'
_cod_database_code               1565993
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.98(4)
 0.02(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 C1-C2
 1.5 with sigma of 0.02
 C4-C5
 1.54 with sigma of 0.02
 C2-C4
 2.45 with sigma of 0.04
 C2-C1 \\sim C2P-C1 \\sim C3P-C2P \\sim C2-C3 \\sim C4-C3 \\sim C3P-C4P \\sim
C5P-C4P
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C3 \\sim C3P: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C4 \\sim C5 \\sim C5P \\sim C4P \\sim C3 \\sim C3P: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(O12W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O13W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Rigid body (RIGU) restrains
 C1, C2P, C3P, C4P, C5P, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
6. Others
 Fixed Sof: P1A(0.667) O1B(0.33333) O1(0.667) O4B(0.33333) O4(0.667) H2B(0.5)
 K1(0.5) O17W(0.5) P1B(0.33333) C2P(0.5) C4P(0.5) C5P(0.25) C3P(0.5) C5(0.25)
 C2(0.5) C3(0.5) C4(0.5) K3(0.16667) O9W(0.25) O13W(0.5) O14W(0.5) O26W(0.75)
 O8W(0.75) K2(0.5) O30W(0.5) O5W(0.5) O16W(0.5) O22W(0.25) O11W(0.5) O10W(0.5)
 K3B(0.33333) O2W(0.5) O7W(0.5) O21W(0.5) O12W(0.5) O19W(0.25) O15W(0.5)
 O6W(0.25) O18W(0.25) O16X(0.5) O33W(0.5)
7.a Ternary CH refined with riding coordinates:
 C1E(H1E), C1B(H1B), C1F(H1F), C1C(H1C), C1A(H1A), C1D(H1D), C2E(H2EA),
 C2A(H2AA), C2F(H2F), C2B(H2BA), C2C(H2C), C3D(H3DA), C3E(H3EA), C3C(H3CA),
 C3B(H3B), C3F(H3FA), C3A(H3AA), C4D(H4D), C4B(H4B), C4F(H4F), C2AA(H2AB),
 C4C(H4C), C5B(H5B), C3AA(H3AB), C5C(H5C), C5F(H5F), C5E(H5E), C5D(H5D)
7.b Secondary CH2 refined with riding coordinates:
 C6C(H6CA,H6CB), C6D(H6DA,H6DB), C6B(H6BA,H6BB), C6E(H6EA,H6EB), C6A(H6AA,
 H6AB), C6F(H6FA,H6FB)
7.c Idealised tetrahedral OH refined as rotating group:
 O2B(H2B), O2A(H2A), O2E(H2E), O3D(H3D), O3C(H3C), O3F(H3F), O3A(H3A),
 O3E(H3E), O6C(H6C), O6B(H6B), O6F(H6F)
;
_shelx_res_checksum              57101
_shelx_hkl_checksum              37855
_olex2_submission_special_instructions 'No special instructions were received'