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_1565992
_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), C8 H16 O8 P2, 4 K, 31.5 (H2 O)'
_chemical_formula_sum            'C80 H199 K4 O99.5 P2'
_chemical_formula_weight         2971.72
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-01
_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                   23.4286(4)
_cell_length_b                   23.4286(4)
_cell_length_c                   24.2838(5)
_cell_measurement_reflns_used    9447
_cell_measurement_temperature    120
_cell_measurement_theta_max      66.06
_cell_measurement_theta_min      4.10
_cell_volume                     13329.4(4)
_computing_cell_refinement       'Bruker APEX2'
_computing_data_collection       'Bruker SAINT'
_computing_data_reduction        'Bruker APEX2'
_computing_molecular_graphics    'Diamond (Brandenburg)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0584
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            157940
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.467
_diffrn_reflns_theta_min         4.190
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.489
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0924 before and 0.0629 after correction. The Ratio of minimum to maximum transmission is 0.8210. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       block
_exptl_crystal_F_000             6324
_exptl_crystal_recrystallization_method 'recristalisation from solvent'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.08(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     974
_refine_ls_number_reflns         12240
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0826
_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^)+(0.1695P)^2^+16.0899P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2328
_refine_ls_wR_factor_ref         0.2433
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                11126
_reflns_number_total             12240
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc05697b2.cif
_cod_data_source_block           jsc340b_f_0m
_cod_depositor_comments
'Adding full bibliography for 1565992--1565995.cif.'
_cod_original_cell_volume        13329.4(5)
_cod_original_formula_sum        'C80 H199 K4 O99.50 P2'
_cod_database_code               1565992
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.754
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.92(4)
 0.08(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups
3. Restrained distances
 O6D-H6D
 0.85 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O5W \\sim O6W: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
O25W: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O31W) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O20W) \\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
5. Others
 Fixed Sof: H2C(0.5) O1(0.75) O1'(0.25) H1AA(0.75) H1AB(0.75) H1BC(0.25)
 H1BD(0.25) C2(0.75) H2G(0.75) H2H(0.75) C2'(0.25) H2'A(0.25) H2'B(0.25)
 H3AA(0.75) H3AB(0.75) H3BC(0.25) H3BD(0.25) K1(0.66667) K3(0.5) O1W(0.5)
 O2W(0.75) O3W(0.5) O5W(0.5) O6W(0.5) O7W(0.5) O8W(0.5) O9W(0.5) O10W(0.25)
 O12W(0.5) O30W(0.25) K2(0.33333) O4W(0.5) O13W(0.5) O14W(0.25) O15W(0.5)
 O17W(0.5) O18W(0.5) O19W(0.5) O20W(0.5) O21W(0.5) O26W(0.75) O29W(0.5)
 O31W(0.5) O32W(0.25) O23W(0.5) O24W(0.25) O25W(0.5)
6.a Riding coordinates:
 O6B(H6B), O6E(H6E), O6F(H6F)
6.b Riding coordinates and stretchable bonds:
 O6D(H6D)
6.c Ternary CH refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C1B(H1B), C2B(H2B),
 C3B(H3B), C4B(H4B), C5B(H5B), C1C(H1C), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C),
  C1D(H1D), C2D(H2D), C3D(H3D), C4D(H4D), C5D(H5D), C1E(H1E), C2E(H2E),
 C3E(H3E), C4E(H4E), C5E(H5E), C1F(H1F), C2F(H2F), C3F(H3F), C4F(H4F), C5F(H5F)
6.d Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C6B(H6BA,H6BB), C6C(H6CA,H6CB), C6D(H6DA,H6DB), C6E(H6EA,
 H6EB), C6F(H6FA,H6FB), C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2G,H2H), C2'(H2'A,
 H2'B), C3(H3AA,H3AB), C3(H3BC,H3BD), C4(H4G,H4H)
;
_shelx_res_checksum              27981
_shelx_hkl_checksum              60410
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_exptl_crystal_mounting_method cryoloop
_olex2_submission_special_instructions 'No special instructions were received'