Dynamics of a [2]rotaxane wheel in a crystalline molecular solid.
Baggi, Giorgio; Wilson, Benjamin H.; Dhara, Ayan; O'Keefe, Christopher A; Schurko, Robert W.; Loeb, Stephen J.; Chemical communications (Cambridge, England) 57 (2021) 8210–8213; doi:10.1039/d1cc03009d

data_7128689
_publ_section_title
;
 Dynamics of a [2]rotaxane wheel in a crystalline molecular solid.
;
_journal_issue                   66
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8210
_journal_page_last               8213
_journal_paper_doi               10.1039/d1cc03009d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety
'5.17(C H2 Cl2), C114 H82 N4, 2(C0.75 H1.5 Cl1.75)'
_chemical_formula_sum            'C120.67 H95.33 Cl13.83 N4'
_chemical_formula_weight         2091.65
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-21 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                76.476(3)
_cell_angle_beta                 89.608(4)
_cell_angle_gamma                89.864(3)
_cell_formula_units_Z            1
_cell_length_a                   12.2864(7)
_cell_length_b                   12.6134(7)
_cell_length_c                   17.4682(10)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      59.87
_cell_measurement_theta_min      2.60
_cell_volume                     2632.0(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      170.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28330
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        58.927
_diffrn_reflns_theta_max         58.927
_diffrn_reflns_theta_min         3.597
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.720
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1178 before and 0.0687 after correction. The Ratio of minimum to maximum transmission is 0.7187. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       block
_exptl_crystal_F_000             1082
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.740
_refine_diff_density_min         -0.819
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         7454
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.1573
_refine_ls_R_factor_gt           0.1323
_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^)+(0.1239P)^2^+20.3668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3131
_refine_ls_wR_factor_ref         0.3326
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5783
_reflns_number_total             7454
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03009d2.cif
_cod_data_source_block           cu_gb061_0m
_cod_depositor_comments
'Adding full bibliography for 7128689--7128690.cif.'
_cod_database_code               7128689
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.643
_shelx_estimated_absorpt_t_min   0.318
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups
2. Restrained distances
 Cl4B-Cl3B
 2.292 with sigma of 0.02
 Cl3B-Cl4B
 3 with sigma of 0.02
 Cl6A-C60
 1.7 with sigma of 0.02
 C60-Cl5A
 1.7 with sigma of 0.02
 Cl8B-C61B
 1.7 with sigma of 0.02
 Cl8B-Cl7B
 2.927 with sigma of 0.02
 C61B-Cl7B
 1.715 with sigma of 0.02
 Cl8A-C61A
 1.715 with sigma of 0.02
 Cl8A-Cl7A
 2.928 with sigma of 0.02
 C60-Cl6B
 1.7 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl3B \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl4B \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl3A \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl4A \\sim C59: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl4B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl3B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl3A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C59 \\sim Cl4A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C60 \\sim Cl5A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
C61B \\sim Cl8B: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Cl8A \\sim C61A \\sim Cl7A: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Cl7B \\sim C61B \\sim Cl8B: within 1.7A with sigma of 0.04 and sigma for
terminal atoms of 0.08
Uanis(C61A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C61B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 Cl3B, Cl3A, C59, Cl4B, Cl4A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl7A, C61A, Cl8A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C61A, Cl8A, Cl7A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: Cl7A(0.33333) Cl8A(0.33333) Cl8B(0.5) C60(0.75) H60C(0.25)
 H60D(0.25) H60A(0.5) H60B(0.5) Cl6B(0.25) C61B(0.5) H61C(0.5) H61D(0.5)
 Cl3A(0.5) C59(0.75) H59B(0.5) H59A(0.5) H59D(0.25) H59C(0.25) Cl3B(0.25)
 Cl4B(0.25) Cl4A(0.5) Cl6A(0.5) Cl5A(0.75) Cl5B(0.25) Cl7B(0.5) C61A(0.33333)
 H61A(0.33333) H61B(0.33333)
6.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C60(H60C,H60D), C60(H60A,H60B), C61B(H61C,H61D), C59(H59B,
 H59A), C59(H59D,H59C), C61A(H61A,H61B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), C20(H20), C45(H45), C35(H35), C41(H41), C22(H22), C47(H47), C12(H12),
 C32(H32), C34(H34), C13(H13), C10(H10), C37(H37), C26(H26), C23(H23), C16(H16),
  C44(H44), C9(H9), C28(H28), C38(H38), C53(H53), C17(H17), C51(H51), C31(H31),
 C5(H5), C4(H4), C57(H57), C19(H19), C18(H18), C48(H48), C30(H30), C24(H24),
 C29(H29), C25(H25), C42(H42), C56(H56), C43(H43), C54(H54), C55(H55), C49(H49),
  C50(H50)
;
_shelx_res_checksum              80498
_olex2_submission_special_instructions 'No special instructions were received'