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_7128690
_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         'C114 H82 N4, C18 H36 O6'
_chemical_formula_sum            'C132 H118 N4 O6'
_chemical_formula_weight         1856.30
_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             2020-10-21
_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                94.140(7)
_cell_angle_beta                 93.355(8)
_cell_angle_gamma                100.854(8)
_cell_formula_units_Z            1
_cell_length_a                   9.0214(9)
_cell_length_b                   13.7471(13)
_cell_length_c                   22.9679(19)
_cell_measurement_reflns_used    6552
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      50.4140
_cell_measurement_theta_min      1.9380
_cell_volume                     2782.6(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f    -10.27 349.73   2.00   60.00  -9.60 -89.16  31.50    --   180
  2  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74 -29.95   52
  3  \f   -339.92  20.08   2.00   38.50 -56.84 -74.16 -59.25    --   180
  4  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74 130.05   52
  5  \w      3.93  99.93   2.00   10.00    --   20.69  59.25 159.92   48
  6  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74-109.95   52
  7  \w      3.93  99.93   2.00   10.00    --   20.69  59.25 -20.08   48
  8  \w    -26.23  71.77   2.00   18.40    --   50.69 -83.74-126.05   49
  9  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25  60.08   48
 10  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74  50.05   52
 11  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25 -19.92   48
 12  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25 140.08   48
 13  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25 -99.92   48
 14  \w     33.93 129.93   2.00   18.40    --   50.69  59.25-125.08   48
 15  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25-179.92   48
 16  \w     33.93 129.93   2.00   18.40    --   50.69  59.25  30.92   48
 17  \w    -26.23  71.77   2.00   18.40    --   50.69 -83.74  80.95   49
 18  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74 170.05   52
 19  \w     33.93 129.93   2.00   18.40    --   50.69  59.25 132.92   48
 20  \w     27.40 123.40   2.00   15.50    --   44.16  59.25 -20.08   48
 21  \w     33.93 129.93   2.00   18.40    --   50.69  59.25-176.08   48
 22  \w     33.93 129.93   2.00   18.40    --   50.69  59.25  81.92   48
 23  \f   -339.92  20.08   2.00   60.00 -71.84 -89.16 -59.25    --   180
 24  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25 -59.92   48
 25  \w     33.93 129.93   2.00   18.40    --   50.69  59.25 -74.08   48
 26  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74  10.05   52
 27  \w      3.93  99.93   2.00   10.00    --   20.69  59.25  69.92   48
 28  \w     42.40 138.40   2.00   24.20    --   59.16  59.25-110.08   48
 29  \w   -120.80 -16.80   2.00   60.00    --  -89.16  83.74-149.95   52
 30  \w    192.04 288.04   2.00   60.00    --  -89.16 -59.25 100.08   48
 31  \w     42.40 138.40   2.00   24.20    --   59.16  59.25 -20.08   48
 32  \w     42.40 138.40   2.00   24.20    --   59.16  59.25 159.92   48
 33  \w      3.93  99.93   2.00   10.00    --   20.69  59.25-110.08   48
 34  \w     27.40 123.40   2.00   15.50    --   44.16  59.25  69.92   48
 35  \w     27.40 123.40   2.00   15.50    --   44.16  59.25 159.92   48
 36  \w     33.93 129.93   2.00   18.40    --   50.69  59.25 -20.08   48
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1350997000
_diffrn_orient_matrix_UB_12      -0.0415535000
_diffrn_orient_matrix_UB_13      -0.0447205000
_diffrn_orient_matrix_UB_21      -0.1068779000
_diffrn_orient_matrix_UB_22      -0.0103255000
_diffrn_orient_matrix_UB_23      0.0500557000
_diffrn_orient_matrix_UB_31      -0.0268946000
_diffrn_orient_matrix_UB_32      0.1062133000
_diffrn_orient_matrix_UB_33      -0.0064592000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1984
_diffrn_reflns_av_unetI/netI     0.1314
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            66583
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        60.015
_diffrn_reflns_theta_max         60.015
_diffrn_reflns_theta_min         1.934
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.520
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94729
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_description       block
_exptl_crystal_F_000             986
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.901
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     694
_refine_ls_number_reflns         8161
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      0.906
_refine_ls_R_factor_all          0.1798
_refine_ls_R_factor_gt           0.0817
_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^)+(0.1205P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.2472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3367
_reflns_number_total             8161
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc03009d2.cif
_cod_data_source_block           cu_gb135
_cod_depositor_comments
'Adding full bibliography for 7128689--7128690.cif.'
_cod_database_code               7128690
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.903
_reflns_odcompleteness_completeness 99.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     59.94
_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
 C66A-C65A
 1.35 with sigma of 0.02
 C67A-C66A
 1.35 with sigma of 0.02
 C65B-C64B
 1.35 with sigma of 0.02
 C64A-C63A
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C64B) \\sim Ueq, Uanis(C65B) \\sim Ueq, Uanis(C62B) \\sim Ueq,
Uanis(C63B) \\sim Ueq, Uanis(O4B) \\sim Ueq, Uanis(C64A) \\sim Ueq, Uanis(C67A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C65A, O2, C60, C59, C61, C58, C62A, O3B, O1, C63A, C62B, C64A, C63B, O4B,
 C66A, C64B, C67A, C65B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C62A(0.5) H62A(0.5) H62B(0.5) H61A(0.5) H61B(0.5) H61C(0.5)
 H61D(0.5) C66A(0.5) H66A(0.5) H66B(0.5) C64A(0.5) H64A(0.5) H64B(0.5)
 C65B(0.5) H65A(0.5) H65B(0.5) C67A(0.5) H67A(0.5) H67B(0.5) C64B(0.5)
 H64C(0.5) H64D(0.5) C65A(0.5) H65C(0.5) H65D(0.5) O4B(0.5) C63B(0.5) H63A(0.5)
 H63B(0.5) C62B(0.5) H62C(0.5) H62D(0.5) O3B(0.5) C63A(0.5) H63C(0.5) H63D(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C62A(H62A,H62B), C60(H60A,H60B), C61(H61A,H61B), C61(H61C,H61D), C59(H59A,
 H59B), C58(H58A,H58B), C66A(H66A,H66B), C64A(H64A,H64B), C65B(H65A,H65B),
 C67A(H67A,H67B), C64B(H64C,H64D), C65A(H65C,H65D), C63B(H63A,H63B), C62B(H62C,
 H62D), C63A(H63C,H63D)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C37(H37), C35(H35), C34(H34), C53(H53), C57(H57), C4(H4), C38(H38),
 C47(H47), C48(H48), C28(H28), C41(H41), C56(H56), C5(H5), C45(H45), C54(H54),
 C16(H16), C20(H20), C55(H55), C32(H32), C49(H49), C24(H24), C51(H51), C23(H23),
  C50(H50), C29(H29), C44(H44), C22(H22), C13(H13), C17(H17), C12(H12),
 C42(H42), C26(H26), C18(H18), C19(H19), C25(H25), C43(H43), C31(H31), C10(H10),
  C9(H9), C30(H30)
;
_shelx_res_checksum              71446
_shelx_fab_checksum              6109
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.201
_oxdiff_exptl_absorpt_empirical_full_min 0.843