Influence of axle length on the rate and mechanism of shuttling in rigid H-shaped [2]rotaxanes
Gholami, Ghazale; Zhu, Kelong; Baggi, Giorgio; Schott, Eduardo; Zarate, Ximena; Loeb, Stephen J.; Chem. Sci.  (2017) –; doi:10.1039/C7SC03736H

data_1547337
_publ_section_title
;
 Influence of axle length on the rate and mechanism of shuttling in rigid
 H-shaped [2]rotaxanes
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03736H
_journal_year                    2017
_chemical_formula_moiety         'C64 H64 N4, C24 H32 O8, 2(C3 H7 N O)'
_chemical_formula_sum            'C94 H110 N6 O10'
_chemical_formula_weight         1483.87
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-07-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-20 deposited with the CCDC.
2017-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                107.703(4)
_cell_angle_beta                 90.106(4)
_cell_angle_gamma                110.238(4)
_cell_formula_units_Z            2
_cell_length_a                   14.3220(13)
_cell_length_b                   15.9818(16)
_cell_length_c                   20.0611(16)
_cell_measurement_reflns_used    5727
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.887
_cell_measurement_theta_min      2.79
_cell_volume                     4074.8(7)
_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  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.2
_diffrn_measured_fraction_theta_full 0.578
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1505
_diffrn_reflns_av_unetI/netI     0.1148
_diffrn_reflns_Laue_measured_fraction_full 0.578
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40316
_diffrn_reflns_point_group_measured_fraction_full 0.578
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         20.815
_diffrn_reflns_theta_min         2.795
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6735
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0846 before and 0.0513 after correction.
The Ratio of minimum to maximum transmission is 0.9035.
The \l/2 correction factor is 0.00150.'
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             1592
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.414
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1007
_refine_ls_number_reflns         8510
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.2001
_refine_ls_R_factor_gt           0.1040
_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^)+(0.0694P)^2^+20.5414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4295
_reflns_number_total             8510
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03736h2.cif
_cod_data_source_block           mo_kz022_0m
_cod_database_code               1547337
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C4S \\sim N2S \\sim C6S \\sim O2S \\sim C5S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O1S \\sim C3S \\sim N1S \\sim C2S \\sim C1S: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(O2S) \\sim Ueq, Uanis(C6S) \\sim Ueq, Uanis(N2S) \\sim Ueq, Uanis(C5S)
\\sim Ueq, Uanis(C4S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(O1S) \\sim Ueq, Uanis(C3S) \\sim Ueq, Uanis(N1S) \\sim Ueq, Uanis(C2S)
\\sim Ueq, Uanis(C1S) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms
of 0.2
Uanis(C3) = Uanis(C3A)
Uanis(C1) = Uanis(C1A)
Uanis(C2) = Uanis(C2A)
3. Same fragment restrains
{C4, C3A, C2A, C1A} sigma for 1-2: 0.02, 1-3: 0.02
as
{C4, C3, C2, C1}
4. Others
 Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=
 Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=
 Sof(H1A)=Sof(H1B)=Sof(H1C)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,
 H75B), C76(H76A,H76B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B),
 C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B)
5.b Me refined with riding coordinates:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C64(H64A,H64B,H64C), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC),
 C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC)
5.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C6(H6), C7(H7), C9(H9), C10(H10), C15(H15), C16(H16),
 C18(H18), C19(H19), C21(H21), C22(H22), C29(H29), C30(H30), C32(H32), C34(H34),
  C35(H35), C37(H37), C44(H44), C45(H45), C47(H47), C48(H48), C50(H50),
 C51(H51), C56(H56), C57(H57), C59(H59), C60(H60), C66(H66), C67(H67), C68(H68),
  C69(H69), C78(H78), C79(H79), C80(H80), C81(H81), C3S(H3S), C6S(H6S)
5.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C3A(H3AA,H3AB,H3AC),
 C2A(H2AA,H2AB,H2AC), C1A(H1AA,H1AB,H1AC)
;
_olex2_submission_special_instructions 'No special instructions were received'