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_1547338
_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         'C20 H10 Br4 N4, C16 H32 O8'
_chemical_formula_sum            'C36 H42 Br4 N4 O8'
_chemical_formula_weight         978.37
_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
_atom_sites_solution_primary     dual
_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                68.379(2)
_cell_angle_beta                 82.740(2)
_cell_angle_gamma                68.992(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6346(14)
_cell_length_b                   10.1658(15)
_cell_length_c                   11.2070(17)
_cell_measurement_reflns_used    6123
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.26
_cell_volume                     952.6(2)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART V5.631 (?, 2016)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0582
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9812
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         1.955
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.281
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5585
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1009 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.7491.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             490
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: ethyl acetate'
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.994
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+0.1474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1042
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3291
_reflns_number_total             3839
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03736h2.cif
_cod_data_source_block           kz71
_cod_database_code               1547338
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.391
_shelx_estimated_absorpt_t_min   0.238
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C016(H01A,H01B), C017(H01C,H01D), C018(H01E,H01F), C021(H02A,H02B), C022(H02C,
 H02D), C024(H02E,H02F), C025(H02G,H02H), C026(H02I,H02J)
2.b Aromatic/amide H refined with riding coordinates:
 N009(H009), C011(H011), C019(H019), C020(H020), C023(H023)
;
_olex2_submission_special_instructions 'No special instructions were received'