Dampened circumrotation by CH⋯π interactions in hydrogen bonded [2]rotaxanes
Berná, Jose; Alajarín, Mateo; Martínez-Espín, Juan S.; Buriol, Lilian; Martins, Marcos A. P.; Orenes, Raúl-Ángel; Chemical Communications (Cambridge, United Kingdom) 48 (2012) 5677–5679; doi:10.1039/c2cc32092d

data_7107765
_publ_section_title
;
 Dampened circumrotation by CH&#x22EF;\p interactions in hydrogen bonded
 [2]rotaxanes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   45
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              5677
_journal_page_last               5679
_journal_paper_doi               10.1039/c2cc32092d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C66 H86 Cl6 N6 O6'
_chemical_formula_weight         1272.11
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                73.492(2)
_cell_angle_beta                 73.172(2)
_cell_angle_gamma                86.333(2)
_cell_formula_units_Z            1
_cell_length_a                   9.9123(13)
_cell_length_b                   11.7727(16)
_cell_length_c                   14.746(2)
_cell_measurement_reflns_used    3792
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.24
_cell_volume                     1578.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.907
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19245
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.80
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.8992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.153
_refine_ls_hydrogen_treatment    'NH free, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7391
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0552P)^2^+1.8721P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1736
_reflns_number_gt                5808
_reflns_number_total             7391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc32092d.txt
_cod_data_source_block           lb059s_compound_1a
_cod_database_code               7107765