Orchestrating Directional Molecular Motions: Kinetically Controlled Supramolecular Pathways of a Helical Host on Rodlike Guests.
Wang, Xiang; Wicher, Barbara; Ferrand, Yann; Huc, Ivan; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b04884

data_4126252
_publ_section_title
;
 Orchestrating Directional Molecular Motions: Kinetically Controlled
 Supramolecular Pathways of a Helical Host on Rodlike Guests.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b04884
_journal_year                    2017
_chemical_formula_moiety
'4(C139 H135 F8 N23 O21), C45 H72 N4 O8, 12(C H Cl3), 4.33(H2 O)'
_chemical_formula_sum            'C613 H632.66 Cl36 F32 N96 O96.33'
_chemical_formula_weight         12770.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_symmetry_space_group_name_Hall  'P -2yc'
_symmetry_space_group_name_H-M   'P 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 105.91(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   36.365(7)
_cell_length_b                   49.686(10)
_cell_length_c                   46.097(9)
_cell_measurement_reflns_used    221131
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.880
_cell_measurement_theta_min      0.736
_cell_volume                     80099(3)
_computing_cell_refinement       'XDS (W. Kabsch, 2010)'
_computing_data_collection       'mX-cube and EDNA, BL13-XALOC, ALBA'
_computing_data_reduction        'XDS (W. Kabsch, 2010)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Superflip, (L. Palatinus, 2007)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_method       'phi scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.850
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 0.930
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       52
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            221131
_diffrn_reflns_point_group_measured_fraction_full 0.778
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        26.880
_diffrn_reflns_theta_max         26.880
_diffrn_reflns_theta_min         0.736
_exptl_absorpt_coefficient_mu    0.308
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.059
_exptl_crystal_description       prsim
_exptl_crystal_F_000             26613
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.891
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.128
_refine_ls_abs_structure_details
;
 Flack x determined using 28313 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.513(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.605
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     10284
_refine_ls_number_reflns         157077
_refine_ls_number_restraints     1332
_refine_ls_restrained_S_all      1.698
_refine_ls_R_factor_all          0.2018
_refine_ls_R_factor_gt           0.1607
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3920
_refine_ls_wR_factor_ref         0.4326
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_full    0.625
_reflns_Friedel_fraction_max     0.625
_reflns_number_gt                93034
_reflns_number_total             157077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04884_si_005.cif
_cod_data_source_block           alba_sq
_cod_original_cell_volume        80098(30)
_cod_database_code               4126252
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.970
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              28237
_shelx_hkl_checksum              65580
_shelx_fab_checksum              5996