Formation of a pillar[5]arene‒based [3]pseudorotaxane in solution and in the solid state
Lingyan Gao; Chengyou Han; Bo Zheng; Shengyi Dong; Feihe Huang; Chem.Commun. 49 (2013) 472–; doi:10.1039/c2cc37646f

data_7108744
_publ_section_title
;
 Formation of a pillar[5]arene--based [3]pseudorotaxane in solution and in
 the solid state
;
_journal_name_full               Chem.Commun.
_journal_page_first              472
_journal_paper_doi               10.1039/c2cc37646f
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C74 H102 Br3 O11'
_chemical_formula_sum            'C74 H102 Br3 O11'
_chemical_formula_weight         1407.29
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 130.180(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.807(3)
_cell_length_b                   20.7165(10)
_cell_length_c                   27.943(3)
_cell_measurement_reflns_used    5301
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      29.0745
_cell_measurement_theta_min      3.0389
_cell_volume                     14510(4)
_computing_cell_refinement       'CrysAlis PRO (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28619
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    1.724
_exptl_absorpt_correction_T_max  0.6627
_exptl_absorpt_correction_T_min  0.5603
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5912
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.569
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     931
_refine_ls_number_reflns         13256
_refine_ls_number_restraints     472
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1805
_refine_ls_R_factor_gt           0.0843
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1056P)^2^+70.5483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2048
_refine_ls_wR_factor_ref         0.2659
_reflns_number_gt                6408
_reflns_number_total             13256
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc37646f.txt
_cod_data_source_block           x
_cod_original_cell_volume        14510(2)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7108744