Four Structural isomers of BMpillar[5]arene: Synthesis, Crystal Structures and Complexation with N-Octyltrimethyl Ammonium Hexafluorophosphate
Zibin Zhang; Yan Luo; Binyuan Xia; Chengyou Han; Yihua Yu; Xiaopeng Chen; Feihe Huang; Chem.Commun. 47 (2011) 2417–; doi:10.1039/c0cc03732j

data_7105992
_publ_section_title
;
 Four Structural isomers of BMpillar[5]arene: Synthesis, Crystal
 Structures and Complexation with N-Octyltrimethyl Ammonium
 Hexafluorophosphate
;
_journal_name_full               Chem.Commun.
_journal_page_first              2417
_journal_paper_doi               10.1039/c0cc03732j
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         '2(C50 H60 O10), 3(C2 H3 N)'
_chemical_formula_sum            'C106 H129 N3 O20'
_chemical_formula_weight         1765.12
_chemical_name_systematic
;
?
;
_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                68.825(5)
_cell_angle_beta                 88.866(4)
_cell_angle_gamma                80.174(4)
_cell_formula_units_Z            2
_cell_length_a                   12.2072(4)
_cell_length_b                   20.6545(12)
_cell_length_c                   21.4041(11)
_cell_measurement_reflns_used    8248
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.9368
_cell_measurement_theta_min      2.5668
_cell_volume                     4953.3(5)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2009)'
_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, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0553
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31785
_diffrn_reflns_theta_full        65.08
_diffrn_reflns_theta_max         65.08
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  0.91
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.53
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1892
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.475
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1130
_refine_ls_number_reflns         16706
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.1031
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2895
_refine_ls_wR_factor_ref         0.3248
_reflns_number_gt                9165
_reflns_number_total             16706
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0CC03732J.TXT
_cod_data_source_block           EMpillar[5]arene
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        4953.3(4)
_cod_database_code               7105992