Pillar[5]arene derivatives with three different kinds of repeating units: first examples, crystal structures and selective preparation
Pan, Mingguang; Xue, Min; RSC Adv. 4 (2014) 260–; doi:10.1039/C3RA44581J

data_7239294
_publ_section_title
;
 Pillar[5]arene derivatives with three different kinds of repeating units:
 first examples, crystal structures and selective preparation
;
_journal_issue                   1
_journal_name_full               'RSC Adv.'
_journal_page_first              260
_journal_paper_doi               10.1039/C3RA44581J
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C53 H58 O18, 4(CH2 Cl2)'
_chemical_formula_sum            'C57 H64 Cl8 O18'
_chemical_formula_weight         1320.68
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 102.2746(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5855(4)
_cell_length_b                   15.4343(3)
_cell_length_c                   21.1972(4)
_cell_measurement_reflns_used    11244
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      66.8747
_cell_measurement_theta_min      3.6760
_cell_volume                     6261.2(2)
_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      170(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28585
_diffrn_reflns_theta_full        66.99
_diffrn_reflns_theta_max         66.99
_diffrn_reflns_theta_min         3.68
_exptl_absorpt_coefficient_mu    3.869
_exptl_absorpt_correction_T_max  0.3899
_exptl_absorpt_correction_T_min  0.3211
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Agilent Technologies, 2011) 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
Two disordered CH2Cl2 solvent were removed from the asymmetric unit.
;
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0657P)^2^+8.5438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                4703
_reflns_number_total             5551
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra44581j.txt
_cod_data_source_block           130419_pmg_71
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7239294