#------------------------------------------------------------------------------
#$Date: 2019-11-28 21:15:00 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244640 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/92/7239294.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7239294
loop_
_publ_author_name
'Pan, Mingguang'
'Xue, Min'
_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       'ω 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/[σ²(Fo²)+(0.0657P)²+8.5438P] where P=(Fo²+2Fc²)/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
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
O1 O 0.68843(8) 0.10267(10) 0.20478(7) 0.0390(4) Uani 1 1 d .
O2 O 0.54960(8) -0.04425(10) 0.38006(7) 0.0393(4) Uani 1 1 d .
O3 O 0.69239(8) 0.42277(9) 0.20442(6) 0.0335(3) Uani 1 1 d .
O4 O 0.66098(8) 0.50066(10) 0.08902(7) 0.0383(4) Uani 1 1 d .
O5 O 0.73722(8) 0.41628(10) 0.05267(6) 0.0397(4) Uani 1 1 d .
O6 O 0.68700(8) 0.23981(9) 0.42757(6) 0.0331(3) Uani 1 1 d .
O7 O 0.66608(9) 0.13674(10) 0.52302(7) 0.0435(4) Uani 1 1 d .
O8 O 0.62057(8) 0.24699(10) 0.56937(7) 0.0417(4) Uani 1 1 d .
O9 O 0.55541(7) 0.52388(11) 0.38126(6) 0.0376(4) Uani 1 1 d .
C1 C 0.5000 -0.08567(17) 0.2500 0.0301(6) Uani 1 2 d S
H1A H 0.4925 -0.1233 0.2857 0.036 Uiso 0.50 1 calc PR
H1B H 0.5075 -0.1233 0.2143 0.036 Uiso 0.50 1 calc PR
C2 C 0.56403(9) -0.02963(12) 0.27316(9) 0.0269(4) Uani 1 1 d .
C3 C 0.59873(10) 0.00595(13) 0.22846(9) 0.0308(4) Uani 1 1 d .
H3 H 0.5845 -0.0095 0.1842 0.037 Uiso 1 1 calc R
C4 C 0.65358(10) 0.06336(12) 0.24719(9) 0.0275(4) Uani 1 1 d .
C5 C 0.67592(9) 0.08692(12) 0.31205(9) 0.0254(4) Uani 1 1 d .
C6 C 0.64171(10) 0.05081(13) 0.35694(9) 0.0281(4) Uani 1 1 d .
H6 H 0.6562 0.0658 0.4012 0.034 Uiso 1 1 calc R
C7 C 0.58650(10) -0.00708(13) 0.33777(9) 0.0290(4) Uani 1 1 d .
C8 C 0.67226(14) 0.0750(2) 0.13980(11) 0.0530(6) Uani 1 1 d .
H8A H 0.6990 0.1094 0.1146 0.079 Uiso 1 1 calc R
H8B H 0.6222 0.0829 0.1222 0.079 Uiso 1 1 calc R
H8C H 0.6844 0.0137 0.1375 0.079 Uiso 1 1 calc R
C9 C 0.57256(18) -0.0254(2) 0.44647(12) 0.0713(10) Uani 1 1 d .
H9A H 0.5660 0.0365 0.4538 0.107 Uiso 1 1 calc R
H9B H 0.6222 -0.0401 0.4602 0.107 Uiso 1 1 calc R
H9C H 0.5454 -0.0595 0.4715 0.107 Uiso 1 1 calc R
C10 C 0.73586(9) 0.15016(12) 0.33265(9) 0.0272(4) Uani 1 1 d .
H10A H 0.7578 0.1397 0.3786 0.033 Uiso 1 1 calc R
H10B H 0.7716 0.1391 0.3069 0.033 Uiso 1 1 calc R
C11 C 0.71327(9) 0.24408(12) 0.32442(8) 0.0238(4) Uani 1 1 d .
C12 C 0.71612(9) 0.28944(12) 0.26804(9) 0.0261(4) Uani 1 1 d .
H12 H 0.7325 0.2609 0.2344 0.031 Uiso 1 1 calc R
C13 C 0.69528(10) 0.37567(13) 0.26030(9) 0.0280(4) Uani 1 1 d .
C14 C 0.67302(9) 0.42001(12) 0.30950(8) 0.0239(4) Uani 1 1 d .
C15 C 0.67046(10) 0.37492(13) 0.36598(8) 0.0270(4) Uani 1 1 d .
H15 H 0.6557 0.4040 0.4003 0.032 Uiso 1 1 calc R
C16 C 0.68924(9) 0.28813(12) 0.37273(8) 0.0247(4) Uani 1 1 d .
C17 C 0.72224(12) 0.38680(14) 0.15579(9) 0.0369(5) Uani 1 1 d .
H17A H 0.7049 0.3270 0.1461 0.044 Uiso 1 1 calc R
H17B H 0.7737 0.3847 0.1702 0.044 Uiso 1 1 calc R
C18 C 0.70222(10) 0.44257(13) 0.09658(9) 0.0301(4) Uani 1 1 d .
C19 C 0.72277(14) 0.46459(18) -0.00710(10) 0.0483(6) Uani 1 1 d .
H19A H 0.7450 0.4358 -0.0388 0.072 Uiso 1 1 calc R
H19B H 0.7414 0.5235 0.0007 0.072 Uiso 1 1 calc R
H19C H 0.6722 0.4673 -0.0238 0.072 Uiso 1 1 calc R
C20 C 0.65708(11) 0.27984(13) 0.47488(9) 0.0303(4) Uani 1 1 d .
H20A H 0.6109 0.3044 0.4549 0.036 Uiso 1 1 calc R
H20B H 0.6875 0.3274 0.4960 0.036 Uiso 1 1 calc R
C21 C 0.64931(10) 0.21161(14) 0.52386(9) 0.0300(4) Uani 1 1 d .
C22 C 0.60916(14) 0.19070(19) 0.61989(11) 0.0537(7) Uani 1 1 d .
H22A H 0.5751 0.1460 0.6017 0.081 Uiso 1 1 calc R
H22B H 0.5913 0.2244 0.6520 0.081 Uiso 1 1 calc R
H22C H 0.6533 0.1631 0.6405 0.081 Uiso 1 1 calc R
C23 C 0.65041(10) 0.51355(12) 0.30155(9) 0.0267(4) Uani 1 1 d .
H23A H 0.6759 0.5428 0.2720 0.032 Uiso 1 1 calc R
H23B H 0.6625 0.5431 0.3439 0.032 Uiso 1 1 calc R
C24 C 0.57275(10) 0.52107(11) 0.27487(8) 0.0246(4) Uani 1 1 d .
C25 C 0.52562(10) 0.52288(13) 0.31605(8) 0.0271(4) Uani 1 1 d .
C26 C 0.45427(10) 0.52256(12) 0.29154(9) 0.0272(4) Uani 1 1 d .
H26 H 0.4232 0.5234 0.3204 0.033 Uiso 1 1 calc R
C27 C 0.50995(14) 0.5302(3) 0.42467(10) 0.0722(10) Uani 1 1 d .
H27A H 0.4776 0.4810 0.4182 0.108 Uiso 1 1 calc R
H27B H 0.4834 0.5844 0.4168 0.108 Uiso 1 1 calc R
H27C H 0.5373 0.5297 0.4691 0.108 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C4 O1 C8 117.60(17) . .
C7 O2 C9 117.28(17) . .
C13 O3 C17 118.32(15) . .
C18 O5 C19 114.94(17) . .
C16 O6 C20 116.91(15) . .
C21 O8 C22 116.70(19) . .
C25 O9 C27 117.50(17) . .
C2 C1 C2 110.5(2) . 2_655
C2 C1 H1A 109.6 . .
C2 C1 H1A 109.6 2_655 .
C2 C1 H1B 109.6 . .
C2 C1 H1B 109.6 2_655 .
H1A C1 H1B 108.1 . .
C7 C2 C3 118.29(17) . .
C7 C2 C1 121.89(15) . .
C3 C2 C1 119.65(15) . .
C4 C3 C2 121.28(18) . .
C4 C3 H3 119.4 . .
C2 C3 H3 119.4 . .
O1 C4 C3 123.79(17) . .
O1 C4 C5 115.55(17) . .
C3 C4 C5 120.64(17) . .
C6 C5 C4 118.19(17) . .
C6 C5 C10 121.09(17) . .
C4 C5 C10 120.72(16) . .
C5 C6 C7 120.90(17) . .
C5 C6 H6 119.5 . .
C7 C6 H6 119.5 . .
O2 C7 C2 115.66(17) . .
O2 C7 C6 123.64(17) . .
C2 C7 C6 120.69(17) . .
O1 C8 H8A 109.5 . .
O1 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
O1 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
O2 C9 H9A 109.5 . .
O2 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
O2 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C11 C10 C5 113.15(15) . .
C11 C10 H10A 108.9 . .
C5 C10 H10A 108.9 . .
C11 C10 H10B 108.9 . .
C5 C10 H10B 108.9 . .
H10A C10 H10B 107.8 . .
C16 C11 C12 117.78(17) . .
C16 C11 C10 121.26(16) . .
C12 C11 C10 120.96(16) . .
C13 C12 C11 121.09(17) . .
C13 C12 H12 119.5 . .
C11 C12 H12 119.5 . .
O3 C13 C12 124.21(16) . .
O3 C13 C14 114.93(17) . .
C12 C13 C14 120.82(16) . .
C13 C14 C15 118.14(17) . .
C13 C14 C23 121.18(16) . .
C15 C14 C23 120.66(16) . .
C16 C15 C14 120.85(17) . .
C16 C15 H15 119.6 . .
C14 C15 H15 119.6 . .
C15 C16 O6 123.31(16) . .
C15 C16 C11 121.27(16) . .
O6 C16 C11 115.41(16) . .
O3 C17 C18 108.14(16) . .
O3 C17 H17A 110.1 . .
C18 C17 H17A 110.1 . .
O3 C17 H17B 110.1 . .
C18 C17 H17B 110.1 . .
H17A C17 H17B 108.4 . .
O4 C18 O5 124.68(18) . .
O4 C18 C17 126.20(17) . .
O5 C18 C17 109.11(16) . .
O5 C19 H19A 109.5 . .
O5 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
O5 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O6 C20 C21 107.58(16) . .
O6 C20 H20A 110.2 . .
C21 C20 H20A 110.2 . .
O6 C20 H20B 110.2 . .
C21 C20 H20B 110.2 . .
H20A C20 H20B 108.5 . .
O7 C21 O8 124.26(18) . .
O7 C21 C20 126.36(18) . .
O8 C21 C20 109.38(17) . .
O8 C22 H22A 109.5 . .
O8 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
O8 C22 H22C 109.5 . .
H22A C22 H22C 109.5 . .
H22B C22 H22C 109.5 . .
C14 C23 C24 111.33(15) . .
C14 C23 H23A 109.4 . .
C24 C23 H23A 109.4 . .
C14 C23 H23B 109.4 . .
C24 C23 H23B 109.4 . .
H23A C23 H23B 108.0 . .
C26 C24 C25 118.06(17) 2_655 .
C26 C24 C23 121.00(16) 2_655 .
C25 C24 C23 120.88(16) . .
O9 C25 C26 123.62(16) . .
O9 C25 C24 115.48(17) . .
C26 C25 C24 120.89(17) . .
C25 C26 C24 121.00(17) . 2_655
C25 C26 H26 119.5 . .
C24 C26 H26 119.5 2_655 .
O9 C27 H27A 109.5 . .
O9 C27 H27B 109.5 . .
H27A C27 H27B 109.5 . .
O9 C27 H27C 109.5 . .
H27A C27 H27C 109.5 . .
H27B C27 H27C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C4 1.379(2) .
O1 C8 1.412(3) .
O2 C7 1.389(2) .
O2 C9 1.414(3) .
O3 C13 1.381(2) .
O3 C17 1.403(2) .
O4 C18 1.195(2) .
O5 C18 1.331(2) .
O5 C19 1.445(3) .
O6 C16 1.390(2) .
O6 C20 1.407(2) .
O7 C21 1.203(3) .
O8 C21 1.333(2) .
O8 C22 1.433(3) .
O9 C25 1.381(2) .
O9 C27 1.413(3) .
C1 C2 1.517(2) .
C1 C2 1.517(2) 2_655
C1 H1A 0.9900 .
C1 H1B 0.9900 .
C2 C7 1.391(3) .
C2 C3 1.391(3) .
C3 C4 1.384(3) .
C3 H3 0.9500 .
C4 C5 1.399(3) .
C5 C6 1.391(3) .
C5 C10 1.518(3) .
C6 C7 1.395(3) .
C6 H6 0.9500 .
C8 H8A 0.9800 .
C8 H8B 0.9800 .
C8 H8C 0.9800 .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.515(3) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C16 1.392(3) .
C11 C12 1.396(3) .
C12 C13 1.392(3) .
C12 H12 0.9500 .
C13 C14 1.393(3) .
C14 C15 1.395(3) .
C14 C23 1.509(3) .
C15 C16 1.388(3) .
C15 H15 0.9500 .
C17 C18 1.504(3) .
C17 H17A 0.9900 .
C17 H17B 0.9900 .
C19 H19A 0.9800 .
C19 H19B 0.9800 .
C19 H19C 0.9800 .
C20 C21 1.509(3) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
C22 H22C 0.9800 .
C23 C24 1.510(3) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C26 1.395(3) 2_655
C24 C25 1.399(3) .
C25 C26 1.384(3) .
C26 C24 1.395(3) 2_655
C26 H26 0.9500 .
C27 H27A 0.9800 .
C27 H27B 0.9800 .
C27 H27C 0.9800 .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.410 0.250 0.358 919 360 ' '
2 0.087 0.750 0.142 919 360 ' '
