#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/04/7220438.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_7220438
loop_
_publ_author_name
'Morohashi, Naoya'
'Nanbu, Kazuki'
'Tonosaki, Ayano'
'Noji, Shintaro'
'Hattori, Tetsutaro'
_publ_section_title
;
 Comparison of inclusion properties between p-tert-butylcalix[4]arene and
 p-tert-butylthiacalix[4]arene towards primary alcohols in crystals
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4799
_journal_paper_doi               10.1039/C5CE00370A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_sum            'C42 H54 O5 S4'
_chemical_formula_weight         767.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           129
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a 2a'
_symmetry_space_group_name_H-M   'P 4/n m m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-04-23 deposited with the CCDC.
2015-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.8115(11)
_cell_length_b                   15.8115(11)
_cell_length_c                   8.2875(12)
_cell_measurement_reflns_used    4483
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.73
_cell_measurement_theta_min      2.46
_cell_volume                     2071.9(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita,Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayered confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            11205
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.520846
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.930
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1341
_refine_ls_number_restraints     124
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0962
_refine_ls_R_factor_gt           0.0864
_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)+(0.1526P)²+2.0350P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2301
_refine_ls_wR_factor_ref         0.2557
_reflns_number_gt                1107
_reflns_number_total             1341
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce00370a2.cif
_cod_data_source_block           2-EtOH
_cod_depositor_comments
'Adding full bibliography for 7220433--7220440.cif.'
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               7220438
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'-y, -x, -z'
'y+1/2, x+1/2, -z'
'y, -x+1/2, z'
'-y+1/2, x, z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z'
'x, -y-1/2, z'
'y, x, z'
'-y-1/2, -x-1/2, z'
'-y, x-1/2, -z'
'y-1/2, -x, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4248(2) 0.2500 1.1998(5) 0.0425(9) Uani 1 2 d S . .
C2 C 0.44900(18) 0.17374(19) 1.1276(4) 0.0451(7) Uani 1 1 d . . .
C3 C 0.4921(2) 0.1750(2) 0.9825(4) 0.0534(8) Uani 1 1 d . . .
H1 H 0.5078 0.1239 0.9354 0.064 Uiso 1 1 calc R . .
C4 C 0.5126(3) 0.2500 0.9046(6) 0.0585(12) Uani 1 2 d S . .
C5 C 0.5577(4) 0.2500 0.7403(8) 0.0859(17) Uani 1 2 d SDU . .
C6A C 0.5224(5) 0.1757(4) 0.6302(7) 0.0926(19) Uani 0.75 1 d PDU A 1
H3 H 0.5510 0.1763 0.5281 0.139 Uiso 0.75 1 calc PR A 1
H4 H 0.4628 0.1834 0.6135 0.139 Uiso 0.75 1 calc PR A 1
H5 H 0.5320 0.1224 0.6827 0.139 Uiso 0.75 1 calc PR A 1
C6B C 0.6167(15) 0.1702(11) 0.720(3) 0.103(5) Uani 0.25 1 d PDU A 2
H6 H 0.6438 0.1722 0.6163 0.154 Uiso 0.25 1 calc PR A 2
H7 H 0.5833 0.1197 0.7277 0.154 Uiso 0.25 1 calc PR A 2
H8 H 0.6588 0.1702 0.8032 0.154 Uiso 0.25 1 calc PR A 2
C7A C 0.6563(7) 0.2500 0.758(3) 0.121(5) Uani 0.50 2 d SPDU A 1
H9 H 0.6817 0.2500 0.6524 0.182 Uiso 0.50 2 calc SPR A 1
H10 H 0.6739 0.2004 0.8155 0.182 Uiso 0.25 1 calc PR A 1
H11 H 0.6739 0.2996 0.8155 0.182 Uiso 0.25 1 calc PR A 1
C7B C 0.6421(7) 0.3039(10) 0.7676(19) 0.064(3) Uani 0.25 1 d PDU A 2
H12 H 0.6736 0.3063 0.6686 0.096 Uiso 0.25 1 calc PR A 2
H13 H 0.6760 0.2774 0.8495 0.096 Uiso 0.25 1 calc PR A 2
H14 H 0.6275 0.3601 0.8010 0.096 Uiso 0.25 1 calc PR A 2
C9 C 0.2500 0.2500 0.907(3) 0.154(7) Uani 1 8 d SDU . .
C8 C 0.3050(19) 0.2500 0.757(3) 0.180(7) Uani 0.25 2 d SPDU . .
O2 O 0.2500 0.2500 0.624(3) 0.210(7) Uani 1 8 d SDU . .
O1 O 0.3782(2) 0.2500 1.3375(4) 0.0502(8) Uani 1 2 d S . .
H2 H 0.359(4) 0.214(4) 1.371(8) 0.036(17) Uiso 0.50 1 d P . .
S1 S 0.42428(5) 0.07572(5) 1.22254(17) 0.0517(5) Uani 1 2 d S . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
O1 C1 C2 120.51(19) . .
O1 C1 C2 120.51(19) . 12_565
C2 C1 C2 119.0(4) . 12_565
C3 C2 C1 119.7(3) . .
C3 C2 S1 120.3(2) . .
C1 C2 S1 120.0(3) . .
C2 C3 C4 122.1(3) . .
C2 C3 H1 119.0 . .
C4 C3 H1 119.0 . .
C3 C4 C3 117.3(4) . 12_565
C3 C4 C5 121.3(2) . .
C3 C4 C5 121.3(2) 12_565 .
C4 C5 C7A 112.4(9) . .
C4 C5 C6B 111.7(9) . 12_565
C7A C5 C6B 54.7(11) . 12_565
C4 C5 C6B 111.7(9) . .
C7A C5 C6B 54.7(11) . .
C6B C5 C6B 106(2) 12_565 .
C4 C5 C6A 110.2(4) . .
C7A C5 C6A 113.7(6) . .
C6B C5 C6A 137.5(10) 12_565 .
C6B C5 C6A 63.5(11) . .
C4 C5 C6A 110.2(4) . 12_565
C7A C5 C6A 113.7(6) . 12_565
C6B C5 C6A 63.5(11) 12_565 12_565
C6B C5 C6A 137.5(10) . 12_565
C6A C5 C6A 95.4(6) . 12_565
C4 C5 C7B 105.2(7) . .
C7A C5 C7B 32.4(6) . .
C6B C5 C7B 25.4(10) 12_565 .
C6B C5 C7B 87.0(14) . .
C6A C5 C7B 140.2(8) . .
C6A C5 C7B 88.9(7) 12_565 .
C4 C5 C7B 105.2(7) . 12_565
C7A C5 C7B 32.4(6) . 12_565
C6B C5 C7B 87.0(14) 12_565 12_565
C6B C5 C7B 25.4(10) . 12_565
C6A C5 C7B 88.9(7) . 12_565
C6A C5 C7B 140.2(8) 12_565 12_565
C7B C5 C7B 64.3(12) . 12_565
C5 C6A H3 109.5 . .
C5 C6A H4 109.5 . .
H3 C6A H4 109.5 . .
C5 C6A H5 109.5 . .
H3 C6A H5 109.5 . .
H4 C6A H5 109.5 . .
C5 C6B H6 109.5 . .
C5 C6B H7 109.5 . .
H6 C6B H7 109.5 . .
C5 C6B H8 109.5 . .
H6 C6B H8 109.5 . .
H7 C6B H8 109.5 . .
C5 C7A H9 109.5 . .
C5 C7A H10 109.5 . .
H9 C7A H10 109.5 . .
C5 C7A H11 109.5 . .
H9 C7A H11 109.5 . .
H10 C7A H11 109.5 . .
C5 C7B H12 109.5 . .
C5 C7B H13 109.5 . .
H12 C7B H13 109.5 . .
C5 C7B H14 109.5 . .
H12 C7B H14 109.5 . .
H13 C7B H14 109.5 . .
C8 C9 C8 70(2) 13 14_665
C8 C9 C8 47.9(15) 13 .
C8 C9 C8 47.9(15) 14_665 .
C8 C9 C8 47.9(15) 13 2
C8 C9 C8 47.9(15) 14_665 2
C8 C9 C8 70(2) . 2
C8 C8 C8 89.998(11) 13 14_665
C8 C8 O2 64.1(8) 13 .
C8 C8 O2 64.1(8) 14_665 .
C8 C8 C9 66.1(8) 13 .
C8 C8 C9 66.1(8) 14_665 .
O2 C8 C9 107(2) . .
C8 C8 C8 44.997(12) 13 2
C8 C8 C8 45.001(8) 14_665 2
O2 C8 C8 51.8(13) . 2
C9 C8 C8 55.0(12) . 2
C8 O2 C8 51.8(16) 13 .
C8 O2 C8 76(3) 13 14_665
C8 O2 C8 51.8(16) . 14_665
C8 O2 C8 51.8(16) 13 2
C8 O2 C8 76(3) . 2
C8 O2 C8 51.8(16) 14_665 2
C1 O1 H2 125(6) . .
C2 S1 C2 100.77(19) . 14_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.358(5) .
C1 C2 1.400(4) .
C1 C2 1.400(4) 12_565
C2 C3 1.382(4) .
C2 S1 1.781(3) .
C3 C4 1.389(4) .
C3 H1 0.9300 .
C4 C3 1.389(4) 12_565
C4 C5 1.537(8) .
C5 C7A 1.566(9) .
C5 C6B 1.578(9) 12_565
C5 C6B 1.578(9) .
C5 C6A 1.589(7) .
C5 C6A 1.590(7) 12_565
C5 C7B 1.600(8) .
C5 C7B 1.600(8) 12_565
C6A H3 0.9600 .
C6A H4 0.9600 .
C6A H5 0.9600 .
C6B H6 0.9600 .
C6B H7 0.9600 .
C6B H8 0.9600 .
C7A H9 0.9600 .
C7A H10 0.9600 .
C7A H11 0.9600 .
C7B H12 0.9600 .
C7B H13 0.9600 .
C7B H14 0.9600 .
C9 C8 1.51(2) 13
C9 C8 1.51(2) 14_665
C9 C8 1.52(2) .
C9 C8 1.52(2) 2
C8 C8 1.23(4) 13
C8 C8 1.23(4) 14_665
C8 O2 1.41(2) .
C8 C8 1.74(6) 2
O2 C8 1.41(2) 13
O2 C8 1.41(2) 14_665
O2 C8 1.41(2) 2
O1 H2 0.70(6) .
S1 C2 1.781(3) 14_665
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
O1 C1 C2 C3 176.1(3) . .
C2 C1 C2 C3 -3.6(5) 12_565 .
O1 C1 C2 S1 -3.8(5) . .
C2 C1 C2 S1 176.46(18) 12_565 .
C1 C2 C3 C4 0.1(5) . .
S1 C2 C3 C4 -180.0(3) . .
C2 C3 C4 C3 3.3(7) . 12_565
C2 C3 C4 C5 -177.8(4) . .
C3 C4 C5 C7A -89.4(4) . .
C3 C4 C5 C7A 89.4(4) 12_565 .
C3 C4 C5 C6B -148.8(12) . 12_565
C3 C4 C5 C6B 30.0(13) 12_565 12_565
C3 C4 C5 C6B -30.0(13) . .
C3 C4 C5 C6B 148.8(12) 12_565 .
C3 C4 C5 C6A 38.6(7) . .
C3 C4 C5 C6A -142.6(4) 12_565 .
C3 C4 C5 C6A 142.6(4) . 12_565
C3 C4 C5 C6A -38.6(7) 12_565 12_565
C3 C4 C5 C7B -122.9(7) . .
C3 C4 C5 C7B 55.9(8) 12_565 .
C3 C4 C5 C7B -55.9(8) . 12_565
C3 C4 C5 C7B 122.9(7) 12_565 12_565
C8 C9 C8 C8 101.4(8) 14_665 13
C8 C9 C8 C8 50.7(4) 2 13
C8 C9 C8 C8 -101.4(8) 13 14_665
C8 C9 C8 C8 -50.7(4) 2 14_665
C8 C9 C8 O2 -50.7(4) 13 .
C8 C9 C8 O2 50.7(4) 14_665 .
C8 C9 C8 O2 -0.002(4) 2 .
C8 C9 C8 C8 -50.7(4) 13 2
C8 C9 C8 C8 50.7(4) 14_665 2
C8 C8 O2 C8 103.7(10) 14_665 13
C9 C8 O2 C8 51.8(5) . 13
C8 C8 O2 C8 51.8(5) 2 13
C8 C8 O2 C8 -103.7(10) 13 14_665
C9 C8 O2 C8 -51.8(5) . 14_665
C8 C8 O2 C8 -51.8(5) 2 14_665
C8 C8 O2 C8 -51.8(5) 13 2
C8 C8 O2 C8 51.8(5) 14_665 2
C9 C8 O2 C8 0.002(7) . 2
C3 C2 S1 C2 -86.8(3) . 14_665
C1 C2 S1 C2 93.1(3) . 14_665
