#------------------------------------------------------------------------------
#$Date: 2024-11-16 00:24:31 +0200 (Sat, 16 Nov 2024) $
#$Revision: 295947 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/50/59/1505913.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_1505913
loop_
_publ_author_name
'Sawada, Tsuyoshi'
'Nishiyama, Yousuke'
'Tabuchi, Wataru'
'Ishikawa, Makoto'
'Tsutsumi, Emi'
'Kuwahara, Yutaka'
'Shosenji, Hideto'
_publ_section_title
;
 Novel calixarene hemisphere synthesized via pinacol rearrangement of
 [2.1.2.1]metacyclophane.
;
_journal_issue                   10
_journal_name_full               'Organic letters'
_journal_page_first              1995
_journal_page_last               1997
_journal_paper_doi               10.1021/ol060286y
_journal_volume                  8
_journal_year                    2006
_chemical_formula_moiety         'C56 H76 O8 '
_chemical_formula_sum            'C56 H76 O8'
_chemical_formula_weight         877.21
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                97.61(3)
_cell_angle_beta                 99.46(3)
_cell_angle_gamma                92.88(3)
_cell_formula_units_Z            1
_cell_length_a                   10.585(4)
_cell_length_b                   12.668(4)
_cell_length_c                   9.841(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298.1
_cell_measurement_theta_max      17.3
_cell_measurement_theta_min      15.4
_cell_volume                     1286.7(8)
_computing_cell_refinement       WinAFC
_computing_data_collection       WinAFC
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9990
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7146
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_standards_decay_%        0.66
_diffrn_standards_interval_count 0
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.918
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             476.00
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.28
_refine_diff_density_min         -0.25
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5902
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.1070P)²+0.1936P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2260
_reflns_number_gt                3000
_reflns_number_total             5902
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            ol060286ysi20060202_101212.cif
_cod_data_source_block           '_bisketal3'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_formula_sum        'C56 H76 O8 '
_cod_database_code               1505913
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
O1 O 0.68934(17) 0.09579(16) 0.7521(2) 0.0562(5) Uani 1 1 d . . .
O2 O 0.39397(17) 0.19197(16) 0.4411(2) 0.0534(5) Uani 1 1 d . . .
O3 O 0.60282(19) 0.38583(14) 0.85371(19) 0.0524(5) Uani 1 1 d . . .
O4 O 0.6101(2) 0.46609(15) 0.6599(2) 0.0617(6) Uani 1 1 d . . .
C1 C 0.5437(3) -0.0852(2) 0.8131(3) 0.0489(7) Uani 1 1 d . . .
H1A H 0.6294 -0.0837 0.7902 0.073 Uiso 1 1 calc R . .
H1B H 0.5516 -0.0925 0.9109 0.073 Uiso 1 1 calc R . .
C2 C 0.4875(2) 0.0210(2) 0.7905(3) 0.0431(6) Uani 1 1 d . . .
C3 C 0.3604(3) 0.0360(2) 0.8016(3) 0.0474(6) Uani 1 1 d . . .
H3 H 0.3088 -0.0220 0.8152 0.071 Uiso 1 1 calc R . .
C4 C 0.3056(3) 0.1337(2) 0.7937(3) 0.0465(6) Uani 1 1 d . A .
C5 C 0.3858(3) 0.2189(2) 0.7755(3) 0.0485(7) Uani 1 1 d . . .
H5 H 0.3532 0.2856 0.7734 0.073 Uiso 1 1 calc R . .
C6 C 0.5133(3) 0.2080(2) 0.7604(3) 0.0457(6) Uani 1 1 d . . .
C7 C 0.5625(2) 0.1085(2) 0.7658(3) 0.0448(6) Uani 1 1 d . . .
C8 C 0.5956(3) 0.3024(2) 0.7378(3) 0.0478(6) Uani 1 1 d . . .
H8 H 0.6822 0.2807 0.7307 0.072 Uiso 1 1 calc R . .
C9 C 0.5468(3) 0.3614(2) 0.6155(3) 0.0495(7) Uani 1 1 d . . .
H9 H 0.4537 0.3655 0.6067 0.074 Uiso 1 1 calc R . .
C10 C 0.5797(3) 0.3151(2) 0.4776(3) 0.0477(6) Uani 1 1 d . . .
C11 C 0.6896(3) 0.3504(2) 0.4347(3) 0.0523(7) Uani 1 1 d . . .
H11 H 0.7433 0.4049 0.4914 0.078 Uiso 1 1 calc R . .
C12 C 0.7228(3) 0.3070(2) 0.3083(3) 0.0508(7) Uani 1 1 d . . .
C13 C 0.6434(3) 0.2242(2) 0.2289(3) 0.0486(7) Uani 1 1 d . . .
H13 H 0.6630 0.1954 0.1436 0.073 Uiso 1 1 calc R . .
C14 C 0.5343(3) 0.1818(2) 0.2717(3) 0.0449(6) Uani 1 1 d . . .
C15 C 0.5025(2) 0.2307(2) 0.3954(3) 0.0460(6) Uani 1 1 d . . .
C16 C 0.1647(3) 0.1431(2) 0.8049(3) 0.0582(8) Uani 1 1 d . . .
C17A C 0.1180(5) 0.2522(5) 0.7844(8) 0.092(3) Uani 0.704(9) 1 d P A 1
H17A H 0.1437 0.2734 0.7022 0.138 Uiso 0.704(9) 1 calc PR A 1
H17B H 0.1548 0.3034 0.8637 0.138 Uiso 0.704(9) 1 calc PR A 1
H17C H 0.0261 0.2489 0.7742 0.138 Uiso 0.704(9) 1 calc PR A 1
C18A C 0.1425(6) 0.1180(8) 0.9467(8) 0.112(3) Uani 0.704(9) 1 d P A 1
H18A H 0.1528 0.0437 0.9518 0.169 Uiso 0.704(9) 1 calc PR A 1
H18B H 0.0571 0.1340 0.9592 0.169 Uiso 0.704(9) 1 calc PR A 1
H18C H 0.2037 0.1606 1.0184 0.169 Uiso 0.704(9) 1 calc PR A 1
C19A C 0.0855(5) 0.0607(6) 0.6902(11) 0.125(4) Uani 0.704(9) 1 d P A 1
H19A H 0.1271 -0.0050 0.6847 0.187 Uiso 0.704(9) 1 calc PR A 1
H19B H 0.0785 0.0873 0.6026 0.187 Uiso 0.704(9) 1 calc PR A 1
H19C H 0.0012 0.0481 0.7117 0.187 Uiso 0.704(9) 1 calc PR A 1
C18B C 0.1573(14) 0.2314(15) 0.9267(19) 0.103(7) Uani 0.296(9) 1 d P A 2
H18D H 0.0691 0.2388 0.9357 0.134 Uiso 0.296(9) 1 calc PR A 2
H18E H 0.1945 0.2978 0.9088 0.134 Uiso 0.296(9) 1 calc PR A 2
H18F H 0.2037 0.2126 1.0113 0.134 Uiso 0.296(9) 1 calc PR A 2
C17B C 0.0925(11) 0.1801(13) 0.6739(17) 0.085(5) Uani 0.296(9) 1 d P A 2
H17D H 0.0039 0.1858 0.6821 0.110 Uiso 0.296(9) 1 calc PR A 2
H17E H 0.0985 0.1293 0.5941 0.110 Uiso 0.296(9) 1 calc PR A 2
H17F H 0.1298 0.2485 0.6632 0.110 Uiso 0.296(9) 1 calc PR A 2
C19B C 0.0892(13) 0.0388(13) 0.828(2) 0.103(7) Uani 0.296(9) 1 d P A 2
H19D H 0.0019 0.0531 0.8341 0.134 Uiso 0.296(9) 1 calc PR A 2
H19E H 0.1290 0.0161 0.9135 0.134 Uiso 0.296(9) 1 calc PR A 2
H19F H 0.0906 -0.0166 0.7521 0.134 Uiso 0.296(9) 1 calc PR A 2
C20 C 0.7052(3) 0.0661(3) 0.6100(4) 0.0703(9) Uani 1 1 d . . .
H20A H 0.7945 0.0584 0.6065 0.106 Uiso 1 1 calc R . .
H20B H 0.6752 0.1205 0.5560 0.106 Uiso 1 1 calc R . .
H20C H 0.6567 -0.0004 0.5726 0.106 Uiso 1 1 calc R . .
C21 C 0.8462(3) 0.3518(3) 0.2647(3) 0.0597(8) Uani 1 1 d . . .
C22 C 0.9603(3) 0.3369(4) 0.3736(5) 0.1073(16) Uani 1 1 d . . .
H22A H 0.9663 0.2622 0.3791 0.161 Uiso 1 1 calc R . .
H22B H 0.9495 0.3734 0.4624 0.161 Uiso 1 1 calc R . .
H22C H 1.0374 0.3657 0.3484 0.161 Uiso 1 1 calc R . .
C23 C 0.8372(4) 0.4706(3) 0.2553(5) 0.0871(12) Uani 1 1 d . . .
H23A H 0.8264 0.5075 0.3438 0.131 Uiso 1 1 calc R . .
H23B H 0.7650 0.4800 0.1860 0.131 Uiso 1 1 calc R . .
H23C H 0.9145 0.4990 0.2301 0.131 Uiso 1 1 calc R . .
C24 C 0.8638(4) 0.2979(4) 0.1224(5) 0.0970(14) Uani 1 1 d . . .
H24A H 0.8700 0.2227 0.1243 0.146 Uiso 1 1 calc R . .
H24B H 0.9410 0.3280 0.0988 0.146 Uiso 1 1 calc R . .
H24C H 0.7916 0.3088 0.0541 0.146 Uiso 1 1 calc R . .
C25 C 0.2807(3) 0.2418(3) 0.3920(4) 0.0763(10) Uani 1 1 d . . .
H25A H 0.2095 0.2120 0.4270 0.114 Uiso 1 1 calc R . .
H25B H 0.2636 0.2296 0.2921 0.114 Uiso 1 1 calc R . .
H25C H 0.2929 0.3171 0.4238 0.114 Uiso 1 1 calc R . .
C26 C 0.6443(3) 0.4819(2) 0.8081(3) 0.0503(7) Uani 1 1 d . . .
C27 C 0.5737(3) 0.5710(2) 0.8698(4) 0.0689(9) Uani 1 1 d . . .
H27A H 0.6006 0.6367 0.8408 0.103 Uiso 1 1 calc R . .
H27B H 0.5923 0.5775 0.9695 0.103 Uiso 1 1 calc R . .
H27C H 0.4830 0.5558 0.8386 0.103 Uiso 1 1 calc R . .
C28 C 0.7892(3) 0.5019(3) 0.8444(4) 0.0752(10) Uani 1 1 d . . .
H28A H 0.8150 0.5671 0.8134 0.113 Uiso 1 1 calc R . .
H28B H 0.8288 0.4437 0.7994 0.113 Uiso 1 1 calc R . .
H28C H 0.8154 0.5077 0.9434 0.113 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 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.011 0.006
;
International Tables for Crystallography
(1992, 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
C7 O1 C20 113.0(2) . .
C15 O2 C25 113.4(2) . .
C26 O3 C8 106.49(19) . .
C26 O4 C9 108.8(2) . .
C14 C1 C2 114.3(2) 2_656 .
C3 C2 C7 117.4(2) . .
C3 C2 C1 120.6(2) . .
C7 C2 C1 122.0(2) . .
C2 C3 C4 123.6(2) . .
C5 C4 C3 116.6(2) . .
C5 C4 C16 123.1(3) . .
C3 C4 C16 120.3(2) . .
C4 C5 C6 122.4(3) . .
C7 C6 C5 118.8(2) . .
C7 C6 C8 120.8(2) . .
C5 C6 C8 120.4(2) . .
O1 C7 C6 119.9(2) . .
O1 C7 C2 118.9(2) . .
C6 C7 C2 121.2(2) . .
O3 C8 C6 109.3(2) . .
O3 C8 C9 101.2(2) . .
C6 C8 C9 117.8(2) . .
O4 C9 C10 110.1(2) . .
O4 C9 C8 102.3(2) . .
C10 C9 C8 115.1(2) . .
C11 C10 C15 118.8(2) . .
C11 C10 C9 121.2(2) . .
C15 C10 C9 119.9(2) . .
C10 C11 C12 122.0(3) . .
C13 C12 C11 117.6(3) . .
C13 C12 C21 122.9(3) . .
C11 C12 C21 119.5(3) . .
C12 C13 C14 122.5(3) . .
C15 C14 C13 117.6(2) . .
C15 C14 C1 121.8(2) . 2_656
C13 C14 C1 120.6(2) . 2_656
C10 C15 C14 121.4(2) . .
C10 C15 O2 118.9(2) . .
C14 C15 O2 119.6(2) . .
C17A C16 C18A 109.0(4) . .
C17A C16 C4 113.6(3) . .
C18A C16 C4 109.5(3) . .
C17A C16 C17B 50.7(6) . .
C18A C16 C17B 140.2(6) . .
C4 C16 C17B 110.2(5) . .
C17A C16 C19A 107.7(5) . .
C18A C16 C19A 109.4(6) . .
C4 C16 C19A 107.4(3) . .
C17B C16 C19A 60.4(7) . .
C17A C16 C18B 56.8(8) . .
C18A C16 C18B 57.7(8) . .
C4 C16 C18B 108.0(6) . .
C17B C16 C18B 106.4(10) . .
C19A C16 C18B 144.5(6) . .
C17A C16 C19B 130.2(6) . .
C18A C16 C19B 55.8(8) . .
C4 C16 C19B 116.1(6) . .
C17B C16 C19B 107.4(9) . .
C19A C16 C19B 54.3(8) . .
C18B C16 C19B 108.3(11) . .
C22 C21 C24 110.3(3) . .
C22 C21 C23 109.5(3) . .
C24 C21 C23 107.1(3) . .
C22 C21 C12 108.8(3) . .
C24 C21 C12 112.0(3) . .
C23 C21 C12 109.2(3) . .
O3 C26 O4 106.6(2) . .
O3 C26 C27 108.1(2) . .
O4 C26 C27 110.1(3) . .
O3 C26 C28 110.8(3) . .
O4 C26 C28 107.7(2) . .
C27 C26 C28 113.4(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C7 1.386(3) .
O1 C20 1.439(4) .
O2 C15 1.391(3) .
O2 C25 1.426(4) .
O3 C26 1.425(3) .
O3 C8 1.438(3) .
O4 C26 1.428(3) .
O4 C9 1.435(3) .
C1 C14 1.509(4) 2_656
C1 C2 1.526(4) .
C2 C3 1.388(4) .
C2 C7 1.402(4) .
C3 C4 1.399(4) .
C4 C5 1.387(4) .
C4 C16 1.523(4) .
C5 C6 1.393(4) .
C6 C7 1.392(4) .
C6 C8 1.506(4) .
C8 C9 1.532(4) .
C9 C10 1.508(4) .
C10 C11 1.375(4) .
C10 C15 1.390(4) .
C11 C12 1.398(4) .
C12 C13 1.377(4) .
C12 C21 1.545(4) .
C13 C14 1.399(4) .
C14 C15 1.391(4) .
C14 C1 1.509(4) 2_656
C16 C17A 1.519(6) .
C16 C18A 1.523(7) .
C16 C17B 1.529(14) .
C16 C19A 1.535(7) .
C16 C18B 1.542(14) .
C16 C19B 1.573(13) .
C21 C22 1.514(5) .
C21 C24 1.519(5) .
C21 C23 1.528(5) .
C26 C27 1.502(4) .
C26 C28 1.516(4) .
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Vaitkus, Antanas' 2024-11-16T00:18:53+02:00
;
 Replaced the '\/Y' character sequence with the backslash character ('\')
 in the '_refine_ls_weighting_details' data value.
;
