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#$Date: 2016-03-22 11:58:54 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178927 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/56/4115621.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_4115621
loop_
_publ_author_name
'Jerry L. Atwood'
'Leonard J. Barbour'
'Timothy J. Ness'
'Colin L. Raston'
'Paul L. Raston'
_publ_section_title
;
 A Well-Resolved Ice-like (H2O)8 Cluster in an Organic Supramolecular
 Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7192
_journal_page_last               7193
_journal_paper_doi               10.1021/ja015757k
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C38 H60 O16'
_chemical_formula_weight         772.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           137
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4ac 2a'
_symmetry_space_group_name_H-M   'P 42/n m c :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.2553(7)
_cell_length_b                   16.2553(7)
_cell_length_c                   15.0336(10)
_cell_measurement_temperature    173(2)
_cell_volume                     3972.4(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0433
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23815
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.9803
_exptl_absorpt_correction_T_min  0.9610
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2363
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0840
_refine_ls_R_factor_gt           0.0441
_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)+(0.0756P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                1489
_reflns_number_total             2363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja015757k_x4a.cif
_cod_data_source_block           d:\xray\people\paul\x4a
_cod_original_sg_symbol_H-M      'P 42/n m c'
_cod_database_code               4115621
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z+1/2'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z+1/2'
'x+1/2, -y, -z'
'-x, y+1/2, -z'
'y+1/2, x+1/2, -z+1/2'
'-y, -x, -z+1/2'
'-x, -y, -z'
'y-1/2, -x, -z-1/2'
'x-1/2, y-1/2, -z'
'-y, x-1/2, -z-1/2'
'-x-1/2, y, z'
'x, -y-1/2, z'
'-y-1/2, -x-1/2, z-1/2'
'y, x, 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
O1A O 0.60373(7) 0.46998(8) 0.09863(9) 0.0313(3) Uani 1 1 d D
C2A C 0.7500 0.46929(15) 0.09458(16) 0.0252(6) Uani 1 2 d S
H2A H 0.7500 0.4285 0.1398 0.030 Uiso 1 2 calc SR
O1B O 0.50814(8) 0.60404(7) 0.12608(9) 0.0363(4) Uani 1 1 d D
C1B C 0.53064(10) 0.67638(10) 0.08418(11) 0.0245(4) Uani 1 1 d .
C3B C 0.57203(9) 0.67427(10) 0.00311(10) 0.0196(4) Uani 1 1 d .
C1A C 0.67614(10) 0.49867(10) 0.06206(10) 0.0220(4) Uani 1 1 d .
C4B C 0.59237(13) 0.7500 -0.03479(15) 0.0192(5) Uani 1 2 d S
H4B H 0.6217 0.7500 -0.0894 0.023 Uiso 1 2 calc SR
C2B C 0.51055(15) 0.7500 0.12443(16) 0.0286(6) Uani 1 2 d S
H2B H 0.4828 0.7500 0.1800 0.034 Uiso 1 2 calc SR
C5A C 0.59325(10) 0.59244(10) -0.04109(10) 0.0191(4) Uani 1 1 d .
H5A H 0.5492 0.5526 -0.0237 0.023 Uiso 1 1 calc R
C3A C 0.67425(9) 0.55787(9) -0.00562(10) 0.0191(4) Uani 1 1 d .
C4A C 0.7500 0.58610(13) -0.03687(14) 0.0182(5) Uani 1 2 d S
H4A H 0.7500 0.6269 -0.0821 0.022 Uiso 1 2 calc SR
C6A C 0.59267(10) 0.59699(10) -0.14286(11) 0.0236(4) Uani 1 1 d .
H6A3 H 0.5397 0.6188 -0.1631 0.035 Uiso 1 1 calc R
H6A1 H 0.6009 0.5418 -0.1675 0.035 Uiso 1 1 calc R
H6A2 H 0.6370 0.6333 -0.1630 0.035 Uiso 1 1 calc R
O1E O 0.38788(8) 0.61212(8) 0.2500 0.0315(4) Uani 1 2 d SD
O1D O 0.2500 0.2500 0.19065(16) 0.0305(6) Uani 1 4 d S
C2D C 0.2500 0.2500 0.2711(2) 0.0323(9) Uani 1 4 d S
C1D C 0.1718(3) 0.2500 0.3220(2) 0.0720(12) Uani 1 2 d S
H1D3 H 0.1281 0.2742 0.2855 0.108 Uiso 0.50 1 calc PR
H1D2 H 0.1787 0.2824 0.3764 0.108 Uiso 0.50 1 calc PR
H1D1 H 0.1571 0.1934 0.3376 0.108 Uiso 0.50 1 calc PR
O1F O 0.2500 0.60009(13) 0.14532(13) 0.0431(5) Uani 1 2 d SD
O1G O 0.62570(9) 0.37430(9) 0.2500 0.0665(7) Uani 1 2 d SD
C2C C 0.7500 0.2500 0.0756(3) 0.0449(11) Uani 1 4 d S
C1C C 0.6717(2) 0.2500 0.0242(2) 0.0603(9) Uani 1 2 d S
H1C3 H 0.6768 0.2128 -0.0268 0.090 Uiso 0.50 1 calc PR
H1C2 H 0.6601 0.3058 0.0031 0.090 Uiso 0.50 1 calc PR
H1C1 H 0.6267 0.2314 0.0626 0.090 Uiso 0.50 1 calc PR
O1C O 0.7500 0.2500 0.15671(19) 0.0626(10) Uani 1 4 d S
H1B H 0.548(2) 0.5624(15) 0.112(3) 0.158(16) Uiso 1 1 d D
H1E H 0.429(2) 0.610(3) 0.205(2) 0.194(19) Uiso 1 1 d D
H1F H 0.3025(18) 0.600(3) 0.185(3) 0.21(2) Uiso 1 1 d D
H1A H 0.607(3) 0.429(2) 0.1403(19) 0.199(19) Uiso 1 1 d D
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'
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
C1A C2A C1A 120.7(2) 13_755 .
C2B C1B O1B 118.35(15) . .
C2B C1B C3B 121.29(16) . .
O1B C1B C3B 120.36(15) . .
C1B C3B C4B 116.74(16) . .
C1B C3B C5A 120.77(14) . .
C4B C3B C5A 122.49(15) . .
O1A C1A C2A 118.91(15) . .
O1A C1A C3A 120.19(14) . .
C2A C1A C3A 120.90(16) . .
C3B C4B C3B 123.7(2) . 14_575
C1B C2B C1B 120.2(2) . 14_575
C3B C5A C3A 111.31(13) . .
C3B C5A C6A 113.04(13) . .
C3A C5A C6A 111.82(13) . .
C4A C3A C1A 116.82(15) . .
C4A C3A C5A 121.46(15) . .
C1A C3A C5A 121.67(13) . .
C3A C4A C3A 123.8(2) 13_755 .
O1D C2D C1D 121.0(2) . 3
O1D C2D C1D 121.0(2) . .
C1D C2D C1D 117.9(4) 3 .
O1C C2C C1C 121.23(19) . .
O1C C2C C1C 121.23(19) . 3_655
C1C C2C C1C 117.5(4) . 3_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1A C1A 1.3802(19) .
C2A C1A 1.382(2) 13_755
C2A C1A 1.382(2) .
O1B C1B 1.3832(19) .
C1B C2B 1.380(2) .
C1B C3B 1.393(2) .
C3B C4B 1.3962(18) .
C3B C5A 1.526(2) .
C1A C3A 1.401(2) .
C4B C3B 1.3962(18) 14_575
C2B C1B 1.380(2) 14_575
C5A C3A 1.528(2) .
C5A C6A 1.532(2) .
C3A C4A 1.3955(18) .
C4A C3A 1.3955(18) 13_755
O1D C2D 1.210(4) .
C2D C1D 1.483(4) 3
C2D C1D 1.483(4) .
C2C O1C 1.220(4) .
C2C C1C 1.488(4) .
C2C C1C 1.488(4) 3_655
