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#$Date: 2023-11-10 21:21:08 +0200 (Fri, 10 Nov 2023) $
#$Revision: 287519 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/72/4327247.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_4327247
loop_
_publ_author_name
'D. Amilan Jose'
'D. Krishna Kumar'
'Bishwajit Ganguly'
'Amitava Das'
_publ_section_title
;
 Rugby-Ball-Shaped Sulfate-Water-Sulfate Adduct Encapsulated in a Neutral
 Molecular Receptor Capsule
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5817
_journal_page_last               5819
_journal_paper_doi               10.1021/ic062466+
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C25.5 H40.53 N5.75 O7.25 S0.5'
_chemical_formula_weight         559.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   17.230(10)
_cell_length_b                   17.230(10)
_cell_length_c                   39.99(5)
_cell_measurement_temperature    100(2)
_cell_volume                     10281(15)
_computing_cell_refinement       'BRUKER AXS SMART 3'
_computing_data_collection       'BRUKER AXS SMART 3'
_computing_data_reduction        'BRUKER AXS SAINT'
_computing_molecular_graphics    'BRUKER SHELXLTL'
_computing_publication_material  'MERCURY 1.4'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0.3
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'BRUKER SMART CCD AREA DETECTOR'
_diffrn_measurement_method       'PHI-OMEGA SCAN'
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            29554
_diffrn_reflns_theta_full        28.59
_diffrn_reflns_theta_max         28.59
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.9967
_exptl_absorpt_correction_T_min  0.9702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             3597
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.189
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         5532
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0624
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1257P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1633
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                3885
_reflns_number_total             5532
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0624662Bsi20061223_050708_3.cif
_cod_data_source_block           adduct
_cod_original_cell_volume        10282(15)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_original_formula_sum        'C25.50 H40.53 N5.75 O7.25 S0.50'
_cod_database_code               4327247
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
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
S1 S 1.0000 1.0000 0.07400(2) 0.0314(2) Uani 1 3 d S . .
O1S O 0.90802(11) 0.93947(11) 0.06218(4) 0.0367(4) Uani 1 1 d . . .
O2S O 1.0000 1.0000 0.11109(6) 0.0438(7) Uani 1 3 d S . .
O3W O 0.85799(16) 0.85799(16) 0.0000 0.0439(6) Uani 1 2 d S . .
H3W H 0.870(3) 0.885(2) 0.0151(8) 0.071(12) Uiso 1 1 d . . .
N1 N 1.0000 1.0000 0.19726(9) 0.0527(9) Uani 1 3 d S . .
C2 C 0.9066(2) 0.9545(2) 0.20805(6) 0.0581(7) Uani 1 1 d . . .
H2A H 0.9027 0.9753 0.2307 0.055(8) Uiso 1 1 calc R . .
H2B H 0.8835 0.8892 0.2091 0.044(7) Uiso 1 1 calc R . .
C3 C 0.8489(2) 0.9734(2) 0.18385(7) 0.0554(7) Uani 1 1 d . . .
H3A H 0.7883 0.9496 0.1935 0.082(11) Uiso 1 1 calc R . .
H3B H 0.8757 1.0389 0.1811 0.054(8) Uiso 1 1 calc R . .
N4 N 0.84179(17) 0.93300(17) 0.15158(5) 0.0514(6) Uani 1 1 d . . .
H4 H 0.8867 0.9593 0.1374 0.056(9) Uiso 1 1 calc R . .
C5 C 0.7684(2) 0.8563(2) 0.14250(6) 0.0513(7) Uani 1 1 d . . .
O6 O 0.70231(16) 0.81550(15) 0.16050(5) 0.0675(6) Uani 1 1 d . . .
N7 N 0.77248(16) 0.82803(16) 0.11066(5) 0.0533(6) Uani 1 1 d . . .
H7 H 0.8165 0.8667 0.0979 0.048(8) Uiso 1 1 calc R . .
C8 C 0.7144(2) 0.7447(2) 0.09641(7) 0.0544(7) Uani 1 1 d . . .
C9 C 0.6478(2) 0.6716(2) 0.11388(8) 0.0705(10) Uani 1 1 d . . .
H9 H 0.6374 0.6783 0.1367 0.065(9) Uiso 1 1 calc R . .
C10 C 0.5972(2) 0.5903(2) 0.09862(9) 0.0740(10) Uani 1 1 d . . .
H10 H 0.5532 0.5404 0.1109 0.049(8) Uiso 1 1 calc R . .
C11 C 0.6107(2) 0.5818(2) 0.06527(9) 0.0683(10) Uani 1 1 d . . .
C12 C 0.6768(2) 0.6529(2) 0.04725(8) 0.0610(8) Uani 1 1 d . . .
H12 H 0.6864 0.6457 0.0243 0.056(8) Uiso 1 1 calc R . .
C13 C 0.7279(2) 0.73311(19) 0.06270(7) 0.0532(7) Uani 1 1 d . . .
H13 H 0.7733 0.7819 0.0504 0.043(7) Uiso 1 1 calc R . .
N14 N 0.5564(2) 0.4953(2) 0.04876(9) 0.0899(11) Uani 1 1 d . . .
O15 O 0.4968(2) 0.4339(2) 0.06481(8) 0.1093(12) Uani 1 1 d . . .
O16 O 0.5711(3) 0.4875(2) 0.02053(9) 0.1308(16) Uani 1 1 d . . .
N17 N 1.0000 0.71456(17) 0.0000 0.0590(9) Uani 1 2 d S . .
C18 C 0.9754(3) 0.7550(2) 0.02892(9) 0.0623(8) Uani 1 1 d . . .
H18A H 1.0300 0.8099 0.0364 0.075 Uiso 1 1 calc R . .
H18B H 0.9323 0.7729 0.0208 0.075 Uiso 1 1 calc R . .
C19 C 0.9347(3) 0.6934(2) 0.05869(10) 0.0758(10) Uani 1 1 d . . .
H19A H 0.9711 0.6654 0.0644 0.067(10) Uiso 1 1 calc R . .
H19B H 0.8734 0.6451 0.0531 0.047(8) Uiso 1 1 calc R . .
C20 C 0.9314(3) 0.7468(2) 0.08865(9) 0.0759(11) Uani 1 1 d . . .
H20A H 0.9932 0.7893 0.0961 0.15(2) Uiso 1 1 calc R . .
H20B H 0.9030 0.7820 0.0818 0.068(9) Uiso 1 1 calc R . .
C21 C 0.8793(4) 0.6862(3) 0.11743(11) 0.1162(19) Uani 1 1 d . . .
H21A H 0.8218 0.6376 0.1092 0.174 Uiso 1 1 calc R . .
H21B H 0.8685 0.7209 0.1343 0.174 Uiso 1 1 calc R . .
H21C H 0.9138 0.6609 0.1274 0.174 Uiso 1 1 calc R . .
C22 C 0.9237(2) 0.6232(2) -0.00974(10) 0.0701(10) Uani 1 1 d . . .
H13A H 0.9446 0.5995 -0.0281 0.054(8) Uiso 1 1 calc R . .
H13B H 0.9096 0.5825 0.0096 0.068(10) Uiso 1 1 calc R . .
C23 C 0.8382(3) 0.6196(3) -0.02089(19) 0.1085(18) Uani 1 1 d . B .
H23A H 0.8459 0.6449 -0.0437 0.30(6) Uiso 1 1 calc R . .
H23B H 0.8235 0.6555 -0.0056 0.16(2) Uiso 1 1 calc R . .
C24 C 0.7602(4) 0.5192(5) -0.0208(3) 0.199(4) Uani 1 1 d D . .
H24A H 0.7778 0.4828 -0.0346 0.239 Uiso 1 1 calc R A 1
H24B H 0.7059 0.5154 -0.0308 0.239 Uiso 1 1 calc R A 1
C25A C 0.7381(19) 0.4798(16) 0.0162(4) 0.166(8) Uiso 0.34 1 d PD B 1
H25A H 0.6738 0.4368 0.0181 0.249 Uiso 0.34 1 calc PR B 1
H25B H 0.7548 0.5287 0.0322 0.249 Uiso 0.34 1 calc PR B 1
H25C H 0.7721 0.4494 0.0211 0.249 Uiso 0.34 1 calc PR B 1
C25B C 0.7836(14) 0.4794(13) -0.0519(4) 0.159(6) Uiso 0.43 1 d PD B 2
C25C C 0.770(2) 0.499(2) -0.0846(8) 0.151(10) Uiso 0.23 1 d P B 2
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'
N N 0.0061 0.0033 '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
O1S S1 O1S 110.23(7) 3_675 2_765
O1S S1 O1S 110.23(7) 3_675 .
O1S S1 O1S 110.22(7) 2_765 .
O1S S1 O1S 110.23(7) 3_675 1
O1S S1 O1S 110.22(7) 2_765 1
O1S S1 O1S 0.0(2) . 1
O1S S1 O2S 108.71(7) 3_675 1
O1S S1 O2S 108.71(7) 2_765 1
O1S S1 O2S 108.71(7) . 1
O1S S1 O2S 108.71(7) 1 1
O1S S1 O2S 108.71(7) 3_675 .
O1S S1 O2S 108.71(7) 2_765 .
O1S S1 O2S 108.71(7) . .
O1S S1 O2S 108.71(7) 1 .
C2 N1 C2 111.63(15) 3_675 2_765
C2 N1 C2 111.63(15) 3_675 .
C2 N1 C2 111.63(15) 2_765 .
N1 C2 C3 110.9(2) . .
N1 C2 H2A 109.5 . .
C3 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
C3 C2 H2B 109.5 . .
H2A C2 H2B 108.0 . .
N4 C3 C2 111.8(3) . .
N4 C3 H3A 109.3 . .
C2 C3 H3A 109.3 . .
N4 C3 H3B 109.3 . .
C2 C3 H3B 109.3 . .
H3A C3 H3B 107.9 . .
C5 N4 C3 121.9(2) . .
C5 N4 H4 119.1 . .
C3 N4 H4 119.1 . .
O6 C5 N4 123.5(3) . .
O6 C5 N7 122.4(3) . .
N4 C5 N7 114.1(2) . .
C5 N7 C8 127.1(2) . .
C5 N7 H7 116.4 . .
C8 N7 H7 116.4 . .
C9 C8 N7 124.6(3) . .
C9 C8 C13 118.3(3) . .
N7 C8 C13 117.0(2) . .
C10 C9 C8 121.1(3) . .
C10 C9 H9 119.4 . .
C8 C9 H9 119.4 . .
C9 C10 C11 119.1(3) . .
C9 C10 H10 120.5 . .
C11 C10 H10 120.5 . .
C10 C11 C12 121.2(3) . .
C10 C11 N14 119.4(3) . .
C12 C11 N14 119.4(3) . .
C13 C12 C11 119.3(3) . .
C13 C12 H12 120.3 . .
C11 C12 H12 120.3 . .
C12 C13 C8 120.9(3) . .
C12 C13 H13 119.6 . .
C8 C13 H13 119.6 . .
O16 N14 O15 122.6(4) . .
O16 N14 C11 118.9(3) . .
O15 N14 C11 118.4(4) . .
C22 N17 C22 105.4(3) . 6_765
C22 N17 C18 112.2(2) . .
C22 N17 C18 110.4(2) 6_765 .
C22 N17 C18 110.4(2) . 6_765
C22 N17 C18 112.2(2) 6_765 6_765
C18 N17 C18 106.4(3) . 6_765
C19 C18 N17 114.6(2) . .
C19 C18 H18A 108.6 . .
N17 C18 H18A 108.6 . .
C19 C18 H18B 108.6 . .
N17 C18 H18B 108.6 . .
H18A C18 H18B 107.6 . .
C18 C19 C20 109.8(3) . .
C18 C19 H19A 109.7 . .
C20 C19 H19A 109.7 . .
C18 C19 H19B 109.7 . .
C20 C19 H19B 109.7 . .
H19A C19 H19B 108.2 . .
C21 C20 C19 111.7(3) . .
C21 C20 H20A 109.3 . .
C19 C20 H20A 109.3 . .
C21 C20 H20B 109.3 . .
C19 C20 H20B 109.3 . .
H20A C20 H20B 107.9 . .
C20 C21 H21A 109.5 . .
C20 C21 H21B 109.5 . .
H21A C21 H21B 109.5 . .
C20 C21 H21C 109.5 . .
H21A C21 H21C 109.5 . .
H21B C21 H21C 109.5 . .
C23 C22 N17 116.2(3) . .
C23 C22 H13A 108.2 . .
N17 C22 H13A 108.2 . .
C23 C22 H13B 108.2 . .
N17 C22 H13B 108.2 . .
H13A C22 H13B 107.4 . .
C22 C23 C24 108.9(4) . .
C22 C23 H23A 109.9 . .
C24 C23 H23A 109.9 . .
C22 C23 H23B 109.9 . .
C24 C23 H23B 109.9 . .
H23A C23 H23B 108.3 . .
C25B C24 C23 102.3(10) . .
C25B C24 C25A 127.6(14) . .
C23 C24 C25A 111.3(10) . .
C25B C24 H24A 18.8 . .
C23 C24 H24A 109.4 . .
C25A C24 H24A 109.4 . .
C25B C24 H24B 95.1 . .
C23 C24 H24B 109.4 . .
C25A C24 H24B 109.4 . .
H24A C24 H24B 108.0 . .
C24 C25A H25A 109.5 . .
C24 C25A H25B 109.5 . .
C24 C25A H25C 109.5 . .
C25C C25B C24 121(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
S1 O1S 1.4730(18) 3_675
S1 O1S 1.4730(18) 2_765
S1 O1S 1.4730(18) .
S1 O1S 1.4730(18) 1
S1 O2S 1.483(3) 1
S1 O2S 1.483(3) .
O3W H3W 0.72(3) .
N1 C2 1.458(3) 3_675
N1 C2 1.458(3) 2_765
N1 C2 1.458(3) .
C2 C3 1.534(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 N4 1.442(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
N4 C5 1.344(4) .
N4 H4 0.8800 .
C5 O6 1.229(4) .
C5 N7 1.378(4) .
N7 C8 1.397(4) .
N7 H7 0.8800 .
C8 C9 1.395(4) .
C8 C13 1.399(4) .
C9 C10 1.368(5) .
C9 H9 0.9500 .
C10 C11 1.375(5) .
C10 H10 0.9500 .
C11 C12 1.387(4) .
C11 N14 1.463(5) .
C12 C13 1.360(4) .
C12 H12 0.9500 .
C13 H13 0.9500 .
N14 O16 1.179(4) .
N14 O15 1.224(4) .
N17 C22 1.513(4) .
N17 C22 1.513(4) 6_765
N17 C18 1.516(4) .
N17 C18 1.516(4) 6_765
C18 C19 1.513(5) .
C18 H18A 0.9900 .
C18 H18B 0.9900 .
C19 C20 1.529(6) .
C19 H19A 0.9900 .
C19 H19B 0.9900 .
C20 C21 1.511(6) .
C20 H20A 0.9900 .
C20 H20B 0.9900 .
C21 H21A 0.9800 .
C21 H21B 0.9800 .
C21 H21C 0.9800 .
C22 C23 1.510(5) .
C22 H13A 0.9900 .
C22 H13B 0.9900 .
C23 C24 1.572(8) .
C23 H23A 0.9900 .
C23 H23B 0.9900 .
C24 C25B 1.569(8) .
C24 C25A 1.592(8) .
C24 H24A 0.9900 .
C24 H24B 0.9900 .
C25A H25A 0.9800 .
C25A H25B 0.9800 .
C25A H25C 0.9800 .
C25B C25C 1.40(3) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3W H3W O1S 0.72(3) 2.06(3) 2.773(3) 168(4) 1
N4 H4 O2S 0.88 2.01 2.870(3) 165.3 1
N7 H7 O1S 0.88 2.03 2.901(3) 170.0 1
C10 H10 O6 0.95 2.51 3.161(5) 126.1 11_565
C13 H13 O1S 0.95 2.58 3.353(4) 138.3 1
C13 H13 O3W 0.95 2.45 3.335(4) 154.9 1
C19 H19A O15 0.99 2.55 3.307(4) 132.9 3_665
_cod_duplicate_entry 4327246
