#------------------------------------------------------------------------------
#$Date: 2016-03-26 21:55:20 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180485 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/54/7215472.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_7215472
loop_
_publ_author_name
'Adalder, Tapas Kumar'
'Dastidar, Parthasarathi'
_publ_section_title
;
 The role of secondary ammonium cations in controlling the conformation of
 C3-symmetric acid moieties and its implication for the design of
 supramolecular capsules
;
_journal_issue                   22
_journal_name_full               CrystEngComm
_journal_page_first              4867
_journal_paper_doi               10.1039/c3ce42655f
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         '2(C15 H18 O6), C2 H6 O'
_chemical_formula_sum            'C32 H42 O13'
_chemical_formula_weight         634.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.387(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1249(7)
_cell_length_b                   4.7655(3)
_cell_length_c                   35.020(3)
_cell_measurement_temperature    293(2)
_cell_volume                     1686.8(2)
_computing_cell_refinement       'BRUKER APEX II'
_computing_data_collection       'BRUKER APEX II'
_computing_data_reduction        'BRUKER APEX II'
_computing_molecular_graphics    'MERCURY 2.3, PLATON'
_computing_publication_material  'MERCURY 2.3, PLATON'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'BRUKER 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  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            13712
_diffrn_reflns_theta_full        24.03
_diffrn_reflns_theta_max         24.03
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9772
_exptl_absorpt_correction_T_min  0.9717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.201
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.042(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         2655
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1049
_refine_ls_R_factor_gt           0.0858
_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)+(0.1735P)²+1.9664P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2555
_refine_ls_wR_factor_ref         0.2743
_reflns_number_gt                1988
_reflns_number_total             2655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce42655f2.cif
_cod_data_source_block           ta0611a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'MONOCLINIC' changed to 'monoclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN'
changed to 'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 7215472--7215483.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7215472
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 1.2307(3) 1.0051(6) 0.17813(11) 0.0505(10) Uani 1 1 d .
O2 O 1.3182(3) 0.6737(7) 0.21605(9) 0.0439(9) Uani 1 1 d .
H2 H 1.3867 0.7582 0.2122 0.066 Uiso 1 1 calc R
O3 O 0.8807(4) 0.7172(8) 0.00441(9) 0.0624(11) Uani 1 1 d .
H3 H 0.9110 0.8267 -0.0109 0.094 Uiso 1 1 calc R
O4 O 0.9958(4) 0.9796(7) 0.04640(8) 0.0517(10) Uani 1 1 d .
O5 O 0.5447(3) 0.9374(7) 0.20060(9) 0.0499(10) Uani 1 1 d .
O6 O 0.4537(3) 1.2550(7) 0.16162(11) 0.0553(11) Uani 1 1 d .
H6 H 0.3853 1.1929 0.1698 0.083 Uiso 1 1 calc R
O7A O 0.5084(12) 0.461(3) 0.0157(4) 0.041(3) Uiso 0.25 1 d P
O7B O 0.496(2) 0.425(5) 0.0376(7) 0.102(6) Uiso 0.25 1 d P
C1 C 1.2186(4) 0.7936(8) 0.19658(11) 0.0301(10) Uani 1 1 d .
C2 C 1.0896(4) 0.6415(8) 0.19940(11) 0.0302(10) Uani 1 1 d .
H2A H 1.0620 0.6582 0.2254 0.036 Uiso 1 1 calc R
H2B H 1.1033 0.4438 0.1943 0.036 Uiso 1 1 calc R
C3 C 0.9796(4) 0.7490(8) 0.17212(11) 0.0274(9) Uani 1 1 d .
C4 C 0.9737(4) 0.6550(8) 0.13415(11) 0.0284(9) Uani 1 1 d .
C5 C 1.0784(4) 0.4624(9) 0.12051(13) 0.0408(11) Uani 1 1 d .
H5A H 1.0541 0.2713 0.1252 0.061 Uiso 1 1 calc R
H5B H 1.1614 0.5033 0.1340 0.061 Uiso 1 1 calc R
H5C H 1.0865 0.4894 0.0936 0.061 Uiso 1 1 calc R
C6 C 0.8689(4) 0.7398(8) 0.10906(11) 0.0301(10) Uani 1 1 d .
C7 C 0.8545(4) 0.6209(9) 0.06884(11) 0.0371(11) Uani 1 1 d .
H7A H 0.8931 0.4345 0.0690 0.045 Uiso 1 1 calc R
H7B H 0.7611 0.6019 0.0615 0.045 Uiso 1 1 calc R
C8 C 0.9179(4) 0.7933(9) 0.03919(12) 0.0349(10) Uani 1 1 d .
C9 C 0.7751(4) 0.9323(8) 0.12079(11) 0.0292(10) Uani 1 1 d .
C10 C 0.6621(4) 1.0229(10) 0.09326(13) 0.0432(12) Uani 1 1 d .
H10A H 0.5927 0.8857 0.0932 0.065 Uiso 1 1 calc R
H10B H 0.6933 1.0393 0.0680 0.065 Uiso 1 1 calc R
H10C H 0.6289 1.2010 0.1012 0.065 Uiso 1 1 calc R
C11 C 0.7851(3) 1.0365(8) 0.15806(11) 0.0265(9) Uani 1 1 d .
C12 C 0.6865(4) 1.2570(8) 0.17006(12) 0.0330(10) Uani 1 1 d .
H12A H 0.7237 1.3552 0.1925 0.040 Uiso 1 1 calc R
H12B H 0.6727 1.3933 0.1496 0.040 Uiso 1 1 calc R
C13 C 0.5549(4) 1.1329(9) 0.17904(11) 0.0305(10) Uani 1 1 d .
C14 C 0.8850(3) 0.9397(8) 0.18443(10) 0.0270(9) Uani 1 1 d .
C15 C 0.8886(4) 1.0403(10) 0.22533(12) 0.0397(11) Uani 1 1 d .
H15A H 0.9593 0.9482 0.2399 0.060 Uiso 1 1 calc R
H15B H 0.8059 0.9972 0.2361 0.060 Uiso 1 1 calc R
H15C H 0.9027 1.2395 0.2260 0.060 Uiso 1 1 calc R
C16A C 0.352(2) 0.586(5) 0.0579(6) 0.061(5) Uiso 0.25 1 d P
C16B C 0.351(2) 0.761(4) 0.0241(6) 0.049(5) Uiso 0.25 1 d P
C17 C 0.4234(12) 0.594(3) 0.0210(3) 0.061(3) Uiso 0.50 1 d P
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
O7B O7A C17 78(2) . .
O7B O7A O7A 161(3) . 3_665
C17 O7A O7A 84.6(15) . 3_665
O7B O7A C17 151(2) . 3_665
C17 O7A C17 130.3(12) . 3_665
O7A O7A C17 45.8(10) 3_665 3_665
O7A O7B C17 61.9(19) . .
O7A O7B C16A 117(3) . .
C17 O7B C16A 55.6(13) . .
O1 C1 O2 122.8(4) . .
O1 C1 C2 123.7(3) . .
O2 C1 C2 113.6(3) . .
C1 C2 C3 113.9(3) . .
C4 C3 C14 120.4(3) . .
C4 C3 C2 118.7(3) . .
C14 C3 C2 120.9(3) . .
C6 C4 C3 119.5(4) . .
C6 C4 C5 120.1(4) . .
C3 C4 C5 120.4(4) . .
C4 C6 C9 120.6(3) . .
C4 C6 C7 120.3(4) . .
C9 C6 C7 119.2(4) . .
C8 C7 C6 114.7(3) . .
O4 C8 O3 123.3(4) . .
O4 C8 C7 124.1(4) . .
O3 C8 C7 112.5(4) . .
C11 C9 C6 119.7(3) . .
C11 C9 C10 120.3(4) . .
C6 C9 C10 120.0(4) . .
C9 C11 C14 120.5(4) . .
C9 C11 C12 119.4(3) . .
C14 C11 C12 120.1(3) . .
C13 C12 C11 112.8(3) . .
O5 C13 O6 123.0(4) . .
O5 C13 C12 122.8(3) . .
O6 C13 C12 114.1(3) . .
C3 C14 C11 119.1(3) . .
C3 C14 C15 121.2(3) . .
C11 C14 C15 119.6(4) . .
C16B C16A O7B 83.8(15) . .
C17 C16B C16A 71.8(16) . .
O7A C17 C16B 168.1(17) . .
C16B C17 O7B 146(2) . .
O7A C17 C16A 123.5(14) . .
C16B C17 C16A 65.0(15) . .
O7B C17 C16A 83.2(16) . .
O7A C17 O7A 49.7(12) . 3_665
C16B C17 O7A 123.4(15) . 3_665
O7B C17 O7A 89.9(17) . 3_665
C16A C17 O7A 168.7(14) . 3_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C1 1.208(5) .
O2 C1 1.314(5) .
O3 C8 1.305(5) .
O4 C8 1.205(5) .
O5 C13 1.208(5) .
O6 C13 1.299(5) .
O7A O7B 0.80(2) .
O7A C17 1.091(15) .
O7A O7A 1.16(3) 3_665
O7A C17 1.516(18) 3_665
O7B C17 1.21(2) .
O7B C16A 1.82(3) .
C1 C2 1.502(5) .
C2 C3 1.513(5) .
C3 C4 1.401(5) .
C3 C14 1.406(5) .
C4 C6 1.397(5) .
C4 C5 1.501(6) .
C6 C9 1.399(6) .
C6 C7 1.517(5) .
C7 C8 1.498(6) .
C9 C11 1.395(5) .
C9 C10 1.515(5) .
C11 C14 1.407(5) .
C11 C12 1.526(5) .
C12 C13 1.508(6) .
C14 C15 1.509(5) .
C16A C16B 1.45(3) .
C16A C17 1.51(3) .
C16B C17 1.09(2) .
C17 O7A 1.516(18) 3_665
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
O2 H2 O5 0.82 1.88 2.698(4) 176.2 1_655
O3 H3 O4 0.82 1.85 2.661(5) 168.8 3_775
