#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/91/4029168.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_4029168
loop_
_publ_author_name
'Basu, Arghya'
'Das, Gopal'
_publ_section_title
;
 A C3v-Symmetric Tripodal Urea Receptor for Anions and Ion Pairs:
 Formation of Dimeric Capsular Assemblies of the Receptor during Anion and
 Ion Pair Coordination.
;
_journal_issue                   6
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2647
_journal_page_last               2656
_journal_paper_doi               10.1021/jo500102e
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C46 H42 N10 O15'
_chemical_formula_weight         974.90
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :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            6
_cell_length_a                   18.3034(14)
_cell_length_b                   18.3034(14)
_cell_length_c                   40.426(8)
_cell_measurement_temperature    298(2)
_cell_volume                     11729(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0357
_diffrn_reflns_av_sigmaI/netI    0.0805
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            8797
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         3.44
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADBAS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    0.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3048.0
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.239
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         6625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1723
_refine_ls_R_factor_gt           0.0981
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2600
_refine_ls_wR_factor_ref         0.2882
_reflns_number_gt                5730
_reflns_number_total             6625
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo500102e_si_002.cif
_cod_data_source_block           Complex4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/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 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        ' C46 H42 N10 O15 '
_cod_database_code               4029168
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, 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'
'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'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -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'
'-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'
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 0.51604(13) 0.69998(13) 0.62041(6) 0.0999(8) Uani 1 1 d .
O2 O 0.80171(16) 0.67220(17) 0.70793(8) 0.1338(10) Uani 1 1 d .
C3 C 0.58831(18) 0.71756(18) 0.63734(9) 0.0850(9) Uani 1 1 d .
C4 C 0.65777(19) 0.79466(18) 0.63176(9) 0.0902(10) Uani 1 1 d .
H4 H 0.6540 0.8324 0.6174 0.108 Uiso 1 1 calc R
C6 C 0.74023(19) 0.76313(19) 0.66894(8) 0.0835(9) Uani 1 1 d .
C5 C 0.7326(2) 0.81694(19) 0.64694(9) 0.0917(10) Uani 1 1 d .
H5 H 0.7794 0.8693 0.6424 0.110 Uiso 1 1 calc R
N2 N 0.81982(16) 0.79207(16) 0.68345(8) 0.1011(9) Uani 1 1 d .
H2N H 0.8554 0.8451 0.6816 0.121 Uiso 1 1 calc R
N1 N 0.3333 0.6667 0.61756(13) 0.0955(14) Uani 1 3 d S
C9 C 0.8467(2) 0.7448(2) 0.70022(10) 0.1027(11) Uani 1 1 d .
N3 N 0.93169(17) 0.79147(18) 0.70703(8) 0.1040(9) Uani 1 1 d .
H3N H 0.9589 0.8408 0.6982 0.125 Uiso 1 1 calc R
C2 C 0.43983(19) 0.62272(19) 0.62768(10) 0.0984(11) Uani 1 1 d .
H2A H 0.4248 0.6223 0.6507 0.118 Uiso 1 1 calc R
H2B H 0.4486 0.5753 0.6240 0.118 Uiso 1 1 calc R
C11 C 1.0627(3) 0.8253(3) 0.73094(11) 0.1228(13) Uani 1 1 d .
H11 H 1.0870 0.8776 0.7206 0.147 Uiso 1 1 calc R
C8 C 0.5930(2) 0.6635(2) 0.65911(9) 0.1041(11) Uani 1 1 d .
H8 H 0.5454 0.6118 0.6637 0.125 Uiso 1 1 calc R
C7 C 0.6708(2) 0.6860(2) 0.67494(11) 0.1053(12) Uani 1 1 d .
H7 H 0.6745 0.6483 0.6893 0.126 Uiso 1 1 calc R
C1 C 0.3688(2) 0.6143(2) 0.60572(11) 0.1083(12) Uani 1 1 d .
H1B H 0.3898 0.6311 0.5834 0.130 Uiso 1 1 calc R
H1A H 0.3244 0.5556 0.6051 0.130 Uiso 1 1 calc R
N4 N 1.1340(5) 0.7151(5) 0.78692(17) 0.186(2) Uani 1 1 d .
O3 O 1.2052(3) 0.7675(4) 0.79152(13) 0.215(2) Uani 1 1 d .
C10 C 0.9776(2) 0.7668(2) 0.72670(10) 0.0992(11) Uani 1 1 d .
C12 C 1.1118(3) 0.8030(4) 0.75160(14) 0.1382(16) Uani 1 1 d .
H12 H 1.1691 0.8406 0.7544 0.166 Uiso 1 1 calc R
C15 C 0.9432(3) 0.6894(3) 0.74406(11) 0.1231(13) Uani 1 1 d .
H15 H 0.8858 0.6508 0.7427 0.148 Uiso 1 1 calc R
C14 C 0.9935(3) 0.6714(3) 0.76263(13) 0.1428(17) Uani 1 1 d .
H14 H 0.9712 0.6188 0.7727 0.171 Uiso 1 1 calc R
O4 O 1.1010(4) 0.6444(5) 0.79956(13) 0.230(2) Uani 1 1 d .
C13 C 1.0759(4) 0.7290(4) 0.76678(13) 0.1355(16) Uani 1 1 d .
O5 O 0.03127(14) 0.95150(13) 0.68095(9) 0.1452(13) Uani 1 1 d .
C16 C 0.0000 1.0000 0.6825(2) 0.115(2) Uani 1 3 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'
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'
K K 0.2009 0.2494 '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
C3 O1 C2 118.4(2) . .
C8 C3 C4 119.6(3) . .
C8 C3 O1 123.7(3) . .
C4 C3 O1 116.6(3) . .
C5 C4 C3 120.8(3) . .
C7 C6 C5 118.4(3) . .
C7 C6 N2 124.6(3) . .
C5 C6 N2 117.0(3) . .
C4 C5 C6 121.3(3) . .
C9 N2 C6 126.9(3) . .
C1 N1 C1 110.1(2) 3_565 2_665
C1 N1 C1 110.1(2) 3_565 .
C1 N1 C1 110.1(2) 2_665 .
O2 C9 N2 124.2(3) . .
O2 C9 N3 124.9(4) . .
N2 C9 N3 111.0(3) . .
C9 N3 C10 126.4(3) . .
O1 C2 C1 110.0(3) . .
C10 C11 C12 118.3(4) . .
C3 C8 C7 120.0(3) . .
C6 C7 C8 119.8(3) . .
N1 C1 C2 112.1(3) . .
O3 N4 O4 123.2(8) . .
O3 N4 C13 123.3(7) . .
O4 N4 C13 113.4(7) . .
N3 C10 C11 116.6(4) . .
N3 C10 C15 124.9(3) . .
C11 C10 C15 118.4(4) . .
C13 C12 C11 120.1(5) . .
C14 C15 C10 120.3(4) . .
C15 C14 C13 120.6(5) . .
C12 C13 C14 122.1(5) . .
C12 C13 N4 113.9(6) . .
C14 C13 N4 124.0(6) . .
O5 C16 O5 119.75(7) 3_465 2_675
O5 C16 O5 119.75(7) 3_465 .
O5 C16 O5 119.75(8) 2_675 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 C3 1.377(3) .
O1 C2 1.435(3) .
O2 C9 1.203(4) .
C3 C8 1.358(4) .
C3 C4 1.365(4) .
C4 C5 1.364(4) .
C6 C7 1.369(4) .
C6 C5 1.385(4) .
C6 N2 1.406(4) .
N2 C9 1.370(4) .
N1 C1 1.480(3) 3_565
N1 C1 1.480(3) 2_665
N1 C1 1.480(3) .
C9 N3 1.376(4) .
N3 C10 1.387(4) .
C2 C1 1.518(5) .
C11 C10 1.391(5) .
C11 C12 1.427(6) .
C8 C7 1.420(4) .
N4 O3 1.184(7) .
N4 O4 1.233(7) .
N4 C13 1.460(8) .
C10 C15 1.416(5) .
C12 C13 1.324(6) .
C15 C14 1.349(6) .
C14 C13 1.351(6) .
O5 C16 1.276(2) .
C16 O5 1.276(2) 3_465
C16 O5 1.276(2) 2_675
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.071 0.381 0.167 1913 224 ' '
2 -0.005 0.065 0.500 1909 224 ' '
3 -0.113 0.338 0.833 1913 224 ' '
