#------------------------------------------------------------------------------
#$Date: 2016-03-26 02:32:55 +0100 (Sat 26 de Mar de 2016) $
#$Revision: 180186 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/82/7108266.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_7108266
loop_
_publ_author_name
'Xiaoju Li'
'Xiahong Xu'
'Daqiang Yuan'
'Xiulan Weng'
_publ_section_title
;
 Hexagonal prismatic dodecameric water cluster: a building unit of the
 five-fold interpenetrating six-connected supramolecular network
;
_journal_name_full               Chem.Commun.
_journal_page_first              9014
_journal_paper_doi               10.1039/c2cc34412b
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C6 H13 N2 O2'
_chemical_formula_weight         145.18
_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            18
_cell_length_a                   21.5759(8)
_cell_length_b                   21.5759(8)
_cell_length_c                   9.3544(6)
_cell_measurement_temperature    173(2)
_cell_volume                     3771.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9897
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.61
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.9531
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1422
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.43
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         1909
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0840P)²+1.1642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1511
_reflns_number_gt                1490
_reflns_number_total             1909
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc34412b.txt
_cod_data_source_block           d:\wrh\wdb\mim-c4\w
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               7108266
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
O1W O 0.46509(9) 0.80526(8) -0.17653(16) 0.0641(4) Uani 1 1 d D
O2W O 0.45679(8) 0.79772(9) -0.47566(16) 0.0635(4) Uani 1 1 d D
N1 N 0.53130(7) 0.98724(7) 0.17687(12) 0.0376(3) Uani 1 1 d .
N2 N 0.54287(7) 0.92084(7) 0.01086(13) 0.0395(3) Uani 1 1 d .
C1 C 0.43165(9) 0.86055(10) 0.1582(2) 0.0521(4) Uani 1 1 d .
H1A H 0.4175 0.8211 0.0903 0.078 Uiso 1 1 calc R
H1B H 0.3954 0.8753 0.1588 0.078 Uiso 1 1 calc R
H1C H 0.4357 0.8447 0.2541 0.078 Uiso 1 1 calc R
C2 C 0.50174(8) 0.92197(8) 0.11482(15) 0.0362(4) Uani 1 1 d .
C3 C 0.60131(8) 0.98895(9) 0.00725(16) 0.0425(4) Uani 1 1 d .
H3 H 0.6404 1.0046 -0.0571 0.051 Uiso 1 1 calc R
C4 C 0.59518(9) 1.03041(9) 0.10811(17) 0.0433(4) Uani 1 1 d .
H4 H 0.6282 1.0793 0.1276 0.052 Uiso 1 1 calc R
C5 C 0.50118(10) 1.00874(10) 0.29426(16) 0.0463(4) Uani 1 1 d .
H5A H 0.4486 0.9846 0.2827 0.056 Uiso 1 1 calc R
H5B H 0.5201 1.0610 0.2887 0.056 Uiso 1 1 calc R
C6 C 0.51824(9) 0.99065(9) 0.44055(15) 0.0434(4) Uani 1 1 d .
H6A H 0.5707 1.0174 0.4556 0.052 Uiso 1 1 calc R
H6B H 0.5020 0.9389 0.4447 0.052 Uiso 1 1 calc R
H1W1 H 0.4685(11) 0.7731(10) -0.158(2) 0.052 Uiso 1 1 d D
H1W2 H 0.4913(10) 0.8387(9) -0.1260(19) 0.052 Uiso 1 1 d D
H2W1 H 0.4529(11) 0.7586(9) -0.490(2) 0.052 Uiso 1 1 d D
H2W2 H 0.4638(11) 0.8061(11) -0.3902(17) 0.052 Uiso 1 1 d D
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1W 0.0813(10) 0.0569(8) 0.0610(9) -0.0184(7) -0.0180(7) 0.0397(8)
O2W 0.0700(9) 0.0717(9) 0.0557(8) 0.0057(7) 0.0076(7) 0.0404(8)
N1 0.0470(7) 0.0416(7) 0.0300(6) 0.0002(5) 0.0010(5) 0.0266(6)
N2 0.0439(7) 0.0448(7) 0.0332(6) 0.0007(5) 0.0040(5) 0.0247(6)
C1 0.0464(9) 0.0511(10) 0.0537(10) 0.0045(8) 0.0115(7) 0.0206(8)
C2 0.0405(8) 0.0408(8) 0.0313(7) 0.0013(6) 0.0006(6) 0.0234(6)
C3 0.0405(8) 0.0495(9) 0.0373(8) 0.0069(7) 0.0062(6) 0.0224(7)
C4 0.0445(8) 0.0404(8) 0.0411(8) 0.0046(6) -0.0001(7) 0.0184(7)
C5 0.0655(11) 0.0582(10) 0.0325(8) -0.0030(7) 0.0008(7) 0.0439(9)
C6 0.0560(9) 0.0519(9) 0.0342(8) -0.0021(6) -0.0001(7) 0.0360(8)
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'
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_3
C2 N1 C4 107.18(12) .
C2 N1 C5 126.77(13) .
C4 N1 C5 126.05(14) .
C2 N2 C3 105.23(12) .
N2 C2 N1 111.26(13) .
N2 C2 C1 125.24(14) .
N1 C2 C1 123.49(13) .
C4 C3 N2 110.41(13) .
C3 C4 N1 105.92(14) .
N1 C5 C6 113.04(12) .
C5 C6 C6 111.41(16) 10_676
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C2 1.3523(19) .
N1 C4 1.377(2) .
N1 C5 1.4645(19) .
N2 C2 1.3249(19) .
N2 C3 1.377(2) .
C1 C2 1.484(2) .
C3 C4 1.351(2) .
C5 C6 1.518(2) .
C6 C6 1.529(3) 10_676
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
O1W H1W2 N2 0.810(15) 2.012(15) 2.8148(19) 171(2) .
O2W H2W2 O1W 0.816(15) 2.000(16) 2.803(2) 168(2) .
O1W H1W1 O2W 0.752(15) 2.112(17) 2.822(2) 158(2) 14_454
O2W H2W1 O1W 0.816(15) 2.072(16) 2.861(2) 162(2) 14_454
