#------------------------------------------------------------------------------
#$Date: 2016-02-13 13:50:18 +0100 (Sat 13 de Feb de 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/2/02/01/2020109.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2020109
loop_
_publ_author_name
'Ponomarova, Vira V.'
'Rusanova, Julia A.'
'Rusanov, Eduard B.'
'Domasevitch, Konstantin V.'
_publ_section_title
;
 Unusual centrosymmetric structure of [M(18-crown-6)]⁺ (M
 = Rb, Cs and NH₄) complexes stabilized in an environment of
 hexachloridoantimonate(V) anions
;
_journal_coeditor_code           EG3188
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229615015430
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[(N H4) (C12 H24 O6)] , [Sb Cl6]'
_chemical_formula_moiety         'N H4 +, C12 H24 O6, Sb Cl6 -'
_chemical_formula_sum            'C12 H28 Cl6 N O6 Sb'
_chemical_formula_weight         616.80
_chemical_name_systematic
;
Ammonium hexachloridoantimonate(V)--1,4,7,10,13,16-hexaoxacyclooctadecane
(1/1)
;
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   14.1069(9)
_cell_length_b                   14.1069(9)
_cell_length_c                   10.1908(8)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      17.22
_cell_measurement_theta_min      12.56
_cell_volume                     1756.3(2)
_computing_cell_refinement
;
CAD4 Express (Enraf--Nonius, 1994)
;
_computing_data_collection
;
CAD4 Express (Enraf--Nonius, 1994)
;
_computing_data_reduction
;
XCAD4 (Harms & Wocadlo, 1995)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD4'
_diffrn_measurement_method       'non-profiled ω--2θ scans'
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2227
_diffrn_reflns_theta_full        25.31
_diffrn_reflns_theta_max         25.31
_diffrn_reflns_theta_min         2.60
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.889
_exptl_absorpt_correction_T_max  0.7638
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
(North et al.,  1968)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.750
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             924
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.445
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0217
_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)+(0.0283P)²+1.1402P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0547
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                673
_reflns_number_total             708
_reflns_threshold_expression     I>2σ(I)
_iucr_refine_instructions_details
;
TITL NH4_Sb in R-3
CELL  0.71073  14.1069  14.1069  10.1908   90.000   90.000  120.000
ZERR     3.00   0.0009   0.0009   0.0008    0.000    0.000    0.000
LATT   3
SYMM  - Y,   X - Y,   Z
SYMM  - X + Y, - X,   Z
SFAC  C    H    N    O    CL   SB
UNIT  36   84   3    18   18   3
MERG   2
EQIV $1 Y, -X+Y, 1-Z
EQIV $2 -X+Y,-X, Z
EQIV $3 -X, -Y, 1-Z
EQIV $4 -Y, X-Y, Z
EQIV $5 X-Y, X, 1-Z
EQIV $6 1/3+X-Y, -1/3+X, 2/3-Z
MPLA 6 O1 O1_$1 O1_$2 O1_$3 O1_$4 O1_$5 N1
RTAB H..O H1 CL1
RTAB H..O H2 O1
RTAB H..O H2A CL1_$6
RTAB O..O N1 CL1
RTAB O..O N1 O1
RTAB O..O C2 CL1_$6
RTAB XHY N1 H1 CL1
RTAB XHY N1 H2 O1
RTAB XHY C2 H2A CL1_$6
FMAP   2
PLAN   10
SIZE     0.18   0.23   0.25
ACTA
BOND   $H
CONF
LIST   4
L.S.   6
TEMP   -50.00
WGHT    0.028200    1.232100
FVAR       0.10291
SB1   6    0.000000    0.000000    0.000000    10.16667    0.03065    0.03065 =
         0.03442    0.00000    0.00000    0.01533
CL1   5    0.158276    0.078815    0.134595    11.00000    0.04550    0.05259 =
         0.05980   -0.00895   -0.01709    0.02281
O1    4    0.224746    0.063128    0.522375    11.00000    0.03656    0.03826 =
         0.05174    0.00028    0.00613    0.01782
N1    3    0.000000    0.000000    0.449453    10.16667    0.03336    0.03336 =
         0.07409    0.00000    0.00000    0.01668
AFIX   3
H1    2    0.000000    0.000000    0.361138    10.16667   -1.50000
H2    2    0.069402    0.032346    0.478891    10.50000   -1.50000
AFIX   0
C1    1    0.247157   -0.015557    0.464278    11.00000    0.03564    0.05284 =
         0.05362   -0.00745   -0.00062    0.02507
AFIX  23
H1A   2    0.323298    0.004486    0.481400    11.00000   -1.20000
H1B   2    0.236736   -0.017092    0.369064    11.00000   -1.20000
AFIX   0
C2    1    0.171628   -0.125948    0.521034    11.00000    0.04618    0.04837 =
         0.05523   -0.00605   -0.00900    0.03203
AFIX  23
H2A   2    0.194178   -0.178160    0.492867    11.00000   -1.20000
H2B   2    0.174645   -0.122038    0.617073    11.00000   -1.20000
HKLF 4
REM  NH4_Sb in R-3
REM R1 =  0.0217 for    673 Fo > 4sig(Fo)  and  0.0236 for all    708 data
REM     42 parameters refined using      0 restraints
END
WGHT      0.0282      1.1485
REM Highest difference peak  0.360,  deepest hole -0.445,  1-sigma level  0.064
Q1    1   0.1024  0.0589  0.1812  11.00000  0.05    0.36
Q2    1   0.1450  0.1198  0.0819  11.00000  0.05    0.27
Q3    1  -0.0434  0.0296  0.0442  11.00000  0.05    0.26
Q4    1   0.1697  0.0329  0.5323  11.00000  0.05    0.20
Q5    1   0.2082 -0.0660  0.5093  11.00000  0.05    0.19
Q6    1   0.0934  0.1117  0.1333  11.00000  0.05    0.16
Q7    1   0.2586 -0.2477  0.5791  11.00000  0.05    0.15
Q8    1   0.2416  0.1086  0.5002  11.00000  0.05    0.15
Q9    1   0.3363  0.0403  0.4493  11.00000  0.05    0.15
Q10   1   0.1664 -0.2744  0.4797  11.00000  0.05    0.15
;
_cod_data_source_file            eg3188sup1.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2020109
_cod_database_fobs_code          2020109
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Sb Sb1 0.0000 0.0000 0.0000 0.03190(15) Uani d S 1 6
Cl Cl1 0.15828(5) 0.07881(6) 0.13460(7) 0.0534(2) Uani d . 1 1
O O1 0.22474(13) 0.06313(13) 0.52237(17) 0.0426(4) Uani d . 1 1
N N1 0.0000 0.0000 0.4495(8) 0.0469(19) Uani d SP 0.50 3
H H1 0.0000 0.0000 0.3611 0.070 Uiso d SPR 0.50 3
H H2 0.0694 0.0323 0.4789 0.070 Uiso d PR 0.50 1
C C1 0.2472(2) -0.0156(2) 0.4643(3) 0.0461(6) Uani d . 1 1
H H1A 0.3233 0.0045 0.4814 0.055 Uiso calc R 1 1
H H1B 0.2367 -0.0171 0.3691 0.055 Uiso calc R 1 1
C C2 0.1716(2) -0.1260(2) 0.5210(3) 0.0462(6) Uani d . 1 1
H H2A 0.1942 -0.1782 0.4929 0.055 Uiso calc R 1 1
H H2B 0.1746 -0.1220 0.6171 0.055 Uiso calc R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sb1 0.03064(17) 0.03064(17) 0.0344(2) 0.01532(8) 0.000 0.000
Cl1 0.0455(4) 0.0526(4) 0.0598(4) 0.0228(3) -0.0171(3) -0.0090(3)
O1 0.0365(9) 0.0382(8) 0.0517(10) 0.0178(7) 0.0061(7) 0.0003(7)
N1 0.033(2) 0.033(2) 0.074(5) 0.0167(10) 0.000 0.000
C1 0.0356(12) 0.0528(15) 0.0536(15) 0.0250(11) -0.0006(10) -0.0075(12)
C2 0.0462(14) 0.0483(14) 0.0553(15) 0.0320(12) -0.0090(11) -0.0060(11)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 Sb1 Cl1 . 10 180 ?
Cl1 Sb1 Cl1 . 2 89.88(3) ?
Cl1 Sb1 Cl1 10 2 90.12(3) ?
Cl1 Sb1 Cl1 . 12 90.12(3) ?
Cl1 Sb1 Cl1 10 12 89.88(3) ?
Cl1 Sb1 Cl1 2 12 90.12(3) ?
Cl1 Sb1 Cl1 . 11 90.12(3) ?
Cl1 Sb1 Cl1 10 11 89.88(3) ?
Cl1 Sb1 Cl1 2 11 180 ?
Cl1 Sb1 Cl1 12 11 89.88(3) ?
Cl1 Sb1 Cl1 . 3 89.88(3) y
Cl1 Sb1 Cl1 10 3 90.12(3) ?
Cl1 Sb1 Cl1 2 3 89.88(3) ?
Cl1 Sb1 Cl1 12 3 180 ?
Cl1 Sb1 Cl1 11 3 90.12(3) ?
C2 O1 C1 12_556 . 112.75(18) ?
H1 N1 H2 . . 109.5 ?
O1 C1 C2 . . 109.3(2) ?
O1 C1 H1A . . 109.8 ?
C2 C1 H1A . . 109.8 ?
O1 C1 H1B . . 109.8 ?
C2 C1 H1B . . 109.8 ?
H1A C1 H1B . . 108.3 ?
O1 C2 C1 11_556 . 109.2(2) ?
O1 C2 H2A 11_556 . 109.8 ?
C1 C2 H2A . . 109.8 ?
O1 C2 H2B 11_556 . 109.8 ?
C1 C2 H2B . . 109.8 ?
H2A C2 H2B . . 108.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sb1 Cl1 . 2.3707(6) y
Sb1 Cl1 10 2.3707(6) ?
Sb1 Cl1 2 2.3707(6) ?
Sb1 Cl1 12 2.3707(6) ?
Sb1 Cl1 11 2.3707(6) ?
Sb1 Cl1 3 2.3707(6) ?
O1 C2 12_556 1.422(3) ?
O1 C1 . 1.426(3) ?
N1 H1 . 0.9000 ?
N1 H2 . 0.9000 ?
C1 C2 . 1.495(4) ?
C1 H1A . 0.9800 ?
C1 H1B . 0.9800 ?
C2 H2A . 0.9800 ?
C2 H2B . 0.9800 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H2 O1 . 0.90 2.06 2.928(3) 162 yes
N1 H1 Cl1 . 0.90 3.01 3.746(7) 140 yes
C2 H2A Cl1 18_545 0.98 3.09 3.798(3) 130 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C2 O1 C1 C2 12_556 . 176.61(17) y
O1 C1 C2 O1 . 11_556 68.8(3) y
