#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/97/2239700.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_2239700
loop_
_publ_author_name
'Kaas, Marina'
'Friedrich, Ute'
'Korber, Nikolaus'
_publ_section_title
;
 (18-Crown-6)potassium(I) diphenylstibate({-}1)
;
_journal_coeditor_code           FF2129
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m260
_journal_paper_doi               10.1107/S1600536814013282
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[K (C12 H24 O6)] [Sb (C6 H5)2]'
_chemical_formula_moiety         'C12 H24 K O6 +, C12 H10 Sb -'
_chemical_formula_sum            'C24 H34 K O6 Sb'
_chemical_formula_weight         579.36
_chemical_name_common
'(18-Crown-6)potassium(I) diphenylstibate(-1)'
_chemical_name_systematic
;
(1,4,7,10,13,16-Hexaoxacyclooctadecane)potassium diphenylstibide
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 112.654(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6933(9)
_cell_length_b                   9.2655(3)
_cell_length_c                   19.1321(10)
_cell_measurement_reflns_used    1900
_cell_measurement_temperature    123
_cell_measurement_theta_max      28.0290
_cell_measurement_theta_min      3.3880
_cell_volume                     2567.3(2)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'OLEX2 (Dolomanov et al., 2009; Bourhis et al., 2011)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      123
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Agilent SuperNova (Single source at offset, Eos)'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4194
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.366
_diffrn_reflns_theta_min         3.104
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.272
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
[CrysAlis PRO (Agilent, 2012), using a multi-faceted crystal
model based on expressions derived by Clark & Reid (1995)]
;
_exptl_crystal_colour            'clear reddish red'
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.4728
_exptl_crystal_size_mid          0.2702
_exptl_crystal_size_min          0.1505
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.562
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0293
_refine_ls_R_factor_gt           0.0232
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0190P)²+0.7904P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0534
_reflns_number_gt                2297
_reflns_number_total             2592
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ff2129sup1.cf
_cod_data_source_block           I
_cod_database_code               2239700
_cod_database_fobs_code          2239700
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
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_occupancy
Sb Sb1 0.7500 1.08580(2) 1.0000 0.02163(8) Uani d 1
K K1 0.7500 0.7500 0.7500 0.02190(15) Uani d 1
O O2 0.62864(10) 0.83061(17) 0.60590(8) 0.0237(3) Uani d 1
O O3 0.74551(10) 1.03820(17) 0.70288(8) 0.0241(4) Uani d 1
O O1 0.60734(10) 0.56706(17) 0.66609(8) 0.0225(3) Uani d 1
C C1 0.67008(14) 0.9316(2) 0.91614(11) 0.0191(5) Uani d 1
C C10 0.54293(15) 0.7554(3) 0.57688(12) 0.0278(5) Uani d 1
H H10A 0.5106 0.7774 0.5236 0.033 Uiso calc 1
H H10B 0.5045 0.7855 0.6036 0.033 Uiso calc 1
C C4 0.56109(15) 0.7424(3) 0.79930(12) 0.0279(5) Uani d 1
H H4 0.5263 0.6798 0.7609 0.033 Uiso calc 1
C C11 0.61898(16) 0.9803(3) 0.58922(12) 0.0292(5) Uani d 1
H H11A 0.5781 1.0236 0.6106 0.035 Uiso calc 1
H H11B 0.5924 0.9947 0.5348 0.035 Uiso calc 1
C C3 0.59436(14) 0.6990(3) 0.87465(12) 0.0249(5) Uani d 1
H H3 0.5813 0.6068 0.8870 0.030 Uiso calc 1
C C7 0.66870(16) 0.3883(3) 0.76152(13) 0.0286(5) Uani d 1
H H7A 0.6253 0.4205 0.7831 0.034 Uiso calc 1
H H7B 0.6779 0.2853 0.7701 0.034 Uiso calc 1
C C2 0.64697(14) 0.7928(3) 0.93162(12) 0.0215(5) Uani d 1
H H2 0.6675 0.7622 0.9817 0.026 Uiso calc 1
C C5 0.58069(15) 0.8799(3) 0.78264(12) 0.0283(6) Uani d 1
H H5 0.5577 0.9111 0.7326 0.034 Uiso calc 1
C C9 0.56103(15) 0.5973(3) 0.58705(12) 0.0256(5) Uani d 1
H H9A 0.5032 0.5446 0.5668 0.031 Uiso calc 1
H H9B 0.5991 0.5670 0.5600 0.031 Uiso calc 1
C C8 0.63067(16) 0.4186(3) 0.67829(13) 0.0267(5) Uani d 1
H H8A 0.6763 0.3946 0.6574 0.032 Uiso calc 1
H H8B 0.5762 0.3600 0.6530 0.032 Uiso calc 1
C C12 0.71193(16) 1.0495(3) 0.62224(12) 0.0276(5) Uani d 1
H H12A 0.7541 1.0016 0.6037 0.033 Uiso calc 1
H H12B 0.7075 1.1502 0.6074 0.033 Uiso calc 1
C C6 0.63440(15) 0.9725(3) 0.83964(12) 0.0248(5) Uani d 1
H H6 0.6471 1.0645 0.8267 0.030 Uiso calc 1
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'
K K 0.2009 0.2494 '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'
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
C1 Sb1 C1 . 2_657 96.89(12)
O2 K1 O2 . 7_666 180.00(6)
O2 K1 O3 7_666 7_666 60.27(4)
O2 K1 O3 7_666 . 119.73(4)
O2 K1 O3 . 7_666 119.73(4)
O2 K1 O3 . . 60.27(4)
O2 K1 C4 . . 86.78(5)
O2 K1 C4 . 7_666 93.22(5)
O2 K1 C4 7_666 . 93.22(5)
O2 K1 C4 7_666 7_666 86.78(5)
O2 K1 C5 . . 77.81(5)
O2 K1 C5 . 7_666 102.19(5)
O2 K1 C5 7_666 7_666 77.81(5)
O2 K1 C5 7_666 . 102.19(5)
O3 K1 O3 . 7_666 180.0
O3 K1 C4 . 7_666 79.08(5)
O3 K1 C4 7_666 7_666 100.92(5)
O3 K1 C4 . . 100.92(5)
O3 K1 C4 7_666 . 79.08(5)
O3 K1 C5 . 7_666 102.44(6)
O3 K1 C5 7_666 7_666 77.56(6)
O3 K1 C5 7_666 . 102.44(6)
O3 K1 C5 . . 77.56(6)
O1 K1 O2 . . 59.91(4)
O1 K1 O2 . 7_666 120.09(5)
O1 K1 O2 7_666 7_666 59.91(5)
O1 K1 O2 7_666 . 120.09(5)
O1 K1 O3 7_666 . 61.31(4)
O1 K1 O3 . 7_666 61.31(4)
O1 K1 O3 7_666 7_666 118.69(4)
O1 K1 O3 . . 118.69(4)
O1 K1 O1 7_666 . 180.0
O1 K1 C4 7_666 . 116.26(5)
O1 K1 C4 . 7_666 116.26(5)
O1 K1 C4 . . 63.74(5)
O1 K1 C4 7_666 7_666 63.74(5)
O1 K1 C5 . . 78.25(5)
O1 K1 C5 7_666 7_666 78.25(5)
O1 K1 C5 7_666 . 101.75(5)
O1 K1 C5 . 7_666 101.75(5)
C4 K1 C4 . 7_666 180.00(10)
C5 K1 C4 . . 23.57(6)
C5 K1 C4 7_666 7_666 23.57(6)
C5 K1 C4 . 7_666 156.43(6)
C5 K1 C4 7_666 . 156.43(6)
C5 K1 C5 7_666 . 180.0
C10 O2 K1 . . 115.99(12)
C11 O2 K1 . . 117.29(12)
C11 O2 C10 . . 112.83(17)
C7 O3 K1 7_666 . 113.46(12)
C7 O3 C12 7_666 . 111.61(16)
C12 O3 K1 . . 111.65(13)
C9 O1 K1 . . 117.40(12)
C8 O1 K1 . . 113.42(12)
C8 O1 C9 . . 110.95(17)
C2 C1 Sb1 . . 125.20(15)
C2 C1 C6 . . 115.9(2)
C6 C1 Sb1 . . 118.81(17)
O2 C10 H10A . . 109.9
O2 C10 H10B . . 109.9
O2 C10 C9 . . 109.03(18)
H10A C10 H10B . . 108.3
C9 C10 H10A . . 109.9
C9 C10 H10B . . 109.9
K1 C4 H4 . . 95.9
C3 C4 K1 . . 105.73(13)
C3 C4 H4 . . 120.7
C5 C4 K1 . . 67.95(13)
C5 C4 H4 . . 120.7
C5 C4 C3 . . 118.7(2)
O2 C11 H11A . . 109.9
O2 C11 H11B . . 109.9
O2 C11 C12 . . 108.82(18)
H11A C11 H11B . . 108.3
C12 C11 H11A . . 109.9
C12 C11 H11B . . 109.9
C4 C3 H3 . . 119.8
C2 C3 C4 . . 120.3(2)
C2 C3 H3 . . 119.8
O3 C7 H7A 7_666 . 109.8
O3 C7 H7B 7_666 . 109.8
O3 C7 C8 7_666 . 109.56(18)
H7A C7 H7B . . 108.2
C8 C7 H7A . . 109.8
C8 C7 H7B . . 109.8
C1 C2 H2 . . 118.9
C3 C2 C1 . . 122.2(2)
C3 C2 H2 . . 118.9
K1 C5 H5 . . 86.5
C4 C5 K1 . . 88.49(14)
C4 C5 H5 . . 119.6
C4 C5 C6 . . 120.8(2)
C6 C5 K1 . . 95.02(14)
C6 C5 H5 . . 119.6
O1 C9 C10 . . 108.91(18)
O1 C9 H9A . . 109.9
O1 C9 H9B . . 109.9
C10 C9 H9A . . 109.9
C10 C9 H9B . . 109.9
H9A C9 H9B . . 108.3
O1 C8 C7 . . 109.22(18)
O1 C8 H8A . . 109.8
O1 C8 H8B . . 109.8
C7 C8 H8A . . 109.8
C7 C8 H8B . . 109.8
H8A C8 H8B . . 108.3
O3 C12 C11 . . 108.62(18)
O3 C12 H12A . . 110.0
O3 C12 H12B . . 110.0
C11 C12 H12A . . 110.0
C11 C12 H12B . . 110.0
H12A C12 H12B . . 108.3
C1 C6 H6 . . 119.0
C5 C6 C1 . . 122.0(2)
C5 C6 H6 . . 119.0
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 C1 . 2.154(2) y
K1 O2 . 2.7823(14) y
K1 O3 . 2.8106(16) y
K1 O1 . 2.7738(15) y
K1 C4 . 3.441(2) ?
K1 C5 . 3.190(2) ?
O2 C10 . 1.424(3) ?
O2 C11 . 1.418(3) ?
O3 C7 7_666 1.426(3) ?
O3 C12 . 1.429(2) ?
O1 C9 . 1.431(2) ?
O1 C8 . 1.419(3) ?
C1 C2 . 1.399(3) ?
C1 C6 . 1.403(3) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C10 C9 . 1.490(3) ?
C4 H4 . 0.9300 ?
C4 C3 . 1.390(3) ?
C4 C5 . 1.376(3) ?
C11 H11A . 0.9700 ?
C11 H11B . 0.9700 ?
C11 C12 . 1.493(3) ?
C3 H3 . 0.9300 ?
C3 C2 . 1.390(3) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C7 C8 . 1.496(3) ?
C2 H2 . 0.9300 ?
C5 H5 . 0.9300 ?
C5 C6 . 1.389(3) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
C8 H8A . 0.9700 ?
C8 H8B . 0.9700 ?
C12 H12A . 0.9700 ?
C12 H12B . 0.9700 ?
C6 H6 . 0.9300 ?
