#------------------------------------------------------------------------------
#$Date: 2016-11-09 04:05:16 +0200 (Wed, 09 Nov 2016) $
#$Revision: 188332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/24/19/2241934.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_2241934
loop_
_publ_author_name
'Liebing, Phil'
'Zaeni, Ahmad'
'Olbrich, Falk'
'Edelmann, Frank T.'
_publ_section_title
;
 Crystal structures of two solvates of (18-crown-6)potassium acetate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1757
_journal_page_last               1761
_journal_paper_doi               10.1107/S2056989016017436
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'[K (C2 H3 O2) (C12 H24 O6) (H2 O)], C2 H4 O2'
_chemical_formula_moiety         'C14 H29 K O9, C2 H4 O2'
_chemical_formula_sum            'C16 H33 K O11'
_chemical_formula_weight         440.52
_chemical_name_common
;
Acetatoaqua(18-crown-6)potassium acetic acid monosolvate
;
_chemical_name_systematic
;
(Acetato-κ²O,O')aqua(1,4,7,10,13,16-hexaoxacyclooctadecane-\
κ⁶O)potassium acetic acid monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/4
_cell_angle_alpha                90
_cell_angle_beta                 99.0530(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.32330(10)
_cell_length_b                   8.54500(10)
_cell_length_c                   23.3869(3)
_cell_measurement_reflns_used    100
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.00
_cell_volume                     2234.67(4)
_computing_cell_refinement
;
SAINT (Bruker, 2001)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT (Bruker, 2001)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 1999)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2016 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            13151
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.998
_diffrn_reflns_theta_min         1.763
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_correction_T_min  0.8933
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2001)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.305
_refine_ls_extinction_coef       0.0064(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2016 (Sheldrick, 2015)
;
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4846
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0407
_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)+(0.0411P)²+0.8233P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                3833
_reflns_number_total             4846
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            hb7621sup1.cif
_cod_data_source_block           2
_cod_database_code               2241934
_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.
;
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.945
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'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
C C1 -0.26514(15) 0.3641(2) 0.59639(8) 0.0344(4) Uani d 1
H H1A -0.295602 0.316810 0.629859 0.041 Uiso calc 1
H H1B -0.325899 0.348656 0.561493 0.041 Uiso calc 1
C C2 -0.24318(16) 0.5356(2) 0.60680(8) 0.0339(4) Uani d 1
H H2A -0.211614 0.582388 0.573534 0.041 Uiso calc 1
H H2B -0.319274 0.588713 0.610600 0.041 Uiso calc 1
C C3 -0.12935(17) 0.7194(2) 0.66672(8) 0.0326(4) Uani d 1
H H3A -0.202139 0.780529 0.670253 0.039 Uiso calc 1
H H3B -0.095777 0.759557 0.632950 0.039 Uiso calc 1
C C4 -0.03993(17) 0.7378(2) 0.72029(8) 0.0322(4) Uani d 1
H H4A -0.027326 0.850197 0.729470 0.039 Uiso calc 1
H H4B -0.069596 0.686669 0.753275 0.039 Uiso calc 1
C C5 0.15966(17) 0.6830(2) 0.76087(8) 0.0318(4) Uani d 1
H H5A 0.136112 0.624324 0.793796 0.038 Uiso calc 1
H H5B 0.169625 0.794519 0.772089 0.038 Uiso calc 1
C C6 0.27450(17) 0.6196(2) 0.74649(9) 0.0347(4) Uani d 1
H H6A 0.292850 0.668968 0.710610 0.042 Uiso calc 1
H H6B 0.340818 0.642839 0.778267 0.042 Uiso calc 1
C C7 0.36809(16) 0.3840(2) 0.72475(9) 0.0357(4) Uani d 1
H H7A 0.436684 0.406551 0.755438 0.043 Uiso calc 1
H H7B 0.386265 0.426119 0.687675 0.043 Uiso calc 1
C C8 0.34709(17) 0.2111(2) 0.71987(9) 0.0374(5) Uani d 1
H H8A 0.421645 0.157251 0.713968 0.045 Uiso calc 1
H H8B 0.322839 0.170756 0.755975 0.045 Uiso calc 1
C C9 0.22477(18) 0.0196(2) 0.66723(9) 0.0373(5) Uani d 1
H H9A 0.188685 -0.013663 0.701176 0.045 Uiso calc 1
H H9B 0.297603 -0.043805 0.666202 0.045 Uiso calc 1
C C10 0.13805(17) -0.0062(2) 0.61311(9) 0.0370(5) Uani d 1
H H10A 0.170412 0.037599 0.579565 0.044 Uiso calc 1
H H10B 0.124689 -0.119710 0.606545 0.044 Uiso calc 1
C C11 -0.05449(18) 0.0615(2) 0.56565(8) 0.0347(4) Uani d 1
H H11A -0.065285 -0.048774 0.552956 0.042 Uiso calc 1
H H11B -0.022018 0.120701 0.535208 0.042 Uiso calc 1
C C12 -0.17179(17) 0.1291(2) 0.57418(8) 0.0341(4) Uani d 1
H H12A -0.230412 0.117291 0.538289 0.041 Uiso calc 1
H H12B -0.202776 0.072861 0.605745 0.041 Uiso calc 1
C C13 0.26513(17) 0.4042(3) 0.54918(9) 0.0395(5) Uani d 1
C C14 0.3933(2) 0.3558(4) 0.54951(12) 0.0628(7) Uani d 1
H H14A 0.441672 0.448409 0.544505 0.075 Uiso calc 1
H H14B 0.397490 0.282164 0.517759 0.075 Uiso calc 1
H H14C 0.424067 0.305288 0.586489 0.075 Uiso calc 1
C C15 0.46601(19) 0.7951(3) 0.60242(11) 0.0458(5) Uani d 1
C C16 0.5436(3) 0.9332(3) 0.59606(15) 0.0734(8) Uani d 1
H H16A 0.588137 0.915124 0.563968 0.088 Uiso calc 1
H H16B 0.599944 0.948428 0.631968 0.088 Uiso calc 1
H H16C 0.493720 1.026816 0.588064 0.088 Uiso calc 1
O O1 -0.15612(11) 0.29088(15) 0.58855(6) 0.0329(3) Uani d 1
O O2 -0.15927(11) 0.55729(14) 0.65841(5) 0.0299(3) Uani d 1
O O3 0.06996(11) 0.66769(15) 0.71136(5) 0.0298(3) Uani d 1
O O4 0.26219(11) 0.45464(14) 0.73867(6) 0.0311(3) Uani d 1
O O5 0.25553(11) 0.18135(14) 0.67223(5) 0.0322(3) Uani d 1
O O6 0.02708(11) 0.06945(14) 0.61872(5) 0.0319(3) Uani d 1
O O7 0.24709(14) 0.5417(2) 0.56419(9) 0.0654(5) Uani d 1
O O8 0.18335(13) 0.30957(19) 0.53554(6) 0.0459(4) Uani d 1
O O9 0.01027(12) 0.64125(16) 0.55199(6) 0.0339(3) Uani d 1
H H2 -0.0421(19) 0.648(3) 0.5168(7) 0.066(8) Uiso d 1
H H1 0.0852(12) 0.616(3) 0.5426(10) 0.054(7) Uiso d 1
O O10 0.47534(17) 0.7214(2) 0.64660(8) 0.0707(5) Uani d 1
O O11 0.39035(17) 0.7625(3) 0.55675(8) 0.0718(6) Uani d 1
H H3 0.337(4) 0.662(6) 0.564(2) 0.165(18) Uiso d 1
K K 0.06834(3) 0.40782(4) 0.63478(2) 0.02625(12) Uani d 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'
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
O1 C1 C2 109.02(15)
O1 C1 H1A 109.9
C2 C1 H1A 109.9
O1 C1 H1B 109.9
C2 C1 H1B 109.9
H1A C1 H1B 108.3
O2 C2 C1 109.61(15)
O2 C2 H2A 109.7
C1 C2 H2A 109.7
O2 C2 H2B 109.7
C1 C2 H2B 109.7
H2A C2 H2B 108.2
O2 C3 C4 109.30(14)
O2 C3 H3A 109.8
C4 C3 H3A 109.8
O2 C3 H3B 109.8
C4 C3 H3B 109.8
H3A C3 H3B 108.3
O3 C4 C3 109.03(14)
O3 C4 H4A 109.9
C3 C4 H4A 109.9
O3 C4 H4B 109.9
C3 C4 H4B 109.9
H4A C4 H4B 108.3
O3 C5 C6 108.58(14)
O3 C5 H5A 110.0
C6 C5 H5A 110.0
O3 C5 H5B 110.0
C6 C5 H5B 110.0
H5A C5 H5B 108.4
O4 C6 C5 108.44(15)
O4 C6 H6A 110.0
C5 C6 H6A 110.0
O4 C6 H6B 110.0
C5 C6 H6B 110.0
H6A C6 H6B 108.4
O4 C7 C8 107.82(15)
O4 C7 H7A 110.1
C8 C7 H7A 110.1
O4 C7 H7B 110.1
C8 C7 H7B 110.1
H7A C7 H7B 108.5
O5 C8 C7 108.89(15)
O5 C8 H8A 109.9
C7 C8 H8A 109.9
O5 C8 H8B 109.9
C7 C8 H8B 109.9
H8A C8 H8B 108.3
O5 C9 C10 109.42(15)
O5 C9 H9A 109.8
C10 C9 H9A 109.8
O5 C9 H9B 109.8
C10 C9 H9B 109.8
H9A C9 H9B 108.2
O6 C10 C9 108.94(15)
O6 C10 H10A 109.9
C9 C10 H10A 109.9
O6 C10 H10B 109.9
C9 C10 H10B 109.9
H10A C10 H10B 108.3
O6 C11 C12 109.49(14)
O6 C11 H11A 109.8
C12 C11 H11A 109.8
O6 C11 H11B 109.8
C12 C11 H11B 109.8
H11A C11 H11B 108.2
O1 C12 C11 109.04(15)
O1 C12 H12A 109.9
C11 C12 H12A 109.9
O1 C12 H12B 109.9
C11 C12 H12B 109.9
H12A C12 H12B 108.3
O8 C13 O7 122.60(19)
O8 C13 C14 120.3(2)
O7 C13 C14 117.1(2)
O8 C13 K 66.57(11)
O7 C13 K 69.97(12)
C14 C13 K 139.36(15)
C13 C14 H14A 109.5
C13 C14 H14B 109.5
H14A C14 H14B 109.5
C13 C14 H14C 109.5
H14A C14 H14C 109.5
H14B C14 H14C 109.5
O10 C15 O11 123.8(2)
O10 C15 C16 121.8(2)
O11 C15 C16 114.4(2)
C15 C16 H16A 109.5
C15 C16 H16B 109.5
H16A C16 H16B 109.5
C15 C16 H16C 109.5
H16A C16 H16C 109.5
H16B C16 H16C 109.5
C1 O1 C12 112.24(14)
C1 O1 K 123.36(10)
C12 O1 K 120.72(10)
C2 O2 C3 110.62(14)
C2 O2 K 105.41(10)
C3 O2 K 104.17(10)
C5 O3 C4 111.74(13)
C5 O3 K 121.11(10)
C4 O3 K 119.97(10)
C7 O4 C6 112.30(14)
C7 O4 K 106.86(10)
C6 O4 K 106.08(10)
C8 O5 C9 112.12(14)
C8 O5 K 121.71(10)
C9 O5 K 117.67(10)
C11 O6 C10 110.78(14)
C11 O6 K 103.03(10)
C10 O6 K 109.26(10)
C13 O7 K 87.18(13)
C13 O7 H3 121.1(19)
K O7 H3 143.3(19)
C13 O8 K 90.94(13)
K O9 H2 134.4(17)
K O9 H1 82.7(15)
H2 O9 H1 106(2)
C15 O11 H3 111(3)
O9 K O1 83.45(4)
O9 K O3 81.74(4)
O1 K O3 116.00(4)
O9 K O5 140.23(4)
O1 K O5 117.15(4)
O3 K O5 113.43(4)
O9 K O6 126.82(4)
O1 K O6 58.76(4)
O3 K O6 146.14(4)
O5 K O6 58.48(4)
O9 K O8 75.08(4)
O1 K O8 94.65(4)
O3 K O8 138.97(4)
O5 K O8 69.91(4)
O6 K O8 72.63(4)
O9 K O2 73.02(4)
O1 K O2 57.81(4)
O3 K O2 58.28(3)
O5 K O2 146.61(4)
O6 K O2 108.51(4)
O8 K O2 139.62(4)
O9 K O7 57.03(5)
O1 K O7 124.80(5)
O3 K O7 96.28(4)
O5 K O7 84.11(4)
O6 K O7 114.05(4)
O8 K O7 42.69(5)
O2 K O7 127.27(4)
O9 K O4 121.61(4)
O1 K O4 149.21(4)
O3 K O4 57.44(3)
O5 K O4 56.23(3)
O6 K O4 108.18(4)
O8 K O4 108.28(4)
O2 K O4 109.28(4)
O7 K O4 85.72(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
C1 O1 1.421(2) ?
C1 C2 1.500(3) ?
C1 H1A 0.9900 ?
C1 H1B 0.9900 ?
C2 O2 1.426(2) ?
C2 H2A 0.9900 ?
C2 H2B 0.9900 ?
C3 O2 1.432(2) ?
C3 C4 1.490(3) ?
C3 H3A 0.9900 ?
C3 H3B 0.9900 ?
C4 O3 1.426(2) ?
C4 H4A 0.9900 ?
C4 H4B 0.9900 ?
C5 O3 1.421(2) ?
C5 C6 1.495(3) ?
C5 H5A 0.9900 ?
C5 H5B 0.9900 ?
C6 O4 1.425(2) ?
C6 H6A 0.9900 ?
C6 H6B 0.9900 ?
C7 O4 1.425(2) ?
C7 C8 1.498(3) ?
C7 H7A 0.9900 ?
C7 H7B 0.9900 ?
C8 O5 1.420(2) ?
C8 H8A 0.9900 ?
C8 H8B 0.9900 ?
C9 O5 1.426(2) ?
C9 C10 1.491(3) ?
C9 H9A 0.9900 ?
C9 H9B 0.9900 ?
C10 O6 1.437(2) ?
C10 H10A 0.9900 ?
C10 H10B 0.9900 ?
C11 O6 1.427(2) ?
C11 C12 1.490(3) ?
C11 H11A 0.9900 ?
C11 H11B 0.9900 ?
C12 O1 1.427(2) ?
C12 H12A 0.9900 ?
C12 H12B 0.9900 ?
C13 O8 1.233(3) ?
C13 O7 1.252(3) ?
C13 C14 1.508(3) ?
C13 K 3.221(2) ?
C14 H14A 0.9800 ?
C14 H14B 0.9800 ?
C14 H14C 0.9800 ?
C15 O10 1.201(3) ?
C15 O11 1.290(3) ?
C15 C16 1.493(3) ?
C16 H16A 0.9800 ?
C16 H16B 0.9800 ?
C16 H16C 0.9800 ?
K O1 2.7861(12) y
K O2 3.0045(13) y
K O3 2.8510(12) y
K O4 3.0337(13) y
K O5 2.9019(13) y
K O6 2.9435(13) y
K O7 3.0303(19) y
K O8 2.9562(16) y
K O9 2.7855(14) y
O9 H2 0.937(10) ?
O9 H1 0.935(10) ?
O11 H3 1.08(5) ?
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
O9 H1 O7 . 0.935(10) 1.93(2) 2.785(7) 151(9)
O9 H2 O8 3_566 0.937(10) 1.89(2) 2.786(7) 160(9)
O11 H3 O7 . 1.08(5) 1.43(5) 2.513(6) 168(5)
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
O1 C1 C2 O2 -61.89(19)
O2 C3 C4 O3 67.56(18)
O3 C5 C6 O4 -67.82(18)
O4 C7 C8 O5 65.00(19)
O5 C9 C10 O6 -67.21(19)
O6 C11 C12 O1 63.41(19)
C2 C1 O1 C12 -175.70(15)
C2 C1 O1 K 25.89(19)
C11 C12 O1 C1 178.99(15)
C11 C12 O1 K -21.96(18)
C1 C2 O2 C3 175.23(15)
C1 C2 O2 K 63.21(15)
C4 C3 O2 C2 -178.92(14)
C4 C3 O2 K -66.11(14)
C6 C5 O3 C4 -175.13(15)
C6 C5 O3 K 34.54(18)
C3 C4 O3 C5 179.29(14)
C3 C4 O3 K -29.99(18)
C8 C7 O4 C6 177.77(15)
C8 C7 O4 K -66.31(15)
C5 C6 O4 C7 -179.99(15)
C5 C6 O4 K 63.62(15)
C7 C8 O5 C9 -175.98(15)
C7 C8 O5 K -28.8(2)
C10 C9 O5 C8 -174.05(15)
C10 C9 O5 K 37.31(18)
C12 C11 O6 C10 175.38(15)
C12 C11 O6 K -67.88(14)
C9 C10 O6 C11 174.01(15)
C9 C10 O6 K 61.18(16)
O8 C13 O7 K 42.6(2)
C14 C13 O7 K -136.11(18)
O7 C13 O8 K -43.9(2)
C14 C13 O8 K 134.79(19)

_cod_database_fobs_code 2241934
