#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:56:20 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179996 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/90/7029097.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_7029097
loop_
_publ_author_name
'Perrin, Andrea'
'Myers, Dominic'
'Fucke, Katharina'
'Musa, Osama M.'
'Steed, Jonathan W.'
_publ_section_title
;
 N-Alkyl pyrrolidone ether podands as versatile alkali metal ion chelants.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3153
_journal_page_last               3161
_journal_paper_doi               10.1039/c3dt53001a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C48 H84 F24 K4 N8 O14 P4'
_chemical_formula_sum            'C48 H84 F24 K4 N8 O14 P4'
_chemical_formula_weight         1733.51
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-25
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 120.757(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   28.4413(11)
_cell_length_b                   12.8337(3)
_cell_length_c                   23.8944(8)
_cell_measurement_reflns_used    14684
_cell_measurement_temperature    120
_cell_measurement_theta_max      32.2487
_cell_measurement_theta_min      2.6810
_cell_volume                     7494.9(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -52.00   38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604   57.0000  120.0000 90

  2 omega -100.00   -3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -57.0000  -30.0000 97

  3 omega -114.00  -35.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  179.0000 -180.0000 79

  4 omega  -35.00   45.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292  -57.0000 -180.0000 80

  5 omega   68.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292  179.0000  -90.0000 25

  6 omega   47.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292 -127.0000  147.0000 49

  7 omega  -18.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3292    0.0000  -30.0000 89

  8 omega -105.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -57.0000   60.0000 103

  9 omega -105.00   -2.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -57.0000 -150.0000 103

 10 omega -119.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  179.0000  -90.0000 87

 11 omega -107.00    5.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.8604  -77.0000  150.0000 112
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0128049000
_diffrn_orient_matrix_UB_12      -0.0044629000
_diffrn_orient_matrix_UB_13      0.0187484000
_diffrn_orient_matrix_UB_21      0.0256829000
_diffrn_orient_matrix_UB_22      0.0071095000
_diffrn_orient_matrix_UB_23      0.0289124000
_diffrn_orient_matrix_UB_31      -0.0043836000
_diffrn_orient_matrix_UB_32      0.0546146000
_diffrn_orient_matrix_UB_33      -0.0022143000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            57703
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.69
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.443
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72909
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3568
_exptl_crystal_size_max          0.941
_exptl_crystal_size_mid          0.6432
_exptl_crystal_size_min          0.3017
_refine_diff_density_max         1.150
_refine_diff_density_min         -1.179
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         8606
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0677
_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)+(0.0654P)²+32.6055P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                7330
_reflns_number_total             8606
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt53001a.txt
_cod_data_source_block           ap61_1
_cod_original_cell_volume        7494.9(4)
_cod_database_code               7029097
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         'C12 H20 N2 O3 K P F6'
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H19A,H19B} of C19, {H20A,H20B} of C20, {H24A,H24B} of C24, {H22A,H22B} of
  C22, {H23A,H23B} of C23, {H2AA,H2AB} of C2A, {H3AA,H3AB} of C3A, {H4AA,H4AB}
  of C4A, {H10C,H10D} of C10A, {H11C,H11D} of C11A, {H12C,H12D} of C12A, {H14A,
  H14B} of C14, {H7A,H7B} of C7, {H1,H5} of C5, {H17A,H17B} of C17, {H15A,H15B}
  of C15, {H18A,H18B} of C18, {H10A,H10B} of C10B, {H16A,H16B} of C16, {H4BA,
  H4BB} of C4B, {H2BA,H2BB} of C2B, {H3BA,H3BB} of C3B, {H11A,H11B} of C11B,
  {H8A,H8B} of C8, {H12A,H12B} of C12B, {H6A,H6B} of C6
2. Others
 1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=
 1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=1-Sof(O1B)=Sof(O1A)=Sof(C1A)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)
 1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-
 Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=1-Sof(C10B)=Sof(O3A)=Sof(C9A)=
 Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=Sof(C12A)=
 Sof(H12C)=Sof(H12D)
 Fixed Sof: O1S(0.5) O2S(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C15(H15A,H15B), C17(H17A,H17B), C5(H1,H5), C7(H7A,H7B),
 C14(H14A,H14B), C10B(H10A,H10B), C16(H16A,H16B), C4B(H4BA,H4BB), C2B(H2BA,
 H2BB), C3B(H3BA,H3BB), C11B(H11A,H11B), C8(H8A,H8B), C12B(H12A,H12B), C6(H6A,
 H6B), C19(H19A,H19B), C20(H20A,H20B), C24(H24A,H24B), C22(H22A,H22B), C23(H23A,
 H23B), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C10A(H10C,H10D),
 C11A(H11C,H11D), C12A(H12C,H12D)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z+1/2'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -z+1/2'
5 '-x, -y, -z'
6 'x, -y, z-1/2'
7 '-x+1/2, -y+1/2, -z'
8 'x+1/2, -y+1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.08137(3) 0.41054(5) 0.30795(4) 0.03617(17) Uani 1 1 d . . .
P2 P 0.11724(3) 0.87079(7) 0.48114(4) 0.03173(19) Uani 1 1 d . . .
K2 K 0.06747(3) 0.73229(6) 0.33339(3) 0.03864(19) Uani 1 1 d . . .
P1 P 0.19229(5) 0.26517(8) 0.30614(6) 0.0508(3) Uani 1 1 d . . .
O2 O 0.12243(9) 0.27565(19) 0.42211(11) 0.0393(5) Uani 1 1 d . A .
O4 O -0.03467(10) 0.8187(2) 0.28831(12) 0.0513(7) Uani 1 1 d . . .
N3 N -0.10379(12) 0.9215(2) 0.27884(15) 0.0434(7) Uani 1 1 d . A .
N1 N 0.01331(14) 0.2003(3) 0.37394(17) 0.0523(8) Uani 1 1 d . . .
F3 F 0.17959(12) 0.1812(3) 0.25312(16) 0.0917(11) Uani 1 1 d . A .
C13 C -0.06373(12) 0.8508(3) 0.30910(16) 0.0402(8) Uani 1 1 d . . .
F2 F 0.13232(14) 0.2380(2) 0.2947(2) 0.1016(13) Uani 1 1 d . A .
F4 F 0.24902(12) 0.2921(3) 0.31467(19) 0.0943(11) Uani 1 1 d . A .
C18 C -0.17242(16) 0.9340(3) 0.16118(19) 0.0498(9) Uani 1 1 d . A .
H18A H -0.2019 0.9512 0.1701 0.060 Uiso 1 1 calc R . .
H18B H -0.1806 0.9690 0.1203 0.060 Uiso 1 1 calc R . .
C15 C -0.10767(18) 0.8749(4) 0.3711(2) 0.0590(11) Uani 1 1 d . . .
H15A H -0.1347 0.8238 0.3687 0.071 Uiso 1 1 calc R A .
H15B H -0.0943 0.9167 0.4113 0.071 Uiso 1 1 calc R . .
C17 C -0.11826(17) 0.9706(3) 0.2164(2) 0.0511(9) Uani 1 1 d . . .
H17A H -0.0894 0.9549 0.2061 0.061 Uiso 1 1 calc R A .
H17B H -0.1195 1.0471 0.2207 0.061 Uiso 1 1 calc R . .
C5 C 0.05151(18) 0.1562(3) 0.3575(2) 0.0549(10) Uani 1 1 d . A .
H1 H 0.0467 0.1910 0.3179 0.066 Uiso 1 1 calc R . .
H5 H 0.0432 0.0813 0.3474 0.066 Uiso 1 1 calc R . .
C9B C 0.0986(6) 0.5114(10) 0.4567(6) 0.036(2) Uani 0.54(2) 1 d P A 2
C7 C 0.17667(16) 0.2891(4) 0.4745(2) 0.0657(13) Uani 1 1 d . . .
H7A H 0.2027 0.2568 0.4638 0.079 Uiso 1 1 calc R A .
H7B H 0.1811 0.2551 0.5141 0.079 Uiso 1 1 calc R . .
C1B C -0.0144(7) 0.2735(12) 0.3443(8) 0.032(3) Uani 0.48(2) 1 d P A 2
N2 N 0.15103(19) 0.4560(3) 0.50246(16) 0.0702(11) Uani 1 1 d . . .
O1B O -0.0132(3) 0.3207(10) 0.2986(6) 0.044(3) Uani 0.48(2) 1 d P . 2
C14 C -0.06063(15) 0.8194(4) 0.37174(19) 0.0590(11) Uani 1 1 d . A .
H14A H -0.0253 0.8411 0.4098 0.071 Uiso 1 1 calc R . .
H14B H -0.0644 0.7429 0.3734 0.071 Uiso 1 1 calc R . .
C10B C 0.0646(7) 0.5350(14) 0.4851(9) 0.060(3) Uani 0.54(2) 1 d P A 2
H10A H 0.0574 0.6107 0.4835 0.072 Uiso 0.54(2) 1 calc PR A 2
H10B H 0.0293 0.4974 0.4617 0.072 Uiso 0.54(2) 1 calc PR A 2
C16 C -0.1331(2) 0.9436(5) 0.3130(3) 0.0785(16) Uani 1 1 d . A .
H16A H -0.1725 0.9278 0.2849 0.094 Uiso 1 1 calc R . .
H16B H -0.1290 1.0178 0.3260 0.094 Uiso 1 1 calc R . .
C4B C -0.0035(9) 0.1346(19) 0.4090(11) 0.069(5) Uani 0.48(2) 1 d P A 2
H4BA H 0.0267 0.1232 0.4543 0.083 Uiso 0.48(2) 1 calc PR A 2
H4BB H -0.0169 0.0665 0.3871 0.083 Uiso 0.48(2) 1 calc PR A 2
F6 F 0.21647(19) 0.1817(3) 0.35877(18) 0.1355(18) Uani 1 1 d . A .
C2B C -0.0486(9) 0.311(2) 0.3711(9) 0.063(4) Uani 0.48(2) 1 d P A 2
H2BA H -0.0854 0.3334 0.3364 0.075 Uiso 0.48(2) 1 calc PR A 2
H2BB H -0.0306 0.3679 0.4030 0.075 Uiso 0.48(2) 1 calc PR A 2
F5 F 0.16445(19) 0.3510(4) 0.2534(3) 0.184(3) Uani 1 1 d . A .
F1 F 0.1989(2) 0.3531(3) 0.3534(3) 0.159(2) Uani 1 1 d . A .
C3B C -0.0510(8) 0.201(3) 0.4067(13) 0.124(12) Uani 0.48(2) 1 d P A 2
H3BA H -0.0442 0.2144 0.4510 0.149 Uiso 0.48(2) 1 calc PR A 2
H3BB H -0.0868 0.1657 0.3806 0.149 Uiso 0.48(2) 1 calc PR A 2
C11B C 0.0975(9) 0.499(3) 0.5526(10) 0.100(8) Uani 0.54(2) 1 d P A 2
H11A H 0.0735 0.4647 0.5659 0.120 Uiso 0.54(2) 1 calc PR A 2
H11B H 0.1156 0.5588 0.5818 0.120 Uiso 0.54(2) 1 calc PR A 2
C8 C 0.1881(2) 0.4033(5) 0.4864(3) 0.0851(18) Uani 1 1 d . A .
H8A H 0.2262 0.4132 0.5226 0.102 Uiso 1 1 calc R . .
H8B H 0.1848 0.4358 0.4470 0.102 Uiso 1 1 calc R . .
C12B C 0.1408(9) 0.4210(15) 0.5585(8) 0.074(5) Uani 0.54(2) 1 d P A 2
H12A H 0.1269 0.3486 0.5517 0.089 Uiso 0.54(2) 1 calc PR A 2
H12B H 0.1747 0.4261 0.6016 0.089 Uiso 0.54(2) 1 calc PR A 2
C6 C 0.10934(16) 0.1676(3) 0.4107(2) 0.0490(9) Uani 1 1 d . . .
H6A H 0.1146 0.1342 0.4509 0.059 Uiso 1 1 calc R A .
H6B H 0.1338 0.1328 0.3984 0.059 Uiso 1 1 calc R . .
F7 F 0.09279(9) 0.91639(17) 0.40878(9) 0.0496(5) Uani 1 1 d . A .
F8 F 0.07010(8) 0.78482(19) 0.45174(10) 0.0516(6) Uani 1 1 d . A .
F9 F 0.14177(9) 0.8231(2) 0.55178(9) 0.0548(6) Uani 1 1 d . . .
F10 F 0.15482(9) 0.79400(19) 0.46853(11) 0.0516(5) Uani 1 1 d . A .
O5 O -0.16959(9) 0.82592(19) 0.15504(11) 0.0385(5) Uani 1 1 d . . .
F11 F 0.16388(11) 0.9564(2) 0.50858(13) 0.0758(9) Uani 1 1 d . . .
F12 F 0.07864(12) 0.9471(3) 0.49172(12) 0.0817(10) Uani 1 1 d . . .
C19 C -0.22082(12) 0.7826(3) 0.10545(15) 0.0432(9) Uani 1 1 d . A .
H19A H -0.2293 0.8074 0.0620 0.052 Uiso 1 1 calc R . .
H19B H -0.2507 0.8052 0.1126 0.052 Uiso 1 1 calc R . .
C20 C -0.21629(12) 0.6669(3) 0.10862(14) 0.0397(8) Uani 1 1 d . . .
H20A H -0.2507 0.6362 0.0733 0.048 Uiso 1 1 calc R A .
H20B H -0.1862 0.6452 0.1018 0.048 Uiso 1 1 calc R . .
N4 N -0.20591(10) 0.6275(2) 0.17083(12) 0.0327(6) Uani 1 1 d . A .
C21 C -0.15648(12) 0.6027(2) 0.21948(15) 0.0310(6) Uani 1 1 d . . .
C24 C -0.24833(15) 0.6252(4) 0.18876(19) 0.0521(10) Uani 1 1 d . . .
H24A H -0.2817 0.5892 0.1551 0.063 Uiso 1 1 calc R A .
H24B H -0.2581 0.6965 0.1950 0.063 Uiso 1 1 calc R . .
O3B O 0.0840(6) 0.5338(6) 0.3994(3) 0.047(2) Uani 0.54(2) 1 d P A 2
O6 O -0.11403(8) 0.60024(18) 0.21706(11) 0.0370(5) Uani 1 1 d . . .
C22 C -0.16054(15) 0.5791(3) 0.27860(17) 0.0452(8) Uani 1 1 d . A .
H22A H -0.1459 0.6375 0.3101 0.054 Uiso 1 1 calc R . .
H22B H -0.1401 0.5148 0.3004 0.054 Uiso 1 1 calc R . .
C23 C -0.22109(16) 0.5650(3) 0.25211(19) 0.0520(10) Uani 1 1 d . A .
H23A H -0.2316 0.5934 0.2827 0.062 Uiso 1 1 calc R . .
H23B H -0.2313 0.4904 0.2444 0.062 Uiso 1 1 calc R . .
O1S O -0.00675(16) 0.5716(3) 0.2821(2) 0.0317(9) Uani 0.50 1 d P . .
O2S O -0.0152(2) 0.5895(5) 0.3445(3) 0.0573(14) Uani 0.50 1 d P A .
O1A O -0.0012(3) 0.3665(8) 0.3267(5) 0.035(2) Uani 0.52(2) 1 d P . 1
C1A C -0.0082(6) 0.3047(13) 0.3591(8) 0.038(3) Uani 0.52(2) 1 d P A 1
C2A C -0.0416(8) 0.312(2) 0.3919(10) 0.093(7) Uani 0.52(2) 1 d P A 1
H2AA H -0.0386 0.3833 0.4093 0.111 Uiso 0.52(2) 1 calc PR A 1
H2AB H -0.0805 0.2987 0.3595 0.111 Uiso 0.52(2) 1 calc PR A 1
C3A C -0.0255(9) 0.2484(17) 0.4367(11) 0.098(6) Uani 0.52(2) 1 d P A 1
H3AA H -0.0574 0.2156 0.4357 0.118 Uiso 0.52(2) 1 calc PR A 1
H3AB H -0.0039 0.2849 0.4789 0.118 Uiso 0.52(2) 1 calc PR A 1
C4A C 0.0073(10) 0.1702(15) 0.4314(9) 0.066(4) Uani 0.52(2) 1 d P A 1
H4AA H -0.0105 0.1013 0.4240 0.079 Uiso 0.52(2) 1 calc PR A 1
H4AB H 0.0436 0.1669 0.4718 0.079 Uiso 0.52(2) 1 calc PR A 1
O3A O 0.1144(6) 0.5437(4) 0.4140(4) 0.031(2) Uani 0.46(2) 1 d P A 1
C9A C 0.1222(8) 0.5178(11) 0.4668(8) 0.042(3) Uani 0.46(2) 1 d P A 1
C10A C 0.0906(9) 0.5538(15) 0.4993(8) 0.062(5) Uani 0.46(2) 1 d P A 1
H10C H 0.0857 0.6304 0.4962 0.074 Uiso 0.46(2) 1 calc PR A 1
H10D H 0.0542 0.5202 0.4789 0.074 Uiso 0.46(2) 1 calc PR A 1
C11A C 0.1250(10) 0.521(3) 0.5672(10) 0.093(8) Uani 0.46(2) 1 d P A 1
H11C H 0.1432 0.5815 0.5959 0.111 Uiso 0.46(2) 1 calc PR A 1
H11D H 0.1031 0.4841 0.5826 0.111 Uiso 0.46(2) 1 calc PR A 1
C12A C 0.1650(8) 0.4511(16) 0.5661(8) 0.066(4) Uani 0.46(2) 1 d P A 1
H12C H 0.2028 0.4761 0.5954 0.079 Uiso 0.46(2) 1 calc PR A 1
H12D H 0.1614 0.3794 0.5787 0.079 Uiso 0.46(2) 1 calc PR A 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'
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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
13 2 22 0.2721 12.9865 1.9981 21.9868 0.2370 0.9834 0.0035
-13 -2 -22 0.2721 -12.9865 -1.9981 -21.9868 -0.2370 -0.9834 -0.0035
-5 18 0 0.4853 -5.0038 17.9876 0.0036 -0.0161 -0.0005 1.0043
8 -17 6 0.3643 8.0005 -16.9884 5.9928 0.0857 0.2580 -0.9762
-29 -1 32 0.1509 -28.9677 -0.9991 31.9723 0.9748 0.1733 0.0016
29 1 -32 0.1509 28.9677 0.9991 -31.9723 -0.9748 -0.1733 -0.0016
-10 12 -16 0.4271 -9.9964 11.9920 -15.9872 -0.2253 -0.6337 0.7342
38 2 -26 0.1689 37.9581 1.9982 -25.9749 -0.9820 0.2381 0.0003
9 14 14 0.3774 8.9843 13.9899 13.9949 0.0849 0.7348 0.6937
-36 -2 28 0.1590 -35.9601 -1.9982 27.9738 0.9938 -0.1290 -0.0134
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
O2 K1 F1 71.35(12) . .
O2 K1 O1S 118.95(9) . .
O2 K1 O1S 152.74(9) . 2
F2 K1 O2 69.38(10) . .
F2 K1 O1B 101.4(3) . .
F2 K1 F1 45.27(9) . .
F2 K1 O6 115.28(8) . 2
F2 K1 O1S 134.72(13) . 2
F2 K1 O1S 161.08(12) . .
F2 K1 O1A 82.9(2) . 2
F2 K1 O3A 130.1(3) . .
O1B K1 O2 75.07(14) . .
O1B K1 O2 113.6(4) 2 .
O1B K1 F2 72.4(3) 2 .
O1B K1 O1B 62.0(5) 2 .
O1B K1 F1 139.39(19) . .
O1B K1 F1 112.53(17) 2 .
O1B K1 O3B 140.7(4) 2 .
O1B K1 O6 110.4(4) 2 2
O1B K1 O1S 88.7(3) 2 .
O1B K1 O1S 72.2(4) 2 2
O1B K1 O1S 67.1(2) . .
O1B K1 O1S 85.84(14) . 2
O1B K1 O1A 77.7(4) 2 .
O1B K1 O1A 69.9(4) . 2
O1B K1 O1A 15.9(2) 2 2
O1B K1 O3A 156.0(3) 2 .
F1 K1 O1S 151.26(11) . .
O3B K1 O2 75.88(13) . .
O3B K1 F2 140.8(2) . .
O3B K1 O1B 86.2(5) . .
O3B K1 F1 106.7(3) . .
O3B K1 O6 77.5(2) . 2
O3B K1 O1S 83.72(18) . 2
O3B K1 O1S 56.1(3) . .
O3B K1 O1A 134.7(3) . 2
O3B K1 O1A 69.3(4) . .
O3B K1 O3A 15.78(14) . .
O6 K1 O2 134.58(7) 2 .
O6 K1 O1B 138.54(18) 2 .
O6 K1 F1 82.04(10) 2 .
O6 K1 O1S 72.17(9) 2 .
O6 K1 O1S 54.91(9) 2 2
O6 K1 O1A 95.3(2) 2 2
O6 K1 O3A 70.38(14) 2 .
O1S K1 F1 132.93(13) 2 .
O1S K1 O1S 33.98(16) 2 .
O1A K1 O2 71.55(12) . .
O1A K1 O2 129.3(2) 2 .
O1A K1 F2 114.2(2) . .
O1A K1 O1B 16.90(15) . .
O1A K1 F1 116.66(14) 2 .
O1A K1 F1 142.45(15) . .
O1A K1 O6 129.95(19) . 2
O1A K1 O1S 58.41(17) . .
O1A K1 O1S 78.98(19) 2 .
O1A K1 O1S 84.50(13) . 2
O1A K1 O1S 57.5(2) 2 2
O1A K1 O1A 83.4(3) . 2
O1A K1 O3A 83.9(4) . .
O3A K1 O2 74.16(13) . .
O3A K1 O1B 100.7(4) . .
O3A K1 F1 91.5(3) . .
O3A K1 O1S 90.9(2) . 2
O3A K1 O1S 68.3(3) . .
O3A K1 O1A 146.9(3) . 2
F7 P2 K2 51.50(8) . .
F8 P2 K2 52.83(9) . .
F8 P2 F7 88.53(12) . .
F9 P2 K2 127.09(10) . .
F9 P2 F7 178.45(14) . .
F9 P2 F8 90.86(13) . .
F9 P2 F10 89.43(13) . .
F9 P2 F11 90.44(14) . .
F9 P2 F12 91.85(14) . .
F10 P2 K2 57.64(9) . .
F10 P2 F7 89.13(12) . .
F10 P2 F8 89.01(13) . .
F11 P2 K2 125.79(13) . .
F11 P2 F7 90.16(13) . .
F11 P2 F8 178.56(15) . .
F11 P2 F10 90.38(15) . .
F11 P2 F12 90.41(18) . .
F12 P2 K2 120.88(10) . .
F12 P2 F7 89.58(14) . .
F12 P2 F8 90.16(16) . .
F12 P2 F10 178.49(14) . .
O4 K2 O4 73.12(11) . 2
O4 K2 F7 77.75(7) . .
O4 K2 F7 99.92(8) 2 .
O4 K2 F8 77.42(7) . .
O4 K2 F8 139.46(9) 2 .
O4 K2 F10 131.90(8) 2 .
O4 K2 F10 116.11(7) . .
O4 K2 O5 74.38(7) 2 2
O4 K2 O5 130.24(9) . 2
O4 K2 O3B 142.14(14) 2 .
O4 K2 O3B 114.2(3) . .
O4 K2 O6 135.70(7) . 2
O4 K2 O1S 85.71(9) . 2
O4 K2 O1S 66.86(10) 2 2
O4 K2 O2S 65.02(12) . .
O4 K2 O2S 117.41(11) 2 .
O4 K2 O3A 128.2(3) . .
O4 K2 O3A 143.53(12) 2 .
F7 K2 F8 46.16(6) . .
F7 K2 F10 45.14(6) . .
F7 K2 O5 71.96(7) . 2
F7 K2 O3B 117.92(13) . .
F7 K2 O1S 161.47(9) . 2
F7 K2 O2S 113.36(12) . .
F7 K2 O3A 112.72(16) . .
F8 K2 F10 44.64(6) . .
F8 K2 O5 106.07(6) . 2
F8 K2 O3B 75.86(12) . .
F8 K2 O1S 137.81(9) . 2
F8 K2 O2S 72.14(12) . .
F8 K2 O3A 76.99(11) . .
F10 K2 O5 64.47(6) . 2
F10 K2 O1S 153.31(9) . 2
F10 K2 O2S 108.11(11) . .
O5 K2 O1S 114.22(9) 2 2
O5 K2 O2S 164.46(12) 2 .
O3B K2 F10 80.3(2) . .
O3B K2 O5 114.7(3) . 2
O3B K2 O1S 76.46(19) . 2
O3B K2 O2S 49.8(3) . .
O3B K2 O3A 14.85(13) . .
O6 K2 O4 76.68(8) 2 2
O6 K2 F7 139.71(7) 2 .
O6 K2 F8 142.46(7) 2 .
O6 K2 F10 108.17(6) 2 .
O6 K2 O5 68.47(6) 2 2
O6 K2 O3B 73.72(18) 2 .
O6 K2 O1S 52.51(9) 2 2
O6 K2 O2S 103.14(12) 2 .
O6 K2 O3A 68.02(14) 2 .
O1S K2 O4 93.55(11) . 2
O1S K2 O4 73.31(10) . .
O1S K2 F7 142.82(10) . .
O1S K2 F8 104.05(10) . .
O1S K2 F10 134.53(10) . .
O1S K2 O5 145.22(10) . 2
O1S K2 O3B 57.2(3) . .
O1S K2 O6 77.08(10) . 2
O1S K2 O1S 33.76(16) . 2
O1S K2 O2S 31.94(14) . .
O1S K2 O3A 70.4(3) . .
O2S K2 O1S 65.68(13) . 2
O3A K2 F10 70.5(2) . .
O3A K2 O5 100.0(3) . 2
O3A K2 O1S 84.1(2) . 2
O3A K2 O2S 64.5(3) . .
F3 P1 K1 121.05(13) . .
F3 P1 F2 85.89(16) . .
F3 P1 F4 93.07(16) . .
F2 P1 K1 43.74(9) . .
F4 P1 K1 136.20(13) . .
F4 P1 F2 178.1(2) . .
F6 P1 K1 112.0(2) . .
F6 P1 F3 90.2(2) . .
F6 P1 F2 88.8(2) . .
F6 P1 F4 92.7(2) . .
F6 P1 F5 176.1(3) . .
F6 P1 F1 94.3(3) . .
F5 P1 K1 64.2(3) . .
F5 P1 F3 91.2(3) . .
F5 P1 F2 87.7(2) . .
F5 P1 F4 90.8(2) . .
F1 P1 K1 53.4(2) . .
F1 P1 F3 173.9(3) . .
F1 P1 F2 90.2(2) . .
F1 P1 F4 90.7(2) . .
F1 P1 F5 84.0(4) . .
C7 O2 K1 119.2(3) . .
C7 O2 C6 110.4(3) . .
C6 O2 K1 117.2(2) . .
K2 O4 K2 88.36(7) . 2
C13 O4 K2 128.1(2) . 2
C13 O4 K2 139.9(2) . .
C13 N3 C17 123.8(3) . .
C13 N3 C16 113.6(3) . .
C16 N3 C17 122.6(3) . .
C5 N1 C4A 126.5(9) . .
C1B N1 C5 120.3(9) . .
C1B N1 C4B 119.5(13) . .
C1B N1 C1A 19.4(9) . .
C1B N1 C4A 113.0(12) . .
C4B N1 C5 116.8(10) . .
C4B N1 C1A 117.7(12) . .
C4B N1 C4A 25.2(10) . .
C1A N1 C5 125.5(7) . .
C1A N1 C4A 103.2(11) . .
O4 C13 N3 124.6(4) . .
O4 C13 C14 126.8(3) . .
N3 C13 C14 108.6(3) . .
P1 F2 K1 112.22(13) . .
O5 C18 C17 108.3(3) . .
C16 C15 C14 107.2(3) . .
N3 C17 C18 112.7(3) . .
N1 C5 C6 112.7(4) . .
C10B C9B N2 113.8(10) . .
O3B C9B N2 124.0(9) . .
O3B C9B C10B 122.2(11) . .
O2 C7 C8 108.7(4) . .
N1 C1B O1B 125.9(14) . .
N1 C1B C2B 111.9(16) . .
O1B C1B C2B 122.0(15) . .
C9B N2 C12B 102.0(9) . .
C8 N2 C9B 127.5(6) . .
C8 N2 C12B 124.4(7) . .
C9A N2 C9B 20.8(9) . .
C9A N2 C8 117.6(9) . .
C9A N2 C12B 117.2(11) . .
C9A N2 C12A 123.4(11) . .
C12A N2 C9B 116.6(10) . .
C12A N2 C8 115.8(9) . .
C12A N2 C12B 27.5(8) . .
K1 O1B K1 95.79(17) 2 .
C1B O1B K1 124.8(9) . .
C1B O1B K1 137.4(9) . 2
C13 C14 C15 105.2(3) . .
C11B C10B C9B 104.1(11) . .
N3 C16 C15 105.2(3) . .
N1 C4B C3B 101.5(15) . .
C1B C2B C3B 98.9(19) . .
P1 F5 K1 90.9(3) . .
P1 F1 K1 102.6(3) . .
C4B C3B C2B 102.4(14) . .
C10B C11B C12B 109.7(15) . .
N2 C8 C7 112.8(5) . .
C11B C12B N2 103.0(12) . .
O2 C6 C5 109.0(3) . .
P2 F7 K2 102.11(10) . .
P2 F8 K2 100.89(10) . .
P2 F10 K2 95.77(10) . .
C18 O5 K2 119.2(2) . 2
C18 O5 C19 112.4(3) . .
C19 O5 K2 116.29(19) . 2
O5 C19 C20 108.6(2) . .
N4 C20 C19 111.5(3) . .
C20 N4 C24 122.5(3) . .
C21 N4 C20 123.5(3) . .
C21 N4 C24 113.5(3) . .
N4 C21 K1 118.4(2) . 2
N4 C21 C22 108.4(3) . .
O6 C21 K1 43.78(16) . 2
O6 C21 N4 125.9(3) . .
O6 C21 C22 125.7(3) . .
C22 C21 K1 112.2(2) . 2
N4 C24 C23 103.0(3) . .
K1 O3B K2 98.40(19) . .
C9B O3B K1 128.2(7) . .
C9B O3B K2 132.1(7) . .
K2 O6 K1 98.94(7) 2 2
C21 O6 K1 118.3(2) . 2
C21 O6 K2 134.2(2) . 2
C21 C22 C23 104.4(3) . .
C22 C23 C24 104.4(3) . .
K1 O1S K1 83.34(11) 2 .
K1 O1S K2 130.07(14) . 2
K1 O1S K2 87.29(11) 2 2
K2 O1S K1 161.93(17) . 2
K2 O1S K1 93.09(12) . .
K2 O1S K2 81.48(11) . 2
O1S O1S K1 69.81(18) 2 .
O1S O1S K1 76.21(19) 2 2
O1S O1S K2 60.32(17) 2 2
O1S O1S K2 85.92(19) 2 .
O2S O1S K1 112.0(3) . 2
O2S O1S K1 113.4(3) . .
O2S O1S K2 115.6(3) . 2
O2S O1S K2 85.8(3) . .
O2S O1S O1S 171.2(3) . 2
O1S O2S K2 62.3(2) . .
K1 O1A K1 91.87(18) . 2
C1A O1A K1 123.7(8) . 2
C1A O1A K1 134.6(8) . .
N1 C1A C2A 103.4(14) . .
O1A C1A N1 125.9(12) . .
O1A C1A C2A 130.6(15) . .
C3A C2A C1A 110.9(17) . .
C2A C3A C4A 111.1(17) . .
C3A C4A N1 106.5(14) . .
K1 O3A K2 94.6(2) . .
C9A O3A K1 125.2(7) . .
C9A O3A K2 133.3(7) . .
N2 C9A O3A 130.2(13) . .
N2 C9A C10A 102.3(12) . .
O3A C9A C10A 127.2(13) . .
C11A C10A C9A 104.0(12) . .
C12A C11A C10A 104.0(15) . .
N2 C12A C11A 102.0(14) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K1 O2 2.923(2) .
K1 F2 2.751(3) .
K1 O1B 2.553(7) 2
K1 O1B 2.829(7) .
K1 F1 3.029(6) .
K1 O3B 2.667(5) .
K1 O6 2.777(2) 2
K1 O1S 3.057(4) .
K1 O1S 2.955(4) 2
K1 O1A 2.667(5) .
K1 O1A 2.893(8) 2
K1 O3A 2.790(7) .
P2 F7 1.608(2) .
P2 F8 1.595(2) .
P2 F9 1.583(2) .
P2 F10 1.592(2) .
P2 F11 1.584(2) .
P2 F12 1.585(2) .
K2 O4 2.789(3) 2
K2 O4 2.762(2) .
K2 F7 2.832(2) .
K2 F8 2.871(2) .
K2 F10 3.003(2) .
K2 O5 3.023(2) 2
K2 O3B 2.906(7) .
K2 O6 2.777(2) 2
K2 O1S 3.158(4) 2
K2 O1S 2.751(4) .
K2 O2S 3.099(6) .
K2 O3A 2.953(7) .
P1 F3 1.558(3) .
P1 F2 1.622(3) .
P1 F4 1.558(3) .
P1 F6 1.522(4) .
P1 F5 1.551(4) .
P1 F1 1.539(3) .
O2 C7 1.415(4) .
O2 C6 1.426(5) .
O4 K2 2.789(3) 2
O4 C13 1.233(4) .
N3 C13 1.343(4) .
N3 C17 1.471(5) .
N3 C16 1.461(5) .
N1 C5 1.446(5) .
N1 C1B 1.198(18) .
N1 C4B 1.43(2) .
N1 C1A 1.440(16) .
N1 C4A 1.518(17) .
C13 C14 1.509(5) .
C18 C17 1.502(6) .
C18 O5 1.402(5) .
C15 C14 1.509(6) .
C15 C16 1.485(6) .
C5 C6 1.485(6) .
C9B N2 1.502(13) .
C9B C10B 1.468(17) .
C9B O3B 1.244(13) .
C7 C8 1.496(8) .
C1B O1B 1.263(19) .
C1B C2B 1.49(3) .
N2 C8 1.459(7) .
N2 C12B 1.574(14) .
N2 C9A 1.146(17) .
N2 C12A 1.363(16) .
O1B K1 2.553(7) 2
C10B C11B 1.47(2) .
C4B C3B 1.58(3) .
C2B C3B 1.67(4) .
C11B C12B 1.53(3) .
O5 K2 3.023(2) 2
O5 C19 1.439(4) .
C19 C20 1.490(6) .
C20 N4 1.450(4) .
N4 C21 1.326(4) .
N4 C24 1.473(4) .
C21 O6 1.238(4) .
C21 C22 1.506(5) .
C24 C23 1.513(5) .
O6 K1 2.778(2) 2
O6 K2 2.777(2) 2
C22 C23 1.511(5) .
O1S K1 2.955(4) 2
O1S K2 3.158(4) 2
O1S O1S 1.760(9) 2
O1S O2S 1.644(7) .
O1A K1 2.892(8) 2
O1A C1A 1.194(17) .
C1A C2A 1.51(2) .
C2A C3A 1.23(3) .
C3A C4A 1.42(3) .
O3A C9A 1.211(16) .
C9A C10A 1.531(19) .
C10A C11A 1.46(3) .
C11A C12A 1.46(3) .
