#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:00:53 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178929 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/58/4115845.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_4115845
loop_
_publ_author_name
'K. C. Kumara Swamy'
'Sudha Kumaraswamy'
'Praveen Kommana'
_publ_section_title
;
 Very Strong C-H...O, N-H...O, and O-H...O Hydrogen Bonds Involving a
 Cyclic Phosphate
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12642
_journal_page_last               12649
_journal_paper_doi               10.1021/ja010713x
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C66 H101 K O16 P2'
_chemical_formula_weight         1251.51
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 111.093(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.9360(12)
_cell_length_b                   19.447(6)
_cell_length_c                   22.983(3)
_cell_measurement_temperature    293(2)
_cell_volume                     7062(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0968
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            12400
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.9308
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_description       'rectangular plates '
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.346
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.00054(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         12400
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0633
_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)+(0.0800P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.2030
_reflns_number_gt                4152
_reflns_number_total             12400
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja010713x_07.cif
_cod_data_source_block           compd4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_calc_flag
_atom_site_refinement_flags
K K 0.09311(7) 0.48374(6) 0.27798(6) 0.0684(4) Uani 1 d .
P1 P 0.42904(8) 0.19093(6) 0.25465(7) 0.0565(4) Uani 1 d .
P2 P 0.27883(8) 0.56795(6) 0.22805(6) 0.0553(4) Uani 1 d .
O5 O 0.37717(19) 0.56713(14) 0.26678(14) 0.0527(8) Uani 1 d .
O1 O 0.4963(2) 0.21625(14) 0.32093(15) 0.0568(8) Uani 1 d .
O3 O 0.44921(19) 0.12125(14) 0.23900(15) 0.0575(9) Uani 1 d .
O4 O 0.3458(2) 0.20849(16) 0.25822(18) 0.0714(11) Uani 1 d .
O6 O 0.27319(19) 0.54010(15) 0.16151(14) 0.0587(9) Uani 1 d .
O2 O 0.43732(19) 0.24710(14) 0.20537(15) 0.0585(9) Uani 1 d .
O7 O 0.2285(2) 0.52786(15) 0.25497(15) 0.0651(9) Uani 1 d .
O8 O 0.2588(2) 0.64411(15) 0.21712(16) 0.0629(9) Uani 1 d .
H8 H 0.298(5) 0.175(4) 0.269(3) 0.16(3) Uiso 1 d .
O12 O -0.0718(2) 0.50080(17) 0.30120(18) 0.0754(10) Uani 1 d .
O11 O 0.0844(3) 0.4995(2) 0.40072(18) 0.0913(12) Uani 1 d .
O9 O 0.1984(3) 0.3630(2) 0.2762(2) 0.0946(13) Uani 1 d .
O14 O 0.0450(3) 0.3641(2) 0.1784(2) 0.1073(14) Uani 1 d .
O13 O -0.0749(3) 0.4532(2) 0.18520(18) 0.0864(12) Uani 1 d .
O10 O 0.2079(3) 0.4087(3) 0.3938(2) 0.1144(15) Uani 1 d .
C1 C 0.5782(3) 0.1896(2) 0.3444(2) 0.0563(13) Uani 1 d .
C2 C 0.6007(4) 0.1453(2) 0.3966(2) 0.0622(14) Uani 1 d .
C3 C 0.6823(4) 0.1206(3) 0.4162(3) 0.0743(16) Uani 1 d .
H3 H 0.6992 0.0907 0.4500 0.089 Uiso 1 calc R
C4 C 0.7415(4) 0.1371(3) 0.3892(3) 0.0718(15) Uani 1 d .
C5 C 0.7167(3) 0.1838(3) 0.3409(2) 0.0629(14) Uani 1 d .
H5 H 0.7554 0.1975 0.3229 0.076 Uiso 1 calc R
C6 C 0.6360(3) 0.2110(2) 0.3185(2) 0.0570(13) Uani 1 d .
C7 C 0.6127(3) 0.2668(2) 0.2685(2) 0.0631(14) Uani 1 d .
H7A H 0.5722 0.2974 0.2760 0.076 Uiso 1 calc R
H7B H 0.6632 0.2936 0.2739 0.076 Uiso 1 calc R
C8 C 0.5764(3) 0.2439(2) 0.2018(2) 0.0563(12) Uani 1 d .
C9 C 0.6280(3) 0.2330(2) 0.1675(3) 0.0616(14) Uani 1 d .
H9 H 0.6862 0.2370 0.1873 0.074 Uiso 1 calc R
C10 C 0.5959(4) 0.2163(2) 0.1050(3) 0.0685(15) Uani 1 d .
C11 C 0.5090(4) 0.2138(2) 0.0755(3) 0.0746(16) Uani 1 d .
H11 H 0.4868 0.2050 0.0329 0.090 Uiso 1 calc R
C12 C 0.4528(3) 0.2241(2) 0.1072(3) 0.0625(14) Uani 1 d .
C13 C 0.4900(3) 0.2365(2) 0.1715(3) 0.0569(13) Uani 1 d .
C24 C 0.4249(3) 0.5189(2) 0.3111(2) 0.0524(12) Uani 1 d .
C25 C 0.4776(3) 0.5437(3) 0.3679(3) 0.0648(14) Uani 1 d .
C26 C 0.5312(3) 0.4957(3) 0.4087(2) 0.0736(15) Uani 1 d .
H26 H 0.5677 0.5107 0.4476 0.088 Uiso 1 calc R
C27 C 0.5321(4) 0.4270(3) 0.3936(3) 0.0737(16) Uani 1 d .
C28 C 0.4759(3) 0.4045(3) 0.3367(3) 0.0668(15) Uani 1 d .
H28 H 0.4744 0.3580 0.3266 0.080 Uiso 1 calc R
C29 C 0.4215(3) 0.4502(2) 0.2941(2) 0.0509(12) Uani 1 d .
C30 C 0.3636(3) 0.4246(2) 0.2313(2) 0.0594(13) Uani 1 d .
H30A H 0.3685 0.3749 0.2300 0.071 Uiso 1 calc R
H30B H 0.3056 0.4353 0.2262 0.071 Uiso 1 calc R
C31 C 0.3828(3) 0.4553(2) 0.1779(2) 0.0550(12) Uani 1 d .
C32 C 0.4456(3) 0.4277(2) 0.1611(2) 0.0642(14) Uani 1 d .
H32 H 0.4759 0.3902 0.1831 0.077 Uiso 1 calc R
C33 C 0.4653(3) 0.4543(3) 0.1120(3) 0.0722(15) Uani 1 d .
C34 C 0.4190(4) 0.5102(3) 0.0803(3) 0.0742(16) Uani 1 d .
H34 H 0.4318 0.5280 0.0472 0.089 Uiso 1 calc R
C35 C 0.3543(3) 0.5417(2) 0.0949(2) 0.0585(13) Uani 1 d .
C36 C 0.3388(3) 0.5124(2) 0.1452(2) 0.0544(12) Uani 1 d .
C14 C 0.5404(4) 0.1257(3) 0.4294(3) 0.0738(16) Uani 1 d .
C15 C 0.4644(4) 0.0850(3) 0.3869(3) 0.0867(18) Uani 1 d .
H15A H 0.4306 0.1139 0.3533 0.130 Uiso 1 calc R
H15B H 0.4310 0.0696 0.4103 0.130 Uiso 1 calc R
H15C H 0.4839 0.0460 0.3702 0.130 Uiso 1 calc R
C16 C 0.5103(5) 0.1911(3) 0.4539(3) 0.121(3) Uani 1 d .
H16A H 0.5585 0.2188 0.4767 0.181 Uiso 1 calc R
H16B H 0.4807 0.1781 0.4808 0.181 Uiso 1 calc R
H16C H 0.4732 0.2170 0.4193 0.181 Uiso 1 calc R
C17 C 0.5834(4) 0.0812(3) 0.4874(3) 0.108(2) Uani 1 d .
H17A H 0.6044 0.0398 0.4755 0.161 Uiso 1 calc R
H17B H 0.5432 0.0698 0.5065 0.161 Uiso 1 calc R
H17C H 0.6297 0.1063 0.5166 0.161 Uiso 1 calc R
C18 C 0.8302(4) 0.1064(3) 0.4131(3) 0.102(2) Uani 1 d .
H18A H 0.8367 0.0774 0.4483 0.152 Uiso 1 calc R
H18B H 0.8713 0.1427 0.4253 0.152 Uiso 1 calc R
H18C H 0.8384 0.0796 0.3806 0.152 Uiso 1 calc R
C19 C 0.6535(4) 0.2019(3) 0.0692(3) 0.103(2) Uani 1 d .
H19A H 0.7061 0.2258 0.0885 0.154 Uiso 1 calc R
H19B H 0.6270 0.2173 0.0269 0.154 Uiso 1 calc R
H19C H 0.6641 0.1533 0.0695 0.154 Uiso 1 calc R
C20 C 0.3569(4) 0.2223(3) 0.0712(3) 0.0793(17) Uani 1 d .
C21 C 0.3350(4) 0.2108(3) 0.0003(3) 0.117(2) Uani 1 d .
H21A H 0.3612 0.2460 -0.0158 0.176 Uiso 1 calc R
H21B H 0.2748 0.2126 -0.0208 0.176 Uiso 1 calc R
H21C H 0.3556 0.1666 -0.0064 0.176 Uiso 1 calc R
C22 C 0.3162(4) 0.2912(3) 0.0784(3) 0.112(2) Uani 1 d .
H22A H 0.3279 0.3000 0.1218 0.168 Uiso 1 calc R
H22B H 0.2561 0.2888 0.0566 0.168 Uiso 1 calc R
H22C H 0.3392 0.3276 0.0612 0.168 Uiso 1 calc R
C23 C 0.3138(4) 0.1635(3) 0.0940(3) 0.104(2) Uani 1 d .
H23A H 0.3422 0.1209 0.0934 0.156 Uiso 1 calc R
H23B H 0.2556 0.1601 0.0670 0.156 Uiso 1 calc R
H23C H 0.3169 0.1731 0.1358 0.156 Uiso 1 calc R
C37 C 0.4788(4) 0.6205(3) 0.3864(3) 0.0752(16) Uani 1 d .
C38 C 0.5030(4) 0.6657(3) 0.3407(3) 0.096(2) Uani 1 d .
H38A H 0.5546 0.6490 0.3374 0.144 Uiso 1 calc R
H38B H 0.5109 0.7122 0.3556 0.144 Uiso 1 calc R
H38C H 0.4586 0.6642 0.3004 0.144 Uiso 1 calc R
C39 C 0.3916(4) 0.6409(3) 0.3871(3) 0.0912(19) Uani 1 d .
H39A H 0.3504 0.6383 0.3456 0.137 Uiso 1 calc R
H39B H 0.3939 0.6871 0.4024 0.137 Uiso 1 calc R
H39C H 0.3760 0.6102 0.4138 0.137 Uiso 1 calc R
C40 C 0.5438(4) 0.6332(3) 0.4523(3) 0.110(2) Uani 1 d .
H40A H 0.5292 0.6062 0.4819 0.166 Uiso 1 calc R
H40B H 0.5437 0.6811 0.4626 0.166 Uiso 1 calc R
H40C H 0.5992 0.6204 0.4536 0.166 Uiso 1 calc R
C41 C 0.5954(4) 0.3773(3) 0.4376(3) 0.108(2) Uani 1 d .
H41A H 0.6204 0.3495 0.4143 0.162 Uiso 1 calc R
H41B H 0.5668 0.3483 0.4574 0.162 Uiso 1 calc R
H41C H 0.6388 0.4029 0.4687 0.162 Uiso 1 calc R
C42 C 0.5327(4) 0.4220(3) 0.0919(3) 0.106(2) Uani 1 d .
H42A H 0.5834 0.4491 0.1072 0.159 Uiso 1 calc R
H42B H 0.5131 0.4201 0.0472 0.159 Uiso 1 calc R
H42C H 0.5445 0.3763 0.1086 0.159 Uiso 1 calc R
C43 C 0.3096(4) 0.6041(3) 0.0586(2) 0.0712(15) Uani 1 d .
C44 C 0.3279(4) 0.6166(3) -0.0010(3) 0.109(2) Uani 1 d .
H44A H 0.3150 0.5758 -0.0261 0.164 Uiso 1 calc R
H44B H 0.3866 0.6279 0.0097 0.164 Uiso 1 calc R
H44C H 0.2936 0.6540 -0.0238 0.164 Uiso 1 calc R
C45 C 0.2135(5) 0.5964(4) 0.0385(3) 0.139(3) Uani 1 d .
H45A H 0.1962 0.5537 0.0166 0.209 Uiso 1 calc R
H45B H 0.1862 0.6339 0.0116 0.209 Uiso 1 calc R
H45C H 0.1979 0.5967 0.0747 0.209 Uiso 1 calc R
C46 C 0.3354(5) 0.6687(3) 0.0993(3) 0.122(3) Uani 1 d .
H46A H 0.3178 0.7088 0.0735 0.183 Uiso 1 calc R
H46B H 0.3957 0.6694 0.1201 0.183 Uiso 1 calc R
H46C H 0.3087 0.6683 0.1297 0.183 Uiso 1 calc R
C47 C 0.2546(5) 0.3358(4) 0.3300(4) 0.112(2) Uani 1 d .
H47A H 0.3039 0.3187 0.3225 0.134 Uiso 1 calc R
H47B H 0.2285 0.2976 0.3435 0.134 Uiso 1 calc R
C48 C 0.2805(4) 0.3891(4) 0.3790(4) 0.108(2) Uani 1 d .
H48A H 0.3245 0.3712 0.4159 0.130 Uiso 1 calc R
H48B H 0.3027 0.4288 0.3645 0.130 Uiso 1 calc R
C49 C 0.2245(5) 0.4589(4) 0.4395(4) 0.143(3) Uani 1 d .
H49A H 0.2415 0.5011 0.4248 0.171 Uiso 1 calc R
H49B H 0.2706 0.4441 0.4766 0.171 Uiso 1 calc R
C50 C 0.1467(6) 0.4720(4) 0.4553(3) 0.125(3) Uani 1 d .
H50A H 0.1268 0.4295 0.4673 0.150 Uiso 1 calc R
H50B H 0.1593 0.5044 0.4895 0.150 Uiso 1 calc R
C51 C 0.0084(5) 0.5175(3) 0.4086(3) 0.095(2) Uani 1 d .
H51A H 0.0199 0.5495 0.4432 0.114 Uiso 1 calc R
H51B H -0.0180 0.4768 0.4180 0.114 Uiso 1 calc R
C52 C -0.0492(4) 0.5498(3) 0.3505(3) 0.0856(19) Uani 1 d .
H52A H -0.0997 0.5663 0.3566 0.103 Uiso 1 calc R
H52B H -0.0214 0.5888 0.3398 0.103 Uiso 1 calc R
C53 C -0.1240(4) 0.5289(3) 0.2444(3) 0.0805(17) Uani 1 d .
H53A H -0.0943 0.5654 0.2320 0.097 Uiso 1 calc R
H53B H -0.1744 0.5483 0.2487 0.097 Uiso 1 calc R
C54 C -0.1476(4) 0.4746(3) 0.1971(3) 0.0913(19) Uani 1 d .
H54A H -0.1715 0.4359 0.2118 0.110 Uiso 1 calc R
H54B H -0.1900 0.4917 0.1590 0.110 Uiso 1 calc R
C55 C -0.0932(5) 0.4025(4) 0.1399(3) 0.111(2) Uani 1 d .
H55A H -0.1375 0.4183 0.1022 0.133 Uiso 1 calc R
H55B H -0.1134 0.3616 0.1544 0.133 Uiso 1 calc R
C56 C -0.0195(6) 0.3861(4) 0.1266(3) 0.117(3) Uani 1 d .
H56A H -0.0331 0.3505 0.0949 0.140 Uiso 1 calc R
H56B H -0.0013 0.4266 0.1100 0.140 Uiso 1 calc R
C57 C 0.1201(5) 0.3506(4) 0.1688(4) 0.117(2) Uani 1 d .
H57A H 0.1450 0.3932 0.1616 0.141 Uiso 1 calc R
H57B H 0.1092 0.3213 0.1326 0.141 Uiso 1 calc R
C58 C 0.1776(4) 0.3164(3) 0.2247(4) 0.093(2) Uani 1 d .
H58A H 0.1508 0.2756 0.2335 0.112 Uiso 1 calc R
H58B H 0.2287 0.3023 0.2181 0.112 Uiso 1 calc R
O15 O 0.1400(7) 0.7036(8) 0.7070(8) 0.292(6) Uani 1 d D
O16 O 0.1927(12) 0.9323(8) 0.8086(10) 0.339(9) Uani 1 d D
C63 C 0.1356(9) 0.9689(10) 0.7613(8) 0.261(9) Uani 1 d D
H63A H 0.0784 0.9635 0.7609 0.313 Uiso 1 calc R
H63B H 0.1373 0.9562 0.7210 0.313 Uiso 1 calc R
C64 C 0.1665(9) 1.0370(8) 0.7786(8) 0.204(6) Uani 1 d D
H64A H 0.1205 1.0666 0.7786 0.244 Uiso 1 calc R
H64B H 0.1894 1.0550 0.7486 0.244 Uiso 1 calc R
C60 C 0.0133(10) 0.6829(6) 0.6370(9) 0.260(9) Uani 1 d D
H60A H 0.0047 0.6336 0.6324 0.312 Uiso 1 calc R
H60B H -0.0302 0.7065 0.6034 0.312 Uiso 1 calc R
C59 C 0.0950(15) 0.7022(16) 0.6415(8) 0.47(2) Uani 1 d D
H59A H 0.0948 0.7471 0.6230 0.568 Uiso 1 calc R
H59B H 0.1191 0.6688 0.6213 0.568 Uiso 1 calc R
C61 C 0.0190(10) 0.7084(11) 0.7012(7) 0.261(9) Uani 1 d D
H61A H -0.0321 0.7325 0.6991 0.313 Uiso 1 calc R
H61B H 0.0292 0.6708 0.7307 0.313 Uiso 1 calc R
C66 C 0.2300(16) 0.9658(13) 0.8613(9) 0.33(2) Uani 1 d D
H66A H 0.2868 0.9487 0.8831 0.391 Uiso 1 calc R
H66B H 0.1976 0.9625 0.8885 0.391 Uiso 1 calc R
C65 C 0.2314(10) 1.0366(10) 0.8396(10) 0.262(10) Uani 1 d D
H65A H 0.2186 1.0692 0.8670 0.314 Uiso 1 calc R
H65B H 0.2861 1.0478 0.8376 0.314 Uiso 1 calc R
C62 C 0.0902(14) 0.7541(9) 0.7173(10) 0.340(14) Uani 1 d D
H62A H 0.0815 0.7929 0.6891 0.408 Uiso 1 calc R
H62B H 0.1094 0.7696 0.7603 0.408 Uiso 1 calc R
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'
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_
_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
O7 K O3 81.88(9) . 2
O7 K O11 120.47(12) . .
O3 K O11 86.17(11) 2 .
O7 K O13 126.66(11) . .
O3 K O13 87.65(10) 2 .
O11 K O13 110.68(13) . .
O7 K O9 71.80(10) . .
O3 K O9 153.45(11) 2 .
O11 K O9 109.90(13) . .
O13 K O9 105.10(13) . .
O7 K O10 90.18(12) . .
O3 K O10 129.79(13) 2 .
O11 K O10 55.92(13) . .
O13 K O10 133.20(13) . .
O9 K O10 55.44(14) . .
O7 K O12 154.96(10) . .
O3 K O12 73.21(9) 2 .
O11 K O12 56.33(12) . .
O13 K O12 55.89(11) . .
O9 K O12 133.21(11) . .
O10 K O12 103.70(12) . .
O7 K O14 96.27(12) . .
O3 K O14 128.70(12) 2 .
O11 K O14 133.96(13) . .
O13 K O14 52.76(13) . .
O9 K O14 53.47(14) . .
O10 K O14 101.37(15) . .
O12 K O14 101.15(12) . .
O3 P1 O4 122.30(19) . .
O3 P1 O2 111.37(18) . .
O4 P1 O2 101.98(18) . .
O3 P1 O1 111.33(18) . .
O4 P1 O1 103.85(19) . .
O2 P1 O1 104.21(16) . .
O7 P2 O8 117.67(19) . .
O7 P2 O5 114.63(18) . .
O8 P2 O5 103.32(18) . .
O7 P2 O6 112.72(19) . .
O8 P2 O6 103.88(18) . .
O5 P2 O6 102.95(17) . .
C24 O5 P2 129.0(3) . .
C1 O1 P1 121.1(3) . .
P1 O3 K 148.70(18) . 2_545
C36 O6 P2 127.4(3) . .
C13 O2 P1 121.7(3) . .
P2 O7 K 159.39(19) . .
C53 O12 C52 112.3(4) . .
C53 O12 K 101.0(3) . .
C52 O12 K 102.2(3) . .
C51 O11 C50 113.8(5) . .
C51 O11 K 121.5(3) . .
C50 O11 K 122.5(4) . .
C47 O9 C58 112.8(5) . .
C47 O9 K 121.4(4) . .
C58 O9 K 123.0(4) . .
C56 O14 C57 114.2(6) . .
C56 O14 K 108.6(4) . .
C57 O14 K 104.0(4) . .
C55 O13 C54 112.3(5) . .
C55 O13 K 125.9(4) . .
C54 O13 K 118.8(3) . .
C49 O10 C48 114.1(6) . .
C49 O10 K 102.5(4) . .
C48 O10 K 104.6(4) . .
C6 C1 O1 118.8(4) . .
C6 C1 C2 122.2(5) . .
O1 C1 C2 118.9(4) . .
C3 C2 C1 115.0(5) . .
C3 C2 C14 121.6(5) . .
C1 C2 C14 123.3(5) . .
C2 C3 C4 124.9(5) . .
C5 C4 C3 116.8(5) . .
C5 C4 C18 121.6(6) . .
C3 C4 C18 121.6(6) . .
C4 C5 C6 121.8(5) . .
C5 C6 C1 118.9(5) . .
C5 C6 C7 120.4(5) . .
C1 C6 C7 120.6(5) . .
C8 C7 C6 117.3(4) . .
C13 C8 C9 117.8(5) . .
C13 C8 C7 121.0(5) . .
C9 C8 C7 121.1(5) . .
C10 C9 C8 122.4(5) . .
C9 C10 C11 118.0(5) . .
C9 C10 C19 121.3(6) . .
C11 C10 C19 120.7(6) . .
C10 C11 C12 122.8(5) . .
C13 C12 C11 116.0(5) . .
C13 C12 C20 124.0(5) . .
C11 C12 C20 120.1(5) . .
C8 C13 O2 118.5(5) . .
C8 C13 C12 122.8(5) . .
O2 C13 C12 118.5(5) . .
C25 C24 C29 123.5(4) . .
C25 C24 O5 117.5(4) . .
C29 C24 O5 118.9(4) . .
C24 C25 C26 116.4(5) . .
C24 C25 C37 122.5(5) . .
C26 C25 C37 121.0(5) . .
C27 C26 C25 122.5(5) . .
C26 C27 C28 118.6(5) . .
C26 C27 C41 121.0(6) . .
C28 C27 C41 120.4(5) . .
C27 C28 C29 121.1(5) . .
C24 C29 C28 117.7(5) . .
C24 C29 C30 122.3(4) . .
C28 C29 C30 119.9(4) . .
C31 C30 C29 113.2(4) . .
C32 C31 C36 118.7(5) . .
C32 C31 C30 119.7(4) . .
C36 C31 C30 121.7(4) . .
C31 C32 C33 121.6(5) . .
C34 C33 C32 117.7(5) . .
C34 C33 C42 120.8(5) . .
C32 C33 C42 121.5(5) . .
C33 C34 C35 124.2(5) . .
C36 C35 C34 114.7(5) . .
C36 C35 C43 125.4(5) . .
C34 C35 C43 119.9(5) . .
C35 C36 C31 123.1(4) . .
C35 C36 O6 117.9(4) . .
C31 C36 O6 118.9(4) . .
C2 C14 C15 111.9(4) . .
C2 C14 C17 112.2(5) . .
C15 C14 C17 107.0(5) . .
C2 C14 C16 109.9(4) . .
C15 C14 C16 110.3(5) . .
C17 C14 C16 105.3(5) . .
C12 C20 C22 110.4(5) . .
C12 C20 C23 111.9(4) . .
C22 C20 C23 108.8(5) . .
C12 C20 C21 112.0(5) . .
C22 C20 C21 106.9(5) . .
C23 C20 C21 106.7(5) . .
C38 C37 C39 110.7(5) . .
C38 C37 C40 108.0(5) . .
C39 C37 C40 107.3(5) . .
C38 C37 C25 110.1(4) . .
C39 C37 C25 109.5(5) . .
C40 C37 C25 111.0(5) . .
C35 C43 C44 113.6(5) . .
C35 C43 C45 110.7(5) . .
C44 C43 C45 106.4(5) . .
C35 C43 C46 110.1(5) . .
C44 C43 C46 108.2(5) . .
C45 C43 C46 107.6(6) . .
O9 C47 C48 109.8(6) . .
O10 C48 C47 108.8(6) . .
O10 C49 C50 110.1(7) . .
O11 C50 C49 106.7(6) . .
O11 C51 C52 108.9(5) . .
O12 C52 C51 109.6(5) . .
O12 C53 C54 108.9(5) . .
O13 C54 C53 109.4(5) . .
O13 C55 C56 110.1(6) . .
O14 C56 C55 111.7(6) . .
O14 C57 C58 107.6(7) . .
O9 C58 C57 109.0(5) . .
C62 O15 C59 93.9(14) . .
C66 O16 C63 116(2) . .
O16 C63 C64 100.3(13) . .
C63 C64 C65 110.0(12) . .
C59 C60 C61 97.2(12) . .
C60 C59 O15 102.8(14) . .
C62 C61 C60 101.8(13) . .
O16 C66 C65 102.3(16) . .
C64 C65 C66 103.6(15) . .
O15 C62 C61 91.4(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
K O7 2.673(3) .
K O3 2.760(3) 2
K O11 2.894(4) .
K O13 2.937(4) .
K O9 2.958(4) .
K O10 3.045(5) .
K O12 3.045(4) .
K O14 3.157(5) .
P1 O3 1.473(3) .
P1 O4 1.482(3) .
P1 O2 1.615(3) .
P1 O1 1.616(3) .
P2 O7 1.448(3) .
P2 O8 1.520(3) .
P2 O5 1.581(3) .
P2 O6 1.593(3) .
O5 C24 1.407(5) .
O1 C1 1.394(5) .
O3 K 2.760(3) 2_545
O6 C36 1.402(5) .
O2 C13 1.395(5) .
O12 C53 1.397(6) .
O12 C52 1.423(6) .
O11 C51 1.408(7) .
O11 C50 1.421(7) .
O9 C47 1.365(7) .
O9 C58 1.430(6) .
O14 C56 1.364(7) .
O14 C57 1.392(7) .
O13 C55 1.386(7) .
O13 C54 1.417(6) .
O10 C49 1.389(7) .
O10 C48 1.438(7) .
C1 C6 1.381(6) .
C1 C2 1.413(6) .
C2 C3 1.377(7) .
C2 C14 1.522(7) .
C3 C4 1.393(7) .
C4 C5 1.378(7) .
C4 C18 1.523(7) .
C5 C6 1.381(6) .
C6 C7 1.525(6) .
C7 C8 1.500(6) .
C8 C13 1.383(6) .
C8 C9 1.387(6) .
C9 C10 1.379(7) .
C10 C11 1.381(7) .
C10 C19 1.512(7) .
C11 C12 1.405(7) .
C12 C13 1.403(7) .
C12 C20 1.535(7) .
C24 C25 1.375(6) .
C24 C29 1.388(6) .
C25 C26 1.401(6) .
C25 C37 1.551(7) .
C26 C27 1.382(7) .
C27 C28 1.383(7) .
C27 C41 1.524(7) .
C28 C29 1.396(6) .
C29 C30 1.509(6) .
C30 C31 1.502(6) .
C31 C32 1.364(6) .
C31 C36 1.397(6) .
C32 C33 1.387(7) .
C33 C34 1.384(7) .
C33 C42 1.514(7) .
C34 C35 1.397(7) .
C35 C36 1.396(6) .
C35 C43 1.513(7) .
C14 C15 1.527(7) .
C14 C17 1.535(7) .
C14 C16 1.549(7) .
C20 C22 1.543(7) .
C20 C23 1.545(7) .
C20 C21 1.553(7) .
C37 C38 1.534(7) .
C37 C39 1.536(7) .
C37 C40 1.539(7) .
C43 C44 1.526(7) .
C43 C45 1.531(8) .
C43 C46 1.532(7) .
C47 C48 1.476(9) .
C49 C50 1.508(10) .
C51 C52 1.481(8) .
C53 C54 1.464(7) .
C55 C56 1.424(9) .
C57 C58 1.465(8) .
O15 C62 1.369(12) .
O15 C59 1.423(14) .
O16 C66 1.320(17) .
O16 C63 1.365(13) .
C63 C64 1.426(13) .
C64 C65 1.437(13) .
C60 C59 1.400(15) .
C60 C61 1.527(13) .
C61 C62 1.436(14) .
C66 C65 1.467(16) .
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
O4 H8 O8 1.14(8) 1.26(8) 2.397(4) 173(6) 2_545
C30 H30B O9 0.97 2.84 3.522(6) 127.7 .
C30 H30B O7 0.97 2.45 3.235(6) 137.9 .
