# Copyright The Royal Society of Chemistry, 1999
# CCDC Number: 182/1151
data_hull4

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C104 H148.66 K2 O16.66'
_chemical_formula_weight          1743.73

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'

_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/n

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'

_cell_length_a                    16.1867(3)
_cell_length_b                    12.1515(2)
_cell_length_c                    26.4092(4)
_cell_angle_alpha                 90.00
_cell_angle_beta                  105.827(2)
_cell_angle_gamma                 90.00
_cell_volume                      4997.57(15)
_cell_formula_units_Z             2
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     16470
_cell_measurement_theta_min       1.79
_cell_measurement_theta_max       26.78

_exptl_crystal_description        block
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.10
_exptl_crystal_size_mid           0.05
_exptl_crystal_size_min           0.03
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.159
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1888
_exptl_absorpt_coefficient_mu     0.157
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?
_exptl_absorpt_process_details    ?

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       160(2)
_diffrn_radiation_wavelength      0.68790
_diffrn_radiation_type            Synchrotron
_diffrn_radiation_source          'Daresbury SRS Station 9.8'
_diffrn_radiation_monochromator   'Silicon 111'
_diffrn_measurement_device_type   'Siemens SMART CCD diffractometer'
_diffrn_measurement_method        '\w rotation with narrow frames'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          0
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         10
_diffrn_reflns_number             25725
_diffrn_reflns_av_R_equivalents   0.0372
_diffrn_reflns_av_sigmaI/netI     0.0526
_diffrn_reflns_limit_h_min        -20
_diffrn_reflns_limit_h_max        17
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        15
_diffrn_reflns_limit_l_min        -34
_diffrn_reflns_limit_l_max        34
_diffrn_reflns_theta_min          1.80
_diffrn_reflns_theta_max          26.99
_reflns_number_total              10828
_reflns_number_gt                 7613
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Siemens SMART'
_computing_cell_refinement        'local programs'
_computing_data_reduction         'Siemens SAINT'
_computing_structure_solution     'Siemens SHELXTL'
_computing_structure_refinement   'Siemens SHELXTL'
_computing_molecular_graphics     'Siemens SHELXTL'
_computing_publication_material   'SHELXTL and local programs'

_refine_special_details
;
 Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F^2^, conventional R-factors R are based
 on F, with F set to zero for negative F^2^. The threshold expression of
 F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F^2^ are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
 'calc w=1/[\s^2^(Fo^2^)+(0.1865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    mixed
_refine_ls_hydrogen_treatment     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          10828
_refine_ls_number_parameters      649
_refine_ls_number_restraints      110
_refine_ls_R_factor_all           0.1014
_refine_ls_R_factor_gt            0.0802
_refine_ls_wR_factor_ref          0.2642
_refine_ls_wR_factor_gt           0.2475
_refine_ls_goodness_of_fit_ref    1.060
_refine_ls_restrained_S_all       1.078
_refine_ls_shift/su_max           0.909
_refine_ls_shift/su_mean          0.018

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 0.05956(4) 1.08936(5) 0.94600(3) 0.0377(2) Uani 1 1 d . . .
O1 O 0.06799(11) 1.08033(16) 1.05886(8) 0.0267(4) Uani 1 1 d D . .
H1O H 0.049(2) 1.108(3) 1.0755(13) 0.035(10) Uiso 1 1 d D . .
O2 O 0.16871(13) 0.91943(16) 0.94542(8) 0.0295(4) Uani 1 1 d D C .
H2O H 0.151(3) 0.905(3) 0.9203(12) 0.056(14) Uiso 1 1 d D . .
O3 O 0.11331(11) 0.86398(14) 0.85076(7) 0.0239(4) Uani 1 1 d . C .
O4 O -0.02027(12) 0.80064(16) 0.87098(8) 0.0289(4) Uani 1 1 d D C .
H4O H 0.020(3) 0.798(6) 0.867(3) 0.18(3) Uiso 1 1 d D . .
C1 C 0.19080(15) 1.2024(2) 1.08146(9) 0.0222(5) Uani 1 1 d . . .
C2 C 0.27916(16) 1.2137(2) 1.09128(10) 0.0268(5) Uani 1 1 d . C .
H2 H 0.3041 1.2842 1.1005 0.032 Uiso 1 1 calc R . .
C3 C 0.33207(16) 1.1266(2) 1.08813(11) 0.0299(6) Uani 1 1 d . . .
C4 C 0.29371(16) 1.0261(2) 1.07329(10) 0.0278(6) Uani 1 1 d . C .
H4 H 0.3288 0.9655 1.0698 0.033 Uiso 1 1 calc R . .
C5 C 0.20596(15) 1.0098(2) 1.06322(9) 0.0231(5) Uani 1 1 d . C .
C6 C 0.15509(15) 1.0988(2) 1.06839(9) 0.0220(5) Uani 1 1 d . C .
C7 C 0.43004(18) 1.1395(3) 1.10033(14) 0.0446(8) Uani 1 1 d DU A .
C8 C 0.4731(4) 1.0467(7) 1.1399(4) 0.083(2) Uani 0.691(7) 1 d PDU A 1
H8A H 0.4522 0.9747 1.1251 0.124 Uiso 0.691(7) 1 calc PR A 1
H8B H 0.4585 1.0572 1.1733 0.124 Uiso 0.691(7) 1 calc PR A 1
H8C H 0.5356 1.0501 1.1462 0.124 Uiso 0.691(7) 1 calc PR A 1
C9 C 0.4565(4) 1.1151(9) 1.0501(3) 0.094(3) Uani 0.691(7) 1 d PDU A 1
H9A H 0.4328 1.0439 1.0358 0.141 Uiso 0.691(7) 1 calc PR A 1
H9B H 0.5193 1.1128 1.0583 0.141 Uiso 0.691(7) 1 calc PR A 1
H9C H 0.4344 1.1730 1.0241 0.141 Uiso 0.691(7) 1 calc PR A 1
C10 C 0.4643(5) 1.2413(7) 1.1269(6) 0.124(5) Uani 0.691(7) 1 d PDU A 1
H10A H 0.5268 1.2423 1.1333 0.186 Uiso 0.691(7) 1 calc PR A 1
H10B H 0.4499 1.2459 1.1606 0.186 Uiso 0.691(7) 1 calc PR A 1
H10C H 0.4392 1.3042 1.1048 0.186 Uiso 0.691(7) 1 calc PR A 1
C8A C 0.4769(7) 1.0425(9) 1.0934(8) 0.073(5) Uani 0.309(7) 1 d PDU A 2
H8A1 H 0.4479 1.0072 1.0599 0.110 Uiso 0.309(7) 1 calc PR A 2
H8A2 H 0.4795 0.9911 1.1223 0.110 Uiso 0.309(7) 1 calc PR A 2
H8A3 H 0.5353 1.0632 1.0932 0.110 Uiso 0.309(7) 1 calc PR A 2
C9A C 0.4458(5) 1.2350(10) 1.0615(5) 0.049(3) Uani 0.309(7) 1 d PDU A 2
H9A1 H 0.4282 1.2086 1.0251 0.073 Uiso 0.309(7) 1 calc PR A 2
H9A2 H 0.5069 1.2544 1.0710 0.073 Uiso 0.309(7) 1 calc PR A 2
H9A3 H 0.4119 1.3001 1.0649 0.073 Uiso 0.309(7) 1 calc PR A 2
C10A C 0.4601(9) 1.1949(18) 1.1517(5) 0.082(6) Uani 0.309(7) 1 d PDU A 2
H10D H 0.4313 1.2663 1.1502 0.123 Uiso 0.309(7) 1 calc PR A 2
H10E H 0.5223 1.2061 1.1601 0.123 Uiso 0.309(7) 1 calc PR A 2
H10F H 0.4466 1.1492 1.1789 0.123 Uiso 0.309(7) 1 calc PR A 2
C11 C 0.16664(16) 0.8975(2) 1.04879(10) 0.0260(5) Uani 1 1 d . . .
H11A H 0.1583 0.8614 1.0807 0.031 Uiso 1 1 calc R C .
H11B H 0.1096 0.9058 1.0231 0.031 Uiso 1 1 calc R . .
C12 C 0.22277(16) 0.8261(2) 1.02533(10) 0.0248(5) Uani 1 1 d . C .
C13 C 0.27855(16) 0.7521(2) 1.05554(10) 0.0271(5) Uani 1 1 d . . .
H13 H 0.2770 0.7401 1.0908 0.032 Uiso 1 1 calc R C .
C14 C 0.33758(17) 0.6935(2) 1.03635(11) 0.0296(6) Uani 1 1 d . C .
C15 C 0.33773(16) 0.7139(2) 0.98474(10) 0.0257(5) Uani 1 1 d . . .
H15 H 0.3774 0.6752 0.9707 0.031 Uiso 1 1 calc R C .
C16 C 0.28268(15) 0.7879(2) 0.95302(10) 0.0231(5) Uani 1 1 d . C .
C17 C 0.22383(15) 0.84458(19) 0.97355(10) 0.0223(5) Uani 1 1 d . . .
C18 C 0.3994(2) 0.6140(3) 1.07307(13) 0.0451(8) Uani 1 1 d . . .
C19 C 0.4477(3) 0.6753(4) 1.12280(17) 0.0737(13) Uani 1 1 d . C .
H19A H 0.4064 0.7076 1.1396 0.111 Uiso 1 1 calc R . .
H19B H 0.4826 0.7338 1.1135 0.111 Uiso 1 1 calc R . .
H19C H 0.4851 0.6238 1.1472 0.111 Uiso 1 1 calc R . .
C20 C 0.3464(3) 0.5258(3) 1.09021(19) 0.0743(13) Uani 1 1 d . C .
H20A H 0.3052 0.5605 1.1064 0.111 Uiso 1 1 calc R . .
H20B H 0.3844 0.4770 1.1158 0.111 Uiso 1 1 calc R . .
H20C H 0.3153 0.4829 1.0595 0.111 Uiso 1 1 calc R . .
C21 C 0.4629(3) 0.5662(4) 1.04843(16) 0.0630(11) Uani 1 1 d . C .
H21A H 0.4963 0.6254 1.0384 0.094 Uiso 1 1 calc R . .
H21B H 0.4329 0.5244 1.0170 0.094 Uiso 1 1 calc R . .
H21C H 0.5015 0.5170 1.0735 0.094 Uiso 1 1 calc R . .
C22 C 0.28916(15) 0.8111(2) 0.89802(10) 0.0251(5) Uani 1 1 d . . .
H22A H 0.3493 0.7985 0.8973 0.030 Uiso 1 1 calc R C .
H22B H 0.2762 0.8899 0.8902 0.030 Uiso 1 1 calc R . .
C23 C 0.23088(15) 0.7433(2) 0.85462(9) 0.0219(5) Uani 1 1 d . C .
C24 C 0.26194(15) 0.6502(2) 0.83610(10) 0.0264(5) Uani 1 1 d . . .
H24 H 0.3200 0.6295 0.8513 0.032 Uiso 1 1 calc R C .
C25 C 0.21150(16) 0.5857(2) 0.79623(10) 0.0283(6) Uani 1 1 d . A .
C26 C 0.12707(16) 0.6198(2) 0.77474(10) 0.0257(5) Uani 1 1 d . . .
H26 H 0.0911 0.5777 0.7471 0.031 Uiso 1 1 calc R C .
C27 C 0.09374(15) 0.7124(2) 0.79210(9) 0.0220(5) Uani 1 1 d . C .
C28 C 0.14602(15) 0.7747(2) 0.83271(9) 0.0220(5) Uani 1 1 d . . .
C29 C 0.24653(19) 0.4837(3) 0.77462(12) 0.0421(7) Uani 1 1 d D . .
C30 C 0.1912(3) 0.3857(4) 0.7768(2) 0.0507(15) Uani 0.691(7) 1 d PD A 1
H30A H 0.1314 0.4025 0.7582 0.076 Uiso 0.838(7) 1 calc PR B 1
H30B H 0.1953 0.3679 0.8136 0.076 Uiso 0.838(7) 1 calc PR B 1
H30C H 0.2108 0.3226 0.7600 0.076 Uiso 0.838(7) 1 calc PR B 1
C31 C 0.2419(3) 0.5094(4) 0.71600(16) 0.0610(14) Uani 0.838(7) 1 d PD A 1
H31A H 0.2779 0.5735 0.7144 0.092 Uiso 0.838(7) 1 calc PR B 1
H31B H 0.1824 0.5251 0.6965 0.092 Uiso 0.838(7) 1 calc PR B 1
H31C H 0.2627 0.4457 0.7003 0.092 Uiso 0.838(7) 1 calc PR B 1
C32 C 0.3388(3) 0.4617(4) 0.8025(2) 0.0633(16) Uani 0.838(7) 1 d PD A 1
H32A H 0.3732 0.5270 0.8003 0.095 Uiso 0.838(7) 1 calc PR B 1
H32B H 0.3594 0.3991 0.7859 0.095 Uiso 0.838(7) 1 calc PR B 1
H32C H 0.3442 0.4447 0.8395 0.095 Uiso 0.838(7) 1 calc PR B 1
C30A C 0.3264(12) 0.5021(19) 0.7586(9) 0.056(6) Uiso 0.162(7) 1 d PD A 2
C31A C 0.2740(13) 0.3984(16) 0.8253(7) 0.047(6) Uiso 0.162(7) 1 d PD A 2
C32A C 0.1830(12) 0.4124(17) 0.7364(8) 0.053(6) Uiso 0.162(7) 1 d PD A 2
C33 C 0.00240(15) 0.7473(2) 0.76723(9) 0.0248(5) Uani 1 1 d . . .
H33A H -0.0125 0.7294 0.7292 0.030 Uiso 1 1 calc R C .
H33B H -0.0014 0.8282 0.7704 0.030 Uiso 1 1 calc R . .
C34 C -0.06345(14) 0.6946(2) 0.79071(10) 0.0227(5) Uani 1 1 d . C .
C35 C -0.12028(16) 0.6180(2) 0.76192(10) 0.0298(6) Uani 1 1 d . . .
H35 H -0.1155 0.5984 0.7280 0.036 Uiso 1 1 calc R C .
C36 C -0.18375(17) 0.5685(2) 0.77992(11) 0.0347(6) Uani 1 1 d . C .
C37 C -0.18699(16) 0.5963(2) 0.83025(11) 0.0287(6) Uani 1 1 d . . .
H37 H -0.2290 0.5624 0.8441 0.034 Uiso 1 1 calc R C .
C38 C -0.13091(15) 0.6717(2) 0.86097(10) 0.0228(5) Uani 1 1 d . C .
C39 C -0.07038(14) 0.72276(19) 0.84057(9) 0.0206(5) Uani 1 1 d . . .
C40 C -0.2476(2) 0.4891(3) 0.74513(14) 0.0538(10) Uani 1 1 d . . .
C41 C -0.3108(3) 0.4450(5) 0.77179(19) 0.0914(19) Uani 1 1 d . C .
H41A H -0.3505 0.3948 0.7479 0.137 Uiso 1 1 calc R . .
H41B H -0.3432 0.5060 0.7813 0.137 Uiso 1 1 calc R . .
H41C H -0.2803 0.4051 0.8037 0.137 Uiso 1 1 calc R . .
C42 C -0.2011(3) 0.3964(4) 0.7267(2) 0.0789(15) Uani 1 1 d . C .
H42A H -0.2430 0.3465 0.7043 0.118 Uiso 1 1 calc R . .
H42B H -0.1665 0.3559 0.7573 0.118 Uiso 1 1 calc R . .
H42C H -0.1635 0.4265 0.7067 0.118 Uiso 1 1 calc R . .
C43 C -0.2975(3) 0.5539(5) 0.69505(18) 0.0852(15) Uani 1 1 d . C .
H43A H -0.3391 0.5049 0.6717 0.128 Uiso 1 1 calc R . .
H43B H -0.2569 0.5815 0.6765 0.128 Uiso 1 1 calc R . .
H43C H -0.3278 0.6160 0.7055 0.128 Uiso 1 1 calc R . .
C44 C -0.13645(16) 0.6982(2) 0.91585(10) 0.0237(5) Uani 1 1 d . . .
H44A H -0.1605 0.6338 0.9299 0.028 Uiso 1 1 calc R C .
H44B H -0.0777 0.7109 0.9388 0.028 Uiso 1 1 calc R . .
O301 O 0.0684(2) 1.07621(19) 0.84456(10) 0.0645(8) Uani 1 1 d D C .
C301 C 0.0383(4) 1.1392(4) 0.7988(2) 0.0809(14) Uani 1 1 d D . .
H30D H -0.0093 1.0999 0.7738 0.097 Uiso 1 1 calc R C .
H30E H 0.0851 1.1499 0.7818 0.097 Uiso 1 1 calc R . .
C302 C 0.0082(4) 1.2454(5) 0.8115(3) 0.121(2) Uani 1 1 d D C .
H30F H -0.0115 1.2892 0.7793 0.182 Uiso 1 1 calc R . .
H30G H 0.0553 1.2840 0.8365 0.182 Uiso 1 1 calc R . .
H30H H -0.0394 1.2347 0.8273 0.182 Uiso 1 1 calc R . .
O201 O 0.0023(3) 1.2897(3) 0.95006(17) 0.1030(12) Uani 1 1 d D C .
C201 C -0.0593(6) 1.3600(7) 0.9513(5) 0.175(5) Uani 1 1 d D . .
H20D H -0.0990 1.3279 0.9699 0.210 Uiso 1 1 calc R C .
H20E H -0.0351 1.4290 0.9691 0.210 Uiso 1 1 calc R . .
C202 C -0.0980(8) 1.3777(10) 0.9030(5) 0.233(8) Uani 1 1 d D C .
H20F H -0.1452 1.4297 0.9007 0.350 Uiso 1 1 calc R . .
H20G H -0.1210 1.3083 0.8861 0.350 Uiso 1 1 calc R . .
H20H H -0.0575 1.4088 0.8853 0.350 Uiso 1 1 calc R . .
O101 O 0.1569(3) 1.2828(4) 0.94743(19) 0.0677(13) Uani 0.656(5) 1 d PDU C 1
C101 C 0.2226(8) 1.3327(7) 0.9494(6) 0.073(3) Uani 0.656(5) 1 d PDU C 1
O102 O 0.2887(3) 1.2827(4) 0.9363(2) 0.0807(16) Uani 0.656(5) 1 d PDU C 1
C102 C 0.2810(3) 1.1619(4) 0.9287(3) 0.0590(16) Uani 0.656(5) 1 d PDU C 1
H10G H 0.2857 1.1225 0.9622 0.071 Uiso 0.656(5) 1 calc PR C 1
H10H H 0.2269 1.1409 0.9025 0.071 Uiso 0.656(5) 1 calc PR C 1
C103 C 0.3536(6) 1.1446(8) 0.9097(4) 0.111(3) Uani 0.656(5) 1 d PDU C 1
H10I H 0.3586 1.0661 0.9026 0.166 Uiso 0.656(5) 1 calc PR C 1
H10J H 0.4054 1.1691 0.9362 0.166 Uiso 0.656(5) 1 calc PR C 1
H10K H 0.3472 1.1866 0.8772 0.166 Uiso 0.656(5) 1 calc PR C 1
O103 O 0.2382(3) 1.4377(4) 0.9532(2) 0.0859(17) Uani 0.656(5) 1 d PDU C 1
C104 C 0.1691(4) 1.5059(5) 0.9562(4) 0.082(2) Uani 0.656(5) 1 d PDU C 1
H10L H 0.1373 1.4665 0.9778 0.098 Uiso 0.656(5) 1 calc PR C 1
H10M H 0.1943 1.5723 0.9763 0.098 Uiso 0.656(5) 1 calc PR C 1
C105 C 0.1120(4) 1.5402(5) 0.9135(3) 0.070(2) Uani 0.656(5) 1 d PDU C 1
H10N H 0.0688 1.5854 0.9235 0.106 Uiso 0.656(5) 1 calc PR C 1
H10O H 0.0840 1.4766 0.8931 0.106 Uiso 0.656(5) 1 calc PR C 1
H10P H 0.1406 1.5841 0.8922 0.106 Uiso 0.656(5) 1 calc PR C 1
O401 O 0.2001(9) 1.2076(9) 0.9337(9) 0.175(9) Uani 0.344(5) 1 d PDU C 2
C401 C 0.2220(18) 1.3198(12) 0.9356(16) 0.094(5) Uani 0.344(5) 1 d PDU C 2
H40A H 0.2248 1.3436 0.9003 0.113 Uiso 0.344(5) 1 calc PR C 2
H40B H 0.2799 1.3295 0.9602 0.113 Uiso 0.344(5) 1 calc PR C 2
C402 C 0.1615(7) 1.3903(8) 0.9526(6) 0.066(4) Uani 0.344(5) 1 d PDU C 2
H40C H 0.1804 1.4670 0.9535 0.099 Uiso 0.344(5) 1 calc PR C 2
H40D H 0.1589 1.3679 0.9878 0.099 Uiso 0.344(5) 1 calc PR C 2
H40E H 0.1043 1.3831 0.9278 0.099 Uiso 0.344(5) 1 calc PR C 2

loop_
 _atom_site_aniso_label
 _atom_site_aniso_U_11
 _atom_site_aniso_U_22
 _atom_site_aniso_U_33
 _atom_site_aniso_U_23
 _atom_site_aniso_U_13
 _atom_site_aniso_U_12
K1 0.0338(4) 0.0387(4) 0.0410(4) -0.0012(3) 0.0111(3) -0.0026(3)
O1 0.0171(8) 0.0307(10) 0.0338(10) -0.0134(8) 0.0094(8) -0.0050(7)
O2 0.0293(10) 0.0298(10) 0.0275(11) -0.0057(8) 0.0044(8) 0.0051(8)
O3 0.0220(8) 0.0232(9) 0.0273(9) -0.0014(7) 0.0079(7) 0.0005(7)
O4 0.0238(9) 0.0345(10) 0.0316(10) -0.0133(8) 0.0128(8) -0.0087(8)
C1 0.0217(12) 0.0259(12) 0.0201(11) -0.0031(9) 0.0075(9) -0.0021(9)
C2 0.0240(12) 0.0270(13) 0.0310(13) -0.0068(10) 0.0101(10) -0.0067(10)
C3 0.0193(12) 0.0338(14) 0.0371(15) -0.0058(11) 0.0083(11) -0.0046(10)
C4 0.0217(12) 0.0299(14) 0.0331(14) -0.0055(10) 0.0095(10) 0.0007(10)
C5 0.0224(12) 0.0256(12) 0.0229(12) -0.0053(9) 0.0088(9) -0.0035(9)
C6 0.0178(11) 0.0289(13) 0.0198(11) -0.0049(9) 0.0063(9) -0.0020(9)
C7 0.0186(13) 0.0497(19) 0.065(2) -0.0144(15) 0.0105(13) -0.0057(12)
C8 0.024(3) 0.102(5) 0.111(6) 0.008(4) -0.002(3) 0.011(3)
C9 0.030(3) 0.181(10) 0.079(4) -0.021(5) 0.027(3) -0.025(4)
C10 0.027(3) 0.078(5) 0.266(14) -0.091(7) 0.038(6) -0.023(3)
C8A 0.016(5) 0.050(6) 0.155(17) 0.006(7) 0.025(7) 0.005(4)
C9A 0.011(4) 0.066(7) 0.073(7) 0.015(6) 0.017(4) -0.009(4)
C10A 0.024(6) 0.155(17) 0.056(7) -0.027(8) -0.006(5) -0.052(8)
C11 0.0248(12) 0.0262(13) 0.0302(13) -0.0090(10) 0.0129(10) -0.0053(10)
C12 0.0241(12) 0.0220(12) 0.0313(13) -0.0064(10) 0.0126(10) -0.0044(9)
C13 0.0288(13) 0.0277(13) 0.0264(13) -0.0028(10) 0.0104(11) -0.0032(10)
C14 0.0286(13) 0.0295(13) 0.0317(14) -0.0009(11) 0.0099(11) 0.0011(10)
C15 0.0215(12) 0.0272(13) 0.0300(13) -0.0061(10) 0.0096(10) -0.0010(10)
C16 0.0181(11) 0.0280(13) 0.0240(12) -0.0067(9) 0.0068(9) -0.0066(9)
C17 0.0189(11) 0.0209(11) 0.0263(12) -0.0043(9) 0.0048(9) -0.0040(9)
C18 0.0494(19) 0.0450(18) 0.0406(17) 0.0106(14) 0.0118(15) 0.0184(15)
C19 0.070(3) 0.084(3) 0.054(2) -0.013(2) -0.007(2) 0.027(2)
C20 0.090(3) 0.060(3) 0.087(3) 0.036(2) 0.049(3) 0.033(2)
C21 0.063(2) 0.074(3) 0.056(2) 0.0179(19) 0.0242(19) 0.038(2)
C22 0.0186(11) 0.0334(13) 0.0251(12) -0.0032(10) 0.0090(10) -0.0056(10)
C23 0.0190(11) 0.0292(13) 0.0192(11) 0.0005(9) 0.0080(9) -0.0035(9)
C24 0.0172(11) 0.0388(15) 0.0238(12) -0.0012(10) 0.0068(10) 0.0025(10)
C25 0.0243(12) 0.0356(14) 0.0261(13) -0.0048(10) 0.0088(10) 0.0043(10)
C26 0.0232(12) 0.0327(13) 0.0215(12) -0.0065(10) 0.0066(10) -0.0013(10)
C27 0.0188(11) 0.0295(13) 0.0193(11) 0.0000(9) 0.0077(9) -0.0006(9)
C28 0.0223(11) 0.0240(12) 0.0228(12) 0.0001(9) 0.0112(10) -0.0014(9)
C29 0.0326(15) 0.0467(18) 0.0441(17) -0.0197(14) 0.0054(13) 0.0093(13)
C30 0.050(3) 0.023(2) 0.075(4) -0.014(2) 0.010(3) 0.0053(19)
C31 0.056(3) 0.085(3) 0.043(2) -0.026(2) 0.014(2) 0.024(2)
C32 0.042(2) 0.066(3) 0.071(3) -0.030(2) -0.004(2) 0.029(2)
C33 0.0221(12) 0.0331(13) 0.0192(11) -0.0004(10) 0.0057(9) 0.0020(10)
C34 0.0164(11) 0.0281(12) 0.0230(12) -0.0012(9) 0.0043(9) 0.0038(9)
C35 0.0239(13) 0.0411(15) 0.0240(13) -0.0108(11) 0.0062(10) -0.0016(11)
C36 0.0270(13) 0.0434(16) 0.0335(15) -0.0168(12) 0.0079(12) -0.0103(12)
C37 0.0242(12) 0.0310(14) 0.0325(14) -0.0097(11) 0.0105(11) -0.0082(10)
C38 0.0200(11) 0.0239(12) 0.0246(12) -0.0043(9) 0.0061(9) 0.0016(9)
C39 0.0158(10) 0.0216(11) 0.0232(12) -0.0035(9) 0.0033(9) 0.0009(9)
C40 0.0434(18) 0.071(2) 0.050(2) -0.0368(18) 0.0177(15) -0.0294(17)
C41 0.085(3) 0.121(4) 0.081(3) -0.062(3) 0.043(3) -0.078(3)
C42 0.074(3) 0.067(3) 0.100(4) -0.050(3) 0.031(3) -0.024(2)
C43 0.056(2) 0.131(4) 0.053(3) -0.020(3) -0.012(2) -0.028(3)
C44 0.0234(12) 0.0244(12) 0.0235(12) -0.0023(9) 0.0071(10) -0.0012(9)
O301 0.112(2) 0.0365(13) 0.0393(13) 0.0048(10) 0.0116(14) 0.0100(13)
C301 0.091(3) 0.076(3) 0.080(3) 0.026(2) 0.032(3) 0.026(3)
C302 0.105(5) 0.110(5) 0.149(6) 0.062(4) 0.034(4) 0.040(4)
O201 0.137(4) 0.057(2) 0.124(3) -0.008(2) 0.051(3) -0.009(2)
C201 0.138(7) 0.122(7) 0.314(15) -0.118(8) 0.144(9) -0.082(6)
C202 0.166(10) 0.186(11) 0.307(17) 0.151(12) -0.007(11) -0.028(8)
O101 0.062(3) 0.058(3) 0.083(3) 0.002(2) 0.021(2) -0.015(2)
C101 0.073(4) 0.067(4) 0.078(8) -0.015(4) 0.019(4) -0.004(3)
O102 0.054(3) 0.064(3) 0.121(4) -0.008(3) 0.020(3) 0.000(2)
C102 0.031(2) 0.044(3) 0.092(5) -0.011(3) 0.000(3) -0.005(2)
C103 0.102(6) 0.111(7) 0.124(8) -0.040(6) 0.039(6) -0.035(5)
O103 0.067(3) 0.060(3) 0.133(5) -0.025(3) 0.032(3) -0.016(2)
C104 0.050(3) 0.040(3) 0.146(7) 0.007(4) 0.011(4) -0.004(3)
C105 0.068(4) 0.064(4) 0.088(5) 0.045(3) 0.035(3) -0.013(3)
O401 0.098(9) 0.075(7) 0.38(3) -0.010(11) 0.122(13) -0.021(7)
C401 0.087(8) 0.091(7) 0.100(14) -0.001(8) 0.016(8) 0.002(7)
C402 0.042(6) 0.035(5) 0.120(11) 0.004(6) 0.022(6) -0.012(4)

_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
K1 O201 2.617(4) . ?
K1 O2 2.7204(19) . ?
K1 O301 2.726(3) . ?
K1 O401 2.783(12) . ?
K1 O101 2.824(4) . ?
K1 O1 2.8959(19) 3_577 ?
K1 O1 2.948(2) . ?
O1 H1O 0.69(3) . ?
O1 C6 1.381(3) . ?
O1 K1 2.8960(19) 3_577 ?
O2 H2O 0.67(3) . ?
O2 C17 1.347(3) . ?
O3 C28 1.350(3) . ?
O4 H4O 0.68(3) . ?
O4 C39 1.358(3) . ?
C1 C6 1.388(3) . ?
C1 C2 1.389(3) . ?
C1 C44 1.507(3) 3_577 ?
C2 C3 1.379(4) . ?
C3 C4 1.377(4) . ?
C3 C7 1.538(4) . ?
C4 C5 1.386(3) . ?
C5 C6 1.389(3) . ?
C5 C11 1.509(3) . ?
C7 C8A 1.440(11) . ?
C7 C10 1.456(7) . ?
C7 C10A 1.473(12) . ?
C7 C9 1.529(7) . ?
C7 C8 1.566(8) . ?
C7 C9A 1.615(10) . ?
C11 C12 1.506(3) . ?
C12 C13 1.367(4) . ?
C12 C17 1.391(4) . ?
C13 C14 1.393(4) . ?
C14 C15 1.386(4) . ?
C14 C18 1.532(4) . ?
C15 C16 1.378(4) . ?
C16 C17 1.399(3) . ?
C16 C22 1.511(3) . ?
C18 C21 1.476(5) . ?
C18 C20 1.517(6) . ?
C18 C19 1.527(5) . ?
C22 C23 1.514(3) . ?
C23 C24 1.381(4) . ?
C23 C28 1.390(3) . ?
C24 C25 1.385(4) . ?
C25 C26 1.392(4) . ?
C25 C29 1.536(4) . ?
C26 C27 1.379(3) . ?
C27 C28 1.394(3) . ?
C27 C33 1.506(3) . ?
C29 C30A 1.483(15) . ?
C29 C32 1.498(5) . ?
C29 C30 1.501(6) . ?
C29 C32A 1.504(15) . ?
C29 C31 1.561(5) . ?
C29 C31A 1.654(14) . ?
C33 C34 1.514(3) . ?
C34 C35 1.382(4) . ?
C34 C39 1.394(3) . ?
C35 C36 1.382(4) . ?
C36 C37 1.386(4) . ?
C36 C40 1.526(4) . ?
C37 C38 1.386(3) . ?
C38 C39 1.387(3) . ?
C38 C44 1.511(3) . ?
C40 C41 1.490(5) . ?
C40 C42 1.507(6) . ?
C40 C43 1.562(7) . ?
C44 C1 1.507(3) 3_577 ?
O301 C301 1.400(5) . ?
C301 C302 1.450(8) . ?
O201 C201 1.321(9) . ?
C201 C202 1.275(12) . ?
O101 C101 1.213(12) . ?
C101 O103 1.299(9) . ?
C101 O102 1.356(10) . ?
O102 C102 1.481(7) . ?
C102 C103 1.414(10) . ?
O103 C104 1.412(8) . ?
C104 C105 1.316(9) . ?
O401 C401 1.407(11) . ?
C401 C402 1.461(12) . ?

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
 _geom_angle_publ_flag
O201 K1 O2 160.72(11) . . ?
O201 K1 O301 102.05(11) . . ?
O2 K1 O301 75.04(7) . . ?
O201 K1 O401 80.5(2) . . ?
O2 K1 O401 80.7(2) . . ?
O301 K1 O401 69.6(5) . . ?
O201 K1 O101 55.09(14) . . ?
O2 K1 O101 105.72(11) . . ?
O301 K1 O101 83.30(12) . . ?
O401 K1 O101 26.0(2) . . ?
O201 K1 O1 114.08(11) . 3_577 ?
O2 K1 O1 85.16(6) . 3_577 ?
O301 K1 O1 98.19(8) . 3_577 ?
O401 K1 O1 163.3(3) . 3_577 ?
O101 K1 O1 168.98(11) . 3_577 ?
O201 K1 O1 84.98(10) . . ?
O2 K1 O1 97.26(6) . . ?
O301 K1 O1 172.27(7) . . ?
O401 K1 O1 108.9(5) . . ?
O101 K1 O1 98.37(11) . . ?
O1 K1 O1 81.61(6) 3_577 . ?
O201 K1 C6 90.24(11) . . ?
O2 K1 C6 84.07(6) . . ?
O301 K1 C6 149.23(8) . . ?
O401 K1 C6 85.1(5) . . ?
O101 K1 C6 80.88(11) . . ?
O1 K1 C6 102.35(6) 3_577 . ?
O1 K1 C6 25.68(5) . . ?
O201 K1 C5 112.61(11) . . ?
O2 K1 C5 60.58(6) . . ?
O301 K1 C5 130.68(8) . . ?
O401 K1 C5 82.4(5) . . ?
O101 K1 C5 88.71(11) . . ?
O1 K1 C5 98.37(6) 3_577 . ?
O1 K1 C5 42.14(5) . . ?
C6 K1 C5 23.50(6) . . ?
O201 K1 K1 102.05(10) . 3_577 ?
O2 K1 K1 91.66(5) . 3_577 ?
O301 K1 K1 138.91(7) . 3_577 ?
O401 K1 K1 147.4(5) . 3_577 ?
O101 K1 K1 137.70(10) . 3_577 ?
O1 K1 K1 41.25(4) 3_577 3_577 ?
O1 K1 K1 40.36(4) . 3_577 ?
C6 K1 K1 62.57(5) . 3_577 ?
C5 K1 K1 66.50(4) . 3_577 ?
H1O O1 C6 115(3) . . ?
H1O O1 K1 86(3) . 3_577 ?
C6 O1 K1 143.50(15) . 3_577 ?
H1O O1 K1 136(3) . . ?
C6 O1 K1 86.66(13) . . ?
K1 O1 K1 98.39(6) 3_577 . ?
H2O O2 C17 114(4) . . ?
H2O O2 K1 96(4) . . ?
C17 O2 K1 147.47(16) . . ?
H4O O4 C39 109(7) . . ?
C6 C1 C2 118.3(2) . . ?
C6 C1 C44 122.0(2) . 3_577 ?
C2 C1 C44 119.7(2) . 3_577 ?
C3 C2 C1 122.5(2) . . ?
C4 C3 C2 117.3(2) . . ?
C4 C3 C7 120.6(2) . . ?
C2 C3 C7 122.1(2) . . ?
C3 C4 C5 122.7(2) . . ?
C4 C5 C6 118.2(2) . . ?
C4 C5 C11 121.2(2) . . ?
C6 C5 C11 120.6(2) . . ?
C4 C5 K1 122.95(17) . . ?
C6 C5 K1 65.99(14) . . ?
C11 C5 K1 83.62(14) . . ?
O1 C6 C1 121.8(2) . . ?
O1 C6 C5 117.3(2) . . ?
C1 C6 C5 120.9(2) . . ?
O1 C6 K1 67.66(12) . . ?
C1 C6 K1 109.83(16) . . ?
C5 C6 K1 90.51(15) . . ?
C8A C7 C10A 116.0(11) . . ?
C10 C7 C9 115.1(6) . . ?
C8A C7 C3 116.1(5) . . ?
C10 C7 C3 115.0(4) . . ?
C10A C7 C3 107.6(6) . . ?
C9 C7 C3 108.4(3) . . ?
C10 C7 C8 104.3(6) . . ?
C9 C7 C8 105.1(5) . . ?
C3 C7 C8 108.2(3) . . ?
C8A C7 C9A 109.1(8) . . ?
C10A C7 C9A 100.7(9) . . ?
C3 C7 C9A 105.8(4) . . ?
C12 C11 C5 111.4(2) . . ?
C13 C12 C17 119.8(2) . . ?
C13 C12 C11 121.0(2) . . ?
C17 C12 C11 118.8(2) . . ?
C12 C13 C14 122.2(2) . . ?
C15 C14 C13 116.9(2) . . ?
C15 C14 C18 124.0(2) . . ?
C13 C14 C18 119.1(2) . . ?
C16 C15 C14 122.7(2) . . ?
C15 C16 C17 118.8(2) . . ?
C15 C16 C22 120.2(2) . . ?
C17 C16 C22 120.9(2) . . ?
O2 C17 C12 117.9(2) . . ?
O2 C17 C16 122.5(2) . . ?
C12 C17 C16 119.6(2) . . ?
C21 C18 C20 111.8(3) . . ?
C21 C18 C19 108.5(3) . . ?
C20 C18 C19 106.7(4) . . ?
C21 C18 C14 112.5(3) . . ?
C20 C18 C14 108.0(3) . . ?
C19 C18 C14 109.2(3) . . ?
C16 C22 C23 115.7(2) . . ?
C24 C23 C28 119.4(2) . . ?
C24 C23 C22 120.1(2) . . ?
C28 C23 C22 120.5(2) . . ?
C23 C24 C25 122.4(2) . . ?
C24 C25 C26 116.8(2) . . ?
C24 C25 C29 122.5(2) . . ?
C26 C25 C29 120.6(2) . . ?
C27 C26 C25 122.4(2) . . ?
C26 C27 C28 119.2(2) . . ?
C26 C27 C33 120.7(2) . . ?
C28 C27 C33 120.0(2) . . ?
O3 C28 C23 120.8(2) . . ?
O3 C28 C27 119.6(2) . . ?
C23 C28 C27 119.6(2) . . ?
C32 C29 C30 111.4(4) . . ?
C30A C29 C32A 112.7(12) . . ?
C30A C29 C25 115.0(10) . . ?
C32 C29 C25 112.4(3) . . ?
C30 C29 C25 110.0(3) . . ?
C32A C29 C25 117.4(9) . . ?
C32 C29 C31 107.1(3) . . ?
C30 C29 C31 109.2(4) . . ?
C25 C29 C31 106.5(3) . . ?
C30A C29 C31A 105.2(11) . . ?
C32A C29 C31A 99.5(11) . . ?
C25 C29 C31A 104.5(8) . . ?
C27 C33 C34 114.8(2) . . ?
C35 C34 C39 118.2(2) . . ?
C35 C34 C33 119.8(2) . . ?
C39 C34 C33 122.0(2) . . ?
C34 C35 C36 123.4(2) . . ?
C35 C36 C37 116.8(2) . . ?
C35 C36 C40 120.9(3) . . ?
C37 C36 C40 122.3(3) . . ?
C36 C37 C38 122.1(2) . . ?
C37 C38 C39 119.2(2) . . ?
C37 C38 C44 120.1(2) . . ?
C39 C38 C44 120.7(2) . . ?
O4 C39 C38 117.0(2) . . ?
O4 C39 C34 122.7(2) . . ?
C38 C39 C34 120.3(2) . . ?
C41 C40 C42 110.6(4) . . ?
C41 C40 C36 112.5(3) . . ?
C42 C40 C36 110.5(3) . . ?
C41 C40 C43 108.6(4) . . ?
C42 C40 C43 107.0(4) . . ?
C36 C40 C43 107.4(3) . . ?
C1 C44 C38 113.9(2) 3_577 . ?
C301 O301 K1 135.8(3) . . ?
O301 C301 C302 110.3(5) . . ?
C201 O201 K1 151.7(4) . . ?
C202 C201 O201 104.7(10) . . ?
C101 O101 K1 153.6(6) . . ?
O101 C101 O103 130.1(9) . . ?
O101 C101 O102 120.6(7) . . ?
O103 C101 O102 108.0(8) . . ?
C101 O102 C102 115.8(6) . . ?
C103 C102 O102 98.5(5) . . ?
C101 O103 C104 116.2(6) . . ?
C105 C104 O103 121.3(8) . . ?
C401 O401 K1 134.6(9) . . ?
O401 C401 C402 113.3(12) . . ?

_diffrn_measured_fraction_theta_max    0.901
_diffrn_reflns_theta_full              25.00
_diffrn_measured_fraction_theta_full   0.995
_refine_diff_density_max    1.229
_refine_diff_density_min   -0.779
_refine_diff_density_rms    0.097