#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:38:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179070 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/32/4303215.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_4303215
loop_
_publ_author_name
'Andrzej W. Misiołek'
'Andrew S. Ichimura'
'Robert A. Gentner'
'Rui H. Huang'
'Vanessa P. McCaffrey'
'James E. Jackson'
_publ_section_title
;
Building Blocks for Molecule-Based Magnets: Radical Anions and Dianions of
Substituted 3,6-Dimethylenecyclohexane-1,2,4,5-tetrones as Paramagnetic
Bridging Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9005
_journal_page_last               9017
_journal_paper_doi               10.1021/ic901390n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C84 H124 K O12'
_chemical_formula_weight         1364.93
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.2809(11)
_cell_angle_beta                 85.5001(12)
_cell_angle_gamma                77.6417(10)
_cell_formula_units_Z            1
_cell_length_a                   9.5055(2)
_cell_length_b                   13.0026(3)
_cell_length_c                   17.1668(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2020.63(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.940
_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  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            22327
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.123
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             743
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     874
_refine_ls_number_reflns         17415
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.1437
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          2.318
_refine_ls_shift/su_mean         0.286
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2361P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.3117
_reflns_number_gt                9758
_reflns_number_total             17415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901390n_si_002_2.cif
_cod_data_source_block           4K.(C4H8O)4
_cod_original_cell_volume        2020.64(7)
_cod_database_code               4303215
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
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
K K 0.5254(3) 0.6177(2) 0.16148(19) 0.0903(5) Uani 1 1 d . . .
C1 C 1.0216(6) 0.6702(5) 0.0754(3) 0.0350(14) Uani 1 1 d . . .
C2 C 1.1564(6) 0.6144(5) 0.1102(4) 0.0360(14) Uani 1 1 d . . .
C3 C 1.1601(6) 0.5616(5) 0.2003(4) 0.0336(13) Uani 1 1 d . . .
C4 C 1.0281(6) 0.5637(4) 0.2486(3) 0.0301(13) Uani 1 1 d . . .
C5 C 0.8924(7) 0.6213(5) 0.2111(3) 0.0385(15) Uani 1 1 d . . .
C6 C 0.8876(6) 0.6729(4) 0.1244(3) 0.0297(12) Uani 1 1 d . . .
C7 C 1.0347(6) 0.5098(5) 0.3287(3) 0.0282(12) Uani 1 1 d . . .
C8 C 0.9434(6) 0.5561(4) 0.3913(3) 0.0304(13) Uani 1 1 d . . .
C9 C 0.8922(7) 0.4898(5) 0.4593(3) 0.0347(14) Uani 1 1 d . . .
H9 H 0.9110 0.4157 0.4630 0.042 Uiso 1 1 calc R . .
C10 C 0.8153(7) 0.5320(5) 0.5202(4) 0.0397(15) Uani 1 1 d . . .
C11 C 0.7954(7) 0.6432(6) 0.5162(4) 0.0420(16) Uani 1 1 d . . .
C12 C 0.8256(7) 0.7131(5) 0.4442(4) 0.0467(17) Uani 1 1 d . . .
C13 C 0.9067(7) 0.6655(5) 0.3850(4) 0.0426(16) Uani 1 1 d . . .
H13 H 0.9370 0.7099 0.3394 0.051 Uiso 1 1 calc R . .
C14 C 0.7503(10) 0.4557(7) 0.5918(4) 0.063(2) Uani 1 1 d . . .
C15 C 0.8125(16) 0.4616(10) 0.6699(5) 0.127(5) Uani 1 1 d . . .
H15A H 0.9154 0.4386 0.6674 0.191 Uiso 1 1 calc R . .
H15B H 0.7729 0.4154 0.7137 0.191 Uiso 1 1 calc R . .
H15C H 0.7883 0.5343 0.6774 0.191 Uiso 1 1 calc R . .
C16 C 0.7576(14) 0.3474(7) 0.5695(6) 0.113(5) Uani 1 1 d . . .
H16A H 0.8536 0.3209 0.5510 0.170 Uiso 1 1 calc R . .
H16B H 0.6914 0.3561 0.5279 0.170 Uiso 1 1 calc R . .
H16C H 0.7322 0.2970 0.6156 0.170 Uiso 1 1 calc R . .
C17 C 0.6103(15) 0.4926(8) 0.6190(9) 0.167(8) Uani 1 1 d . . .
H17A H 0.5439 0.4982 0.5782 0.250 Uiso 1 1 calc R . .
H17B H 0.6034 0.5621 0.6313 0.250 Uiso 1 1 calc R . .
H17C H 0.5873 0.4430 0.6661 0.250 Uiso 1 1 calc R . .
O18 O 0.7305(5) 0.6861(4) 0.5799(3) 0.0539(13) Uani 1 1 d . . .
C19 C 0.8277(13) 0.6963(12) 0.6330(7) 0.123(5) Uani 1 1 d . . .
H19A H 0.7758 0.7271 0.6754 0.184 Uiso 1 1 calc R . .
H19B H 0.8905 0.7422 0.6053 0.184 Uiso 1 1 calc R . .
H19C H 0.8838 0.6266 0.6549 0.184 Uiso 1 1 calc R . .
C20 C 0.7810(10) 0.8365(6) 0.4296(6) 0.078(3) Uani 1 1 d . . .
C21 C 0.8090(12) 0.8914(6) 0.3481(7) 0.096(3) Uani 1 1 d . . .
H21A H 0.9066 0.8649 0.3320 0.144 Uiso 1 1 calc R . .
H21B H 0.7947 0.9674 0.3457 0.144 Uiso 1 1 calc R . .
H21C H 0.7442 0.8782 0.3130 0.144 Uiso 1 1 calc R . .
C22 C 0.6336(14) 0.8709(8) 0.4587(9) 0.152(7) Uani 1 1 d . . .
H22A H 0.6212 0.8318 0.5123 0.227 Uiso 1 1 calc R . .
H22B H 0.5673 0.8570 0.4248 0.227 Uiso 1 1 calc R . .
H22C H 0.6154 0.9466 0.4581 0.227 Uiso 1 1 calc R . .
C23 C 0.883(3) 0.8797(9) 0.4833(11) 0.253(13) Uani 1 1 d . . .
H23A H 0.9824 0.8583 0.4677 0.380 Uiso 1 1 calc R . .
H23B H 0.8688 0.8492 0.5388 0.380 Uiso 1 1 calc R . .
H23C H 0.8575 0.9568 0.4747 0.380 Uiso 1 1 calc R . .
O24 O 0.7753(4) 0.6251(5) 0.2474(3) 0.0712(18) Uani 1 1 d . . .
O25 O 1.2752(5) 0.6133(4) 0.0751(3) 0.0620(15) Uani 1 1 d . . .
O26 O 0.7682(5) 0.7124(4) 0.0958(3) 0.0555(14) Uani 1 1 d . . .
O27 O 1.2816(4) 0.5298(4) 0.2269(2) 0.0480(12) Uani 1 1 d . . .
C28 C 1.1262(6) 0.4030(4) 0.3531(3) 0.0295(12) Uani 1 1 d . . .
C29 C 1.1494(6) 0.3306(4) 0.3012(3) 0.0321(13) Uani 1 1 d . . .
H29 H 1.1180 0.3557 0.2492 0.039 Uiso 1 1 calc R . .
C30 C 1.2181(7) 0.2218(5) 0.3245(4) 0.0396(15) Uani 1 1 d . . .
C31 C 1.2421(10) 0.1502(6) 0.2614(4) 0.060(2) Uani 1 1 d . . .
C32 C 1.3919(11) 0.0780(8) 0.2671(5) 0.100(4) Uani 1 1 d . . .
H32A H 1.4634 0.1216 0.2606 0.150 Uiso 1 1 calc R . .
H32B H 1.4060 0.0370 0.2260 0.150 Uiso 1 1 calc R . .
H32C H 1.4006 0.0298 0.3185 0.150 Uiso 1 1 calc R . .
C33 C 1.2353(12) 0.2196(7) 0.1752(4) 0.092(3) Uani 1 1 d . . .
H33A H 1.3091 0.2614 0.1670 0.139 Uiso 1 1 calc R . .
H33B H 1.1426 0.2669 0.1679 0.139 Uiso 1 1 calc R . .
H33C H 1.2499 0.1734 0.1375 0.139 Uiso 1 1 calc R . .
C34 C 1.1242(15) 0.0831(9) 0.2700(6) 0.113(4) Uani 1 1 d . . .
H34A H 1.1243 0.0393 0.3230 0.169 Uiso 1 1 calc R . .
H34B H 1.1428 0.0378 0.2317 0.169 Uiso 1 1 calc R . .
H34C H 1.0319 0.1305 0.2609 0.169 Uiso 1 1 calc R . .
C35 C 1.2630(7) 0.1890(5) 0.4025(4) 0.0428(16) Uani 1 1 d . . .
O36 O 1.3178(8) 0.0780(4) 0.4303(3) 0.081(2) Uani 1 1 d . . .
C37 C 1.1814(19) 0.0233(8) 0.4658(7) 0.163(7) Uani 1 1 d . . .
H37A H 1.2146 -0.0524 0.4857 0.245 Uiso 1 1 calc R . .
H37B H 1.1146 0.0340 0.4242 0.245 Uiso 1 1 calc R . .
H37C H 1.1344 0.0561 0.5085 0.245 Uiso 1 1 calc R . .
C38 C 1.2550(7) 0.2573(4) 0.4560(4) 0.0366(14) Uani 1 1 d . . .
C39 C 1.3198(9) 0.2246(5) 0.5372(4) 0.056(2) Uani 1 1 d . . .
C40 C 1.2193(19) 0.1863(17) 0.6004(5) 0.198(9) Uani 1 1 d . . .
H40A H 1.2658 0.1661 0.6508 0.297 Uiso 1 1 calc R . .
H40B H 1.1898 0.1251 0.5892 0.297 Uiso 1 1 calc R . .
H40C H 1.1363 0.2427 0.6029 0.297 Uiso 1 1 calc R . .
C41 C 1.3305(13) 0.3217(7) 0.5717(5) 0.091(3) Uani 1 1 d . . .
H41A H 1.3957 0.3612 0.5388 0.137 Uiso 1 1 calc R . .
H41B H 1.3654 0.2972 0.6250 0.137 Uiso 1 1 calc R . .
H41C H 1.2369 0.3675 0.5730 0.137 Uiso 1 1 calc R . .
C42 C 1.4858(15) 0.1566(12) 0.5323(8) 0.157(6) Uani 1 1 d . . .
H42A H 1.5367 0.1923 0.4875 0.235 Uiso 1 1 calc R . .
H42B H 1.4846 0.0852 0.5259 0.235 Uiso 1 1 calc R . .
H42C H 1.5333 0.1524 0.5806 0.235 Uiso 1 1 calc R . .
C43 C 1.1857(6) 0.3657(5) 0.4286(3) 0.0306(13) Uani 1 1 d . . .
H43 H 1.1795 0.4139 0.4621 0.037 Uiso 1 1 calc R . .
C44 C 1.0181(6) 0.7270(4) -0.0068(3) 0.0343(14) Uani 1 1 d . . .
C45 C 0.9270(6) 0.8360(4) -0.0299(3) 0.0291(12) Uani 1 1 d . . .
C46 C 0.8675(7) 0.8724(5) -0.1050(3) 0.0355(14) Uani 1 1 d . . .
H46 H 0.8745 0.8242 -0.1386 0.043 Uiso 1 1 calc R . .
C47 C 0.7985(7) 0.9778(5) -0.1312(4) 0.0405(15) Uani 1 1 d . . .
C48 C 0.7960(8) 1.0510(4) -0.0812(4) 0.0424(16) Uani 1 1 d . . .
C49 C 0.8357(7) 1.0127(5) 0.0003(3) 0.0360(14) Uani 1 1 d . . .
C50 C 0.9043(6) 0.9063(5) 0.0207(3) 0.0328(13) Uani 1 1 d . . .
H50 H 0.9373 0.8804 0.0724 0.039 Uiso 1 1 calc R . .
C51 C 0.8096(8) 1.0844(5) 0.0624(4) 0.0502(17) Uani 1 1 d . . .
C52 C 0.8218(17) 1.0181(8) 0.1444(5) 0.108(4) Uani 1 1 d . . .
H52A H 0.9130 0.9686 0.1491 0.162 Uiso 1 1 calc R . .
H52B H 0.7453 0.9786 0.1555 0.162 Uiso 1 1 calc R . .
H52C H 0.8148 1.0639 0.1820 0.162 Uiso 1 1 calc R . .
C53 C 0.6642(11) 1.1635(7) 0.0537(6) 0.084(3) Uani 1 1 d . . .
H53A H 0.6574 1.2059 0.0003 0.126 Uiso 1 1 calc R . .
H53B H 0.6564 1.2100 0.0909 0.126 Uiso 1 1 calc R . .
H53C H 0.5877 1.1241 0.0646 0.126 Uiso 1 1 calc R . .
C54 C 0.9308(12) 1.1524(10) 0.0527(8) 0.119(5) Uani 1 1 d . . .
H54A H 1.0234 1.1049 0.0582 0.178 Uiso 1 1 calc R . .
H54B H 0.9166 1.1946 0.0931 0.178 Uiso 1 1 calc R . .
H54C H 0.9261 1.1994 0.0009 0.178 Uiso 1 1 calc R . .
O55 O 0.7421(9) 1.1564(4) -0.1090(3) 0.085(2) Uani 1 1 d . . .
C56 C 0.8304(15) 1.2198(9) -0.1367(6) 0.109(4) Uani 1 1 d . . .
H56A H 0.7770 1.2920 -0.1536 0.163 Uiso 1 1 calc R . .
H56B H 0.8853 1.1966 -0.1813 0.163 Uiso 1 1 calc R . .
H56C H 0.8945 1.2180 -0.0956 0.163 Uiso 1 1 calc R . .
C57 C 0.7275(9) 1.0127(6) -0.2158(4) 0.054(2) Uani 1 1 d . . .
C58 C 0.7031(15) 0.9186(7) -0.2416(6) 0.120(5) Uani 1 1 d . . .
H58A H 0.7918 0.8666 -0.2405 0.180 Uiso 1 1 calc R . .
H58B H 0.6686 0.9397 -0.2951 0.180 Uiso 1 1 calc R . .
H58C H 0.6328 0.8875 -0.2064 0.180 Uiso 1 1 calc R . .
C59 C 0.5956(16) 1.0852(13) -0.2153(7) 0.213(11) Uani 1 1 d . . .
H59A H 0.6086 1.1467 -0.1966 0.319 Uiso 1 1 calc R . .
H59B H 0.5275 1.0507 -0.1806 0.319 Uiso 1 1 calc R . .
H59C H 0.5600 1.1078 -0.2685 0.319 Uiso 1 1 calc R . .
C60 C 0.8098(16) 1.0865(7) -0.2741(5) 0.120(4) Uani 1 1 d . . .
H60A H 0.9058 1.0481 -0.2829 0.181 Uiso 1 1 calc R . .
H60B H 0.8139 1.1478 -0.2524 0.181 Uiso 1 1 calc R . .
H60C H 0.7616 1.1102 -0.3240 0.181 Uiso 1 1 calc R . .
C61 C 1.1091(6) 0.6820(5) -0.0684(3) 0.0359(14) Uani 1 1 d . . .
C62 C 1.1604(6) 0.7464(5) -0.1352(3) 0.0381(15) Uani 1 1 d . . .
H62 H 1.1449 0.8201 -0.1377 0.046 Uiso 1 1 calc R . .
C63 C 1.2349(6) 0.7052(5) -0.1997(4) 0.0364(14) Uani 1 1 d . . .
C64 C 1.2589(6) 0.5949(5) -0.1924(4) 0.0372(15) Uani 1 1 d . . .
C65 C 1.2197(7) 0.5238(5) -0.1236(4) 0.0415(15) Uani 1 1 d . . .
C66 C 1.1457(6) 0.5697(5) -0.0632(3) 0.0376(15) Uani 1 1 d . . .
H66 H 1.1188 0.5247 -0.0170 0.045 Uiso 1 1 calc R . .
C67 C 1.2837(8) 0.7866(7) -0.2700(4) 0.0566(19) Uani 1 1 d . . .
C68 C 1.3012(11) 0.8858(7) -0.2471(6) 0.089(3) Uani 1 1 d . . .
H68A H 1.3329 0.9333 -0.2930 0.133 Uiso 1 1 calc R . .
H68B H 1.3716 0.8680 -0.2065 0.133 Uiso 1 1 calc R . .
H68C H 1.2107 0.9206 -0.2269 0.133 Uiso 1 1 calc R . .
C69 C 1.4588(15) 0.7336(12) -0.2810(11) 0.170(8) Uani 1 1 d . . .
H69A H 1.4692 0.6656 -0.2964 0.255 Uiso 1 1 calc R . .
H69B H 1.5053 0.7231 -0.2314 0.255 Uiso 1 1 calc R . .
H69C H 1.5025 0.7816 -0.3217 0.255 Uiso 1 1 calc R . .
C70 C 1.1657(14) 0.8301(12) -0.3311(6) 0.172(8) Uani 1 1 d . . .
H70A H 1.1446 0.7716 -0.3508 0.259 Uiso 1 1 calc R . .
H70B H 1.1979 0.8807 -0.3747 0.259 Uiso 1 1 calc R . .
H70C H 1.0804 0.8652 -0.3062 0.259 Uiso 1 1 calc R . .
O71 O 1.3179(5) 0.5532(4) -0.2589(3) 0.0477(12) Uani 1 1 d . . .
C72 C 1.2198(12) 0.5410(10) -0.3137(6) 0.099(4) Uani 1 1 d . . .
H72A H 1.2730 0.5122 -0.3566 0.149 Uiso 1 1 calc R . .
H72B H 1.1609 0.6099 -0.3349 0.149 Uiso 1 1 calc R . .
H72C H 1.1596 0.4928 -0.2864 0.149 Uiso 1 1 calc R . .
C73 C 1.2693(11) 0.4017(6) -0.1095(6) 0.073(3) Uani 1 1 d . . .
C74 C 1.284(2) 0.3576(8) -0.0186(7) 0.247(13) Uani 1 1 d . . .
H74A H 1.3162 0.2808 -0.0085 0.370 Uiso 1 1 calc R . .
H74B H 1.1924 0.3753 0.0081 0.370 Uiso 1 1 calc R . .
H74C H 1.3530 0.3892 0.0010 0.370 Uiso 1 1 calc R . .
C75 C 1.4291(14) 0.3660(11) -0.1356(8) 0.146(6) Uani 1 1 d . . .
H75A H 1.4553 0.2889 -0.1240 0.219 Uiso 1 1 calc R . .
H75B H 1.4896 0.3944 -0.1070 0.219 Uiso 1 1 calc R . .
H75C H 1.4415 0.3928 -0.1919 0.219 Uiso 1 1 calc R . .
C76 C 1.165(2) 0.3491(9) -0.1300(19) 0.321(19) Uani 1 1 d . . .
H76A H 1.2008 0.2727 -0.1189 0.481 Uiso 1 1 calc R . .
H76B H 1.1455 0.3738 -0.1858 0.481 Uiso 1 1 calc R . .
H76C H 1.0773 0.3653 -0.0990 0.481 Uiso 1 1 calc R . .
O101 O 0.6346(7) 0.4093(6) 0.2396(7) 0.146(4) Uani 1 1 d . . .
C102 C 0.5680(13) 0.3330(9) 0.2507(11) 0.136(6) Uani 1 1 d . . .
H10A H 0.5591 0.3129 0.2004 0.164 Uiso 1 1 calc R . .
H10B H 0.4721 0.3547 0.2730 0.164 Uiso 1 1 calc R . .
C103 C 0.6535(14) 0.2380(9) 0.3084(8) 0.127(4) Uani 1 1 d . . .
H10C H 0.5918 0.2148 0.3537 0.152 Uiso 1 1 calc R . .
H10D H 0.6870 0.1783 0.2818 0.152 Uiso 1 1 calc R . .
C104 C 0.7692(14) 0.2666(14) 0.3347(12) 0.183(8) Uani 1 1 d . . .
H10E H 0.8593 0.2198 0.3238 0.220 Uiso 1 1 calc R . .
H10F H 0.7595 0.2672 0.3913 0.220 Uiso 1 1 calc R . .
C105 C 0.757(2) 0.3769(13) 0.2848(18) 0.35(2) Uani 1 1 d . . .
H10G H 0.7548 0.4271 0.3193 0.423 Uiso 1 1 calc R . .
H10H H 0.8411 0.3793 0.2494 0.423 Uiso 1 1 calc R . .
O201 O 0.4078(11) 0.8310(9) 0.0907(8) 0.166(5) Uani 1 1 d . . .
C202 C 0.5010(11) 0.9025(10) 0.0514(14) 0.181(9) Uani 1 1 d . . .
H20A H 0.5953 0.8629 0.0384 0.217 Uiso 1 1 calc R . .
H20B H 0.5117 0.9526 0.0838 0.217 Uiso 1 1 calc R . .
C203 C 0.433(2) 0.949(3) -0.0098(15) 0.295(18) Uani 1 1 d . . .
H20C H 0.4346 1.0252 -0.0171 0.354 Uiso 1 1 calc R . .
H20D H 0.4883 0.9243 -0.0544 0.354 Uiso 1 1 calc R . .
C204 C 0.3014(18) 0.9432(13) -0.0175(7) 0.137(5) Uani 1 1 d . . .
H20E H 0.2924 0.9063 -0.0597 0.165 Uiso 1 1 calc R . .
H20F H 0.2377 1.0134 -0.0269 0.165 Uiso 1 1 calc R . .
C205 C 0.2756(9) 0.8765(11) 0.0651(12) 0.174(8) Uani 1 1 d . . .
H20G H 0.2236 0.9219 0.1002 0.209 Uiso 1 1 calc R . .
H20H H 0.2214 0.8223 0.0620 0.209 Uiso 1 1 calc R . .
O301 O 0.4168(9) 0.6945(10) 0.3073(7) 0.151(4) Uani 1 1 d . . .
C302 C 0.2846(12) 0.7451(12) 0.3195(10) 0.144(6) Uani 1 1 d . . .
H30A H 0.2154 0.7108 0.3018 0.173 Uiso 1 1 calc R . .
H30B H 0.2699 0.8196 0.2911 0.173 Uiso 1 1 calc R . .
C303 C 0.2692(14) 0.738(2) 0.4110(12) 0.223(12) Uani 1 1 d . . .
H30C H 0.3125 0.7889 0.4293 0.268 Uiso 1 1 calc R . .
H30D H 0.1713 0.7394 0.4323 0.268 Uiso 1 1 calc R . .
C304 C 0.351(4) 0.639(3) 0.421(2) 0.38(2) Uani 1 1 d . . .
H30E H 0.2908 0.5917 0.4114 0.461 Uiso 1 1 calc R . .
H30F H 0.3750 0.6170 0.4768 0.461 Uiso 1 1 calc R . .
C305 C 0.4831(12) 0.6179(13) 0.3746(8) 0.131(5) Uani 1 1 d . . .
H30G H 0.5635 0.6385 0.3944 0.157 Uiso 1 1 calc R . .
H30H H 0.5091 0.5447 0.3662 0.157 Uiso 1 1 calc R . .
O401 O 0.6165(11) 0.5379(9) 0.0065(7) 0.173(5) Uani 1 1 d . . .
C402 C 0.7779(19) 0.493(2) -0.0300(16) 0.292(19) Uani 1 1 d . . .
H40D H 0.8529 0.5076 -0.0014 0.351 Uiso 1 1 calc R . .
H40E H 0.7940 0.4161 -0.0280 0.351 Uiso 1 1 calc R . .
C403 C 0.7720(19) 0.5557(15) -0.1145(9) 0.164(6) Uani 1 1 d . . .
H40F H 0.8435 0.6007 -0.1245 0.197 Uiso 1 1 calc R . .
H40G H 0.7908 0.5074 -0.1516 0.197 Uiso 1 1 calc R . .
C404 C 0.646(2) 0.6136(16) -0.1232(12) 0.202(8) Uani 1 1 d . . .
H40H H 0.5858 0.5828 -0.1511 0.242 Uiso 1 1 calc R . .
H40I H 0.6484 0.6864 -0.1519 0.242 Uiso 1 1 calc R . .
C405 C 0.602(6) 0.612(2) -0.0519(15) 0.54(4) Uani 1 1 d . . .
H40J H 0.6400 0.6677 -0.0365 0.646 Uiso 1 1 calc R . .
H40K H 0.4987 0.6384 -0.0551 0.646 Uiso 1 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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O101 K O201 176.7(5) . . ?
O101 K O27 74.31(19) . 1_455 ?
O201 K O27 104.1(3) . 1_455 ?
O101 K O26 107.01(19) . . ?
O201 K O26 74.6(2) . . ?
O27 K O26 178.4(2) 1_455 . ?
O101 K O301 95.0(4) . . ?
O201 K O301 81.8(4) . . ?
O27 K O301 69.71(18) 1_455 . ?
O26 K O301 109.2(2) . . ?
O101 K O25 107.6(2) . 1_455 ?
O201 K O25 73.1(3) . 1_455 ?
O27 K O25 53.45(13) 1_455 1_455 ?
O26 K O25 126.39(15) . 1_455 ?
O301 K O25 107.1(2) . 1_455 ?
O101 K O24 73.1(2) . . ?
O201 K O24 106.1(3) . . ?
O27 K O24 126.93(16) 1_455 . ?
O26 K O24 53.21(14) . . ?
O301 K O24 72.7(2) . . ?
O25 K O24 179.3(2) 1_455 . ?
O101 K O401 86.2(4) . . ?
O201 K O401 97.0(4) . . ?
O27 K O401 106.9(3) 1_455 . ?
O26 K O401 74.1(3) . . ?
O301 K O401 175.9(3) . . ?
O25 K O401 68.8(2) 1_455 . ?
O24 K O401 111.4(2) . . ?
C2 C1 C44 120.1(5) . . ?
C2 C1 C6 120.0(5) . . ?
C44 C1 C6 119.9(5) . . ?
O25 C2 C1 124.5(5) . . ?
O25 C2 C3 115.6(5) . . ?
C1 C2 C3 119.5(5) . . ?
O27 C3 C4 124.4(6) . . ?
O27 C3 C2 114.6(5) . . ?
C4 C3 C2 120.6(5) . . ?
C7 C4 C3 119.0(5) . . ?
C7 C4 C5 122.6(5) . . ?
C3 C4 C5 118.4(5) . . ?
O24 C5 C4 122.5(5) . . ?
O24 C5 C6 115.8(6) . . ?
C4 C5 C6 121.5(5) . . ?
O26 C6 C1 122.2(5) . . ?
O26 C6 C5 117.7(5) . . ?
C1 C6 C5 120.0(5) . . ?
C4 C7 C28 121.3(5) . . ?
C4 C7 C8 121.1(5) . . ?
C28 C7 C8 117.5(5) . . ?
C13 C8 C9 118.0(5) . . ?
C13 C8 C7 120.7(5) . . ?
C9 C8 C7 121.4(5) . . ?
C10 C9 C8 121.6(5) . . ?
C9 C10 C11 118.6(6) . . ?
C9 C10 C14 119.7(6) . . ?
C11 C10 C14 121.7(6) . . ?
C10 C11 O18 119.7(6) . . ?
C10 C11 C12 120.5(6) . . ?
O18 C11 C12 119.3(6) . . ?
C13 C12 C11 116.9(6) . . ?
C13 C12 C20 119.1(6) . . ?
C11 C12 C20 123.9(6) . . ?
C8 C13 C12 122.8(6) . . ?
C17 C14 C15 91.5(10) . . ?
C17 C14 C16 108.7(8) . . ?
C15 C14 C16 120.6(9) . . ?
C17 C14 C10 117.5(8) . . ?
C15 C14 C10 109.2(7) . . ?
C16 C14 C10 109.0(6) . . ?
C11 O18 C19 113.7(6) . . ?
C22 C20 C21 113.2(8) . . ?
C22 C20 C12 111.6(8) . . ?
C21 C20 C12 114.2(7) . . ?
C22 C20 C23 105.3(13) . . ?
C21 C20 C23 103.7(11) . . ?
C12 C20 C23 108.1(8) . . ?
C5 O24 K 118.3(5) . . ?
C2 O25 K 120.0(4) . 1_655 ?
C6 O26 K 119.0(4) . . ?
C3 O27 K 124.2(4) . 1_655 ?
C43 C28 C29 117.2(5) . . ?
C43 C28 C7 123.1(5) . . ?
C29 C28 C7 119.6(5) . . ?
C28 C29 C30 122.9(5) . . ?
C35 C30 C29 116.1(5) . . ?
C35 C30 C31 125.4(6) . . ?
C29 C30 C31 118.4(6) . . ?
C34 C31 C33 106.9(8) . . ?
C34 C31 C30 110.9(7) . . ?
C33 C31 C30 111.2(6) . . ?
C34 C31 C32 111.1(8) . . ?
C33 C31 C32 105.6(8) . . ?
C30 C31 C32 111.0(6) . . ?
C30 C35 C38 124.8(5) . . ?
C30 C35 O36 117.3(6) . . ?
C38 C35 O36 117.9(6) . . ?
C35 O36 C37 107.0(7) . . ?
C35 C38 C43 116.1(5) . . ?
C35 C38 C39 124.8(5) . . ?
C43 C38 C39 119.1(5) . . ?
C40 C39 C38 112.7(8) . . ?
C40 C39 C41 93.8(9) . . ?
C38 C39 C41 112.4(6) . . ?
C40 C39 C42 120.2(11) . . ?
C38 C39 C42 110.7(7) . . ?
C41 C39 C42 105.4(8) . . ?
C28 C43 C38 122.5(5) . . ?
C1 C44 C61 121.2(5) . . ?
C1 C44 C45 120.5(5) . . ?
C61 C44 C45 118.2(5) . . ?
C50 C45 C46 117.6(5) . . ?
C50 C45 C44 120.8(5) . . ?
C46 C45 C44 121.4(5) . . ?
C47 C46 C45 122.1(5) . . ?
C46 C47 C48 118.1(5) . . ?
C46 C47 C57 119.4(6) . . ?
C48 C47 C57 122.5(5) . . ?
O55 C48 C47 119.0(5) . . ?
O55 C48 C49 120.3(5) . . ?
C47 C48 C49 120.4(5) . . ?
C50 C49 C48 115.9(5) . . ?
C50 C49 C51 120.7(5) . . ?
C48 C49 C51 123.4(5) . . ?
C45 C50 C49 124.4(5) . . ?
C53 C51 C52 110.2(8) . . ?
C53 C51 C49 112.7(6) . . ?
C52 C51 C49 110.7(6) . . ?
C53 C51 C54 107.6(7) . . ?
C52 C51 C54 105.6(9) . . ?
C49 C51 C54 109.7(6) . . ?
C56 O55 C48 118.9(9) . . ?
C59 C57 C58 108.1(10) . . ?
C59 C57 C60 97.9(11) . . ?
C58 C57 C60 116.8(8) . . ?
C59 C57 C47 112.4(6) . . ?
C58 C57 C47 110.2(5) . . ?
C60 C57 C47 110.8(7) . . ?
C62 C61 C66 117.1(5) . . ?
C62 C61 C44 122.1(5) . . ?
C66 C61 C44 120.8(5) . . ?
C61 C62 C63 123.0(6) . . ?
C64 C63 C62 116.4(5) . . ?
C64 C63 C67 126.5(6) . . ?
C62 C63 C67 117.0(6) . . ?
O71 C64 C63 117.6(5) . . ?
O71 C64 C65 118.7(5) . . ?
C63 C64 C65 123.6(5) . . ?
C66 C65 C64 116.7(5) . . ?
C66 C65 C73 119.4(6) . . ?
C64 C65 C73 123.5(6) . . ?
C65 C66 C61 122.9(5) . . ?
C68 C67 C63 113.0(6) . . ?
C68 C67 C70 101.7(9) . . ?
C63 C67 C70 110.5(6) . . ?
C68 C67 C69 97.4(8) . . ?
C63 C67 C69 102.5(7) . . ?
C70 C67 C69 131.0(10) . . ?
C64 O71 C72 117.4(5) . . ?
C65 C73 C76 113.1(9) . . ?
C65 C73 C75 113.0(8) . . ?
C76 C73 C75 118.7(14) . . ?
C65 C73 C74 108.1(8) . . ?
C76 C73 C74 103.4(15) . . ?
C75 C73 C74 98.2(10) . . ?
C102 O101 C105 108.9(11) . . ?
C102 O101 K 124.6(7) . . ?
C105 O101 K 125.5(7) . . ?
O101 C102 C103 107.8(10) . . ?
C104 C103 C102 110.4(10) . . ?
C103 C104 C105 99.6(12) . . ?
O101 C105 C104 113.0(11) . . ?
C205 O201 C202 106.5(10) . . ?
C205 O201 K 130.6(9) . . ?
C202 O201 K 120.1(7) . . ?
O201 C202 C203 101.1(13) . . ?
C204 C203 C202 122(2) . . ?
C203 C204 C205 98.4(15) . . ?
O201 C205 C204 104.0(11) . . ?
C302 O301 C305 116.2(11) . . ?
C302 O301 K 125.1(9) . . ?
C305 O301 K 108.6(7) . . ?
O301 C302 C303 104.8(13) . . ?
O301 C302 C304 71.4(13) . . ?
C303 C302 C304 41.2(13) . . ?
C304 C303 C302 88.6(18) . . ?
C303 C304 C305 121(2) . . ?
C303 C304 C302 50.2(15) . . ?
C305 C304 C302 83.0(14) . . ?
O301 C305 C304 89.4(17) . . ?
C405 O401 C402 88(2) . . ?
C405 O401 K 111.8(13) . . ?
C402 O401 K 130.5(14) . . ?
C403 C402 O401 102.2(13) . . ?
C404 C403 C402 106.7(17) . . ?
C403 C404 C405 102(3) . . ?
O401 C405 C404 130(3) . . ?
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
K O101 2.763(8) . ?
K O201 2.796(10) . ?
K O27 2.845(5) 1_455 ?
K O26 2.884(5) . ?
K O301 2.929(10) . ?
K O25 2.917(6) 1_455 ?
K O24 2.922(6) . ?
K O401 3.061(12) . ?
C1 C2 1.434(8) . ?
C1 C44 1.440(8) . ?
C1 C6 1.470(7) . ?
C2 O25 1.236(7) . ?
C2 C3 1.547(8) . ?
C3 O27 1.228(7) . ?
C3 C4 1.449(7) . ?
C4 C7 1.398(8) . ?
C4 C5 1.464(9) . ?
C5 O24 1.229(7) . ?
C5 C6 1.492(8) . ?
C6 O26 1.233(7) . ?
C7 C28 1.465(8) . ?
C7 C8 1.477(7) . ?
C8 C13 1.372(8) . ?
C8 C9 1.411(8) . ?
C9 C10 1.374(8) . ?
C10 C11 1.405(9) . ?
C10 C14 1.575(9) . ?
C11 O18 1.380(7) . ?
C11 C12 1.412(9) . ?
C12 C13 1.401(9) . ?
C12 C20 1.538(10) . ?
C14 C17 1.396(13) . ?
C14 C15 1.530(13) . ?
C14 C16 1.525(11) . ?
O18 C19 1.393(12) . ?
C20 C22 1.461(13) . ?
C20 C21 1.455(13) . ?
C20 C23 1.645(18) . ?
O25 K 2.917(6) 1_655 ?
O27 K 2.845(5) 1_655 ?
C28 C43 1.399(7) . ?
C28 C29 1.407(8) . ?
C29 C30 1.409(8) . ?
C30 C35 1.384(9) . ?
C30 C31 1.552(8) . ?
C31 C34 1.541(13) . ?
C31 C33 1.553(11) . ?
C31 C32 1.526(11) . ?
C35 C38 1.400(8) . ?
C35 O36 1.412(8) . ?
O36 C37 1.624(15) . ?
C38 C43 1.414(8) . ?
C38 C39 1.505(9) . ?
C39 C40 1.463(14) . ?
C39 C41 1.532(10) . ?
C39 C42 1.641(14) . ?
C44 C61 1.457(8) . ?
C44 C45 1.482(7) . ?
C45 C50 1.369(8) . ?
C45 C46 1.391(8) . ?
C46 C47 1.379(8) . ?
C47 C48 1.410(9) . ?
C47 C57 1.583(9) . ?
C48 O55 1.348(7) . ?
C48 C49 1.431(8) . ?
C49 C50 1.378(8) . ?
C49 C51 1.538(9) . ?
C51 C53 1.532(12) . ?
C51 C52 1.479(12) . ?
C51 C54 1.574(12) . ?
O55 C56 1.292(13) . ?
C57 C59 1.399(12) . ?
C57 C58 1.457(11) . ?
C57 C60 1.520(13) . ?
C61 C62 1.385(8) . ?
C61 C66 1.410(8) . ?
C62 C63 1.410(8) . ?
C63 C64 1.382(8) . ?
C63 C67 1.534(9) . ?
C64 O71 1.400(7) . ?
C64 C65 1.409(9) . ?
C65 C66 1.380(8) . ?
C65 C73 1.526(10) . ?
C67 C68 1.472(12) . ?
C67 C70 1.526(13) . ?
C67 C69 1.673(15) . ?
O71 C72 1.430(10) . ?
C73 C76 1.426(18) . ?
C73 C75 1.551(14) . ?
C73 C74 1.546(16) . ?
O101 C102 1.261(13) . ?
O101 C105 1.383(14) . ?
C102 C103 1.525(18) . ?
C103 C104 1.370(17) . ?
C104 C105 1.485(19) . ?
O201 C205 1.333(14) . ?
O201 C202 1.444(16) . ?
C202 C203 1.24(3) . ?
C203 C204 1.29(2) . ?
C204 C205 1.523(19) . ?
O301 C302 1.312(13) . ?
O301 C305 1.436(15) . ?
C302 C303 1.55(2) . ?
C302 C304 2.02(4) . ?
C303 C304 1.33(4) . ?
C304 C305 1.44(3) . ?
O401 C405 1.22(3) . ?
O401 C402 1.65(2) . ?
C402 C403 1.50(2) . ?
C403 C404 1.27(2) . ?
C404 C405 1.26(3) . ?
