#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/37/4113746.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_4113746
loop_
_publ_author_name
'Tracy A. Hanna'
'Lihua Liu'
'Alfredo M. Angeles-Boza'
'Xiaodi Kou'
'C. David Gutsche'
'Krzysztof Ejsmont'
'William H. Watson'
'Lev N. Zakharov'
'Christopher D. Incarvito'
'Arnold L. Rheingold'
_publ_contact_author             'Tracy A. Hanna'
_publ_contact_author_email       T.Hanna@tcu.edu
_publ_section_title
;
 Synthesis, Structures, and Conformational Characteristics of Calixarene
 Monoanions and Dianions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6228
_journal_page_last               6238
_journal_paper_doi               10.1021/ja0289797
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C57 H72 K O12 Rb'
_chemical_formula_weight         1073.72
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 107.9540(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5123(8)
_cell_length_b                   24.7889(13)
_cell_length_c                   14.8909(8)
_cell_measurement_temperature    100.0(1)
_cell_volume                     5096.1(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 0.939
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0587
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32715
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    1.118
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_density_meas      0
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.895
_refine_diff_density_min         -1.053
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         11905
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.891
_refine_ls_R_factor_all          0.0811
_refine_ls_R_factor_gt           0.0644
_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)+(0.0934P)²+13.5677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1707
_reflns_number_gt                8901
_reflns_number_total             11905
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0289797si20021230_042221_11.cif
_cod_data_source_block           36
_cod_original_formula_sum        'C57 H72 K1 O12 Rb1'
_cod_database_code               4113746
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Rb1 Rb 0.49145(3) 0.222388(14) 0.08478(3) 0.02814(11) Uani 1 1 d .
K1 K 0.60422(5) 0.37219(3) 0.20275(5) 0.01868(15) Uani 1 1 d .
O1 O 0.52600(19) 0.19777(10) 0.40164(17) 0.0198(5) Uani 1 1 d .
O2 O 0.69389(17) 0.23141(9) 0.46856(16) 0.0201(5) Uani 1 1 d .
O3 O 0.61917(19) 0.32404(11) 0.47917(18) 0.0223(5) Uani 1 1 d .
O4 O 0.42718(18) 0.40812(10) 0.21660(18) 0.0203(5) Uani 1 1 d .
O5 O 0.30262(15) 0.36118(9) 0.08034(15) 0.0177(5) Uani 1 1 d .
O6 O 0.32740(17) 0.26666(10) 0.14617(17) 0.0185(5) Uani 1 1 d .
O7 O 0.5179(2) 0.28781(11) 0.2628(2) 0.0237(6) Uani 1 1 d .
O8 O 0.6771(2) 0.28474(12) 0.1425(2) 0.0323(6) Uani 1 1 d .
O9 O 0.4688(2) 0.34117(16) 0.0462(2) 0.0411(8) Uani 1 1 d .
O10 O 0.3204(2) 0.18096(12) -0.0507(2) 0.0382(7) Uani 1 1 d .
O11 O 0.6620(3) 0.45987(12) 0.1176(2) 0.0490(8) Uani 1 1 d .
C1 C 0.5029(2) 0.16688(13) 0.3226(2) 0.0175(6) Uani 1 1 d .
C2 C 0.4051(2) 0.16597(13) 0.2685(2) 0.0170(6) Uani 1 1 d .
C3 C 0.3776(3) 0.13351(13) 0.1885(2) 0.0209(7) Uani 1 1 d .
H3A H 0.3072 0.1260 0.1577 0.025 Uiso 1 1 calc R
C4 C 0.4456(3) 0.10311(13) 0.1620(2) 0.0233(7) Uani 1 1 d .
H4A H 0.4227 0.0730 0.1158 0.028 Uiso 1 1 calc R
C5 C 0.5426(3) 0.10496(14) 0.2161(2) 0.0238(7) Uani 1 1 d .
H5A H 0.5888 0.0784 0.2033 0.029 Uiso 1 1 calc R
C6 C 0.5728(3) 0.13665(13) 0.2970(2) 0.0212(7) Uani 1 1 d .
C7 C 0.6785(2) 0.13527(14) 0.3601(3) 0.0229(7) Uani 1 1 d .
H7A H 0.6791 0.1327 0.4266 0.028 Uiso 1 1 calc R
H7B H 0.7089 0.1020 0.3454 0.028 Uiso 1 1 calc R
C8 C 0.7402(2) 0.18262(14) 0.3516(2) 0.0212(7) Uani 1 1 d .
C9 C 0.7463(2) 0.22871(14) 0.4089(2) 0.0201(7) Uani 1 1 d .
C10 C 0.8083(2) 0.27166(14) 0.4041(2) 0.0215(7) Uani 1 1 d .
C11 C 0.8628(2) 0.26819(15) 0.3421(3) 0.0238(7) Uani 1 1 d .
H11A H 0.9049 0.2969 0.3390 0.029 Uiso 1 1 calc R
C12 C 0.8564(3) 0.22287(16) 0.2842(3) 0.0280(8) Uani 1 1 d .
H12A H 0.8934 0.2211 0.2416 0.034 Uiso 1 1 calc R
C13 C 0.7956(3) 0.18085(15) 0.2896(2) 0.0255(7) Uani 1 1 d .
H13A H 0.7914 0.1501 0.2504 0.031 Uiso 1 1 calc R
C14 C 0.8183(2) 0.32010(14) 0.4692(3) 0.0241(7) Uani 1 1 d .
H14A H 0.8104 0.3075 0.5295 0.029 Uiso 1 1 calc R
H14B H 0.8850 0.3344 0.4833 0.029 Uiso 1 1 calc R
C15 C 0.7479(2) 0.36623(13) 0.4325(2) 0.0204(7) Uani 1 1 d .
C16 C 0.6537(2) 0.36603(13) 0.4399(2) 0.0177(6) Uani 1 1 d .
C17 C 0.5900(2) 0.40937(13) 0.4068(2) 0.0169(6) Uani 1 1 d .
C18 C 0.6233(2) 0.45410(13) 0.3696(2) 0.0193(6) Uani 1 1 d .
H18A H 0.5833 0.4878 0.3572 0.023 Uiso 1 1 calc R
C19 C 0.7166(3) 0.45577(14) 0.3638(3) 0.0237(7) Uani 1 1 d .
H19A H 0.7426 0.4901 0.3460 0.028 Uiso 1 1 calc R
C20 C 0.7775(3) 0.41204(15) 0.3942(3) 0.0254(7) Uani 1 1 d .
H20A H 0.8457 0.4142 0.3923 0.031 Uiso 1 1 calc R
C21 C 0.4883(2) 0.40511(13) 0.4136(2) 0.0189(6) Uani 1 1 d .
H21A H 0.4643 0.3683 0.3935 0.023 Uiso 1 1 calc R
H21B H 0.4926 0.4087 0.4810 0.023 Uiso 1 1 calc R
C22 C 0.4132(2) 0.44443(13) 0.3585(2) 0.0174(6) Uani 1 1 d .
C23 C 0.3807(2) 0.44250(12) 0.2595(2) 0.0174(6) Uani 1 1 d .
C24 C 0.3025(2) 0.47414(12) 0.2064(2) 0.0180(6) Uani 1 1 d .
C25 C 0.2558(2) 0.50713(13) 0.2546(2) 0.0213(7) Uani 1 1 d .
H25A H 0.2012 0.5278 0.2199 0.026 Uiso 1 1 calc R
C26 C 0.2876(2) 0.51036(13) 0.3526(3) 0.0222(7) Uani 1 1 d .
H26A H 0.2557 0.5333 0.3846 0.027 Uiso 1 1 calc R
C27 C 0.3666(2) 0.47968(13) 0.4032(2) 0.0198(6) Uani 1 1 d .
H27A H 0.3895 0.4828 0.4701 0.024 Uiso 1 1 calc R
C28 C 0.2718(2) 0.47420(13) 0.0991(2) 0.0213(7) Uani 1 1 d .
H28A H 0.2503 0.5111 0.0770 0.026 Uiso 1 1 calc R
H28B H 0.3296 0.4661 0.0794 0.026 Uiso 1 1 calc R
C29 C 0.1921(2) 0.43519(14) 0.0490(2) 0.0202(7) Uani 1 1 d .
C30 C 0.2123(2) 0.38008(13) 0.0411(2) 0.0186(6) Uani 1 1 d .
C31 C 0.1378(2) 0.34511(13) -0.0102(2) 0.0191(6) Uani 1 1 d .
C32 C 0.0459(3) 0.36523(16) -0.0541(3) 0.0278(8) Uani 1 1 d .
H32A H -0.0038 0.3416 -0.0890 0.033 Uiso 1 1 calc R
C33 C 0.0258(3) 0.41915(17) -0.0479(3) 0.0340(9) Uani 1 1 d .
H33A H -0.0372 0.4327 -0.0788 0.041 Uiso 1 1 calc R
C34 C 0.0981(3) 0.45353(16) 0.0038(3) 0.0315(9) Uani 1 1 d .
H34A H 0.0834 0.4906 0.0086 0.038 Uiso 1 1 calc R
C35 C 0.1584(3) 0.28548(13) -0.0168(2) 0.0207(7) Uani 1 1 d .
H35A H 0.2228 0.2814 -0.0259 0.025 Uiso 1 1 calc R
H35B H 0.1097 0.2703 -0.0732 0.025 Uiso 1 1 calc R
C36 C 0.1568(2) 0.25298(13) 0.0690(2) 0.0200(7) Uani 1 1 d .
C37 C 0.2410(2) 0.24394(13) 0.1442(2) 0.0174(6) Uani 1 1 d .
C38 C 0.2396(2) 0.21083(13) 0.2203(2) 0.0195(6) Uani 1 1 d .
C39 C 0.1519(3) 0.18864(15) 0.2215(3) 0.0250(7) Uani 1 1 d .
H39A H 0.1499 0.1662 0.2725 0.030 Uiso 1 1 calc R
C40 C 0.0673(3) 0.19908(17) 0.1487(3) 0.0304(8) Uani 1 1 d .
H40A H 0.0074 0.1844 0.1506 0.036 Uiso 1 1 calc R
C41 C 0.0703(3) 0.23061(16) 0.0739(3) 0.0270(8) Uani 1 1 d .
H41A H 0.0122 0.2374 0.0243 0.032 Uiso 1 1 calc R
C42 C 0.3326(2) 0.19978(13) 0.2983(2) 0.0170(6) Uani 1 1 d .
H42A H 0.3168 0.1811 0.3504 0.020 Uiso 1 1 calc R
H42B H 0.3632 0.2347 0.3231 0.020 Uiso 1 1 calc R
C43 C 0.2497(3) 0.15688(15) -0.0980(3) 0.0270(8) Uani 1 1 d .
C44 C 0.1829(3) 0.1288(2) -0.0544(3) 0.0396(10) Uani 1 1 d .
H44A H 0.2062 0.1337 0.0142 0.059 Uiso 1 1 calc R
H44B H 0.1810 0.0902 -0.0693 0.059 Uiso 1 1 calc R
H44C H 0.1177 0.1440 -0.0796 0.059 Uiso 1 1 calc R
C45 C 0.2243(3) 0.15332(16) -0.2030(3) 0.0318(8) Uani 1 1 d .
H45A H 0.2724 0.1731 -0.2240 0.048 Uiso 1 1 calc R
H45B H 0.1600 0.1691 -0.2321 0.048 Uiso 1 1 calc R
H45C H 0.2237 0.1154 -0.2219 0.048 Uiso 1 1 calc R
C46 C 0.6425(4) 0.50707(17) 0.1250(3) 0.0386(10) Uani 1 1 d .
C47 C 0.7172(4) 0.55008(18) 0.1411(4) 0.0453(11) Uani 1 1 d .
H47A H 0.7796 0.5340 0.1437 0.068 Uiso 1 1 calc R
H47B H 0.7231 0.5684 0.2010 0.068 Uiso 1 1 calc R
H47C H 0.6982 0.5763 0.0894 0.068 Uiso 1 1 calc R
C48 C 0.5433(4) 0.5241(2) 0.1190(3) 0.0454(11) Uani 1 1 d .
H48A H 0.5009 0.4925 0.1086 0.068 Uiso 1 1 calc R
H48B H 0.5191 0.5494 0.0663 0.068 Uiso 1 1 calc R
H48C H 0.5440 0.5418 0.1780 0.068 Uiso 1 1 calc R
H1O H 0.577(3) 0.2032(16) 0.422(3) 0.015(10) Uiso 1 1 d .
H3O H 0.648(3) 0.3030(18) 0.480(3) 0.019(12) Uiso 1 1 d .
H4O H 0.392(3) 0.3963(16) 0.181(3) 0.014(11) Uiso 1 1 d .
H6O H 0.317(3) 0.2919(17) 0.126(3) 0.016(11) Uiso 1 1 d .
H7C H 0.531(4) 0.2799(19) 0.309(4) 0.031(14) Uiso 1 1 d .
H7D H 0.467(4) 0.288(2) 0.245(4) 0.037(15) Uiso 1 1 d .
H8D H 0.721(4) 0.271(2) 0.179(4) 0.049(16) Uiso 1 1 d .
H8C H 0.693(3) 0.2801(17) 0.089(3) 0.032(12) Uiso 1 1 d .
H9D H 0.423(4) 0.349(2) 0.037(4) 0.06(2) Uiso 1 1 d .
H9C H 0.480(4) 0.337(2) -0.002(4) 0.047(15) Uiso 1 1 d .
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'
Rb Rb -0.9393 2.9676 '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
O10 Rb1 O8 153.59(9) . .
O10 Rb1 O9 101.38(9) . .
O8 Rb1 O9 65.39(9) . .
O10 Rb1 O3 91.98(8) . 4_565
O8 Rb1 O3 72.68(8) . 4_565
O9 Rb1 O3 108.93(8) . 4_565
O10 Rb1 O6 75.50(7) . .
O8 Rb1 O6 116.80(7) . .
O9 Rb1 O6 69.52(8) . .
O3 Rb1 O6 166.49(7) 4_565 .
O10 Rb1 O7 131.07(8) . .
O8 Rb1 O7 67.19(8) . .
O9 Rb1 O7 67.60(8) . .
O3 Rb1 O7 136.95(8) 4_565 .
O6 Rb1 O7 55.76(7) . .
O10 Rb1 C4 72.62(9) . .
O8 Rb1 C4 128.35(9) . .
O9 Rb1 C4 157.06(9) . .
O3 Rb1 C4 93.57(8) 4_565 .
O6 Rb1 C4 87.56(8) . .
O7 Rb1 C4 99.13(8) . .
O10 Rb1 C3 69.54(9) . .
O8 Rb1 C3 136.47(8) . .
O9 Rb1 C3 133.17(9) . .
O3 Rb1 C3 117.03(8) 4_565 .
O6 Rb1 C3 63.71(8) . .
O7 Rb1 C3 84.11(8) . .
C4 Rb1 C3 23.89(8) . .
O10 Rb1 C5 94.87(9) . .
O8 Rb1 C5 104.78(8) . .
O9 Rb1 C5 157.96(8) . .
O3 Rb1 C5 85.07(8) 4_565 .
O6 Rb1 C5 100.79(8) . .
O7 Rb1 C5 90.49(8) . .
C4 Rb1 C5 23.58(9) . .
C3 Rb1 C5 41.10(9) . .
O10 Rb1 O1 87.45(8) . 4_565
O8 Rb1 O1 66.57(7) . 4_565
O9 Rb1 O1 48.25(7) . 4_565
O3 Rb1 O1 63.44(7) 4_565 4_565
O6 Rb1 O1 110.16(7) . 4_565
O7 Rb1 O1 111.48(7) . 4_565
C4 Rb1 O1 149.37(7) . 4_565
C3 Rb1 O1 156.94(7) . 4_565
C5 Rb1 O1 148.50(7) . 4_565
O10 Rb1 C2 88.11(8) . .
O8 Rb1 C2 118.22(8) . .
O9 Rb1 C2 118.75(8) . .
O3 Rb1 C2 131.31(7) 4_565 .
O6 Rb1 C2 54.61(7) . .
O7 Rb1 C2 61.70(7) . .
C4 Rb1 C2 40.55(8) . .
C3 Rb1 C2 22.54(7) . .
C5 Rb1 C2 46.51(8) . .
O1 Rb1 C2 164.77(7) 4_565 .
O10 Rb1 C6 112.09(8) . .
O8 Rb1 C6 91.69(8) . .
O9 Rb1 C6 135.85(8) . .
O3 Rb1 C6 98.14(7) 4_565 .
O6 Rb1 C6 91.38(7) . .
O7 Rb1 C6 68.77(8) . .
C4 Rb1 C6 39.98(8) . .
C3 Rb1 C6 46.26(8) . .
C5 Rb1 C6 22.16(8) . .
O1 Rb1 C6 154.35(7) 4_565 .
C2 Rb1 C6 39.13(7) . .
O10 Rb1 H6O 76.7(7) . .
O8 Rb1 H6O 110.7(7) . .
O9 Rb1 H6O 58.3(7) . .
O3 Rb1 H6O 159.7(7) 4_565 .
O6 Rb1 H6O 11.6(7) . .
O7 Rb1 H6O 56.6(7) . .
C4 Rb1 H6O 98.8(7) . .
C3 Rb1 H6O 75.1(7) . .
C5 Rb1 H6O 112.3(7) . .
O1 Rb1 H6O 98.9(7) 4_565 .
C2 Rb1 H6O 65.9(7) . .
C6 Rb1 H6O 101.7(7) . .
O10 Rb1 H7D 117.8(11) . .
O8 Rb1 H7D 78.8(10) . .
O9 Rb1 H7D 65.4(10) . .
O3 Rb1 H7D 150.1(11) 4_565 .
O6 Rb1 H7D 42.4(11) . .
O7 Rb1 H7D 13.4(10) . .
C4 Rb1 H7D 97.2(10) . .
C3 Rb1 H7D 78.4(10) . .
C5 Rb1 H7D 93.9(10) . .
O1 Rb1 H7D 112.8(10) 4_565 .
C2 Rb1 H7D 57.2(10) . .
C6 Rb1 H7D 73.7(10) . .
H6O Rb1 H7D 43.6(13) . .
O10 Rb1 H8C 139.0(9) . .
O8 Rb1 H8C 15.9(9) . .
O9 Rb1 H8C 67.3(8) . .
O3 Rb1 H8C 58.8(9) 4_565 .
O6 Rb1 H8C 128.8(8) . .
O7 Rb1 H8C 82.8(9) . .
C4 Rb1 H8C 131.6(8) . .
C3 Rb1 H8C 147.1(8) . .
C5 Rb1 H8C 109.0(8) . .
O1 Rb1 H8C 55.0(8) 4_565 .
C2 Rb1 H8C 132.5(9) . .
C6 Rb1 H8C 100.8(8) . .
H6O Rb1 H8C 120.6(11) . .
H7D Rb1 H8C 93.9(14) . .
O10 Rb1 H9C 96.5(10) . .
O8 Rb1 H9C 64.8(9) . .
O9 Rb1 H9C 14.7(11) . .
O3 Rb1 H9C 95.4(11) 4_565 .
O6 Rb1 H9C 81.2(11) . .
O7 Rb1 H9C 81.4(11) . .
C4 Rb1 H9C 166.1(10) . .
C3 Rb1 H9C 144.3(10) . .
C5 Rb1 H9C 168.6(10) . .
O1 Rb1 H9C 33.6(11) 4_565 .
C2 Rb1 H9C 132.9(11) . .
C6 Rb1 H9C 147.7(10) . .
H6O Rb1 H9C 69.7(13) . .
H7D Rb1 H9C 80.0(14) . .
H8C Rb1 H9C 62.3(12) . .
O9 K1 O8 74.56(10) . .
O9 K1 O7 77.03(11) . .
O8 K1 O7 76.00(9) . .
O9 K1 O11 94.10(11) . .
O8 K1 O11 105.92(10) . .
O7 K1 O11 170.19(11) . .
O9 K1 O4 73.04(9) . .
O8 K1 O4 138.58(9) . .
O7 K1 O4 72.15(8) . .
O11 K1 O4 101.48(9) . .
O9 K1 C18 137.65(10) . .
O8 K1 C18 146.63(9) . .
O7 K1 C18 99.98(9) . .
O11 K1 C18 83.70(9) . .
O4 K1 C18 66.11(8) . .
O9 K1 C19 155.60(11) . .
O8 K1 C19 127.55(9) . .
O7 K1 C19 115.44(9) . .
O11 K1 C19 71.34(10) . .
O4 K1 C19 90.36(8) . .
C18 K1 C19 25.11(9) . .
O9 K1 C17 131.38(10) . .
O8 K1 C17 133.49(9) . .
O7 K1 C17 75.07(8) . .
O11 K1 C17 108.75(9) . .
O4 K1 C17 60.86(8) . .
C18 K1 C17 25.07(8) . .
C19 K1 C17 43.99(9) . .
O9 K1 C20 178.21(11) . .
O8 K1 C20 104.79(9) . .
O7 K1 C20 104.48(9) . .
O11 K1 C20 84.47(10) . .
O4 K1 C20 108.27(9) . .
C18 K1 C20 43.31(9) . .
C19 K1 C20 24.41(9) . .
C17 K1 C20 50.26(9) . .
O9 K1 C16 139.84(10) . .
O8 K1 C16 109.49(9) . .
O7 K1 C16 66.06(9) . .
O11 K1 C16 121.06(9) . .
O4 K1 C16 80.85(8) . .
C18 K1 C16 42.94(8) . .
C19 K1 C16 49.72(8) . .
C17 K1 C16 24.35(8) . .
C20 K1 C16 41.92(8) . .
O9 K1 C15 157.49(10) . .
O8 K1 C15 96.78(9) . .
O7 K1 C15 80.73(9) . .
O11 K1 C15 108.33(10) . .
O4 K1 C15 103.41(8) . .
C18 K1 C15 50.28(8) . .
C19 K1 C15 42.84(8) . .
C17 K1 C15 43.08(8) . .
C20 K1 C15 23.88(8) . .
C16 K1 C15 23.86(8) . .
O9 K1 Rb1 44.98(9) . .
O8 K1 Rb1 44.91(7) . .
O7 K1 Rb1 45.77(6) . .
O11 K1 Rb1 129.26(7) . .
O4 K1 Rb1 93.67(6) . .
C18 K1 Rb1 145.45(7) . .
C19 K1 Rb1 157.33(7) . .
C17 K1 Rb1 120.80(6) . .
C20 K1 Rb1 135.58(7) . .
C16 K1 Rb1 108.98(6) . .
C15 K1 Rb1 114.69(6) . .
O9 K1 H4O 61.1(8) . .
O8 K1 H4O 127.7(8) . .
O7 K1 H4O 68.5(8) . .
O11 K1 H4O 103.7(8) . .
O4 K1 H4O 12.2(8) . .
C18 K1 H4O 78.3(8) . .
C19 K1 H4O 102.4(8) . .
C17 K1 H4O 71.8(8) . .
C20 K1 H4O 120.3(8) . .
C16 K1 H4O 90.0(8) . .
C15 K1 H4O 113.4(8) . .
Rb1 K1 H4O 83.1(8) . .
O9 K1 H7D 68.5(10) . .
O8 K1 H7D 82.5(10) . .
O7 K1 H7D 12.1(10) . .
O11 K1 H7D 158.3(10) . .
O4 K1 H7D 62.0(10) . .
C18 K1 H7D 100.3(10) . .
C19 K1 H7D 119.7(10) . .
C17 K1 H7D 76.6(10) . .
C20 K1 H7D 113.2(10) . .
C16 K1 H7D 72.5(10) . .
C15 K1 H7D 90.0(10) . .
Rb1 K1 H7D 45.3(9) . .
H4O K1 H7D 57.2(12) . .
O9 K1 H9D 10.6(12) . .
O8 K1 H9D 84.6(12) . .
O7 K1 H9D 75.8(12) . .
O11 K1 H9D 94.7(11) . .
O4 K1 H9D 62.5(12) . .
C18 K1 H9D 127.1(12) . .
C19 K1 H9D 147.0(12) . .
C17 K1 H9D 121.7(12) . .
C20 K1 H9D 170.4(12) . .
C16 K1 H9D 133.6(12) . .
C15 K1 H9D 155.4(12) . .
Rb1 K1 H9D 51.0(11) . .
H4O K1 H9D 50.7(14) . .
H7D K1 H9D 65.7(15) . .
C1 O1 Rb1 158.6(2) . 4_566
C1 O1 H1O 115(3) . .
Rb1 O1 H1O 87(3) 4_566 .
C16 O3 Rb1 152.2(2) . 4_566
C16 O3 H3O 107(4) . .
Rb1 O3 H3O 100(4) 4_566 .
C23 O4 K1 146.7(2) . .
C23 O4 H4O 106(3) . .
K1 O4 H4O 107(3) . .
C37 O6 Rb1 130.5(2) . .
C37 O6 H6O 106(3) . .
Rb1 O6 H6O 107(3) . .
K1 O7 Rb1 94.07(9) . .
K1 O7 H7C 122(4) . .
Rb1 O7 H7C 130(4) . .
K1 O7 H7D 113(4) . .
Rb1 O7 H7D 81(4) . .
H7C O7 H7D 109(6) . .
K1 O8 Rb1 95.78(9) . .
K1 O8 H8D 116(4) . .
Rb1 O8 H8D 117(4) . .
K1 O8 H8C 129(3) . .
Rb1 O8 H8C 98(3) . .
H8D O8 H8C 101(5) . .
K1 O9 Rb1 96.22(11) . .
K1 O9 H9D 122(5) . .
Rb1 O9 H9D 112(5) . .
K1 O9 H9C 122(4) . .
Rb1 O9 H9C 91(4) . .
H9D O9 H9C 108(6) . .
C43 O10 Rb1 169.7(3) . .
C46 O11 K1 126.9(3) . .
O1 C1 C2 116.3(3) . .
O1 C1 C6 122.0(3) . .
C2 C1 C6 121.6(3) . .
C3 C2 C1 118.3(3) . .
C3 C2 C42 122.0(3) . .
C1 C2 C42 119.7(3) . .
C3 C2 Rb1 69.58(18) . .
C1 C2 Rb1 84.40(18) . .
C42 C2 Rb1 116.16(19) . .
C2 C3 C4 121.0(3) . .
C2 C3 Rb1 87.87(19) . .
C4 C3 Rb1 74.68(19) . .
C2 C3 H3A 118.9 . .
C4 C3 H3A 118.9 . .
Rb1 C3 H3A 118.9 . .
C5 C4 C3 119.8(3) . .
C5 C4 Rb1 84.0(2) . .
C3 C4 Rb1 81.43(19) . .
C5 C4 H4A 119.0 . .
C3 C4 H4A 119.0 . .
Rb1 C4 H4A 119.0 . .
C4 C5 C6 120.8(3) . .
C4 C5 Rb1 72.42(19) . .
C6 C5 Rb1 88.3(2) . .
C4 C5 H5A 119.1 . .
C6 C5 H5A 119.1 . .
Rb1 C5 H5A 119.1 . .
C5 C6 C1 118.3(3) . .
C5 C6 C7 120.5(3) . .
C1 C6 C7 121.1(3) . .
C5 C6 Rb1 69.57(19) . .
C1 C6 Rb1 81.81(18) . .
C7 C6 Rb1 122.3(2) . .
C8 C7 C6 116.1(3) . .
C8 C7 H7A 108.3 . .
C6 C7 H7A 108.3 . .
C8 C7 H7B 108.3 . .
C6 C7 H7B 108.3 . .
H7A C7 H7B 107.4 . .
C13 C8 C9 118.9(3) . .
C13 C8 C7 120.6(3) . .
C9 C8 C7 120.5(3) . .
O2 C9 C10 119.8(3) . .
O2 C9 C8 120.0(3) . .
C10 C9 C8 120.2(3) . .
C11 C10 C9 119.3(3) . .
C11 C10 C14 120.6(3) . .
C9 C10 C14 120.1(3) . .
C10 C11 C12 121.0(3) . .
C10 C11 H11A 119.5 . .
C12 C11 H11A 119.5 . .
C13 C12 C11 119.4(3) . .
C13 C12 H12A 120.3 . .
C11 C12 H12A 120.3 . .
C12 C13 C8 121.4(3) . .
C12 C13 H13A 119.3 . .
C8 C13 H13A 119.3 . .
C15 C14 C10 116.4(3) . .
C15 C14 H14A 108.2 . .
C10 C14 H14A 108.2 . .
C15 C14 H14B 108.2 . .
C10 C14 H14B 108.2 . .
H14A C14 H14B 107.4 . .
C20 C15 C16 117.7(3) . .
C20 C15 C14 120.1(3) . .
C16 C15 C14 122.1(3) . .
C20 C15 K1 74.1(2) . .
C16 C15 K1 76.72(18) . .
C14 C15 K1 121.9(2) . .
O3 C16 C17 116.5(3) . .
O3 C16 C15 122.1(3) . .
C17 C16 C15 121.4(3) . .
O3 C16 K1 119.64(19) . .
C17 C16 K1 72.16(17) . .
C15 C16 K1 79.42(19) . .
C18 C17 C16 118.5(3) . .
C18 C17 C21 123.2(3) . .
C16 C17 C21 118.2(3) . .
C18 C17 K1 73.94(18) . .
C16 C17 K1 83.50(19) . .
C21 C17 K1 112.85(19) . .
C19 C18 C17 121.0(3) . .
C19 C18 K1 79.6(2) . .
C17 C18 K1 80.99(18) . .
C19 C18 H18A 119.1 . .
C17 C18 H18A 119.1 . .
K1 C18 H18A 119.1 . .
C20 C19 C18 119.7(3) . .
C20 C19 K1 82.2(2) . .
C18 C19 K1 75.26(19) . .
C20 C19 H19A 119.9 . .
C18 C19 H19A 119.9 . .
K1 C19 H19A 119.9 . .
C19 C20 C15 121.6(3) . .
C19 C20 K1 73.4(2) . .
C15 C20 K1 82.1(2) . .
C19 C20 H20A 119.1 . .
C15 C20 H20A 119.1 . .
K1 C20 H20A 119.1 . .
C22 C21 C17 118.4(3) . .
C22 C21 H21A 107.7 . .
C17 C21 H21A 107.7 . .
C22 C21 H21B 107.7 . .
C17 C21 H21B 107.7 . .
H21A C21 H21B 107.1 . .
C27 C22 C23 117.9(3) . .
C27 C22 C21 121.5(3) . .
C23 C22 C21 120.2(3) . .
O4 C23 C22 117.3(3) . .
O4 C23 C24 121.1(3) . .
C22 C23 C24 121.5(3) . .
C25 C24 C23 118.4(3) . .
C25 C24 C28 120.6(3) . .
C23 C24 C28 121.0(3) . .
C26 C25 C24 121.1(3) . .
C26 C25 H25A 119.5 . .
C24 C25 H25A 119.5 . .
C27 C26 C25 119.3(3) . .
C27 C26 H26A 120.3 . .
C25 C26 H26A 120.3 . .
C26 C27 C22 121.6(3) . .
C26 C27 H27A 119.2 . .
C22 C27 H27A 119.2 . .
C29 C28 C24 116.6(3) . .
C29 C28 H28A 108.1 . .
C24 C28 H28A 108.1 . .
C29 C28 H28B 108.1 . .
C24 C28 H28B 108.1 . .
H28A C28 H28B 107.3 . .
C34 C29 C30 118.1(3) . .
C34 C29 C28 120.9(3) . .
C30 C29 C28 120.9(3) . .
O5 C30 C29 120.1(3) . .
O5 C30 C31 120.1(3) . .
C29 C30 C31 119.8(3) . .
C32 C31 C30 120.0(3) . .
C32 C31 C35 120.0(3) . .
C30 C31 C35 120.0(3) . .
C33 C32 C31 120.7(3) . .
C33 C32 H32A 119.6 . .
C31 C32 H32A 119.6 . .
C32 C33 C34 119.6(3) . .
C32 C33 H33A 120.2 . .
C34 C33 H33A 120.2 . .
C33 C34 C29 121.8(3) . .
C33 C34 H34A 119.1 . .
C29 C34 H34A 119.1 . .
C31 C35 C36 114.1(3) . .
C31 C35 H35A 108.7 . .
C36 C35 H35A 108.7 . .
C31 C35 H35B 108.7 . .
C36 C35 H35B 108.7 . .
H35A C35 H35B 107.6 . .
C41 C36 C37 118.2(3) . .
C41 C36 C35 120.2(3) . .
C37 C36 C35 121.6(3) . .
O6 C37 C36 121.4(3) . .
O6 C37 C38 117.7(3) . .
C36 C37 C38 120.9(3) . .
C39 C38 C37 118.8(3) . .
C39 C38 C42 121.5(3) . .
C37 C38 C42 119.7(3) . .
C40 C39 C38 120.5(3) . .
C40 C39 H39A 119.7 . .
C38 C39 H39A 119.7 . .
C41 C40 C39 119.8(3) . .
C41 C40 H40A 120.1 . .
C39 C40 H40A 120.1 . .
C40 C41 C36 121.6(3) . .
C40 C41 H41A 119.2 . .
C36 C41 H41A 119.2 . .
C38 C42 C2 114.3(3) . .
C38 C42 H42A 108.7 . .
C2 C42 H42A 108.7 . .
C38 C42 H42B 108.7 . .
C2 C42 H42B 108.7 . .
H42A C42 H42B 107.6 . .
O10 C43 C45 122.1(4) . .
O10 C43 C44 121.7(4) . .
C45 C43 C44 116.3(3) . .
C43 C44 H44A 109.5 . .
C43 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C43 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
C43 C45 H45A 109.5 . .
C43 C45 H45B 109.5 . .
H45A C45 H45B 109.5 . .
C43 C45 H45C 109.5 . .
H45A C45 H45C 109.5 . .
H45B C45 H45C 109.5 . .
O11 C46 C48 121.3(4) . .
O11 C46 C47 121.8(5) . .
C48 C46 C47 117.0(4) . .
C46 C47 H47A 109.5 . .
C46 C47 H47B 109.5 . .
H47A C47 H47B 109.5 . .
C46 C47 H47C 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C46 C48 H48A 109.5 . .
C46 C48 H48B 109.5 . .
H48A C48 H48B 109.5 . .
C46 C48 H48C 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rb1 O10 2.863(3) .
Rb1 O8 2.993(3) .
Rb1 O9 2.999(4) .
Rb1 O3 3.005(3) 4_565
Rb1 O6 3.008(2) .
Rb1 O7 3.029(3) .
Rb1 C4 3.314(3) .
Rb1 C3 3.398(3) .
Rb1 C5 3.457(3) .
Rb1 O1 3.528(2) 4_565
Rb1 C2 3.623(3) .
Rb1 C6 3.688(3) .
Rb1 H6O 3.28(4) .
Rb1 H7D 3.00(5) .
Rb1 H8C 3.24(5) .
Rb1 H9C 3.12(5) .
K1 O9 2.658(3) .
K1 O8 2.685(3) .
K1 O7 2.727(3) .
K1 O11 2.773(3) .
K1 O4 2.786(3) .
K1 C18 3.154(3) .
K1 C19 3.208(3) .
K1 C17 3.242(3) .
K1 C20 3.318(4) .
K1 C16 3.384(3) .
K1 C15 3.417(3) .
K1 H4O 3.05(4) .
K1 H7D 3.07(5) .
K1 H9D 3.06(6) .
O1 C1 1.357(4) .
O1 Rb1 3.528(2) 4_566
O1 H1O 0.72(4) .
O2 C9 1.338(4) .
O3 C16 1.362(4) .
O3 Rb1 3.005(3) 4_566
O3 H3O 0.66(4) .
O4 C23 1.362(4) .
O4 H4O 0.67(4) .
O5 C30 1.345(4) .
O6 C37 1.366(4) .
O6 H6O 0.69(4) .
O7 H7C 0.68(5) .
O7 H7D 0.70(5) .
O8 H8D 0.78(6) .
O8 H8C 0.90(5) .
O9 H9D 0.66(6) .
O9 H9C 0.79(6) .
O10 C43 1.208(4) .
O11 C46 1.217(5) .
C1 C2 1.400(5) .
C1 C6 1.404(5) .
C2 C3 1.390(4) .
C2 C42 1.514(4) .
C3 C4 1.391(5) .
C3 H3A 1.0000 .
C4 C5 1.390(5) .
C4 H4A 1.0000 .
C5 C6 1.391(5) .
C5 H5A 1.0000 .
C6 C7 1.533(5) .
C7 C8 1.505(5) .
C7 H7A 0.9900 .
C7 H7B 0.9900 .
C8 C13 1.399(5) .
C8 C9 1.412(5) .
C9 C10 1.410(5) .
C10 C11 1.391(5) .
C10 C14 1.522(5) .
C11 C12 1.402(5) .
C11 H11A 0.9500 .
C12 C13 1.383(5) .
C12 H12A 0.9500 .
C13 H13A 0.9500 .
C14 C15 1.518(5) .
C14 H14A 0.9900 .
C14 H14B 0.9900 .
C15 C20 1.397(5) .
C15 C16 1.406(5) .
C16 C17 1.404(4) .
C17 C18 1.391(5) .
C17 C21 1.513(4) .
C18 C19 1.384(5) .
C18 H18A 1.0000 .
C19 C20 1.384(5) .
C19 H19A 1.0000 .
C20 H20A 1.0000 .
C21 C22 1.503(4) .
C21 H21A 0.9900 .
C21 H21B 0.9900 .
C22 C27 1.394(4) .
C22 C23 1.404(5) .
C23 C24 1.405(4) .
C24 C25 1.393(5) .
C24 C28 1.521(5) .
C25 C26 1.391(5) .
C25 H25A 0.9500 .
C26 C27 1.389(5) .
C26 H26A 0.9500 .
C27 H27A 0.9500 .
C28 C29 1.516(5) .
C28 H28A 0.9900 .
C28 H28B 0.9900 .
C29 C34 1.399(5) .
C29 C30 1.410(5) .
C30 C31 1.412(5) .
C31 C32 1.385(5) .
C31 C35 1.517(5) .
C32 C33 1.377(6) .
C32 H32A 0.9500 .
C33 C34 1.386(5) .
C33 H33A 0.9500 .
C34 H34A 0.9500 .
C35 C36 1.517(5) .
C35 H35A 0.9900 .
C35 H35B 0.9900 .
C36 C41 1.394(5) .
C36 C37 1.398(4) .
C37 C38 1.404(5) .
C38 C39 1.392(5) .
C38 C42 1.510(4) .
C39 C40 1.390(5) .
C39 H39A 0.9500 .
C40 C41 1.372(5) .
C40 H40A 0.9500 .
C41 H41A 0.9500 .
C42 H42A 0.9900 .
C42 H42B 0.9900 .
C43 C45 1.494(5) .
C43 C44 1.495(6) .
C44 H44A 0.9800 .
C44 H44B 0.9800 .
C44 H44C 0.9800 .
C45 H45A 0.9800 .
C45 H45B 0.9800 .
C45 H45C 0.9800 .
C46 C48 1.477(7) .
C46 C47 1.486(6) .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
