# Supplementary Material (ESI) for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2010

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Kang Min Ok'
_publ_contact_author_email       KMOK@CAU.AC.KR

_publ_section_title              
;
CAU-1 and CAU-2: The first tubular alkali
metal-organic framework materials,
A3[C6H3(CO2)(CO2H0.5)(CO2H)]2 (A = K or Rb)
;
loop_
_publ_author_name
'Kang Min Ok.'
'Vinna Jo.'
'Min Kyung Kim.'
'Dong Woo Lee.'
'Il-Wun Shim.'

# Attachment 'CAU.cif'

data_CAU1
_database_code_depnum_ccdc_archive 'CCDC 745346'

#TrackingRef 'CAU.cif'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'C18 H9 K3 O12'
_chemical_formula_weight         534.55

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_cell_length_a                   3.9802(8)
_cell_length_b                   13.615(3)
_cell_length_c                   17.671(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.72(3)
_cell_angle_gamma                90
_cell_volume                     955.6(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    298.0(2)

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    1.858
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             540
_exptl_crystal_description       Rod
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.785
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
;
SADABS(Blessing, 1995)
;
_exptl_absorpt_correction_T_min  0.92
_exptl_absorpt_correction_T_max  0.96

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      298.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0811
_diffrn_reflns_number            7696
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             2786
_reflns_number_gt                1533
_reflns_threshold_expression     >2\(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.0326P)^2^+5.4274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method     none
_refine_ls_number_reflns         2786
_refine_ls_number_parameters     151
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0685
_refine_ls_wR_factor_ref         0.1953
_refine_ls_wR_factor_gt          0.1311
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_restrained_S_all      1.118
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.987
_refine_diff_density_rms         0.178

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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_
_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 0.5 0 0 0.0342(4) Uani 1 2 d S . .
K2 K 0.7094(3) 0.28863(10) 0.06321(8) 0.0381(3) Uani 1 1 d . . .
O1 O 0.2128(11) 0.1563(3) 0.0976(2) 0.0357(10) Uani 1 1 d . . .
O2 O 0.0509(10) 0.0032(3) 0.11886(19) 0.0301(8) Uani 1 1 d . . .
O3 O 0.4828(11) -0.1836(3) 0.0681(2) 0.0358(10) Uani 1 1 d . . .
O4 O 0.3956(10) -0.1380(3) 0.1867(2) 0.0354(10) Uani 1 1 d . . .
H1 H 0.2947 -0.0925 0.165 0.053 Uiso 1 1 calc R . .
O5 O 0.2451(10) 0.4181(3) 0.1096(2) 0.0338(9) Uani 1 1 d . . .
O6 O 0.6845(9) 0.4506(3) -0.0376(2) 0.0296(8) Uani 1 1 d . . .
H6 H 0.605 0.419 0.0043 0.036 Uiso 0.5 1 calc PR . .
C1 C 0.1291(12) 0.1118(4) 0.2249(3) 0.0251(11) Uani 1 1 d . . .
C2 C 0.0212(13) 0.5474(4) 0.2253(3) 0.0263(11) Uani 1 1 d . . .
H2 H 0.1159 0.4888 0.2434 0.032 Uiso 1 1 calc R . .
C3 C 0.0286(12) 0.5710(4) 0.1490(3) 0.0218(10) Uani 1 1 d . . .
C4 C 0.8785(13) -0.3440(4) 0.1220(3) 0.0247(10) Uani 1 1 d . . .
H3 H 0.8869 -0.3281 0.071 0.03 Uiso 1 1 calc R . .
C5 C 0.7124(13) -0.2806(4) 0.1701(3) 0.0248(10) Uani 1 1 d . . .
C6 C 0.7235(13) -0.3017(4) 0.2472(3) 0.0253(10) Uani 1 1 d . . .
H4 H 0.6316 -0.2577 0.2804 0.03 Uiso 1 1 calc R . .
C7 C 0.1308(13) 0.0891(4) 0.1413(3) 0.0261(11) Uani 1 1 d . . .
C8 C 0.2050(13) 0.5057(4) 0.0959(3) 0.0251(10) Uani 1 1 d . . .
C9 C 0.5246(13) -0.1956(4) 0.1362(3) 0.0271(11) Uani 1 1 d . . .

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 0.0437(10) 0.0339(9) 0.0255(8) 0.0025(7) 0.0074(7) 0.0016(8)
K2 0.0389(7) 0.0327(7) 0.0432(7) 0.0025(6) 0.0059(5) 0.0020(6)
O1 0.059(3) 0.0230(19) 0.0256(19) 0.0025(16) 0.0101(18) -0.0054(19)
O2 0.043(2) 0.0255(19) 0.0220(17) -0.0032(16) 0.0009(15) 0.0009(18)
O3 0.058(3) 0.031(2) 0.0191(17) 0.0027(16) 0.0090(17) 0.0066(19)
O4 0.050(3) 0.031(2) 0.0257(19) -0.0009(16) 0.0054(17) 0.0153(19)
O5 0.048(2) 0.0193(18) 0.036(2) 0.0016(16) 0.0095(18) 0.0067(17)
O6 0.036(2) 0.029(2) 0.0243(17) -0.0004(16) 0.0094(15) 0.0012(17)
C1 0.022(2) 0.031(3) 0.022(2) -0.003(2) 0.0022(18) -0.001(2)
C2 0.025(3) 0.028(3) 0.026(2) 0.001(2) 0.001(2) 0.002(2)
C3 0.019(2) 0.022(2) 0.025(2) 0.001(2) 0.0016(18) 0.0001(19)
C4 0.025(3) 0.029(3) 0.020(2) 0.000(2) 0.0016(18) -0.002(2)
C5 0.029(3) 0.021(2) 0.024(2) 0.001(2) 0.0055(19) 0.002(2)
C6 0.027(3) 0.021(2) 0.028(2) 0.000(2) 0.005(2) -0.003(2)
C7 0.026(3) 0.029(3) 0.022(2) 0.000(2) -0.0003(19) 0.004(2)
C8 0.027(3) 0.028(3) 0.020(2) -0.004(2) 0.0031(18) -0.002(2)
C9 0.029(3) 0.023(2) 0.029(2) 0.002(2) 0.004(2) -0.002(2)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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 O3 2.776(4) 3_655 ?
K1 O3 2.776(4) . ?
K1 O2 2.845(4) . ?
K1 O2 2.845(4) 3_655 ?
K1 O2 2.936(4) 1_655 ?
K1 O2 2.936(4) 3 ?
K1 O1 3.012(4) . ?
K1 O1 3.012(4) 3_655 ?
K1 C7 3.216(5) . ?
K1 C7 3.216(5) 3_655 ?
K1 K1 3.9802(9) 1_655 ?
K1 K1 3.9802(9) 1_455 ?
K2 O5 2.719(4) . ?
K2 O1 2.733(5) 1_655 ?
K2 O1 2.771(4) . ?
K2 O3 2.790(4) 3_655 ?
K2 O6 2.832(4) . ?
K2 O5 2.846(4) 1_655 ?
K2 C7 3.434(5) 1_655 ?
K2 K2 3.9802(19) 1_455 ?
K2 K2 3.9802(19) 1_655 ?
O1 C7 1.253(6) . ?
O1 K2 2.733(4) 1_455 ?
O2 C7 1.269(6) . ?
O2 K1 2.936(4) 1_455 ?
O3 C9 1.217(6) . ?
O3 K2 2.790(4) 3_655 ?
O4 C9 1.317(6) . ?
O5 C8 1.225(6) . ?
O5 K2 2.846(4) 1_455 ?
O6 C8 1.291(6) 3_665 ?
C1 C6 1.392(7) 2_655 ?
C1 C2 1.404(7) 2_545 ?
C1 C7 1.509(7) . ?
C2 C3 1.388(7) . ?
C2 C1 1.404(7) 2 ?
C3 C4 1.373(7) 1_465 ?
C3 C8 1.500(7) . ?
C4 C3 1.373(7) 1_645 ?
C4 C5 1.406(7) . ?
C5 C6 1.390(7) . ?
C5 C9 1.482(7) . ?
C6 C1 1.392(7) 2_645 ?
C7 K2 3.434(5) 1_455 ?
C8 O6 1.291(6) 3_665 ?

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
O3 K1 O3 180.00(15) 3_655 . ?
O3 K1 O2 109.89(11) 3_655 . ?
O3 K1 O2 70.11(11) . . ?
O3 K1 O2 70.11(11) 3_655 3_655 ?
O3 K1 O2 109.89(11) . 3_655 ?
O2 K1 O2 180.00(14) . 3_655 ?
O3 K1 O2 104.95(11) 3_655 1_655 ?
O3 K1 O2 75.05(11) . 1_655 ?
O2 K1 O2 86.99(9) . 1_655 ?
O2 K1 O2 93.01(9) 3_655 1_655 ?
O3 K1 O2 75.05(11) 3_655 3 ?
O3 K1 O2 104.95(11) . 3 ?
O2 K1 O2 93.01(9) . 3 ?
O2 K1 O2 86.99(9) 3_655 3 ?
O2 K1 O2 180.00(10) 1_655 3 ?
O3 K1 O1 68.46(10) 3_655 . ?
O3 K1 O1 111.54(10) . . ?
O2 K1 O1 44.45(10) . . ?
O2 K1 O1 135.55(10) 3_655 . ?
O2 K1 O1 82.71(11) 1_655 . ?
O2 K1 O1 97.29(11) 3 . ?
O3 K1 O1 111.54(10) 3_655 3_655 ?
O3 K1 O1 68.46(10) . 3_655 ?
O2 K1 O1 135.55(10) . 3_655 ?
O2 K1 O1 44.45(10) 3_655 3_655 ?
O2 K1 O1 97.29(11) 1_655 3_655 ?
O2 K1 O1 82.71(11) 3 3_655 ?
O1 K1 O1 180.0(2) . 3_655 ?
O3 K1 C7 91.25(12) 3_655 . ?
O3 K1 C7 88.75(12) . . ?
O2 K1 C7 23.14(12) . . ?
O2 K1 C7 156.86(12) 3_655 . ?
O2 K1 C7 78.27(12) 1_655 . ?
O2 K1 C7 101.73(12) 3 . ?
O1 K1 C7 22.92(12) . . ?
O1 K1 C7 157.08(12) 3_655 . ?
O3 K1 C7 88.75(12) 3_655 3_655 ?
O3 K1 C7 91.25(12) . 3_655 ?
O2 K1 C7 156.86(12) . 3_655 ?
O2 K1 C7 23.14(12) 3_655 3_655 ?
O2 K1 C7 101.73(12) 1_655 3_655 ?
O2 K1 C7 78.27(12) 3 3_655 ?
O1 K1 C7 157.08(12) . 3_655 ?
O1 K1 C7 22.92(12) 3_655 3_655 ?
C7 K1 C7 180.00(18) . 3_655 ?
O3 K1 K1 86.97(9) 3_655 1_655 ?
O3 K1 K1 93.03(9) . 1_655 ?
O2 K1 K1 132.55(7) . 1_655 ?
O2 K1 K1 47.45(7) 3_655 1_655 ?
O2 K1 K1 45.55(7) 1_655 1_655 ?
O2 K1 K1 134.44(7) 3 1_655 ?
O1 K1 K1 114.63(8) . 1_655 ?
O1 K1 K1 65.37(8) 3_655 1_655 ?
C7 K1 K1 120.49(9) . 1_655 ?
C7 K1 K1 59.51(9) 3_655 1_655 ?
O3 K1 K1 93.03(9) 3_655 1_455 ?
O3 K1 K1 86.97(9) . 1_455 ?
O2 K1 K1 47.45(7) . 1_455 ?
O2 K1 K1 132.55(7) 3_655 1_455 ?
O2 K1 K1 134.45(7) 1_655 1_455 ?
O2 K1 K1 45.56(7) 3 1_455 ?
O1 K1 K1 65.37(8) . 1_455 ?
O1 K1 K1 114.63(8) 3_655 1_455 ?
C7 K1 K1 59.51(9) . 1_455 ?
C7 K1 K1 120.49(9) 3_655 1_455 ?
K1 K1 K1 180 1_655 1_455 ?
O5 K2 O1 149.64(12) . 1_655 ?
O5 K2 O1 81.19(12) . . ?
O1 K2 O1 92.63(12) 1_655 . ?
O5 K2 O3 115.37(13) . 3_655 ?
O1 K2 O3 90.26(12) 1_655 3_655 ?
O1 K2 O3 71.84(12) . 3_655 ?
O5 K2 O6 71.85(11) . . ?
O1 K2 O6 130.40(12) 1_655 . ?
O1 K2 O6 130.38(13) . . ?
O3 K2 O6 83.08(11) 3_655 . ?
O5 K2 O5 91.30(12) . 1_655 ?
O1 K2 O5 79.59(12) 1_655 1_655 ?
O1 K2 O5 150.59(12) . 1_655 ?
O3 K2 O5 135.82(12) 3_655 1_655 ?
O6 K2 O5 72.19(11) . 1_655 ?
O5 K2 C7 135.68(12) . 1_655 ?
O1 K2 C7 19.52(12) 1_655 1_655 ?
O1 K2 C7 74.60(13) . 1_655 ?
O3 K2 C7 91.65(12) 3_655 1_655 ?
O6 K2 C7 149.82(12) . 1_655 ?
O5 K2 C7 92.11(12) 1_655 1_655 ?
O5 K2 K2 45.63(9) . 1_455 ?
O1 K2 K2 135.94(9) 1_655 1_455 ?
O1 K2 K2 43.31(9) . 1_455 ?
O3 K2 K2 77.28(9) 3_655 1_455 ?
O6 K2 K2 90.34(8) . 1_455 ?
O5 K2 K2 136.93(8) 1_655 1_455 ?
C7 K2 K2 117.54(9) 1_655 1_455 ?
O5 K2 K2 134.37(9) . 1_655 ?
O1 K2 K2 44.06(9) 1_655 1_655 ?
O1 K2 K2 136.68(9) . 1_655 ?
O3 K2 K2 102.72(9) 3_655 1_655 ?
O6 K2 K2 89.66(8) . 1_655 ?
O5 K2 K2 43.07(8) 1_655 1_655 ?
C7 K2 K2 62.46(9) 1_655 1_655 ?
K2 K2 K2 180 1_455 1_655 ?
O5 K2 K1 124.47(10) . . ?
O1 K2 K1 64.40(9) 1_655 . ?
O1 K2 K1 46.43(8) . . ?
O3 K2 K1 41.59(8) 3_655 . ?
O6 K2 K1 124.67(8) . . ?
O5 K2 K1 142.82(9) 1_655 . ?
C7 K2 K1 56.23(9) 1_655 . ?
K2 K2 K1 79.450(18) 1_455 . ?
K2 K2 K1 100.550(18) 1_655 . ?
C7 O1 K2 113.7(3) . 1_455 ?
C7 O1 K2 145.9(4) . . ?
K2 O1 K2 92.63(12) 1_455 . ?
C7 O1 K1 87.7(3) . . ?
K2 O1 K1 129.66(14) 1_455 . ?
K2 O1 K1 91.77(12) . . ?
C7 O2 K1 95.0(3) . . ?
C7 O2 K1 113.4(3) . 1_455 ?
K1 O2 K1 86.99(9) . 1_455 ?
C9 O3 K1 123.0(4) . . ?
C9 O3 K2 140.1(4) . 3_655 ?
K1 O3 K2 96.58(11) . 3_655 ?
C8 O5 K2 130.8(3) . . ?
C8 O5 K2 117.4(3) . 1_455 ?
K2 O5 K2 91.30(12) . 1_455 ?
C8 O6 K2 149.4(3) 3_665 . ?
C6 C1 C2 119.5(4) 2_655 2_545 ?
C6 C1 C7 119.4(5) 2_655 . ?
C2 C1 C7 121.1(5) 2_545 . ?
C3 C2 C1 120.1(5) . 2 ?
C4 C3 C2 119.8(5) 1_465 . ?
C4 C3 C8 119.5(4) 1_465 . ?
C2 C3 C8 120.7(5) . . ?
C3 C4 C5 121.2(5) 1_645 . ?
C6 C5 C4 118.6(5) . . ?
C6 C5 C9 122.7(5) . . ?
C4 C5 C9 118.7(4) . . ?
C5 C6 C1 120.6(5) . 2_645 ?
O1 C7 O2 123.4(5) . . ?
O1 C7 C1 118.1(5) . . ?
O2 C7 C1 118.5(5) . . ?
O1 C7 K1 69.4(3) . . ?
O2 C7 K1 61.8(3) . . ?
C1 C7 K1 150.2(3) . . ?
O1 C7 K2 46.8(3) . 1_455 ?
O2 C7 K2 119.8(3) . 1_455 ?
C1 C7 K2 101.4(3) . 1_455 ?
K1 C7 K2 102.87(14) . 1_455 ?
O5 C8 O6 124.1(5) . 3_665 ?
O5 C8 C3 120.9(4) . . ?
O6 C8 C3 115.0(5) 3_665 . ?
O3 C9 O4 123.8(5) . . ?
O3 C9 C5 122.6(5) . . ?
O4 C9 C5 113.6(4) . . ?

#===END

data_CAU2
_database_code_depnum_ccdc_archive 'CCDC 745347'
#TrackingRef 'CAU.cif'

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
?
;
_chemical_formula_sum            'C18 H9 O12 Rb3'
_chemical_formula_weight         673.66

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_cell_length_a                   4.0727(8)
_cell_length_b                   13.891(3)
_cell_length_c                   17.853(4)
_cell_angle_alpha                90
_cell_angle_beta                 93.81(3)
_cell_angle_gamma                90
_cell_volume                     1007.8(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    298.0(2)

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_density_diffrn    2.22
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_exptl_crystal_description       Rod
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.324
_exptl_absorpt_correction_type   EMPIRICAL
_exptl_absorpt_process_details   
;
SADABS(Blessing, 1995)
;
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_T_max  0.70

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       CCD
_diffrn_ambient_temperature      298.0(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.1032
_diffrn_reflns_number            5787
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.86
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_full        25.49
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_reflns_number_total             1847
_reflns_number_gt                1186
_reflns_threshold_expression     >2\(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_extinction_method     none
_refine_ls_number_reflns         1847
_refine_ls_number_parameters     161
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.16
_refine_ls_R_factor_gt           0.1196
_refine_ls_wR_factor_ref         0.3088
_refine_ls_wR_factor_gt          0.2811
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         4.606
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.336

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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_
_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
Rb1 Rb 0.5 0 0 0.0360(8) Uani 0.903(6) 2 d SP . .
Rb1' Rb 0.107(7) -0.001(2) -0.0013(15) 0.0360(8) Uani 0.050(3) 1 d P . .
Rb2 Rb 0.7212(4) 0.28479(11) 0.06880(9) 0.0396(6) Uani 0.923(4) 1 d P . .
Rb2' Rb 0.231(5) 0.2846(13) 0.0694(10) 0.0396(6) Uani 0.076(4) 1 d P . .
O1 O 0.217(3) 0.1441(7) 0.1031(5) 0.040(3) Uani 1 1 d . . .
O2 O 0.065(3) -0.0058(7) 0.1266(5) 0.043(3) Uani 1 1 d . . .
O3 O 0.504(3) -0.1873(8) 0.0703(5) 0.051(3) Uani 1 1 d . . .
O4 O 0.400(3) -0.1488(7) 0.1880(5) 0.047(3) Uani 1 1 d . . .
H1 H 0.3054 -0.103 0.1672 0.07 Uiso 1 1 calc R . .
O5 O 0.254(3) 0.4197(7) 0.1087(6) 0.048(3) Uani 1 1 d . . .
O6 O 0.683(3) 0.4514(6) -0.0364(5) 0.038(2) Uani 1 1 d . . .
H6 H 0.6106 0.4209 0.0058 0.045 Uiso 0.5 1 calc PR . .
C1 C 0.132(4) 0.1045(10) 0.2290(6) 0.031(3) Uani 1 1 d . . .
C2 C 0.023(4) 0.5431(10) 0.2213(7) 0.032(3) Uani 1 1 d . . .
H2 H 0.1159 0.4854 0.2386 0.039 Uiso 1 1 calc R . .
C3 C 0.036(3) 0.5692(9) 0.1458(7) 0.024(3) Uani 1 1 d . . .
C4 C 0.883(4) -0.3471(10) 0.1208(7) 0.034(3) Uani 1 1 d . . .
H3 H 0.8945 -0.3293 0.0709 0.041 Uiso 1 1 calc R . .
C5 C 0.714(4) -0.2886(9) 0.1678(7) 0.029(3) Uani 1 1 d . . .
C6 C 0.716(3) -0.3110(9) 0.2447(7) 0.028(3) Uani 1 1 d . . .
H4 H 0.6168 -0.2699 0.2776 0.034 Uiso 1 1 calc R . .
C7 C 0.141(4) 0.0787(11) 0.1458(7) 0.034(3) Uani 1 1 d . . .
C8 C 0.216(4) 0.5066(10) 0.0946(8) 0.039(4) Uani 1 1 d . . .
C9 C 0.533(4) -0.2043(10) 0.1363(8) 0.037(4) Uani 1 1 d . . .

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
Rb1 0.0619(17) 0.0231(11) 0.0241(11) 0.0024(8) 0.0119(9) 0.0050(10)
Rb1' 0.0619(17) 0.0231(11) 0.0241(11) 0.0024(8) 0.0119(9) 0.0050(10)
Rb2 0.0499(11) 0.0255(9) 0.0436(10) 0.0032(6) 0.0064(7) 0.0027(7)
Rb2' 0.0499(11) 0.0255(9) 0.0436(10) 0.0032(6) 0.0064(7) 0.0027(7)
O1 0.070(8) 0.028(5) 0.024(5) 0.003(4) 0.016(5) 0.010(5)
O2 0.066(8) 0.033(6) 0.031(5) -0.006(4) 0.005(5) -0.004(5)
O3 0.090(10) 0.039(6) 0.026(5) 0.000(5) 0.012(5) 0.013(6)
O4 0.075(8) 0.031(5) 0.036(6) -0.006(5) 0.011(5) 0.018(5)
O5 0.077(9) 0.027(6) 0.042(6) 0.000(5) 0.015(5) 0.007(5)
O6 0.060(7) 0.026(5) 0.028(5) 0.002(4) 0.010(5) -0.003(5)
C1 0.052(10) 0.027(7) 0.013(6) 0.002(5) -0.001(6) 0.001(6)
C2 0.042(9) 0.026(7) 0.029(7) -0.005(6) 0.008(6) 0.004(6)
C3 0.025(7) 0.025(6) 0.021(6) -0.005(5) 0.001(5) -0.006(5)
C4 0.049(10) 0.034(8) 0.020(7) 0.008(6) 0.002(6) 0.006(7)
C5 0.052(9) 0.020(6) 0.017(6) 0.000(5) 0.006(6) 0.004(6)
C6 0.034(8) 0.028(7) 0.024(6) -0.002(5) 0.010(6) 0.000(6)
C7 0.035(9) 0.039(9) 0.029(7) 0.003(6) 0.011(6) 0.012(7)
C8 0.059(11) 0.024(8) 0.036(8) 0.000(6) 0.005(7) 0.011(7)
C9 0.055(10) 0.030(7) 0.024(7) -0.001(6) 0.001(7) 0.002(7)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_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
Rb1 Rb1' 1.60(3) 3_655 ?
Rb1 Rb1' 1.60(3) . ?
Rb1 Rb1' 2.47(3) 1_655 ?
Rb1 Rb1' 2.47(3) 3 ?
Rb1 O3 2.888(10) . ?
Rb1 O3 2.888(10) 3_655 ?
Rb1 O2 2.964(11) 3_655 ?
Rb1 O2 2.964(11) . ?
Rb1 O1 3.000(9) 3_655 ?
Rb1 O1 3.000(9) . ?
Rb1 O2 3.117(11) 3 ?
Rb1 O2 3.117(11) 1_655 ?
Rb1' Rb1' 0.88(6) 3 ?
Rb1' O2 2.30(3) . ?
Rb1' O2 2.30(3) 3 ?
Rb1' Rb1 2.47(3) 1_455 ?
Rb1' O1 2.76(3) . ?
Rb1' C7 2.84(3) . ?
Rb1' C7 2.92(3) 3 ?
Rb1' O1 2.95(3) 3 ?
Rb1' Rb1' 3.20(6) 3_655 ?
Rb1' O3 3.27(3) . ?
Rb1' O3 3.33(3) 3_655 ?
Rb2 Rb2' 2.00(2) . ?
Rb2 Rb2' 2.08(2) 1_655 ?
Rb2 O5 2.796(11) . ?
Rb2 O1 2.848(10) 1_655 ?
Rb2 O5 2.920(12) 1_655 ?
Rb2 O3 2.921(11) 3_655 ?
Rb2 O1 2.927(11) . ?
Rb2 O6 2.978(9) . ?
Rb2 C7 3.563(14) 1_655 ?
Rb2 C8 3.694(16) 1_655 ?
Rb2 C8 3.749(14) . ?
Rb2 Rb2 4.0727(8) 1_455 ?
Rb2' O5 2.00(2) . ?
Rb2' O1 2.04(2) . ?
Rb2' Rb2 2.08(2) 1_455 ?
Rb2' O3 3.09(2) 3_655 ?
Rb2' C8 3.12(2) . ?
Rb2' C7 3.20(2) . ?
Rb2' C4 3.51(2) 3_655 ?
Rb2' C6 3.57(2) 2_655 ?
Rb2' O6 3.58(2) . ?
Rb2' Rb2' 4.0727(8) 1_455 ?
Rb2' Rb2' 4.0727(8) 1_655 ?
O1 C7 1.240(17) . ?
O1 Rb2 2.848(10) 1_455 ?
O1 Rb1' 2.95(3) 3 ?
O2 C7 1.256(17) . ?
O2 Rb1' 2.30(3) 3 ?
O2 Rb1 3.117(11) 1_455 ?
O3 C9 1.200(16) . ?
O3 Rb2 2.921(11) 3_655 ?
O3 Rb2' 3.09(2) 3_655 ?
O3 Rb1' 3.33(3) 3_655 ?
O4 C9 1.343(17) . ?
O5 C8 1.240(16) . ?
O5 Rb2 2.920(12) 1_455 ?
O6 C8 1.283(18) 3_665 ?
C1 C6 1.395(19) 2_655 ?
C1 C2 1.409(18) 2_545 ?
C1 C7 1.531(18) . ?
C2 C3 1.401(18) . ?
C2 C1 1.409(18) 2 ?
C3 C4 1.378(18) 1_465 ?
C3 C8 1.491(19) . ?
C4 C3 1.378(18) 1_645 ?
C4 C5 1.384(19) . ?
C4 Rb2' 3.51(2) 3_655 ?
C5 C6 1.407(17) . ?
C5 C9 1.474(19) . ?
C6 C1 1.395(19) 2_645 ?
C6 Rb2' 3.57(2) 2_645 ?
C7 Rb1' 2.92(3) 3 ?
C7 Rb2 3.563(14) 1_455 ?
C7 Rb1 3.726(15) 1_455 ?
C8 O6 1.283(18) 3_665 ?
C8 Rb2 3.694(16) 1_455 ?

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
Rb1' Rb1 Rb1' 180 3_655 . ?
Rb1' Rb1 Rb1' 1.4(16) 3_655 1_655 ?
Rb1' Rb1 Rb1' 178.6(16) . 1_655 ?
Rb1' Rb1 Rb1' 178.6(16) 3_655 3 ?
Rb1' Rb1 Rb1' 1.4(16) . 3 ?
Rb1' Rb1 Rb1' 180 1_655 3 ?
Rb1' Rb1 O3 91.3(10) 3_655 . ?
Rb1' Rb1 O3 88.7(10) . . ?
Rb1' Rb1 O3 91.4(7) 1_655 . ?
Rb1' Rb1 O3 88.6(7) 3 . ?
Rb1' Rb1 O3 88.7(10) 3_655 3_655 ?
Rb1' Rb1 O3 91.3(10) . 3_655 ?
Rb1' Rb1 O3 88.6(7) 1_655 3_655 ?
Rb1' Rb1 O3 91.4(7) 3 3_655 ?
O3 Rb1 O3 180.0(3) . 3_655 ?
Rb1' Rb1 O2 50.4(10) 3_655 3_655 ?
Rb1' Rb1 O2 129.6(10) . 3_655 ?
Rb1' Rb1 O2 49.1(7) 1_655 3_655 ?
Rb1' Rb1 O2 130.9(7) 3 3_655 ?
O3 Rb1 O2 111.7(3) . 3_655 ?
O3 Rb1 O2 68.3(3) 3_655 3_655 ?
Rb1' Rb1 O2 129.6(10) 3_655 . ?
Rb1' Rb1 O2 50.4(10) . . ?
Rb1' Rb1 O2 130.9(7) 1_655 . ?
Rb1' Rb1 O2 49.1(7) 3 . ?
O3 Rb1 O2 68.3(3) . . ?
O3 Rb1 O2 111.7(3) 3_655 . ?
O2 Rb1 O2 180.0(6) 3_655 . ?
Rb1' Rb1 O1 65.7(10) 3_655 3_655 ?
Rb1' Rb1 O1 114.3(10) . 3_655 ?
Rb1' Rb1 O1 64.4(7) 1_655 3_655 ?
Rb1' Rb1 O1 115.6(7) 3 3_655 ?
O3 Rb1 O1 71.0(3) . 3_655 ?
O3 Rb1 O1 109.0(3) 3_655 3_655 ?
O2 Rb1 O1 43.7(3) 3_655 3_655 ?
O2 Rb1 O1 136.3(3) . 3_655 ?
Rb1' Rb1 O1 114.3(10) 3_655 . ?
Rb1' Rb1 O1 65.7(10) . . ?
Rb1' Rb1 O1 115.6(7) 1_655 . ?
Rb1' Rb1 O1 64.4(7) 3 . ?
O3 Rb1 O1 109.0(3) . . ?
O3 Rb1 O1 71.0(3) 3_655 . ?
O2 Rb1 O1 136.3(3) 3_655 . ?
O2 Rb1 O1 43.7(3) . . ?
O1 Rb1 O1 180.0(4) 3_655 . ?
Rb1' Rb1 O2 134.4(10) 3_655 3 ?
Rb1' Rb1 O2 45.6(10) . 3 ?
Rb1' Rb1 O2 133.1(7) 1_655 3 ?
Rb1' Rb1 O2 46.9(7) 3 3 ?
O3 Rb1 O2 108.7(3) . 3 ?
O3 Rb1 O2 71.3(3) 3_655 3 ?
O2 Rb1 O2 84.1(2) 3_655 3 ?
O2 Rb1 O2 95.9(2) . 3 ?
O1 Rb1 O2 82.4(3) 3_655 3 ?
O1 Rb1 O2 97.6(3) . 3 ?
Rb1' Rb1 O2 45.6(10) 3_655 1_655 ?
Rb1' Rb1 O2 134.4(10) . 1_655 ?
Rb1' Rb1 O2 46.9(7) 1_655 1_655 ?
Rb1' Rb1 O2 133.1(7) 3 1_655 ?
O3 Rb1 O2 71.3(3) . 1_655 ?
O3 Rb1 O2 108.7(3) 3_655 1_655 ?
O2 Rb1 O2 95.9(2) 3_655 1_655 ?
O2 Rb1 O2 84.1(2) . 1_655 ?
O1 Rb1 O2 97.6(3) 3_655 1_655 ?
O1 Rb1 O2 82.4(3) . 1_655 ?
O2 Rb1 O2 180 3 1_655 ?
Rb1' Rb1' Rb1 176(5) 3 . ?
Rb1' Rb1' O2 79(3) 3 . ?
Rb1 Rb1' O2 97.3(14) . . ?
Rb1' Rb1' O2 79(4) 3 3 ?
Rb1 Rb1' O2 104.7(12) . 3 ?
O2 Rb1' O2 158.0(14) . 3 ?
Rb1' Rb1' Rb1 3(3) 3 1_455 ?
Rb1 Rb1' Rb1 178.6(17) . 1_455 ?
O2 Rb1' Rb1 81.4(8) . 1_455 ?
O2 Rb1' Rb1 76.6(10) 3 1_455 ?
Rb1' Rb1' O1 94(4) 3 . ?
Rb1 Rb1' O1 82.4(12) . . ?
O2 Rb1' O1 51.1(6) . . ?
O2 Rb1' O1 130.8(12) 3 . ?
Rb1 Rb1' O1 96.3(9) 1_455 . ?
Rb1' Rb1' C7 86(4) 3 . ?
Rb1 Rb1' C7 89.9(13) . . ?
O2 Rb1' C7 25.6(5) . . ?
O2 Rb1' C7 151.1(13) 3 . ?
Rb1 Rb1' C7 88.7(8) 1_455 . ?
O1 Rb1' C7 25.5(4) . . ?
Rb1' Rb1' C7 76(4) 3 3 ?
Rb1 Rb1' C7 107.6(12) . 3 ?
O2 Rb1' C7 145.2(13) . 3 ?
O2 Rb1' C7 24.4(5) 3 3 ?
Rb1 Rb1' C7 73.8(8) 1_455 3 ?
O1 Rb1' C7 154.1(12) . 3 ?
C7 Rb1' C7 162.5(11) . 3 ?
Rb1' Rb1' O1 69(4) 3 3 ?
Rb1 Rb1' O1 114.8(13) . 3 ?
O2 Rb1' O1 122.0(11) . 3 ?
O2 Rb1' O1 48.1(7) 3 3 ?
Rb1 Rb1' O1 66.5(7) 1_455 3 ?
O1 Rb1' O1 162.7(11) . 3 ?
C7 Rb1' O1 145.4(11) . 3 ?
C7 Rb1' O1 24.4(4) 3 3 ?
Rb1' Rb1' Rb1' 176(5) 3 3_655 ?
Rb1 Rb1' Rb1' 0 . 3_655 ?
O2 Rb1' Rb1' 97.3(14) . 3_655 ?
O2 Rb1' Rb1' 104.7(12) 3 3_655 ?
Rb1 Rb1' Rb1' 178.6(16) 1_455 3_655 ?
O1 Rb1' Rb1' 82.4(12) . 3_655 ?
C7 Rb1' Rb1' 89.9(13) . 3_655 ?
C7 Rb1' Rb1' 107.6(12) 3 3_655 ?
O1 Rb1' Rb1' 114.8(13) 3 3_655 ?
Rb1' Rb1' O3 118(4) 3 . ?
Rb1 Rb1' O3 62.1(9) . . ?
O2 Rb1' O3 69.8(7) . . ?
O2 Rb1' O3 121.4(11) 3 . ?
Rb1 Rb1' O3 117.9(10) 1_455 . ?
O1 Rb1' O3 105.1(9) . . ?
C7 Rb1' O3 87.4(8) . . ?
C7 Rb1' O3 100.6(9) 3 . ?
O1 Rb1' O3 83.9(8) 3 . ?
Rb1' Rb1' O3 62.1(9) 3_655 . ?
Rb1' Rb1' O3 120(4) 3 3_655 ?
Rb1 Rb1' O3 60.0(9) . 3_655 ?
O2 Rb1' O3 117.4(11) . 3_655 ?
O2 Rb1' O3 74.4(8) 3 3_655 ?
Rb1 Rb1' O3 120.0(10) 1_455 3_655 ?
O1 Rb1' O3 67.6(7) . 3_655 ?
C7 Rb1' O3 92.4(9) . 3_655 ?
C7 Rb1' O3 96.3(8) 3 3_655 ?
O1 Rb1' O3 120.4(9) 3 3_655 ?
Rb1' Rb1' O3 60.0(9) 3_655 3_655 ?
O3 Rb1' O3 122.1(9) . 3_655 ?
Rb2' Rb2 Rb2' 179.4(11) . 1_655 ?
Rb2' Rb2 O5 45.8(6) . . ?
Rb2' Rb2 O5 134.2(6) 1_655 . ?
Rb2' Rb2 O1 133.9(6) . 1_655 ?
Rb2' Rb2 O1 45.8(5) 1_655 1_655 ?
O5 Rb2 O1 152.9(3) . 1_655 ?
Rb2' Rb2 O5 136.6(6) . 1_655 ?
Rb2' Rb2 O5 43.3(6) 1_655 1_655 ?
O5 Rb2 O5 90.8(3) . 1_655 ?
O1 Rb2 O5 83.3(3) 1_655 1_655 ?
Rb2' Rb2 O3 75.3(6) . 3_655 ?
Rb2' Rb2 O3 105.1(6) 1_655 3_655 ?
O5 Rb2 O3 110.3(3) . 3_655 ?
O1 Rb2 O3 92.4(3) 1_655 3_655 ?
O5 Rb2 O3 133.7(3) 1_655 3_655 ?
Rb2' Rb2 O1 44.2(6) . . ?
Rb2' Rb2 O1 135.5(5) 1_655 . ?
O5 Rb2 O1 84.0(3) . . ?
O1 Rb2 O1 89.7(3) 1_655 . ?
O5 Rb2 O1 153.8(3) 1_655 . ?
O3 Rb2 O1 71.6(3) 3_655 . ?
Rb2' Rb2 O6 89.7(6) . . ?
Rb2' Rb2 O6 90.8(5) 1_655 . ?
O5 Rb2 O6 68.4(3) . . ?
O1 Rb2 O6 132.5(3) 1_655 . ?
O5 Rb2 O6 70.2(3) 1_655 . ?
O3 Rb2 O6 79.9(3) 3_655 . ?
O1 Rb2 O6 130.0(3) . . ?
Rb2' Rb2 C7 116.8(6) . 1_655 ?
Rb2' Rb2 C7 62.8(5) 1_655 1_655 ?
O5 Rb2 C7 139.2(3) . 1_655 ?
O1 Rb2 C7 18.3(3) 1_655 1_655 ?
O5 Rb2 C7 95.3(3) 1_655 1_655 ?
O3 Rb2 C7 94.0(3) 3_655 1_655 ?
O1 Rb2 C7 73.0(3) . 1_655 ?
O6 Rb2 C7 150.6(3) . 1_655 ?
Rb2' Rb2 C8 122.6(6) . 1_655 ?
Rb2' Rb2 C8 57.5(5) 1_655 1_655 ?
O5 Rb2 C8 77.5(3) . 1_655 ?
O1 Rb2 C8 99.9(3) 1_655 1_655 ?
O5 Rb2 C8 16.9(3) 1_655 1_655 ?
O3 Rb2 C8 129.1(3) 3_655 1_655 ?
O1 Rb2 C8 156.2(3) . 1_655 ?
O6 Rb2 C8 55.6(3) . 1_655 ?
C7 Rb2 C8 112.2(3) 1_655 1_655 ?
Rb2' Rb2 C8 56.2(6) . . ?
Rb2' Rb2 C8 123.9(6) 1_655 . ?
O5 Rb2 C8 14.1(3) . . ?
O1 Rb2 C8 157.6(3) 1_655 . ?
O5 Rb2 C8 81.2(3) 1_655 . ?
O3 Rb2 C8 110.0(3) 3_655 . ?
O1 Rb2 C8 97.2(3) . . ?
O6 Rb2 C8 55.5(3) . . ?
C7 Rb2 C8 150.0(3) 1_655 . ?
C8 Rb2 C8 66.3(2) 1_655 . ?
Rb2' Rb2 Rb2 0.3(6) . 1_455 ?
Rb2' Rb2 Rb2 179.7(5) 1_655 1_455 ?
O5 Rb2 Rb2 45.8(2) . 1_455 ?
O1 Rb2 Rb2 134.0(2) 1_655 1_455 ?
O5 Rb2 Rb2 136.6(2) 1_655 1_455 ?
O3 Rb2 Rb2 75.1(3) 3_655 1_455 ?
O1 Rb2 Rb2 44.4(2) . 1_455 ?
O6 Rb2 Rb2 89.4(2) . 1_455 ?
C7 Rb2 Rb2 117.0(2) 1_655 1_455 ?
C8 Rb2 Rb2 122.5(2) 1_655 1_455 ?
C8 Rb2 Rb2 56.2(3) . 1_455 ?
O5 Rb2' Rb2 88.7(9) . . ?
O5 Rb2' O1 142.4(11) . . ?
Rb2 Rb2' O1 92.8(9) . . ?
O5 Rb2' Rb2 91.4(9) . 1_455 ?
Rb2 Rb2' Rb2 179.4(11) . 1_455 ?
O1 Rb2' Rb2 87.5(8) . 1_455 ?
O5 Rb2' O3 132.9(9) . 3_655 ?
Rb2 Rb2' O3 66.0(6) . 3_655 ?
O1 Rb2' O3 80.7(7) . 3_655 ?
Rb2 Rb2' O3 113.6(8) 1_455 3_655 ?
O5 Rb2' C8 12.5(5) . . ?
Rb2 Rb2' C8 91.6(7) . . ?
O1 Rb2' C8 154.2(9) . . ?
Rb2 Rb2' C8 88.3(7) 1_455 . ?
O3 Rb2' C8 124.0(7) 3_655 . ?
O5 Rb2' C7 133.8(9) . . ?
Rb2 Rb2' C7 98.4(7) . . ?
O1 Rb2' C7 10.0(4) . . ?
Rb2 Rb2' C7 82.0(6) 1_455 . ?
O3 Rb2' C7 90.5(6) 3_655 . ?
C8 Rb2' C7 144.9(7) . . ?
O5 Rb2' C4 96.2(7) . 3_655 ?
Rb2 Rb2' C4 93.6(7) . 3_655 ?
O1 Rb2' C4 121.1(8) . 3_655 ?
Rb2 Rb2' C4 85.8(6) 1_455 3_655 ?
O3 Rb2' C4 50.1(4) 3_655 3_655 ?
C8 Rb2' C4 83.8(5) . 3_655 ?
C7 Rb2' C4 128.5(7) . 3_655 ?
O5 Rb2' C6 91.4(7) . 2_655 ?
Rb2 Rb2' C6 90.4(7) . 2_655 ?
O1 Rb2' C6 51.1(5) . 2_655 ?
Rb2 Rb2' C6 90.2(7) 1_455 2_655 ?
O3 Rb2' C6 125.7(6) 3_655 2_655 ?
C8 Rb2' C6 103.5(6) . 2_655 ?
C7 Rb2' C6 43.3(4) . 2_655 ?
C4 Rb2' C6 171.5(7) 3_655 2_655 ?
O5 Rb2' O6 64.2(6) . . ?
Rb2 Rb2' O6 56.4(5) . . ?
O1 Rb2' O6 143.0(9) . . ?
Rb2 Rb2' O6 123.1(7) 1_455 . ?
O3 Rb2' O6 68.8(5) 3_655 . ?
C8 Rb2' O6 56.7(4) . . ?
C7 Rb2' O6 151.8(7) . . ?
C4 Rb2' O6 50.8(4) 3_655 . ?
C6 Rb2' O6 136.9(7) 2_655 . ?
O5 Rb2' Rb2' 91.4(7) . 1_455 ?
Rb2 Rb2' Rb2' 179.7(6) . 1_455 ?
O1 Rb2' Rb2' 87.3(7) . 1_455 ?
Rb2 Rb2' Rb2' 0.3(5) 1_455 1_455 ?
O3 Rb2' Rb2' 113.8(5) 3_655 1_455 ?
C8 Rb2' Rb2' 88.4(5) . 1_455 ?
C7 Rb2' Rb2' 81.8(5) . 1_455 ?
C4 Rb2' Rb2' 86.1(4) 3_655 1_455 ?
C6 Rb2' Rb2' 89.9(4) 2_655 1_455 ?
O6 Rb2' Rb2' 123.4(4) . 1_455 ?
O5 Rb2' Rb2' 88.6(7) . 1_655 ?
Rb2 Rb2' Rb2' 0.3(5) . 1_655 ?
O1 Rb2' Rb2' 92.7(7) . 1_655 ?
Rb2 Rb2' Rb2' 179.7(6) 1_455 1_655 ?
O3 Rb2' Rb2' 66.2(5) 3_655 1_655 ?
C8 Rb2' Rb2' 91.6(5) . 1_655 ?
C7 Rb2' Rb2' 98.2(5) . 1_655 ?
C4 Rb2' Rb2' 93.9(4) 3_655 1_655 ?
C6 Rb2' Rb2' 90.1(4) 2_655 1_655 ?
O6 Rb2' Rb2' 56.6(4) . 1_655 ?
Rb2' Rb2' Rb2' 180.0000(10) 1_455 1_655 ?
C7 O1 Rb2' 153.4(11) . . ?
C7 O1 Rb1' 81.1(10) . . ?
Rb2' O1 Rb1' 120.2(9) . . ?
C7 O1 Rb2 115.6(9) . 1_455 ?
Rb2' O1 Rb2 46.7(6) . 1_455 ?
Rb1' O1 Rb2 105.9(7) . 1_455 ?
C7 O1 Rb2 145.7(10) . . ?
Rb2' O1 Rb2 43.0(6) . . ?
Rb1' O1 Rb2 115.5(6) . . ?
Rb2 O1 Rb2 89.7(3) 1_455 . ?
C7 O1 Rb1' 76.3(10) . 3 ?
Rb2' O1 Rb1' 118.9(9) . 3 ?
Rb1' O1 Rb1' 17.3(11) . 3 ?
Rb2 O1 Rb1' 92.8(6) 1_455 3 ?
Rb2 O1 Rb1' 127.9(6) . 3 ?
C7 O1 Rb1 90.6(8) . . ?
Rb2' O1 Rb1 115.9(7) . . ?
Rb1' O1 Rb1 31.9(6) . . ?
Rb2 O1 Rb1 128.4(3) 1_455 . ?
Rb2 O1 Rb1 90.8(3) . . ?
Rb1' O1 Rb1 49.1(5) 3 . ?
C7 O2 Rb1' 102.0(11) . . ?
C7 O2 Rb1' 106.4(11) . 3 ?
Rb1' O2 Rb1' 22.0(14) . 3 ?
C7 O2 Rb1 91.9(8) . . ?
Rb1' O2 Rb1 32.3(7) . . ?
Rb1' O2 Rb1 54.3(7) 3 . ?
C7 O2 Rb1 109.3(9) . 1_455 ?
Rb1' O2 Rb1 51.7(7) . 1_455 ?
Rb1' O2 Rb1 29.7(7) 3 1_455 ?
Rb1 O2 Rb1 84.1(2) . 1_455 ?
C9 O3 Rb1 126.9(9) . . ?
C9 O3 Rb2 138.5(10) . 3_655 ?
Rb1 O3 Rb2 93.2(3) . 3_655 ?
C9 O3 Rb2' 133.5(11) . 3_655 ?
Rb1 O3 Rb2' 92.0(4) . 3_655 ?
Rb2 O3 Rb2' 38.7(4) 3_655 3_655 ?
C9 O3 Rb1' 123.7(11) . . ?
Rb1 O3 Rb1' 29.3(5) . . ?
Rb2 O3 Rb1' 85.2(6) 3_655 . ?
Rb2' O3 Rb1' 102.8(6) 3_655 . ?
C9 O3 Rb1' 119.9(11) . 3_655 ?
Rb1 O3 Rb1' 28.6(5) . 3_655 ?
Rb2 O3 Rb1' 100.3(6) 3_655 3_655 ?
Rb2' O3 Rb1' 81.0(6) 3_655 3_655 ?
Rb1' O3 Rb1' 57.9(9) . 3_655 ?
C8 O5 Rb2' 146.9(12) . . ?
C8 O5 Rb2 132.6(10) . . ?
Rb2' O5 Rb2 45.6(6) . . ?
C8 O5 Rb2 119.7(11) . 1_455 ?
Rb2' O5 Rb2 45.3(7) . 1_455 ?
Rb2 O5 Rb2 90.8(3) . 1_455 ?
C8 O6 Rb2 149.2(9) 3_665 . ?
C8 O6 Rb2' 157.8(10) 3_665 . ?
Rb2 O6 Rb2' 34.0(3) . . ?
C6 C1 C2 120.3(11) 2_655 2_545 ?
C6 C1 C7 119.0(12) 2_655 . ?
C2 C1 C7 120.7(13) 2_545 . ?
C3 C2 C1 119.7(12) . 2 ?
C4 C3 C2 119.0(12) 1_465 . ?
C4 C3 C8 121.6(11) 1_465 . ?
C2 C3 C8 119.3(12) . . ?
C3 C4 C5 122.1(12) 1_645 . ?
C3 C4 Rb2' 123.4(9) 1_645 3_655 ?
C5 C4 Rb2' 113.7(9) . 3_655 ?
C4 C5 C6 119.3(12) . . ?
C4 C5 C9 119.4(11) . . ?
C6 C5 C9 121.2(12) . . ?
C1 C6 C5 119.3(12) 2_645 . ?
C1 C6 Rb2' 90.1(8) 2_645 2_645 ?
C5 C6 Rb2' 145.2(9) . 2_645 ?
O1 C7 O2 125.8(13) . . ?
O1 C7 C1 116.6(13) . . ?
O2 C7 C1 117.5(12) . . ?
O1 C7 Rb1' 73.4(9) . . ?
O2 C7 Rb1' 52.4(9) . . ?
C1 C7 Rb1' 169.8(12) . . ?
O1 C7 Rb1' 79.3(10) . 3 ?
O2 C7 Rb1' 49.2(9) . 3 ?
C1 C7 Rb1' 156.4(12) . 3 ?
Rb1' C7 Rb1' 17.5(11) . 3 ?
O1 C7 Rb2' 16.6(7) . . ?
O2 C7 Rb2' 138.8(10) . . ?
C1 C7 Rb2' 102.4(9) . . ?
Rb1' C7 Rb2' 87.3(8) . . ?
Rb1' C7 Rb2' 89.9(7) 3 . ?
O1 C7 Rb1 67.0(7) . . ?
O2 C7 Rb1 65.4(7) . . ?
C1 C7 Rb1 153.5(10) . . ?
Rb1' C7 Rb1 29.4(6) . . ?
Rb1' C7 Rb1 46.8(6) 3 . ?
Rb2' C7 Rb1 83.6(5) . . ?
O1 C7 Rb2 46.1(7) . 1_455 ?
O2 C7 Rb2 122.8(10) . 1_455 ?
C1 C7 Rb2 98.3(8) . 1_455 ?
Rb1' C7 Rb2 87.9(7) . 1_455 ?
Rb1' C7 Rb2 80.1(6) 3 1_455 ?
Rb2' C7 Rb2 35.2(4) . 1_455 ?
Rb1 C7 Rb2 101.0(4) . 1_455 ?
O1 C7 Rb1 88.8(9) . 1_455 ?
O2 C7 Rb1 52.2(7) . 1_455 ?
C1 C7 Rb1 133.3(9) . 1_455 ?
Rb1' C7 Rb1 41.6(6) . 1_455 ?
Rb1' C7 Rb1 24.1(5) 3 1_455 ?
Rb2' C7 Rb1 93.4(5) . 1_455 ?
Rb1 C7 Rb1 71.0(3) . 1_455 ?
Rb2 C7 Rb1 70.7(3) 1_455 1_455 ?
O5 C8 O6 124.4(13) . 3_665 ?
O5 C8 C3 120.2(13) . . ?
O6 C8 C3 115.3(12) 3_665 . ?
O5 C8 Rb2' 20.5(8) . . ?
O6 C8 Rb2' 108.8(9) 3_665 . ?
C3 C8 Rb2' 132.9(10) . . ?
O5 C8 Rb2 43.4(8) . 1_455 ?
O6 C8 Rb2 118.6(9) 3_665 1_455 ?
C3 C8 Rb2 106.0(9) . 1_455 ?
Rb2' C8 Rb2 34.2(4) . 1_455 ?
O5 C8 Rb2 33.3(8) . . ?
O6 C8 Rb2 93.9(8) 3_665 . ?
C3 C8 Rb2 148.5(9) . . ?
Rb2' C8 Rb2 32.2(4) . . ?
Rb2 C8 Rb2 66.3(2) 1_455 . ?
O3 C9 O4 122.9(14) . . ?
O3 C9 C5 123.1(13) . . ?
O4 C9 C5 114.0(11) . . ?
O3 C9 Rb1 38.2(7) . . ?
O4 C9 Rb1 90.7(8) . . ?
C5 C9 Rb1 147.9(10) . . ?

#===END