# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004



data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Thomas Rauchfuss'
'Matthew L. Kuhlman'
'Haijun Yao'

_publ_contact_author_name        'Prof Thomas Rauchfuss'
_publ_contact_author_address     
;
Department of Chemistry
University of Illinois at Urbana-Champaign
A328 CLSL, 600 South Mathews Ave.
Urbana
Illinois
6180
UNITED STATES OF AMERICA
;

_publ_contact_author_email       RAUCHFUZ@UIUC.EDU

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Synthesis and Characterization of the Hexagonal
Prismatic Cage {THFÌ[PhB(CN)3]6[Cp*Rh]6}6+
;

_publ_section_references         
;

Farrugia, L.J. (1999).  J. Appl. Cryst. 32, 837-838.

Spek, A. L. and van der Sluis, P. (1990).  Acta Cryst. A46, 194-201.

Sheldrick, G.M. (2001).  SHELX-97-2.  Program for crystal structure solution
and refinement.  Institute fur anorg chemie, Gottingen, Germany.

Bruker AXS, Inc.  (2001).  Madison, Wisconsin, USA.
;

_publ_section_figure_captions    
;
Figure 1.  SHELXTL (Bruker, 2000) plot showing 35% probability ellipsoids
for non-H atoms and circles of arbitrary size for H atoms; anion and solvate
positions were omitted for clarity.
;

_publ_section_exptl_prep         
;
Crystals were grown by vapor diffusion of tetrahydrofuran into a nitromethane
solution.  Four frame series were filtered for statistical outliers then
corrected for absorption by integration using SHELXTL/XPREP (Bruker, 2001)
before using SAINT/SADABS (Bruker, 2001) to sort, merge, and scale the
combined data.  A series of identical frames was collected twice during the
experiment to monitor decay.  No decay correction was applied.
;

_publ_section_exptl_refinement   
;
Systematic conditions suggested the ambiguous space group.   Structure
was solved by direct methods (Sheldrick, 2001).  Anion and solvate positions
were severely disordered.  Phenyl rings on the host cation were disordered
over four sites.  Anion and solvate molecules were refined as idealized
groups using an effective standard deviation of 0.01\%A for bond lengths
and 0.02\%A for bond angles.  Disordered phenyl rings were refined as rigid
idealized groups.  Crystallographic -3m symmetry was imposed on the host
cation and the disordered THF solvate molecules.  Inversion or 3-fold
symmetry was imposed on disordered anions.  A structural model consisting
of the host cation, three disordered anion sites and two disordered THF
solvate molecules was developed; however, positions for the idealized
anion and solvate molecules were poorly determined.  This model convergered
with wR2 = 0.225 and R1 = 0.068 for 311 parameters with 366 restraints
against 2741 data.  Since positions for the anion and solvate molecules were
poorly determined a second structural model was refined with contributions
from the anion and solvate molecules removed from the diffraction data using
the bypass procedure in PLATON (Spek, 1990).  No positions for the host
network differed by more than two su's between these two refined models.  The
electron count from the "squeeze" model converged in good agreement with the
number of solvate molecules predicted by the complete refinement.  The
"squeeze" data are reported here.  H atoms were included as riding idealized
contributors.  Methyl H atom U's were assigned as 1.5 times Ueq of adjacent
atom; remaining H atom U's were assigned as 1.2 times adjacent Ueq.  The
space group choice was confirmed by successful convergence of the full-matrix
least-squares refinement on F^2^ (Sheldrick, 2001).  The highest peaks in
the final difference Fourier map were in the vicinity of the disordered phenyl
ring and atom Rh1; the final map had no other significant features.  A final
analysis of variance between observed and calculated structure factors showed
dependence on resolution.
;

_publ_section_acknowledgements   
;
The Materials Chemistry Laboratory at the Univeristy of Illinois was
supported in part by Grant No. NSF CHE 95-03145 from the National Science
Foundation.
;

data_p44ym
_database_code_depnum_ccdc_archive 'CCDC 230644'

_audit_creation_method           SHELXL-97
_audit_update_record             
;
2003-12-03   text and data added, mlk
;

_chemical_name_systematic        
;
?
;

_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C114 H120 B6 N18 Rh6, 6(C F3 O3 S), 2(C4 H8 O)
;
_chemical_formula_sum            'C128 H136 B6 F18 N18 O20 Rh6 S6'
_chemical_formula_structural     ?
_chemical_formula_weight         3463.23

_chemical_absolute_configuration .
_chemical_formula_analytical     ?
_chemical_compound_source        ?

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   'P -3 m 1  '
_symmetry_space_group_name_Hall  '-P 3 2" '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'-x, -x+y, -z'
'x-y, -y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'x, x-y, z'
'-x+y, y, z'

_cell_length_a                   18.325(6)
_cell_length_b                   18.325(6)
_cell_length_c                   13.871(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     4034(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    968
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      24.4
_exptl_crystal_description       tabular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1748
_exptl_crystal_id                p44ym

_exptl_crystal_preparation       
;
The data crystal was mounted using oil (Parantone-N, Exxon) to a
0.3 mm cryo-loop (Hampton Research) with the (-1 0 0) scattering planes
roughly normal to the spindle axis.
;

_exptl_absorpt_coefficient_mu    0.760
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.7957
_exptl_absorpt_correction_T_max  0.9032
_exptl_absorpt_process_details   '(Bruker, 2001)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  p44ym
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_device       'Siemens Platform/CCD'
_diffrn_measurement_method       'profile data from \w scans'

_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         208
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  305

_diffrn_standards_decay_%        0.2
_diffrn_reflns_number            31922

_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.44
_reflns_number_total             2741
_reflns_number_gt                2144
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART V5.625 (Bruker, 2001)'
_computing_cell_refinement       'SAINT V6.22 (Bruker, 2001)'
_computing_data_reduction        'SAINT V6.22 (Bruker, 2001)'
_computing_structure_solution    'SHELXTL V6.10 (Bruker, 2001)'
_computing_structure_refinement  'SHELXTL V6.10 (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL V6.10 (Bruker, 2001)'
_computing_publication_material  'CIFTAB (Sheldrick, 2001)'

_refine_special_details          
;
?
;

_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^)+(0.0961P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2741
_refine_ls_number_parameters     176
_refine_ls_number_restraints     163
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.015
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

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
Rh1 Rh -0.155535(12) 0.155535(12) 0.19848(3) 0.03933(19) Uani 1 2 d S . .
N1 N -0.0277(2) 0.1938(2) 0.1840(2) 0.0459(7) Uani 1 1 d . . .
N2 N 0.15586(13) 0.3117(3) -0.0477(3) 0.0423(10) Uani 1 2 d S . .
C1 C 0.0420(3) 0.2273(3) 0.1693(2) 0.0447(9) Uani 1 1 d . A .
C2 C 0.14978(15) 0.2996(3) 0.0334(4) 0.0424(12) Uani 1 2 d S A .
C11 C -0.2226(2) 0.2226(2) 0.2135(5) 0.087(2) Uani 1 2 d S . .
C12 C -0.1419(4) 0.2683(3) 0.2581(4) 0.0732(14) Uani 1 1 d . . .
C13 C -0.1393(3) 0.2176(3) 0.3342(3) 0.0654(12) Uani 1 1 d . . .
C14 C -0.2526(2) 0.2526(2) 0.1307(6) 0.138(4) Uani 1 2 d S . .
H14A H -0.3108 0.2086 0.1149 0.207 Uiso 0.50 1 d PR . .
H14B H -0.2166 0.2623 0.0747 0.207 Uiso 0.50 1 d PR . .
H14C H -0.2522 0.3044 0.1480 0.207 Uiso 0.50 1 d PR . .
C15 C -0.0741(5) 0.3544(4) 0.2362(5) 0.134(3) Uani 1 1 d . . .
H15A H -0.0908 0.3759 0.1808 0.202 Uiso 1 1 d R . .
H15B H -0.0223 0.3537 0.2208 0.202 Uiso 1 1 d R . .
H15C H -0.0644 0.3908 0.2921 0.202 Uiso 1 1 d R . .
C16 C -0.0684(4) 0.2402(4) 0.4027(4) 0.107(2) Uani 1 1 d . . .
H16A H -0.0220 0.2969 0.3880 0.160 Uiso 1 1 d R . .
H16B H -0.0879 0.2389 0.4688 0.160 Uiso 1 1 d R . .
H16C H -0.0487 0.1996 0.3964 0.160 Uiso 1 1 d R . .
B1 B 0.1417(2) 0.2834(4) 0.1478(4) 0.0441(13) Uani 1 2 d SD . .
C21 C 0.1932(8) 0.3674(5) 0.2103(9) 0.049(3) Uani 0.287(9) 1 d PGDU A 1
C22 C 0.2710(9) 0.4290(7) 0.1753(7) 0.069(3) Uani 0.287(9) 1 d PGU A 1
H22 H 0.2899 0.4223 0.1139 0.082 Uiso 0.287(9) 1 d PG A 1
C23 C 0.3212(8) 0.5004(7) 0.2301(9) 0.080(4) Uani 0.287(9) 1 d PGU A 1
H23 H 0.3744 0.5424 0.2062 0.097 Uiso 0.287(9) 1 d PG A 1
C24 C 0.2936(8) 0.5102(6) 0.3199(8) 0.082(4) Uani 0.287(9) 1 d PGU A 1
H24 H 0.3279 0.5590 0.3574 0.098 Uiso 0.287(9) 1 d PG A 1
C25 C 0.2158(8) 0.4486(8) 0.3549(8) 0.073(3) Uani 0.287(9) 1 d PGU A 1
H25 H 0.1969 0.4553 0.4163 0.088 Uiso 0.287(9) 1 d PG A 1
C26 C 0.1656(7) 0.3773(7) 0.3001(10) 0.059(3) Uani 0.287(9) 1 d PGU A 1
H26 H 0.1124 0.3352 0.3240 0.070 Uiso 0.287(9) 1 d PG A 1
C31 C 0.1792(18) 0.3676(6) 0.2096(10) 0.050(3) Uani 0.213(9) 1 d PGDU A 2
C32 C 0.2057(14) 0.4460(9) 0.1680(7) 0.062(4) Uani 0.213(9) 1 d PGU A 2
H32 H 0.2013 0.4506 0.1003 0.074 Uiso 0.213(9) 1 d PG A 2
C33 C 0.2388(16) 0.5176(6) 0.2256(9) 0.073(4) Uani 0.213(9) 1 d PGU A 2
H33 H 0.2570 0.5712 0.1972 0.088 Uiso 0.213(9) 1 d PG A 2
C34 C 0.2453(17) 0.5109(6) 0.3246(9) 0.071(4) Uani 0.213(9) 1 d PGU A 2
H34 H 0.2679 0.5599 0.3639 0.086 Uiso 0.213(9) 1 d PG A 2
C35 C 0.219(2) 0.4326(9) 0.3662(8) 0.072(3) Uani 0.213(9) 1 d SPGU A 2
H35 H 0.2232 0.4280 0.4339 0.087 Uiso 0.213(9) 1 d PG A 2
C36 C 0.186(3) 0.3609(7) 0.3086(11) 0.056(3) Uani 0.213(9) 1 d PGU A 2
H36 H 0.1675 0.3073 0.3370 0.067 Uiso 0.213(9) 1 d PG A 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
Rh1 0.0421(2) 0.0421(2) 0.0353(3) -0.00231(8) 0.00231(8) 0.0221(2)
N1 0.0427(19) 0.0545(19) 0.0379(16) -0.0050(14) -0.0034(14) 0.0224(16)
N2 0.0414(18) 0.046(3) 0.041(3) -0.0018(19) -0.0009(10) 0.0229(13)
C1 0.053(2) 0.058(2) 0.0304(18) -0.0101(16) -0.0046(17) 0.034(2)
C2 0.041(2) 0.046(3) 0.042(3) -0.006(2) -0.0029(12) 0.0232(15)
C11 0.125(6) 0.125(6) 0.069(5) -0.0080(16) 0.0080(16) 0.106(6)
C12 0.108(4) 0.056(3) 0.068(3) -0.008(2) 0.015(3) 0.050(3)
C13 0.082(3) 0.073(3) 0.046(2) -0.017(2) 0.005(2) 0.043(2)
C14 0.200(10) 0.200(10) 0.113(7) 0.008(2) -0.008(2) 0.174(10)
C15 0.212(8) 0.054(4) 0.113(5) -0.001(4) 0.029(5) 0.049(4)
C16 0.107(5) 0.138(5) 0.063(3) -0.045(3) -0.024(3) 0.052(4)
B1 0.043(2) 0.052(3) 0.041(3) -0.001(3) -0.0007(14) 0.0258(17)
C21 0.058(6) 0.055(4) 0.046(4) -0.006(3) -0.001(5) 0.036(5)
C22 0.067(6) 0.065(5) 0.064(5) -0.013(4) -0.004(5) 0.026(5)
C23 0.078(7) 0.068(6) 0.081(6) -0.027(5) -0.001(5) 0.025(6)
C24 0.080(6) 0.071(5) 0.076(5) -0.027(4) -0.003(5) 0.024(5)
C25 0.075(6) 0.071(5) 0.060(4) -0.023(4) -0.001(6) 0.027(6)
C26 0.065(6) 0.059(5) 0.053(4) -0.011(4) 0.003(5) 0.032(5)
C31 0.058(6) 0.055(4) 0.048(4) -0.007(4) -0.001(6) 0.037(6)
C32 0.064(7) 0.061(5) 0.060(5) -0.010(4) -0.004(5) 0.031(5)
C33 0.076(7) 0.061(5) 0.076(5) -0.020(5) -0.003(5) 0.029(5)
C34 0.072(7) 0.067(5) 0.070(5) -0.026(5) -0.005(6) 0.032(6)
C35 0.074(6) 0.072(5) 0.059(5) -0.019(4) -0.002(6) 0.027(6)
C36 0.059(6) 0.063(5) 0.052(4) -0.011(4) 0.001(6) 0.036(6)

_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
Rh1 N1 2.092(3) 10 ?
Rh1 N1 2.092(3) . ?
Rh1 N2 2.092(5) 9 ?
Rh1 C12 2.120(4) . ?
Rh1 C12 2.120(4) 10 ?
Rh1 C11 2.139(6) . ?
Rh1 C13 2.142(4) . ?
Rh1 C13 2.142(4) 10 ?
N1 C1 1.125(5) . ?
N2 C2 1.141(7) . ?
N2 Rh1 2.092(5) 8 ?
C1 B1 1.614(6) . ?
C2 B1 1.607(8) . ?
C11 C12 1.426(7) . ?
C11 C12 1.426(7) 10 ?
C11 C14 1.492(10) . ?
C12 C13 1.423(7) . ?
C12 C15 1.471(8) . ?
C13 C13 1.434(10) 10 ?
C13 C16 1.491(7) . ?
C14 H14A 0.9879 . ?
C14 H14B 0.9762 . ?
C14 H14C 0.9761 . ?
C15 H15A 0.9799 . ?
C15 H15B 0.9802 . ?
C15 H15C 0.9799 . ?
C16 H16A 0.9801 . ?
C16 H16B 0.9798 . ?
C16 H16C 0.9801 . ?
B1 C31 1.591(9) . ?
B1 C21 1.600(8) . ?
B1 C1 1.614(6) 12 ?
C21 C26 1.3899 . ?
C21 C22 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 C24 1.3899 . ?
C23 H23 0.9500 . ?
C24 C25 1.3899 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9502 . ?
C26 H26 0.9500 . ?
C31 C36 1.3900 . ?
C31 C32 1.3901 . ?
C32 C33 1.3900 . ?
C32 H32 0.9500 . ?
C33 C34 1.3900 . ?
C33 H33 0.9499 . ?
C34 C35 1.3901 . ?
C34 H34 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35 0.9499 . ?
C36 H36 0.9499 . ?

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
N1 Rh1 N1 93.31(18) 10 . ?
N1 Rh1 N2 84.68(11) 10 9 ?
N1 Rh1 N2 84.68(11) . 9 ?
N1 Rh1 C12 159.80(16) 10 . ?
N1 Rh1 C12 98.29(17) . . ?
N2 Rh1 C12 112.73(17) 9 . ?
N1 Rh1 C12 98.29(17) 10 10 ?
N1 Rh1 C12 159.80(16) . 10 ?
N2 Rh1 C12 112.73(17) 9 10 ?
C12 Rh1 C12 66.2(3) . 10 ?
N1 Rh1 C11 133.29(9) 10 . ?
N1 Rh1 C11 133.29(9) . . ?
N2 Rh1 C11 95.3(2) 9 . ?
C12 Rh1 C11 39.12(17) . . ?
C12 Rh1 C11 39.12(17) 10 . ?
N1 Rh1 C13 123.95(16) 10 . ?
N1 Rh1 C13 94.10(15) . . ?
N2 Rh1 C13 151.33(16) 9 . ?
C12 Rh1 C13 39.00(19) . . ?
C12 Rh1 C13 65.70(19) 10 . ?
C11 Rh1 C13 65.0(2) . . ?
N1 Rh1 C13 94.10(15) 10 10 ?
N1 Rh1 C13 123.95(16) . 10 ?
N2 Rh1 C13 151.33(16) 9 10 ?
C12 Rh1 C13 65.70(19) . 10 ?
C12 Rh1 C13 39.00(19) 10 10 ?
C11 Rh1 C13 65.0(2) . 10 ?
C13 Rh1 C13 39.1(3) . 10 ?
C1 N1 Rh1 167.4(3) . . ?
C2 N2 Rh1 170.0(4) . 8 ?
N1 C1 B1 174.7(4) . . ?
N2 C2 B1 179.5(6) . . ?
C12 C11 C12 108.6(6) . 10 ?
C12 C11 C14 125.7(3) . . ?
C12 C11 C14 125.7(3) 10 . ?
C12 C11 Rh1 69.7(3) . . ?
C12 C11 Rh1 69.7(3) 10 . ?
C14 C11 Rh1 124.1(5) . . ?
C13 C12 C11 107.6(5) . . ?
C13 C12 C15 124.6(6) . . ?
C11 C12 C15 127.6(6) . . ?
C13 C12 Rh1 71.3(2) . . ?
C11 C12 Rh1 71.2(3) . . ?
C15 C12 Rh1 126.1(4) . . ?
C12 C13 C13 108.0(3) . 10 ?
C12 C13 C16 126.9(5) . . ?
C13 C13 C16 125.1(3) 10 . ?
C12 C13 Rh1 69.7(2) . . ?
C13 C13 Rh1 70.44(14) 10 . ?
C16 C13 Rh1 125.3(3) . . ?
C11 C14 H14A 108.5 . . ?
C11 C14 H14B 109.8 . . ?
H14A C14 H14B 109.1 . . ?
C11 C14 H14C 110.2 . . ?
H14A C14 H14C 109.1 . . ?
H14B C14 H14C 110.1 . . ?
C12 C15 H15A 109.2 . . ?
C12 C15 H15B 109.6 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.6 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.6 . . ?
C13 C16 H16B 109.4 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.4 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C31 B1 C2 113.4(7) . . ?
C21 B1 C2 113.7(6) . . ?
C31 B1 C1 108.7(11) . . ?
C21 B1 C1 116.6(6) . . ?
C2 B1 C1 105.7(3) . . ?
C31 B1 C1 114.0(11) . 12 ?
C21 B1 C1 105.7(6) . 12 ?
C2 B1 C1 105.7(3) . 12 ?
C1 B1 C1 108.8(4) . 12 ?
C26 C21 C22 120.0 . . ?
C26 C21 B1 122.2(8) . . ?
C22 C21 B1 117.6(8) . . ?
C23 C22 C21 120.0 . . ?
C24 C23 C22 120.0 . . ?
C25 C24 C23 120.0 . . ?
C24 C25 C26 120.0 . . ?
C21 C26 C25 120.0 . . ?
C36 C31 C32 120.0 . . ?
C36 C31 B1 117.5(10) . . ?
C32 C31 B1 122.5(10) . . ?
C33 C32 C31 120.0 . . ?
C33 C32 H32 120.0 . . ?
C31 C32 H32 120.0 . . ?
C32 C33 C34 120.0 . . ?
C32 C33 H33 120.0 . . ?
C34 C33 H33 120.0 . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34 120.0 . . ?
C35 C34 H34 120.0 . . ?
C36 C35 C34 120.0 . . ?
C36 C35 H35 120.0 . . ?
C34 C35 H35 120.0 . . ?
C35 C36 C31 120.0 . . ?
C35 C36 H36 120.0 . . ?
C31 C36 H36 120.0 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.44
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.087

#loop_
#_exptl_crystal_face_index_h
#_exptl_crystal_face_index_k
#_exptl_crystal_face_index_l
#_exptl_crystal_face_perp_dist
#0.00    0.00   -1.00    0.0700
#0.00    0.00    1.00    0.0700
#0.00   -1.00    0.00    0.0800
#1.00    1.00    0.00    0.1200
#-1.00    1.00    0.00    0.1800
#1.00   -1.00    0.00    0.1800
#_vrf_CHEMW03_p44ym
#;
#PROBLEM: ALERT: The ratio of given/expected molecular weight as
#RESPONSE: Since positions for the anion and solvate molecules were
#poorly determined a second structural model was refined with
#contributions from the anion and solvate molecules removed from the
#diffraction data using the bypass procedure in PLATON (Spek, 1990).
#The "squeeze" data are reported here.
#;
#_vrf_PLAT043_p44ym
#;
#PROBLEM: Check Reported Molecular Weight ................    3463.23
#RESPONSE: Since positions for the anion and solvate molecules were
#poorly determined a second structural model was refined with
#contributions from the anion and solvate molecules removed from the
#diffraction data using the bypass procedure in PLATON (Spek, 1990).
#The "squeeze" data are reported here.
#;
#_vrf_PLAT044_p44ym
#;
#PROBLEM: Calculated and Reported Dx Differ ..............          ?
#RESPONSE: Since positions for the anion and solvate molecules were
#poorly determined a second structural model was refined with
#contributions from the anion and solvate molecules removed from the
#diffraction data using the bypass procedure in PLATON (Spek, 1990).
#The "squeeze" data are reported here.
#;
#_vrf_PLAT051_p44ym
#;
#PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by .      16.11 Perc.
#RESPONSE: Since positions for the anion and solvate molecules were
#poorly determined a second structural model was refined with
#contributions from the anion and solvate molecules removed from the
#diffraction data using the bypass procedure in PLATON (Spek, 1990).
#The "squeeze" data are reported here.
#;
#_vrf_PLAT601_p44ym
#;
#PROBLEM: Structure Contains Solvent Accessible VOIDS of .     581.00 A**3
#RESPONSE: Since positions for the anion and solvate molecules were
#poorly determined a second structural model was refined with
#contributions from the anion and solvate molecules removed from the
#diffraction data using the bypass procedure in PLATON (Spek, 1990).
#The "squeeze" data are reported here.
#;

# end Validation Reply Form