# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_global

data_1
#TrackingRef 'Bi2PtI12.cif'

# start Validation Reply Form
_vrf_PLAT601_I                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS of . 460 A**3
RESPONSE: The unit cell contains a number of solvent acetone molecules, which
were not located but are included in the final formula as 3 molecules per
formula unit. See PLATON/SQUEEZE details below.

;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.333 0.667 0.167 459 91 ' '
2 0.000 0.000 0.500 456 90 ' '
3 -0.333 0.333 0.833 459 91 ' '
_platon_squeeze_details          
;
The solvent acetone molecules appeared to be highly disordered and it
was difficult to model their positions reliably. Therefore, the structure
was treated via PLATON/SQUEEZE (van der Sluis & Spek, 1990; Spek, 2003)
procedure to remove the contribution of the electron density in the solvent
regions from the intensity data, and the solvent-free model was emplyed from
the final refinement. The total potential solvent accessible void volume was
estimated to be 1376.2 Ang**3 and the electron count per unit cell was 271,
which were assigned to 9 acetone molecules per unit cell or 3 acetone
molecules per formula unit.
;


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C45 H90 Na4 O15, 2(Bi2 I12 Pt), 3(C3 H6 O)'
_chemical_formula_sum            'C54 H108 Bi4 I24 Na4 O18 Pt2'
_chemical_formula_weight         5409.06

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'
Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   'R 32'
_symmetry_space_group_name_Hall  'R 3 2"'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'

_cell_length_a                   13.9687(9)
_cell_length_b                   13.9687(9)
_cell_length_c                   57.126(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     9653.3(16)
_cell_formula_units_Z            3
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1658
_cell_measurement_theta_min      2.92
_cell_measurement_theta_max      26.25

_exptl_crystal_description       plate
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7140
_exptl_absorpt_coefficient_mu    13.427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1409
_exptl_absorpt_correction_T_max  0.8774
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_detector_area_resol_mean 25
_diffrn_standards_number         0
_diffrn_reflns_number            7335
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_sigmaI/netI    0.1053
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -71
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         26.37
_reflns_number_total             4335
_reflns_number_gt                3366
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'

_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^)+(0.1334P)^2^] 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    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.020(17)
_refine_ls_number_reflns         4335
_refine_ls_number_parameters     136
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0775
_refine_ls_wR_factor_ref         0.2043
_refine_ls_wR_factor_gt          0.1885
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.980
_refine_ls_shift/su_max          0.000
_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
Bi1 Bi 0.6667 0.3333 -0.03886(2) 0.0246(3) Uani 1 3 d S . .
Pt1 Pt 0.6667 0.3333 0.03616(2) 0.0192(3) Uani 1 3 d S . .
I1 I 0.51934(14) 0.13591(14) -0.06383(3) 0.0401(4) Uani 1 1 d . . .
Na1 Na 0.0000 0.0000 0.0301(2) 0.025(3) Uani 1 3 d S . .
O1 O 0.1198(15) 0.0000 0.0000 0.020(4) Uani 1 2 d S . .
Bi2 Bi 0.6667 0.3333 0.10795(2) 0.0303(4) Uani 1 3 d S . .
I2 I 0.61602(13) 0.15865(12) 0.00889(2) 0.0284(4) Uani 1 1 d . . .
Na2 Na 0.0000 0.0000 0.0873(2) 0.037(4) Uani 1 3 d S . .
O2 O 0.1197(12) 0.1318(13) 0.0585(3) 0.030(4) Uani 1 1 d . . .
I3 I 0.49299(12) 0.20735(13) 0.06356(2) 0.0306(4) Uani 1 1 d . . .
O3 O -0.014(2) 0.140(2) 0.1056(4) 0.077(7) Uani 1 1 d DU . .
I4 I 0.5067(2) 0.3709(2) 0.13205(4) 0.0629(6) Uani 1 1 d . . .
C11 C 0.208(2) 0.0000 0.0000 0.028(7) Uani 1 2 d S . .
C12 C 0.280(2) 0.032(2) 0.0210(5) 0.041(7) Uani 1 1 d . . .
H12A H 0.3534 0.0926 0.0170 0.062 Uiso 1 1 calc R . .
H12B H 0.2850 -0.0318 0.0265 0.062 Uiso 1 1 calc R . .
H12C H 0.2477 0.0557 0.0334 0.062 Uiso 1 1 calc R . .
C21 C 0.1948(18) 0.2274(17) 0.0592(4) 0.024(5) Uani 1 1 d . . .
C22 C 0.252(2) 0.298(2) 0.0382(5) 0.044(7) Uani 1 1 d . . .
H22A H 0.2347 0.2516 0.0243 0.066 Uiso 1 1 calc R . .
H22B H 0.3321 0.3385 0.0408 0.066 Uiso 1 1 calc R . .
H22C H 0.2265 0.3516 0.0358 0.066 Uiso 1 1 calc R . .
C23 C 0.248(3) 0.281(2) 0.0830(5) 0.047(7) Uani 1 1 d . . .
H23A H 0.2090 0.2289 0.0957 0.070 Uiso 1 1 calc R . .
H23B H 0.2422 0.3479 0.0853 0.070 Uiso 1 1 calc R . .
H23C H 0.3258 0.3014 0.0830 0.070 Uiso 1 1 calc R . .
C31 C -0.028(4) 0.188(3) 0.1216(5) 0.085(7) Uani 1 1 d DU . .
C32 C -0.003(4) 0.307(3) 0.1211(8) 0.085(7) Uani 1 1 d D . .
H32A H 0.0565 0.3499 0.1100 0.128 Uiso 1 1 calc R . .
H32B H 0.0186 0.3396 0.1368 0.128 Uiso 1 1 calc R . .
H32C H -0.0700 0.3087 0.1162 0.128 Uiso 1 1 calc R . .
C33 C -0.080(4) 0.124(3) 0.1440(6) 0.085(7) Uani 1 1 d D . .
H33A H -0.1519 0.1181 0.1464 0.128 Uiso 1 1 calc R . .
H33B H -0.0315 0.1621 0.1573 0.128 Uiso 1 1 calc R . .
H33C H -0.0895 0.0495 0.1426 0.128 Uiso 1 1 calc R . .

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
Bi1 0.0213(4) 0.0213(4) 0.0312(6) 0.000 0.000 0.0107(2)
Pt1 0.0171(4) 0.0171(4) 0.0233(6) 0.000 0.000 0.00856(19)
I1 0.0289(9) 0.0273(8) 0.0576(10) -0.0098(8) -0.0076(8) 0.0092(7)
Na1 0.028(5) 0.028(5) 0.018(6) 0.000 0.000 0.014(2)
O1 0.022(8) 0.011(9) 0.025(9) -0.009(8) -0.005(4) 0.005(5)
Bi2 0.0332(5) 0.0332(5) 0.0246(6) 0.000 0.000 0.0166(3)
I2 0.0342(8) 0.0208(7) 0.0313(7) -0.0027(6) -0.0025(6) 0.0145(7)
Na2 0.040(6) 0.040(6) 0.030(7) 0.000 0.000 0.020(3)
O2 0.016(8) 0.023(8) 0.048(9) 0.005(7) -0.009(7) 0.008(7)
I3 0.0201(7) 0.0298(8) 0.0333(7) 0.0002(6) 0.0023(6) 0.0061(6)
O3 0.069(10) 0.086(11) 0.082(10) -0.021(8) 0.014(8) 0.044(8)
I4 0.0626(14) 0.0791(16) 0.0598(12) -0.0027(11) 0.0134(10) 0.0451(13)
C11 0.010(9) 0.025(17) 0.054(19) 0.007(15) 0.003(8) 0.012(8)
C12 0.020(12) 0.059(18) 0.053(15) -0.009(14) -0.006(12) 0.026(13)
C21 0.022(11) 0.013(10) 0.039(11) 0.011(9) 0.006(9) 0.009(9)
C22 0.044(16) 0.037(15) 0.061(16) 0.013(13) 0.021(14) 0.028(14)
C23 0.049(17) 0.036(15) 0.055(15) -0.009(13) -0.009(14) 0.022(14)
C31 0.081(10) 0.090(11) 0.084(10) -0.001(8) 0.011(8) 0.043(8)
C32 0.081(10) 0.090(11) 0.084(10) -0.001(8) 0.011(8) 0.043(8)
C33 0.081(10) 0.090(11) 0.084(10) -0.001(8) 0.011(8) 0.043(8)

_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
Bi1 I1 2.8634(17) 2_655 ?
Bi1 I1 2.8634(17) . ?
Bi1 I1 2.8634(17) 3_665 ?
Bi1 I2 3.4883(18) . ?
Bi1 I2 3.4883(18) 2_655 ?
Bi1 I2 3.4883(18) 3_665 ?
Pt1 I2 2.6750(15) . ?
Pt1 I2 2.6750(15) 2_655 ?
Pt1 I2 2.6750(15) 3_665 ?
Pt1 I3 2.6763(16) 2_655 ?
Pt1 I3 2.6763(16) 3_665 ?
Pt1 I3 2.6763(16) . ?
Na1 O2 2.398(17) . ?
Na1 O2 2.398(17) 2 ?
Na1 O2 2.398(17) 3 ?
Na1 O1 2.399(17) . ?
Na1 O1 2.399(17) 3 ?
Na1 O1 2.399(17) 2 ?
O1 C11 1.23(4) . ?
O1 Na1 2.399(17) 4 ?
Bi2 I4 2.887(2) 2_655 ?
Bi2 I4 2.887(2) 3_665 ?
Bi2 I4 2.887(2) . ?
Bi2 I3 3.3383(17) . ?
Bi2 I3 3.3384(17) 2_655 ?
Bi2 I3 3.3384(17) 3_665 ?
Na2 O3 2.31(2) . ?
Na2 O3 2.31(2) 2 ?
Na2 O3 2.31(2) 3 ?
Na2 O2 2.409(18) 2 ?
Na2 O2 2.409(18) 3 ?
Na2 O2 2.409(18) . ?
O2 C21 1.22(3) . ?
O3 C31 1.206(18) . ?
C11 C12 1.48(3) . ?
C11 C12 1.48(3) 4 ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C21 C22 1.51(3) . ?
C21 C23 1.55(3) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C31 C32 1.520(19) . ?
C31 C33 1.522(19) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?

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
I1 Bi1 I1 97.35(6) 2_655 . ?
I1 Bi1 I1 97.35(6) 2_655 3_665 ?
I1 Bi1 I1 97.35(6) . 3_665 ?
I1 Bi1 I2 113.21(5) 2_655 . ?
I1 Bi1 I2 85.36(4) . . ?
I1 Bi1 I2 148.79(5) 3_665 . ?
I1 Bi1 I2 85.36(4) 2_655 2_655 ?
I1 Bi1 I2 148.79(5) . 2_655 ?
I1 Bi1 I2 113.21(5) 3_665 2_655 ?
I2 Bi1 I2 65.35(4) . 2_655 ?
I1 Bi1 I2 148.79(5) 2_655 3_665 ?
I1 Bi1 I2 113.21(5) . 3_665 ?
I1 Bi1 I2 85.36(4) 3_665 3_665 ?
I2 Bi1 I2 65.35(4) . 3_665 ?
I2 Bi1 I2 65.35(4) 2_655 3_665 ?
I2 Pt1 I2 89.49(5) . 2_655 ?
I2 Pt1 I2 89.49(5) . 3_665 ?
I2 Pt1 I2 89.49(5) 2_655 3_665 ?
I2 Pt1 I3 91.17(5) . 2_655 ?
I2 Pt1 I3 90.08(5) 2_655 2_655 ?
I2 Pt1 I3 179.21(5) 3_665 2_655 ?
I2 Pt1 I3 179.21(5) . 3_665 ?
I2 Pt1 I3 91.17(5) 2_655 3_665 ?
I2 Pt1 I3 90.08(5) 3_665 3_665 ?
I3 Pt1 I3 89.26(5) 2_655 3_665 ?
I2 Pt1 I3 90.08(5) . . ?
I2 Pt1 I3 179.21(5) 2_655 . ?
I2 Pt1 I3 91.17(5) 3_665 . ?
I3 Pt1 I3 89.26(5) 2_655 . ?
I3 Pt1 I3 89.26(5) 3_665 . ?
O2 Na1 O2 79.1(7) . 2 ?
O2 Na1 O2 79.1(7) . 3 ?
O2 Na1 O2 79.1(7) 2 3 ?
O2 Na1 O1 105.5(5) . . ?
O2 Na1 O1 175.4(5) 2 . ?
O2 Na1 O1 101.1(5) 3 . ?
O2 Na1 O1 175.4(5) . 3 ?
O2 Na1 O1 101.1(5) 2 3 ?
O2 Na1 O1 105.5(5) 3 3 ?
O1 Na1 O1 74.3(6) . 3 ?
O2 Na1 O1 101.1(5) . 2 ?
O2 Na1 O1 105.5(5) 2 2 ?
O2 Na1 O1 175.4(5) 3 2 ?
O1 Na1 O1 74.3(6) . 2 ?
O1 Na1 O1 74.3(6) 3 2 ?
C11 O1 Na1 134.2(4) . 4 ?
C11 O1 Na1 134.2(4) . . ?
Na1 O1 Na1 91.6(8) 4 . ?
I4 Bi2 I4 99.15(7) 2_655 3_665 ?
I4 Bi2 I4 99.15(7) 2_655 . ?
I4 Bi2 I4 99.15(6) 3_665 . ?
I4 Bi2 I3 96.97(6) 2_655 . ?
I4 Bi2 I3 158.69(6) 3_665 . ?
I4 Bi2 I3 91.93(6) . . ?
I4 Bi2 I3 91.93(6) 2_655 2_655 ?
I4 Bi2 I3 96.97(6) 3_665 2_655 ?
I4 Bi2 I3 158.69(6) . 2_655 ?
I3 Bi2 I3 68.56(5) . 2_655 ?
I4 Bi2 I3 158.68(6) 2_655 3_665 ?
I4 Bi2 I3 91.93(6) 3_665 3_665 ?
I4 Bi2 I3 96.97(6) . 3_665 ?
I3 Bi2 I3 68.56(5) . 3_665 ?
I3 Bi2 I3 68.55(5) 2_655 3_665 ?
Pt1 I2 Bi1 87.06(5) . . ?
O3 Na2 O3 101.2(9) . 2 ?
O3 Na2 O3 101.2(9) . 3 ?
O3 Na2 O3 101.2(9) 2 3 ?
O3 Na2 O2 88.9(7) . 2 ?
O3 Na2 O2 89.0(8) 2 2 ?
O3 Na2 O2 163.9(9) 3 2 ?
O3 Na2 O2 163.9(9) . 3 ?
O3 Na2 O2 88.9(7) 2 3 ?
O3 Na2 O2 89.0(8) 3 3 ?
O2 Na2 O2 78.7(7) 2 3 ?
O3 Na2 O2 89.0(8) . . ?
O3 Na2 O2 163.9(9) 2 . ?
O3 Na2 O2 88.9(7) 3 . ?
O2 Na2 O2 78.7(7) 2 . ?
O2 Na2 O2 78.7(7) 3 . ?
C21 O2 Na1 138.7(15) . . ?
C21 O2 Na2 134.7(16) . . ?
Na1 O2 Na2 85.6(6) . . ?
Pt1 I3 Bi2 85.22(5) . . ?
C31 O3 Na2 157(2) . . ?
O1 C11 C12 121.7(13) . . ?
O1 C11 C12 121.7(13) . 4 ?
C12 C11 C12 117(3) . 4 ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C21 C22 125(2) . . ?
O2 C21 C23 120(2) . . ?
C22 C21 C23 114(2) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O3 C31 C32 126(3) . . ?
O3 C31 C33 118(3) . . ?
C32 C31 C33 116(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         6.997
_refine_diff_density_min         -2.703
_refine_diff_density_rms         0.419
_database_code_depnum_ccdc_archive 'CCDC 930537'