# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 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_CaBTB

#==============================================================================
# start Validation Reply Form
_vrf_PLAT029_I                   
;
PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.930 Note
RESPONSE: When the intensity data were collected with synchrotron radiation,
the detector could not cover enough diffraction angles. 
;
_vrf_PLAT411_I                   
;
PROBLEM: PLAT411_ALERT_2_A Short Inter H...H Contact H15C .. H8TB .. 1.74 Ang.
RESPONSE: H15C and H8TB are respectively bonded to the C atoms (C15T and C8T)
of the occluded THF molecules which show large thermal motions. 
H10B and H23E are also the THF carbons atoms, C10T and C23', respectively. 
The THF H15C atom is engaged in a bad contact with H52A, the H atom of the
BTB linker. Thus, all the bad contacts are ascribed to the large thermal 
motion of the free THF guest in the pore. 
;

#==============================================================================
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'O0.50), 2(C2 H4 O0.50),2(H2 O)'

_chemical_formula_sum            'C156 H174 Ca5 O44'
_chemical_formula_weight         2953.35

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0050 0.0020 '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 0.0150 0.0080 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2690 0.3960 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14

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'

_cell_length_a                   16.135(3)
_cell_length_b                   26.792(5)
_cell_length_c                   18.630(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 110.57(3)
_cell_angle_gamma                90.00
_cell_volume                     7540(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3124
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.80000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            23192
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0437
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.57
_diffrn_reflns_theta_max         28.07
_reflns_number_total             11946
_reflns_number_gt                9436
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELX-TL
_computing_publication_material  SHELX-TL

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
TITL CaBTB in P2(1)/c
CELL 0.80000  16.1350  26.7920  18.6300  90.000 110.574  90.000
ZERR 2.00      0.0032   0.0054   0.0037   0.000   0.030   0.000
LATT 1
SYMM -X, 0.5+Y, 0.5-Z
SFAC C H O Ca
DISP C 0.005 0.002 14.981
DISP Ca 0.269 0.396 1814.419
DISP H -0 0 0.629
DISP O 0.015 0.008 44.819
UNIT 312 348 88 10
L.S. 24
Damp
ACTA
BOND
EQIV $1   x-1, y, z
EQIV $5   -x+1, y+1/2, -z+1/2
EQIV $12 -x, -y, -z
EQIV $13 x+1, -y+1/2, z+1/2
HTAB O1W O10_$5
HTAB O1W O6'
HTAB O1W O6T
HTAB O2W O9_$12
HTAB O2W O2T
HTAB O3W O5_$13
HTAB O3W O4W
HTAB O4W O1T
HTAB O4W O8_$13
HTAB O4  O1_$1
DELU C23T C24T
REM SIMU C18T C19T
FMAP 2
PLAN 10
SHEL 999 0.85
TEMP -173
WGHT    0.200000
EXTI    0.007372
FVAR       0.19959
CA1   4    0.952259    0.432049    0.970845    11.00000    0.02614    0.05798 =
         0.02406   -0.00484    0.00859   -0.00143
CA2   4    0.278707   -0.063006    0.444780    11.00000    0.02983    0.05317 =
         0.02222   -0.00049    0.01025   -0.00081
CA3   4    0.500000    0.000000    0.500000    10.50000    0.02516    0.05100 =
         0.02239    0.00021    0.00851    0.00024
O1W   3    0.870495    0.480352    0.864763    11.00000    0.03778    0.07899 =
         0.03322    0.00053    0.00382   -0.00568
 
DFIX 2.74 0.005 Ca1 H1WA Ca1 H1WB
DFIX 0.84 0.001 O1W H1WA O1W H1WB
DFIX 1.34 0.005 H1WA H1WB
H1WA  2    0.834521    0.498314    0.876496    11.00000   -1.20000
H1WB  2    0.839697    0.461663    0.829191    11.00000   -1.20000
 
O2W   3    0.175710   -0.122866    0.376437    11.00000    0.03935    0.08747 =
         0.03913   -0.01253    0.01692   -0.01271
DFIX 2.74 0.005 Ca2 H2WA Ca2 H2WB
DFIX 0.84 0.001 O2W H2WA O2W H2WB
DFIX 1.34 0.005 H2WA H2WB
 
H2WA  2    0.125117   -0.115277    0.376233    11.00000   -1.20000
H2WB  2    0.171912   -0.122927    0.330301    11.00000   -1.20000
O3W   3    1.063075    0.493865    0.956424    11.00000    0.02372    0.06748 =
         0.02547   -0.00285    0.00847    0.00038
DFIX 2.90 0.005 Ca1 H3WA Ca1 H3WB
DFIX 0.84 0.001 O3W H3WA O3W H3WB
DFIX 1.34 0.005 H3WA H3WB
H3WA  2    1.114062    0.481713    0.976193    11.00000   -1.20000
H3WB  2    1.054511    0.497251    0.909533    11.00000   -1.20000
 
O4W   3    1.057198    0.508552    0.813127    11.00000    0.03889    0.09755 =
         0.03248   -0.00280    0.01189   -0.00628
DFIX 0.84 0.001 O4W H4WA O4W H4WB
DFIX 1.34 0.005 H4WA H4WB
H4WA  2    1.027470    0.491171    0.775309    11.00000   -1.20000
H4WB  2    1.105319    0.514447    0.806821    11.00000   -1.20000
 
O1    3    0.852446    0.364837    0.908698    11.00000    0.02924    0.07544 =
         0.05354   -0.02361    0.02156   -0.00841
O2    3    0.787524    0.414684    0.964817    11.00000    0.02771    0.06256 =
         0.02471   -0.00617    0.01004   -0.00185
O3    3    0.023818    0.384809    0.897722    11.00000    0.03304    0.06344 =
         0.03804   -0.01209    0.01718   -0.00443
O4    3   -0.061024    0.320725    0.836829    11.00000    0.03719    0.08631 =
         0.06222   -0.03503    0.02727   -0.01433
FLAT O3 O4 C20 H4O
DFIX 2.20 O3 H4O
DFIX 0.84 O4 H4O
H4O   2   -0.089201    0.333414    0.861667    11.00000   -1.20000
O5    3    0.240763    0.016942    0.483785    11.00000    0.02639    0.06016 =
         0.02593   -0.00431    0.00730   -0.00114
O6    3    0.380526   -0.004747    0.545726    11.00000    0.02678    0.05505 =
         0.02640   -0.00087    0.01142    0.00244
O7    3    0.375904   -0.006152    0.386630    11.00000    0.03670    0.06247 =
         0.02292    0.00384    0.00732    0.00215
O8    3    0.234267   -0.023223    0.324938    11.00000    0.03722    0.06697 =
         0.02647    0.00613    0.01007   -0.00483
O9    3   -0.029593    0.117377   -0.412431    11.00000    0.03645    0.07560 =
         0.03163   -0.00158    0.00634    0.00237
O10   3    0.084303    0.073990   -0.415932    11.00000    0.03268    0.07293 =
         0.02854   -0.00154    0.00719   -0.00160
O11   3    0.502629    0.415188   -0.004457    11.00000    0.05292    0.05377 =
         0.03857   -0.00029    0.02372   -0.00333
O12   3    0.626649    0.376789    0.066756    11.00000    0.04071    0.06120 =
         0.05296   -0.00240    0.01985   -0.00727
C1    1    0.452062    0.272400    0.789475    11.00000    0.02877    0.05724 =
         0.02346   -0.00202    0.00954   -0.00273
C2    1    0.377447    0.291264    0.801728    11.00000    0.03318    0.05572 =
         0.02499   -0.00500    0.01162   -0.00068
AFIX  43
H2A   2    0.383569    0.319705    0.833638    11.00000   -1.20000
AFIX   0
C3    1    0.294204    0.269479    0.768388    11.00000    0.02985    0.06359 =
         0.02342    0.00127    0.01165   -0.00112
C4    1    0.286636    0.227172    0.723182    11.00000    0.03009    0.05623 =
         0.02536   -0.00251    0.01084   -0.00188
AFIX  43
H4A   2    0.230262    0.212063    0.699797    11.00000   -1.20000
AFIX   0
C5    1    0.360435    0.206510    0.711555    11.00000    0.03204    0.05632 =
         0.02392   -0.00261    0.01010   -0.00207
C6    1    0.442376    0.229933    0.744344    11.00000    0.02774    0.05580 =
         0.02956   -0.00109    0.01174    0.00108
AFIX  43
H6A   2    0.492583    0.216589    0.735652    11.00000   -1.20000
AFIX   0
C7    1    0.538944    0.299103    0.823646    11.00000    0.02995    0.06307 =
         0.02654   -0.00424    0.00933   -0.00393
C8    1    0.618369    0.276736    0.826961    11.00000    0.03469    0.05827 =
         0.05163   -0.01715    0.01606   -0.00357
AFIX  43
H8A   2    0.618170    0.243754    0.808177    11.00000   -1.20000
AFIX   0
C9    1    0.697687    0.302586    0.857655    11.00000    0.02543    0.07311 =
         0.05431   -0.01980    0.01326    0.00100
AFIX  43
H9A   2    0.751118    0.287379    0.858261    11.00000   -1.20000
AFIX   0
C10   1    0.700111    0.349992    0.887274    11.00000    0.02911    0.05877 =
         0.03045   -0.00862    0.01165   -0.00230
C11   1    0.621004    0.371865    0.884020    11.00000    0.03222    0.05664 =
         0.02625   -0.00452    0.00817   -0.00018
AFIX  43
H11A  2    0.621288    0.404544    0.903897    11.00000   -1.20000
AFIX   0
C12   1    0.542271    0.346846    0.852408    11.00000    0.02703    0.06080 =
         0.02690   -0.00412    0.00758    0.00141
AFIX  43
H12A  2    0.488832    0.362752    0.850272    11.00000   -1.20000
AFIX   0
C13   1    0.784786    0.378355    0.922719    11.00000    0.03047    0.05973 =
         0.02896   -0.00526    0.01178   -0.00216
C14   1    0.217386    0.290151    0.785281    11.00000    0.03077    0.05611 =
         0.02482   -0.00038    0.01185    0.00376
C15   1    0.215574    0.340474    0.804505    11.00000    0.03155    0.06210 =
         0.02508   -0.00071    0.01104   -0.00257
AFIX  43
H15A  2    0.260752    0.362225    0.801527    11.00000   -1.20000
AFIX   0
C16   1    0.148970    0.359216    0.827856    11.00000    0.03468    0.05827 =
         0.03077   -0.00364    0.01123   -0.00016
AFIX  43
H16A  2    0.149941    0.393161    0.842871    11.00000   -1.20000
AFIX   0
C17   1    0.080464    0.327735    0.829096    11.00000    0.03347    0.06094 =
         0.03201   -0.00752    0.01140    0.00061
C18   1    0.079068    0.277948    0.805584    11.00000    0.03054    0.07398 =
         0.03507   -0.00947    0.01470   -0.00714
AFIX  43
H18A  2    0.031239    0.256812    0.804153    11.00000   -1.20000
AFIX   0
C19   1    0.147252    0.259585    0.784476    11.00000    0.03542    0.05703 =
         0.03297   -0.00951    0.01312   -0.00267
AFIX  43
H19A  2    0.146254    0.225688    0.769230    11.00000   -1.20000
AFIX   0
C20   1    0.012331    0.347465    0.857913    11.00000    0.03116    0.06777 =
         0.03587   -0.00750    0.01472   -0.00210
C21   1    0.350374    0.160581    0.664685    11.00000    0.03113    0.05375 =
         0.03012   -0.00167    0.01300   -0.00257
C22   1    0.272560    0.151667    0.602044    11.00000    0.02989    0.05876 =
         0.02587   -0.00295    0.01003    0.00113
AFIX  43
H22A  2    0.226676    0.175916    0.588218    11.00000   -1.20000
AFIX   0
C23   1    0.261796    0.108129    0.560241    11.00000    0.03023    0.05783 =
         0.02544   -0.00188    0.01141   -0.00091
AFIX  43
H23A  2    0.208670    0.102641    0.517949    11.00000   -1.20000
AFIX   0
C24   1    0.328267    0.072212    0.579645    11.00000    0.02633    0.05450 =
         0.02605   -0.00080    0.01260   -0.00128
C25   1    0.406836    0.081002    0.641370    11.00000    0.02587    0.05892 =
         0.02900   -0.00190    0.00814    0.00193
AFIX  43
H25A  2    0.453226    0.057080    0.654101    11.00000   -1.20000
AFIX   0
C26   1    0.417165    0.124381    0.683881    11.00000    0.02548    0.06156 =
         0.02937   -0.00471    0.00860   -0.00058
AFIX  43
H26A  2    0.470068    0.129654    0.726491    11.00000   -1.20000
AFIX   0
C27   1    0.315606    0.025849    0.533484    11.00000    0.02852    0.05906 =
         0.02275   -0.00028    0.01185   -0.00408
C28   1    0.295347    0.126103    0.076548    11.00000    0.04988    0.06520 =
         0.02552    0.00265    0.00809   -0.01139
C29   1    0.241399    0.112789    0.002754    11.00000    0.05032    0.06912 =
         0.02699    0.00172    0.00650   -0.01809
AFIX  43
H29A  2    0.204479    0.084207   -0.004663    11.00000   -1.20000
AFIX   0
C30   1    0.240758    0.140912   -0.060697    11.00000    0.05278    0.06502 =
         0.02972    0.00340    0.01290   -0.01037
C31   1    0.293392    0.182589   -0.049089    11.00000    0.05021    0.06864 =
         0.01835    0.00224    0.00579   -0.01006
AFIX  43
H31A  2    0.294137    0.201298   -0.092175    11.00000   -1.20000
AFIX   0
C32   1    0.346081    0.198270    0.024693    11.00000    0.04426    0.06158 =
         0.02801    0.00317    0.01098   -0.00784
C33   1    0.347314    0.169402    0.086935    11.00000    0.04066    0.06876 =
         0.02533    0.00234    0.00333   -0.01029
AFIX  43
H33A  2    0.383773    0.179057    0.137192    11.00000   -1.20000
AFIX   0
C34   1    0.297760    0.094769    0.142442    11.00000    0.04460    0.06431 =
         0.02660    0.00311    0.00586   -0.01048
C35   1    0.376388    0.087209    0.204720    11.00000    0.04051    0.07124 =
         0.03095    0.00147    0.00814   -0.01440
AFIX  43
H35A  2    0.429070    0.103164    0.204971    11.00000   -1.20000
AFIX   0
C36   1    0.379242    0.057296    0.265463    11.00000    0.04087    0.06231 =
         0.02519   -0.00008    0.00467   -0.00662
AFIX  43
H36A  2    0.433228    0.053461    0.307461    11.00000   -1.20000
AFIX   0
C37   1    0.303608    0.032615    0.265821    11.00000    0.03856    0.05301 =
         0.02561   -0.00109    0.00877   -0.00460
C38   1    0.223732    0.040464    0.203922    11.00000    0.03608    0.06063 =
         0.02672    0.00004    0.00616   -0.00690
AFIX  43
H38A  2    0.171148    0.024466    0.203827    11.00000   -1.20000
AFIX   0
C39   1    0.220956    0.070629    0.144356    11.00000    0.04483    0.06091 =
         0.02542    0.00360    0.00414   -0.00807
AFIX  43
H39A  2    0.166371    0.075493    0.103403    11.00000   -1.20000
AFIX   0
C40   1    0.304143   -0.001207    0.329775    11.00000    0.03744    0.05615 =
         0.02372   -0.00257    0.00956   -0.00067
C41   1    0.188880    0.126078   -0.140603    11.00000    0.05112    0.05907 =
         0.03046    0.00096    0.00944   -0.01555
C42   1    0.097547    0.130693   -0.169391    11.00000    0.05511    0.08342 =
         0.02926   -0.00712    0.01446   -0.00814
AFIX  43
H42A  2    0.066795    0.139824   -0.136252    11.00000   -1.20000
AFIX   0
C43   1    0.050628    0.121963   -0.246938    11.00000    0.04863    0.07809 =
         0.03555   -0.00553    0.00910   -0.00218
AFIX  43
H43A  2   -0.011941    0.125512   -0.266573    11.00000   -1.20000
AFIX   0
C44   1    0.094964    0.108146   -0.295360    11.00000    0.04235    0.05897 =
         0.02837   -0.00045    0.01065   -0.00698
C45   1    0.185219    0.102456   -0.266418    11.00000    0.04581    0.08781 =
         0.02492   -0.00297    0.00987   -0.01133
AFIX  43
H45A  2    0.215537    0.091334   -0.298906    11.00000   -1.20000
AFIX   0
C46   1    0.232433    0.112866   -0.189931    11.00000    0.04744    0.08494 =
         0.02784    0.00217    0.00796   -0.01179
AFIX  43
H46A  2    0.295224    0.110911   -0.171233    11.00000   -1.20000
AFIX   0
C47   1    0.046501    0.099169   -0.379472    11.00000    0.03565    0.05891 =
         0.03105   -0.00090    0.01142   -0.00744
C48   1    0.397916    0.244952    0.031968    11.00000    0.04175    0.06092 =
         0.02235   -0.00157    0.01061   -0.00535
C49   1    0.357093    0.286301   -0.011384    11.00000    0.04095    0.06136 =
         0.02422    0.00172    0.01066   -0.00441
AFIX  43
H49A  2    0.296293    0.284539   -0.042676    11.00000   -1.20000
AFIX   0
C50   1    0.403360    0.329566   -0.009595    11.00000    0.03759    0.06095 =
         0.02244    0.00141    0.01128    0.00152
AFIX  43
H50A  2    0.374185    0.357679   -0.038626    11.00000   -1.20000
AFIX   0
C51   1    0.493596    0.332327    0.035007    11.00000    0.03668    0.05628 =
         0.03120   -0.00302    0.01699   -0.00173
C52   1    0.534216    0.291178    0.079369    11.00000    0.04086    0.06071 =
         0.03438    0.00063    0.01336   -0.00236
AFIX  43
H52A  2    0.595092    0.292905    0.110452    11.00000   -1.20000
AFIX   0
C53   1    0.487486    0.248175    0.078780    11.00000    0.04484    0.05988 =
         0.03369    0.00426    0.01238   -0.00332
AFIX  43
H53A  2    0.515766    0.220684    0.110003    11.00000   -1.20000
AFIX   0
C54   1    0.544601    0.378196    0.032442    11.00000    0.04224    0.05398 =
         0.03415   -0.00470    0.02048   -0.00372
O1T   3    0.971626    0.463209    0.672724    11.00000    0.14985    0.15216 =
         0.06941   -0.04202   -0.04011    0.03915
C1T   1    0.950307    0.415602    0.653325    11.00000    0.13973    0.12518 =
         0.07728   -0.00936   -0.03553   -0.01224
AFIX  23
H1TA  2    0.917307    0.401034    0.684135    11.00000   -1.20000
H1TB  2    1.003861    0.395261    0.660538    11.00000   -1.20000
AFIX   0
C2T   1    0.894118    0.418493    0.571506    11.00000    0.35248    0.18181 =
         0.10231   -0.05695   -0.11478    0.12989
AFIX  23
H2TA  2    0.930152    0.413012    0.538792    11.00000   -1.20000
H2TB  2    0.847175    0.392739    0.559028    11.00000   -1.20000
AFIX   0
C3T   1    0.857031    0.465670    0.559225    11.00000    0.25285    0.15579 =
         0.13562   -0.01199   -0.09578    0.02606
AFIX  23
H3TA  2    0.796600    0.465158    0.561384    11.00000   -1.20000
H3TB  2    0.854029    0.478795    0.508696    11.00000   -1.20000
AFIX   0
C4T   1    0.914074    0.494778    0.618982    11.00000    0.32736    0.11270 =
         0.16185   -0.04073   -0.15267    0.06978
AFIX  23
H4TA  2    0.947978    0.518063    0.598531    11.00000   -1.20000
H4TB  2    0.879308    0.514656    0.643216    11.00000   -1.20000
AFIX   0
SAME O1T > C4T
O2T   3    0.152615   -0.147651    0.226347    11.00000    0.14722    0.17166 =
         0.10448    0.00780    0.04159    0.01585
C5T   1    0.140165   -0.106783    0.171154    11.00000    0.17692    0.13161 =
         0.10343    0.00722    0.07243    0.01337
AFIX  23
H5TA  2    0.090076   -0.114257    0.123369    11.00000   -1.20000
H5TB  2    0.127282   -0.075254    0.192898    11.00000   -1.20000
AFIX   0
C6T   1    0.220293   -0.102301    0.155655    11.00000    0.12334    0.12593 =
         0.16094   -0.03171    0.04792    0.00687
AFIX  23
H6TA  2    0.237430   -0.066832    0.155488    11.00000   -1.20000
H6TB  2    0.213841   -0.117316    0.105419    11.00000   -1.20000
AFIX   0
C7T   1    0.286851   -0.129886    0.218998    11.00000    0.12764    0.20079 =
         0.13933    0.04069    0.04785    0.00757
AFIX  23
H7TA  2    0.337306   -0.141252    0.204640    11.00000   -1.20000
H7TB  2    0.309089   -0.109712    0.266473    11.00000   -1.20000
AFIX   0
C8T   1    0.232656   -0.171286    0.226574    11.00000    0.19230    0.20377 =
         0.25954    0.08589    0.13840    0.10171
AFIX  23
H8TA  2    0.220540   -0.194781    0.183066    11.00000   -1.20000
H8TB  2    0.261789   -0.189607    0.275085    11.00000   -1.20000
SAME O1T > C4T
AFIX   0
O3T   3    0.438397   -0.138035    0.122155    11.00000    0.12377    0.25748 =
         0.11451   -0.01858    0.04743    0.00128
C9T   1    0.500112   -0.153839    0.086785    11.00000    0.14276    0.30880 =
         0.08659    0.01644    0.05939    0.04229
AFIX  23
H9TA  2    0.484603   -0.187584    0.064437    11.00000   -1.20000
H9TB  2    0.560921   -0.154808    0.125062    11.00000   -1.20000
AFIX   0
C10T  1    0.494479   -0.117762    0.027235    11.00000    0.29148    0.36560 =
         0.19721    0.15719    0.15689    0.21570
AFIX  23
H10A  2    0.554589   -0.107538    0.030295    11.00000   -1.20000
H10B  2    0.463736   -0.132624   -0.023903    11.00000   -1.20000
AFIX   0
C11T  1    0.445760   -0.074981    0.038420    11.00000    0.29457    0.28701 =
         0.21218   -0.07449    0.17456   -0.00388
AFIX  23
H11B  2    0.484935   -0.045502    0.054530    11.00000   -1.20000
H11C  2    0.396219   -0.066767   -0.009381    11.00000   -1.20000
AFIX   0
C12T  1    0.413434   -0.089625    0.097114    11.00000    0.40234    0.15388 =
         0.42238    0.11947    0.31479    0.12678
AFIX  23
H12B  2    0.436447   -0.066400    0.140999    11.00000   -1.20000
H12C  2    0.348029   -0.087280    0.077442    11.00000   -1.20000
AFIX   0
SAME 0.005 O1T > C4T
O4T   3    0.761959    0.306958    0.623401    11.00000    0.61460    0.21553 =
         0.49929   -0.19473    0.17923   -0.07872
C13T  1    0.721276    0.296066    0.549470    11.00000    0.16670    0.25099 =
         0.41905    0.25861   -0.02850   -0.01633
AFIX  23
H13B  2    0.744692    0.316681    0.516792    11.00000   -1.20000
H13C  2    0.656661    0.301592    0.533778    11.00000   -1.20000
AFIX   0
C14T  1    0.741269    0.242734    0.543971    11.00000    0.36619    0.21069 =
         0.09809   -0.00045    0.12381   -0.07038
AFIX  23
H14B  2    0.687436    0.224623    0.512090    11.00000   -1.20000
H14C  2    0.787279    0.238824    0.520552    11.00000   -1.20000
AFIX   0
C15T  1    0.771171    0.224345    0.617960    11.00000    0.09961    0.10952 =
         0.24535   -0.06707    0.00544    0.00636
AFIX  23
H15B  2    0.812094    0.195858    0.623752    11.00000   -1.20000
H15C  2    0.721571    0.214096    0.634316    11.00000   -1.20000
AFIX   0
C16T  1    0.815487    0.266785    0.658644    11.00000    0.48518    0.23295 =
         0.16339    0.02818   -0.15920   -0.21548
AFIX  23
H16B  2    0.821908    0.264594    0.713389    11.00000   -1.20000
H16C  2    0.874991    0.270073    0.654992    11.00000   -1.20000
AFIX   0
SAME O1T > C4T
O5T   3    1.059272    0.316228    0.550345    11.00000    0.19648    0.16785 =
         0.27124   -0.06149    0.09613   -0.05352
C17T  1    1.105162    0.272894    0.531305    11.00000    0.11731    0.14733 =
         0.25461    0.05345    0.04027    0.06033
AFIX  23
H17B  2    1.106245    0.276118    0.478705    11.00000   -1.20000
H17C  2    1.166826    0.270512    0.567742    11.00000   -1.20000
AFIX   0
C18T  1    1.055454    0.229987    0.537173    11.00000    0.20135    0.11910 =
         0.21166   -0.06067    0.02699   -0.04524
AFIX  23
H18B  2    1.071324    0.218525    0.590856    11.00000   -1.20000
H18C  2    1.062358    0.202118    0.504832    11.00000   -1.20000
AFIX   0
C19T  1    0.966453    0.251606    0.507577    11.00000    0.10387    0.35022 =
         0.76533   -0.40302   -0.00394    0.02202
AFIX  23
H19B  2    0.940275    0.246173    0.451524    11.00000   -1.20000
H19C  2    0.928152    0.235022    0.531845    11.00000   -1.20000
AFIX   0
C20T  1    0.970972    0.304225    0.523826    11.00000    0.06769    0.21294 =
         0.36024   -0.18630    0.00907    0.01373
AFIX  23
H20B  2    0.938880    0.323417    0.476843    11.00000   -1.20000
H20C  2    0.944406    0.311705    0.563112    11.00000   -1.20000
PART 1
AFIX   0
PART 1
SAME O1T > C4T
O6T   3    0.735551    0.465028    0.721541    10.50000    0.05400    0.12000 =
         0.08521   -0.00761    0.00462   -0.01262
C21T  1    0.705588    0.413219    0.708464    10.50000    0.06709    0.08551 =
         0.03497   -0.00576    0.01535   -0.00225
AFIX  23
H21B  2    0.737705    0.392121    0.753241    10.50000   -1.20000
H21C  2    0.714594    0.399464    0.662428    10.50000   -1.20000
AFIX   0
C22T  1    0.610979    0.415868    0.697308    10.50000    0.09035    0.13005 =
         0.05299   -0.00051    0.03393   -0.00738
AFIX  23
H22B  2    0.592427    0.386823    0.720866    10.50000   -1.20000
H22C  2    0.574346    0.417275    0.642141    10.50000   -1.20000
AFIX   0
C23T  1    0.604002    0.462761    0.736651    10.50000    0.12439    0.10920 =
         0.12331    0.02063    0.08940   -0.00678
AFIX  23
H23B  2    0.542981    0.476202    0.716585    10.50000   -1.20000
H23C  2    0.621573    0.457620    0.792657    10.50000   -1.20000
AFIX   0
C24T  1    0.665241    0.495636    0.718840    10.50000    0.12569    0.12620 =
         0.11853    0.03413    0.05820   -0.03202
AFIX  23
H24B  2    0.637602    0.510481    0.667232    10.50000   -1.20000
H24C  2    0.685013    0.522830    0.757067    10.50000   -1.20000
PART 2
AFIX   0
PART 2
SAME O1T > C4T
O6'   3    0.713705    0.448122    0.761752    10.50000    0.05443    0.14699 =
         0.08748   -0.03277   -0.02030    0.00108
C21'  1    0.630849    0.475499    0.735355    10.50000    0.08807    0.10641 =
         0.07739    0.02281    0.03768    0.01592
AFIX  23
H21D  2    0.641182    0.511145    0.727287    10.50000   -1.20000
H21E  2    0.600342    0.473063    0.772970    10.50000   -1.20000
AFIX   0
C22'  1    0.577987    0.451371    0.662143    10.50000    0.07093    0.18348 =
         0.07402    0.04367   -0.00364   -0.00575
AFIX  23
H22D  2    0.514009    0.451779    0.654182    10.50000   -1.20000
H22E  2    0.587633    0.467595    0.617980    10.50000   -1.20000
AFIX   0
C23'  1    0.613951    0.400111    0.674183    10.50000    0.09570    0.13268 =
         0.05972   -0.00456    0.00071   -0.01700
AFIX  23
H23D  2    0.591533    0.380999    0.709048    10.50000   -1.20000
H23E  2    0.599571    0.381899    0.625063    10.50000   -1.20000
AFIX   0
C24'  1    0.708224    0.409559    0.708843    10.50000    0.13518    0.20047 =
         0.29076   -0.11726    0.12023   -0.05286
AFIX  23
H24D  2    0.740073    0.379394    0.735122    10.50000   -1.20000
H24E  2    0.733260    0.420307    0.669849    10.50000   -1.20000
PART 0
 
PART 0
HKLF 4
 
REM  CaBTB in P2(1)/c
REM R1 =  0.0864 for   9436 Fo > 4sig(Fo)  and  0.1006 for all  11946 data
REM    998 parameters refined using    182 restraints
 
END  
     
WGHT      0.2000      0.0000 
REM Highest difference peak  1.047,  deepest hole -0.851,  1-sigma level  0.149
Q1    1   0.3112 -0.1610  0.1824  11.00000  0.05    1.05
Q2    1   0.7179  0.3089  0.5896  11.00000  0.05    0.95
Q3    1   0.1458 -0.1501  0.1421  11.00000  0.05    0.95
Q4    1   0.1024 -0.1389  0.1182  11.00000  0.05    0.93
Q5    1   0.2226 -0.1657  0.1190  11.00000  0.05    0.89
Q6    1   1.0059  0.2896  0.5747  11.00000  0.05    0.75
Q7    1   0.4728 -0.0223  0.0349  11.00000  0.05    0.75
Q8    1   0.9760  0.2781  0.4551  11.00000  0.05    0.70
Q9    1   0.8342  0.2559  0.6335  11.00000  0.05    0.69
Q10   1   1.0620  0.2483  0.4844  11.00000  0.05    0.66
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0074(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11946
_refine_ls_number_parameters     998
_refine_ls_number_restraints     182
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0864
_refine_ls_wR_factor_ref         0.2786
_refine_ls_wR_factor_gt          0.2614
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_restrained_S_all      1.219
_refine_ls_shift/su_max          0.001
_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
Ca1 Ca 0.95226(5) 0.43205(3) 0.97084(4) 0.0361(3) Uani 1 1 d D . .
Ca2 Ca 0.27871(5) -0.06301(3) 0.44478(4) 0.0348(3) Uani 1 1 d D . .
Ca3 Ca 0.5000 0.0000 0.5000 0.0328(3) Uani 1 2 d S . .
O1W O 0.87049(19) 0.48035(12) 0.86476(17) 0.0523(7) Uani 1 1 d D . .
H1WA H 0.8345(17) 0.4983(10) 0.8765(7) 0.063 Uiso 1 1 d D . .
H1WB H 0.8397(19) 0.4617(2) 0.8292(8) 0.063 Uiso 1 1 d D . .
O2W O 0.17571(19) -0.12287(12) 0.37644(17) 0.0545(8) Uani 1 1 d D . .
H2WA H 0.1251(5) -0.1153(8) 0.3762(18) 0.065 Uiso 1 1 d D . .
H2WB H 0.1719(18) -0.1229(10) 0.3303(5) 0.065 Uiso 1 1 d D . .
O3W O 1.06307(16) 0.49387(10) 0.95642(15) 0.0389(6) Uani 1 1 d D . .
H3WA H 1.1141(3) 0.4817(6) 0.9762(16) 0.047 Uiso 1 1 d D . .
H3WB H 1.0545(14) 0.4973(9) 0.9095(2) 0.047 Uiso 1 1 d D . .
O4W O 1.0572(2) 0.50855(14) 0.81313(17) 0.0565(8) Uani 1 1 d D . .
H4WA H 1.027(2) 0.4912(16) 0.7753(18) 0.068 Uiso 1 1 d D . .
H4WB H 1.1053(16) 0.5144(17) 0.807(3) 0.068 Uiso 1 1 d D . .
O1 O 0.85245(18) 0.36484(11) 0.90870(18) 0.0509(8) Uani 1 1 d . . .
O2 O 0.78752(16) 0.41468(10) 0.96482(14) 0.0381(6) Uani 1 1 d . . .
O3 O 0.02382(17) 0.38481(10) 0.89772(16) 0.0436(7) Uani 1 1 d D . .
O4 O -0.06102(19) 0.32073(13) 0.8368(2) 0.0593(9) Uani 1 1 d D . .
H4O H -0.0892(18) 0.3334(12) 0.862(2) 0.071 Uiso 1 1 d D . .
O5 O 0.24076(16) 0.01694(10) 0.48378(14) 0.0380(6) Uani 1 1 d . . .
O6 O 0.38053(15) -0.00475(9) 0.54573(14) 0.0355(6) Uani 1 1 d . . .
O7 O 0.37590(18) -0.00615(10) 0.38663(15) 0.0415(6) Uani 1 1 d . . .
O8 O 0.23427(17) -0.02322(11) 0.32494(15) 0.0439(6) Uani 1 1 d . . .
O9 O -0.02959(18) 0.11738(11) -0.41243(16) 0.0494(7) Uani 1 1 d . . .
O10 O 0.08430(17) 0.07399(11) -0.41593(15) 0.0457(7) Uani 1 1 d . . .
O11 O 0.50263(19) 0.41519(11) -0.00446(16) 0.0464(7) Uani 1 1 d . . .
O12 O 0.62665(19) 0.37679(11) 0.06676(18) 0.0507(7) Uani 1 1 d . . .
C1 C 0.4521(2) 0.27240(14) 0.7895(2) 0.0364(8) Uani 1 1 d . . .
C2 C 0.3774(2) 0.29126(15) 0.8017(2) 0.0376(8) Uani 1 1 d . . .
H2A H 0.3836 0.3197 0.8336 0.045 Uiso 1 1 calc R . .
C3 C 0.2942(2) 0.26948(15) 0.7684(2) 0.0383(8) Uani 1 1 d . . .
C4 C 0.2866(2) 0.22717(14) 0.7232(2) 0.0369(8) Uani 1 1 d . . .
H4A H 0.2303 0.2121 0.6998 0.044 Uiso 1 1 calc R . .
C5 C 0.3604(2) 0.20651(15) 0.7116(2) 0.0374(8) Uani 1 1 d . . .
C6 C 0.4424(2) 0.22993(14) 0.7443(2) 0.0373(8) Uani 1 1 d . . .
H6A H 0.4926 0.2166 0.7357 0.045 Uiso 1 1 calc R . .
C7 C 0.5389(2) 0.29910(15) 0.8236(2) 0.0400(9) Uani 1 1 d . . .
C8 C 0.6184(3) 0.27674(16) 0.8270(3) 0.0480(10) Uani 1 1 d . . .
H8A H 0.6182 0.2438 0.8082 0.058 Uiso 1 1 calc R . .
C9 C 0.6977(3) 0.30259(17) 0.8577(3) 0.0512(11) Uani 1 1 d . . .
H9A H 0.7511 0.2874 0.8583 0.061 Uiso 1 1 calc R . .
C10 C 0.7001(2) 0.34999(15) 0.8873(2) 0.0391(9) Uani 1 1 d . . .
C11 C 0.6210(2) 0.37187(15) 0.8840(2) 0.0389(8) Uani 1 1 d . . .
H11A H 0.6213 0.4045 0.9039 0.047 Uiso 1 1 calc R . .
C12 C 0.5423(2) 0.34685(15) 0.8524(2) 0.0388(8) Uani 1 1 d . . .
H12A H 0.4888 0.3628 0.8503 0.047 Uiso 1 1 calc R . .
C13 C 0.7848(2) 0.37835(15) 0.9227(2) 0.0394(9) Uani 1 1 d . . .
C14 C 0.2174(2) 0.29015(14) 0.7853(2) 0.0367(8) Uani 1 1 d . . .
C15 C 0.2156(2) 0.34047(15) 0.8045(2) 0.0393(9) Uani 1 1 d . . .
H15A H 0.2608 0.3622 0.8015 0.047 Uiso 1 1 calc R . .
C16 C 0.1490(2) 0.35922(16) 0.8279(2) 0.0413(9) Uani 1 1 d . . .
H16A H 0.1499 0.3932 0.8429 0.050 Uiso 1 1 calc R . .
C17 C 0.0805(3) 0.32774(16) 0.8291(2) 0.0422(9) Uani 1 1 d . . .
C18 C 0.0791(3) 0.27795(17) 0.8056(2) 0.0457(10) Uani 1 1 d . . .
H18A H 0.0312 0.2568 0.8042 0.055 Uiso 1 1 calc R . .
C19 C 0.1473(2) 0.25958(16) 0.7845(2) 0.0415(9) Uani 1 1 d . . .
H19A H 0.1463 0.2257 0.7692 0.050 Uiso 1 1 calc R . .
C20 C 0.0123(3) 0.34747(16) 0.8579(2) 0.0441(9) Uani 1 1 d D . .
C21 C 0.3504(2) 0.16058(15) 0.6647(2) 0.0377(8) Uani 1 1 d . . .
C22 C 0.2726(2) 0.15167(15) 0.6020(2) 0.0381(8) Uani 1 1 d . . .
H22A H 0.2267 0.1759 0.5882 0.046 Uiso 1 1 calc R . .
C23 C 0.2618(2) 0.10813(14) 0.5602(2) 0.0374(8) Uani 1 1 d . . .
H23A H 0.2087 0.1026 0.5179 0.045 Uiso 1 1 calc R . .
C24 C 0.3283(2) 0.07221(14) 0.5796(2) 0.0347(8) Uani 1 1 d . . .
C25 C 0.4068(2) 0.08100(15) 0.6414(2) 0.0383(8) Uani 1 1 d . . .
H25A H 0.4532 0.0571 0.6541 0.046 Uiso 1 1 calc R . .
C26 C 0.4172(2) 0.12438(15) 0.6839(2) 0.0391(9) Uani 1 1 d . . .
H26A H 0.4701 0.1297 0.7265 0.047 Uiso 1 1 calc R . .
C27 C 0.3156(2) 0.02585(15) 0.5335(2) 0.0360(8) Uani 1 1 d . . .
C28 C 0.2953(3) 0.12610(16) 0.0765(2) 0.0482(10) Uani 1 1 d . . .
C29 C 0.2414(3) 0.11279(17) 0.0028(2) 0.0507(10) Uani 1 1 d . . .
H29A H 0.2045 0.0842 -0.0047 0.061 Uiso 1 1 calc R . .
C30 C 0.2408(3) 0.14091(17) -0.0607(2) 0.0496(10) Uani 1 1 d . . .
C31 C 0.2934(3) 0.18259(16) -0.0491(2) 0.0474(10) Uani 1 1 d . . .
H31A H 0.2941 0.2013 -0.0922 0.057 Uiso 1 1 calc R . .
C32 C 0.3461(3) 0.19827(16) 0.0247(2) 0.0451(10) Uani 1 1 d . . .
C33 C 0.3473(3) 0.16940(16) 0.0869(2) 0.0471(10) Uani 1 1 d . . .
H33A H 0.3838 0.1791 0.1372 0.057 Uiso 1 1 calc R . .
C34 C 0.2978(3) 0.09477(16) 0.1424(2) 0.0469(10) Uani 1 1 d . . .
C35 C 0.3764(3) 0.08721(17) 0.2047(2) 0.0487(10) Uani 1 1 d . . .
H35A H 0.4291 0.1032 0.2050 0.058 Uiso 1 1 calc R . .
C36 C 0.3792(3) 0.05730(16) 0.2655(2) 0.0446(9) Uani 1 1 d . . .
H36A H 0.4332 0.0535 0.3075 0.054 Uiso 1 1 calc R . .
C37 C 0.3036(3) 0.03261(15) 0.2658(2) 0.0397(9) Uani 1 1 d . . .
C38 C 0.2237(3) 0.04046(15) 0.2039(2) 0.0424(9) Uani 1 1 d . . .
H38A H 0.1711 0.0245 0.2038 0.051 Uiso 1 1 calc R . .
C39 C 0.2210(3) 0.07063(15) 0.1444(2) 0.0459(10) Uani 1 1 d . . .
H39A H 0.1664 0.0755 0.1034 0.055 Uiso 1 1 calc R . .
C40 C 0.3041(3) -0.00121(15) 0.3298(2) 0.0394(9) Uani 1 1 d . . .
C41 C 0.1889(3) 0.12608(16) -0.1406(2) 0.0482(10) Uani 1 1 d . . .
C42 C 0.0975(3) 0.13069(19) -0.1694(2) 0.0560(11) Uani 1 1 d . . .
H42A H 0.0668 0.1398 -0.1363 0.067 Uiso 1 1 calc R . .
C43 C 0.0506(3) 0.12196(18) -0.2469(3) 0.0556(11) Uani 1 1 d . . .
H43A H -0.0119 0.1255 -0.2666 0.067 Uiso 1 1 calc R . .
C44 C 0.0950(3) 0.10815(16) -0.2954(2) 0.0437(9) Uani 1 1 d . . .
C45 C 0.1852(3) 0.10246(19) -0.2664(2) 0.0535(11) Uani 1 1 d . . .
H45A H 0.2155 0.0913 -0.2989 0.064 Uiso 1 1 calc R . .
C46 C 0.2324(3) 0.11287(18) -0.1899(2) 0.0548(11) Uani 1 1 d . . .
H46A H 0.2952 0.1109 -0.1712 0.066 Uiso 1 1 calc R . .
C47 C 0.0465(3) 0.09917(15) -0.3795(2) 0.0420(9) Uani 1 1 d . . .
C48 C 0.3979(3) 0.24495(15) 0.0320(2) 0.0418(9) Uani 1 1 d . . .
C49 C 0.3571(3) 0.28630(15) -0.0114(2) 0.0424(9) Uani 1 1 d . . .
H49A H 0.2963 0.2845 -0.0427 0.051 Uiso 1 1 calc R . .
C50 C 0.4034(3) 0.32957(15) -0.0096(2) 0.0401(9) Uani 1 1 d . . .
H50A H 0.3742 0.3577 -0.0386 0.048 Uiso 1 1 calc R . .
C51 C 0.4936(3) 0.33233(15) 0.0350(2) 0.0400(9) Uani 1 1 d . . .
C52 C 0.5342(3) 0.29118(16) 0.0794(2) 0.0453(9) Uani 1 1 d . . .
H52A H 0.5951 0.2929 0.1105 0.054 Uiso 1 1 calc R . .
C53 C 0.4875(3) 0.24818(16) 0.0788(2) 0.0465(9) Uani 1 1 d . . .
H53A H 0.5158 0.2207 0.1100 0.056 Uiso 1 1 calc R . .
C54 C 0.5446(3) 0.37820(15) 0.0324(2) 0.0416(9) Uani 1 1 d . . .
O1T O 0.9716(4) 0.4632(2) 0.6727(3) 0.145(3) Uani 1 1 d D . .
C1T C 0.9503(6) 0.4156(3) 0.6533(4) 0.134(4) Uani 1 1 d D . .
H1TA H 0.9173 0.4010 0.6841 0.160 Uiso 1 1 calc R . .
H1TB H 1.0039 0.3953 0.6605 0.160 Uiso 1 1 calc R . .
C2T C 0.8941(11) 0.4185(4) 0.5715(6) 0.264(11) Uani 1 1 d D . .
H2TA H 0.9302 0.4130 0.5388 0.317 Uiso 1 1 calc R . .
H2TB H 0.8472 0.3927 0.5590 0.317 Uiso 1 1 calc R . .
C3T C 0.8570(9) 0.4657(4) 0.5592(6) 0.225(9) Uani 1 1 d D . .
H3TA H 0.7966 0.4652 0.5614 0.270 Uiso 1 1 calc R . .
H3TB H 0.8540 0.4788 0.5087 0.270 Uiso 1 1 calc R . .
C4T C 0.9141(10) 0.4948(3) 0.6190(7) 0.264(12) Uani 1 1 d D . .
H4TA H 0.9480 0.5181 0.5985 0.317 Uiso 1 1 calc R . .
H4TB H 0.8793 0.5147 0.6432 0.317 Uiso 1 1 calc R . .
O2T O 0.1526(5) -0.1477(3) 0.2263(4) 0.142(2) Uani 1 1 d D . .
C5T C 0.1402(7) -0.1068(3) 0.1712(5) 0.131(3) Uani 1 1 d D . .
H5TA H 0.0901 -0.1143 0.1234 0.157 Uiso 1 1 calc R . .
H5TB H 0.1273 -0.0753 0.1929 0.157 Uiso 1 1 calc R . .
C6T C 0.2203(7) -0.1023(4) 0.1557(6) 0.137(3) Uani 1 1 d D . .
H6TA H 0.2374 -0.0668 0.1555 0.165 Uiso 1 1 calc R . .
H6TB H 0.2138 -0.1173 0.1054 0.165 Uiso 1 1 calc R . .
C7T C 0.2869(7) -0.1299(5) 0.2190(7) 0.156(4) Uani 1 1 d D . .
H7TA H 0.3373 -0.1413 0.2046 0.187 Uiso 1 1 calc R . .
H7TB H 0.3091 -0.1097 0.2665 0.187 Uiso 1 1 calc R . .
C8T C 0.2327(8) -0.1713(5) 0.2266(10) 0.203(7) Uani 1 1 d D . .
H8TA H 0.2205 -0.1948 0.1831 0.243 Uiso 1 1 calc R . .
H8TB H 0.2618 -0.1896 0.2751 0.243 Uiso 1 1 calc R . .
O3T O 0.4384(5) -0.1380(4) 0.1222(4) 0.164(3) Uani 1 1 d D . .
C9T C 0.5001(8) -0.1538(5) 0.0868(6) 0.174(5) Uani 1 1 d D . .
H9TA H 0.4846 -0.1876 0.0644 0.209 Uiso 1 1 calc R . .
H9TB H 0.5609 -0.1548 0.1251 0.209 Uiso 1 1 calc R . .
C10T C 0.4945(12) -0.1178(6) 0.0272(9) 0.266(12) Uani 1 1 d D . .
H10A H 0.5546 -0.1075 0.0303 0.319 Uiso 1 1 calc R . .
H10B H 0.4637 -0.1326 -0.0239 0.319 Uiso 1 1 calc R . .
C11T C 0.4458(13) -0.0750(5) 0.0384(9) 0.242(9) Uani 1 1 d D . .
H11B H 0.4849 -0.0455 0.0545 0.290 Uiso 1 1 calc R . .
H11C H 0.3962 -0.0668 -0.0094 0.290 Uiso 1 1 calc R . .
C12T C 0.4134(14) -0.0896(5) 0.0971(13) 0.281(13) Uani 1 1 d D . .
H12B H 0.4364 -0.0664 0.1410 0.337 Uiso 1 1 calc R . .
H12C H 0.3480 -0.0873 0.0774 0.337 Uiso 1 1 calc R . .
O4T O 0.7620(16) 0.3070(4) 0.6234(11) 0.448(17) Uani 1 1 d D . .
C13T C 0.7213(10) 0.2961(5) 0.5495(9) 0.314(17) Uani 1 1 d D . .
H13B H 0.7447 0.3167 0.5168 0.377 Uiso 1 1 calc R . .
H13C H 0.6567 0.3016 0.5338 0.377 Uiso 1 1 calc R . .
C14T C 0.7413(12) 0.2427(5) 0.5440(6) 0.214(8) Uani 1 1 d D . .
H14B H 0.6874 0.2246 0.5121 0.256 Uiso 1 1 calc R . .
H14C H 0.7873 0.2388 0.5206 0.256 Uiso 1 1 calc R . .
C15T C 0.7712(6) 0.2243(3) 0.6180(7) 0.166(6) Uani 1 1 d D . .
H15B H 0.8121 0.1959 0.6238 0.199 Uiso 1 1 calc R . .
H15C H 0.7216 0.2141 0.6343 0.199 Uiso 1 1 calc R . .
C16T C 0.8155(13) 0.2668(5) 0.6586(8) 0.37(2) Uani 1 1 d D . .
H16B H 0.8219 0.2646 0.7134 0.440 Uiso 1 1 calc R . .
H16C H 0.8750 0.2701 0.6550 0.440 Uiso 1 1 calc R . .
O5T O 1.0593(7) 0.3162(3) 0.5503(7) 0.208(4) Uani 1 1 d D . .
C17T C 1.1052(7) 0.2729(4) 0.5313(9) 0.180(6) Uani 1 1 d D . .
H17B H 1.1062 0.2761 0.4787 0.216 Uiso 1 1 calc R . .
H17C H 1.1668 0.2705 0.5677 0.216 Uiso 1 1 calc R . .
C18T C 1.0555(9) 0.2300(4) 0.5372(9) 0.190(6) Uani 1 1 d D . .
H18B H 1.0713 0.2185 0.5909 0.227 Uiso 1 1 calc R . .
H18C H 1.0624 0.2021 0.5048 0.227 Uiso 1 1 calc R . .
C19T C 0.9665(9) 0.2516(6) 0.5076(16) 0.45(3) Uani 1 1 d D . .
H19B H 0.9403 0.2462 0.4515 0.538 Uiso 1 1 calc R . .
H19C H 0.9282 0.2350 0.5318 0.538 Uiso 1 1 calc R . .
C20T C 0.9710(6) 0.3042(4) 0.5238(10) 0.231(10) Uani 1 1 d D . .
H20B H 0.9389 0.3234 0.4768 0.278 Uiso 1 1 calc R . .
H20C H 0.9444 0.3117 0.5631 0.278 Uiso 1 1 calc R . .
O6T O 0.7356(6) 0.4650(4) 0.7215(7) 0.092(3) Uani 0.50 1 d PD A 1
C21T C 0.7056(9) 0.4132(4) 0.7085(7) 0.063(5) Uani 0.50 1 d PD A 1
H21B H 0.7377 0.3921 0.7532 0.076 Uiso 0.50 1 calc PR A 1
H21C H 0.7146 0.3995 0.6624 0.076 Uiso 0.50 1 calc PR A 1
C22T C 0.6110(12) 0.4159(7) 0.6973(11) 0.089(6) Uani 0.50 1 d PD A 1
H22B H 0.5924 0.3868 0.7209 0.107 Uiso 0.50 1 calc PR A 1
H22C H 0.5743 0.4173 0.6421 0.107 Uiso 0.50 1 calc PR A 1
C23T C 0.6040(16) 0.4628(7) 0.7367(17) 0.107(9) Uani 0.50 1 d PDU A 1
H23B H 0.5430 0.4762 0.7166 0.128 Uiso 0.50 1 calc PR A 1
H23C H 0.6216 0.4576 0.7927 0.128 Uiso 0.50 1 calc PR A 1
C24T C 0.6652(11) 0.4956(5) 0.7188(12) 0.119(7) Uani 0.50 1 d PDU A 1
H24B H 0.6376 0.5105 0.6672 0.143 Uiso 0.50 1 calc PR A 1
H24C H 0.6850 0.5228 0.7571 0.143 Uiso 0.50 1 calc PR A 1
O6' O 0.7137(6) 0.4481(5) 0.7618(7) 0.108(4) Uani 0.50 1 d PD B 2
C21' C 0.6308(11) 0.4755(7) 0.7354(10) 0.088(6) Uani 0.50 1 d PD B 2
H21D H 0.6412 0.5111 0.7273 0.106 Uiso 0.50 1 calc PR B 2
H21E H 0.6003 0.4731 0.7730 0.106 Uiso 0.50 1 calc PR B 2
C22' C 0.5780(9) 0.4514(7) 0.6621(8) 0.117(6) Uani 0.50 1 d PD B 2
H22D H 0.5140 0.4518 0.6542 0.141 Uiso 0.50 1 calc PR B 2
H22E H 0.5876 0.4676 0.6180 0.141 Uiso 0.50 1 calc PR B 2
C23' C 0.6140(14) 0.4001(7) 0.6742(12) 0.103(7) Uani 0.50 1 d PD B 2
H23D H 0.5915 0.3810 0.7090 0.124 Uiso 0.50 1 calc PR B 2
H23E H 0.5996 0.3819 0.6251 0.124 Uiso 0.50 1 calc PR B 2
C24' C 0.7082(15) 0.4096(10) 0.7088(18) 0.197(19) Uani 0.50 1 d PD B 2
H24D H 0.7401 0.3794 0.7351 0.236 Uiso 0.50 1 calc PR B 2
H24E H 0.7333 0.4203 0.6698 0.236 Uiso 0.50 1 calc PR B 2


_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
Ca1 O1W 2.343(3) . ?
Ca1 O10 2.420(3) 4_667 ?
Ca1 O1 2.422(3) . ?
Ca1 O3 2.428(3) 1_655 ?
Ca1 O3W 2.464(3) 3_767 ?
Ca1 O9 2.474(3) 4_667 ?
Ca1 O3W 2.520(3) . ?
Ca1 O2 2.662(3) . ?
Ca1 C47 2.794(4) 4_667 ?
Ca1 C13 2.911(4) . ?
Ca1 Ca1 3.9541(17) 3_767 ?
Ca2 O12 2.283(3) 2_645 ?
Ca2 O2W 2.338(3) . ?
Ca2 O8 2.347(3) . ?
Ca2 O2 2.367(3) 2_646 ?
Ca2 O5 2.409(3) . ?
Ca2 O6 2.550(3) . ?
Ca2 O7 2.673(3) . ?
Ca2 C27 2.839(4) . ?
Ca2 C40 2.849(4) . ?
Ca2 C54 3.153(4) 2_645 ?
Ca2 Ca3 3.7517(11) . ?
Ca3 O11 2.275(3) 2_645 ?
Ca3 O11 2.275(3) 4_566 ?
Ca3 O7 2.351(3) . ?
Ca3 O7 2.351(3) 3_656 ?
Ca3 O6 2.369(2) 3_656 ?
Ca3 O6 2.369(2) . ?
Ca3 Ca2 3.7517(11) 3_656 ?
O3W Ca1 2.464(3) 3_767 ?
O1 C13 1.262(5) . ?
O2 C13 1.241(5) . ?
O2 Ca2 2.367(3) 2_656 ?
O3 C20 1.220(5) . ?
O3 Ca1 2.428(3) 1_455 ?
O4 C20 1.320(5) . ?
O5 C27 1.260(4) . ?
O6 C27 1.286(4) . ?
O7 C40 1.272(5) . ?
O8 C40 1.247(5) . ?
O9 C47 1.262(5) . ?
O9 Ca1 2.474(3) 4_464 ?
O10 C47 1.257(5) . ?
O10 Ca1 2.420(3) 4_464 ?
O11 C54 1.259(5) . ?
O11 Ca3 2.275(3) 2_655 ?
O12 C54 1.252(5) . ?
O12 Ca2 2.283(3) 2_655 ?
C1 C6 1.391(5) . ?
C1 C2 1.396(5) . ?
C1 C7 1.502(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.392(5) . ?
C3 C14 1.489(5) . ?
C4 C5 1.397(5) . ?
C5 C6 1.395(5) . ?
C5 C21 1.484(5) . ?
C7 C12 1.381(6) . ?
C7 C8 1.396(6) . ?
C8 C9 1.389(6) . ?
C9 C10 1.380(6) . ?
C10 C11 1.386(5) . ?
C10 C13 1.499(5) . ?
C11 C12 1.373(5) . ?
C14 C19 1.393(6) . ?
C14 C15 1.398(6) . ?
C15 C16 1.387(5) . ?
C16 C17 1.397(6) . ?
C17 C18 1.402(6) . ?
C17 C20 1.480(5) . ?
C18 C19 1.382(6) . ?
C21 C26 1.400(5) . ?
C21 C22 1.402(5) . ?
C22 C23 1.379(5) . ?
C23 C24 1.391(5) . ?
C24 C25 1.400(5) . ?
C24 C27 1.484(5) . ?
C25 C26 1.383(5) . ?
C28 C29 1.391(6) . ?
C28 C33 1.404(6) . ?
C28 C34 1.476(6) . ?
C29 C30 1.399(6) . ?
C30 C31 1.373(6) . ?
C30 C41 1.483(6) . ?
C31 C32 1.403(6) . ?
C32 C33 1.388(6) . ?
C32 C48 1.484(6) . ?
C34 C35 1.401(6) . ?
C34 C39 1.409(6) . ?
C35 C36 1.374(6) . ?
C36 C37 1.390(6) . ?
C37 C38 1.411(5) . ?
C37 C40 1.495(5) . ?
C38 C39 1.361(6) . ?
C41 C46 1.385(7) . ?
C41 C42 1.385(7) . ?
C42 C43 1.395(6) . ?
C43 C44 1.384(6) . ?
C44 C45 1.372(6) . ?
C44 C47 1.505(5) . ?
C45 C46 1.388(6) . ?
C47 Ca1 2.794(4) 4_464 ?
C48 C49 1.393(6) . ?
C48 C53 1.404(6) . ?
C49 C50 1.373(6) . ?
C50 C51 1.402(6) . ?
C51 C52 1.395(6) . ?
C51 C54 1.489(6) . ?
C52 C53 1.375(6) . ?
C54 Ca2 3.153(4) 2_655 ?
O1T C1T 1.337(8) . ?
O1T C4T 1.388(8) . ?
C1T C2T 1.477(9) . ?
C2T C3T 1.383(9) . ?
C3T C4T 1.405(9) . ?
O2T C8T 1.437(10) . ?
O2T C5T 1.467(9) . ?
C5T C6T 1.425(10) . ?
C6T C7T 1.484(11) . ?
C7T C8T 1.450(12) . ?
O3T C12T 1.389(10) . ?
O3T C9T 1.437(10) . ?
C9T C10T 1.450(12) . ?
C10T C11T 1.446(13) . ?
C11T C12T 1.422(13) . ?
O4T C13T 1.333(9) . ?
O4T C16T 1.392(9) . ?
C13T C14T 1.476(10) . ?
C14T C15T 1.381(10) . ?
C15T C16T 1.413(10) . ?
O5T C20T 1.372(10) . ?
O5T C17T 1.485(11) . ?
C17T C18T 1.428(12) . ?
C18T C19T 1.465(13) . ?
C19T C20T 1.438(12) . ?
O6T C24T 1.386(14) . ?
O6T C21T 1.462(13) . ?
C21T C22T 1.468(14) . ?
C22T C23T 1.479(16) . ?
C23T C24T 1.447(14) . ?
O6' C24' 1.409(15) . ?
O6' C21' 1.451(14) . ?
C21' C22' 1.479(15) . ?
C22' C23' 1.477(16) . ?
C23' C24' 1.451(16) . ?

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
O1W Ca1 O10 146.57(11) . 4_667 ?
O1W Ca1 O1 85.68(12) . . ?
O10 Ca1 O1 126.93(11) 4_667 . ?
O1W Ca1 O3 93.01(11) . 1_655 ?
O10 Ca1 O3 90.44(10) 4_667 1_655 ?
O1 Ca1 O3 73.24(9) . 1_655 ?
O1W Ca1 O3W 83.30(11) . 3_767 ?
O10 Ca1 O3W 78.60(9) 4_667 3_767 ?
O1 Ca1 O3W 133.10(9) . 3_767 ?
O3 Ca1 O3W 152.59(9) 1_655 3_767 ?
O1W Ca1 O9 153.48(10) . 4_667 ?
O10 Ca1 O9 53.28(9) 4_667 4_667 ?
O1 Ca1 O9 82.86(11) . 4_667 ?
O3 Ca1 O9 106.34(10) 1_655 4_667 ?
O3W Ca1 O9 87.22(10) 3_767 4_667 ?
O1W Ca1 O3W 75.96(10) . . ?
O10 Ca1 O3W 72.33(9) 4_667 . ?
O1 Ca1 O3W 144.61(10) . . ?
O3 Ca1 O3W 77.74(9) 1_655 . ?
O3W Ca1 O3W 75.01(9) 3_767 . ?
O9 Ca1 O3W 125.19(10) 4_667 . ?
O1W Ca1 O2 78.64(10) . . ?
O10 Ca1 O2 125.83(9) 4_667 . ?
O1 Ca1 O2 50.47(8) . . ?
O3 Ca1 O2 123.36(9) 1_655 . ?
O3W Ca1 O2 82.66(8) 3_767 . ?
O9 Ca1 O2 75.61(9) 4_667 . ?
O3W Ca1 O2 147.77(9) . . ?
O1W Ca1 C47 162.72(12) . 4_667 ?
O10 Ca1 C47 26.68(11) 4_667 4_667 ?
O1 Ca1 C47 106.96(12) . 4_667 ?
O3 Ca1 C47 101.80(11) 1_655 4_667 ?
O3W Ca1 C47 79.45(10) 3_767 4_667 ?
O9 Ca1 C47 26.85(11) 4_667 4_667 ?
O3W Ca1 C47 98.36(11) . 4_667 ?
O2 Ca1 C47 100.07(10) . 4_667 ?
O1W Ca1 C13 80.01(11) . . ?
O10 Ca1 C13 132.31(11) 4_667 . ?
O1 Ca1 C13 25.30(10) . . ?
O3 Ca1 C13 98.20(10) 1_655 . ?
O3W Ca1 C13 107.80(10) 3_767 . ?
O9 Ca1 C13 79.43(11) 4_667 . ?
O3W Ca1 C13 155.33(10) . . ?
O2 Ca1 C13 25.23(9) . . ?
C47 Ca1 C13 106.27(12) 4_667 . ?
O1W Ca1 Ca1 76.86(8) . 3_767 ?
O10 Ca1 Ca1 71.54(7) 4_667 3_767 ?
O1 Ca1 Ca1 160.98(8) . 3_767 ?
O3 Ca1 Ca1 114.70(7) 1_655 3_767 ?
O3W Ca1 Ca1 37.99(6) 3_767 3_767 ?
O9 Ca1 Ca1 109.70(8) 4_667 3_767 ?
O3W Ca1 Ca1 37.01(6) . 3_767 ?
O2 Ca1 Ca1 117.35(6) . 3_767 ?
C47 Ca1 Ca1 88.77(9) 4_667 3_767 ?
C13 Ca1 Ca1 140.32(8) . 3_767 ?
O12 Ca2 O2W 80.51(11) 2_645 . ?
O12 Ca2 O8 102.84(11) 2_645 . ?
O2W Ca2 O8 82.67(11) . . ?
O12 Ca2 O2 111.89(10) 2_645 2_646 ?
O2W Ca2 O2 78.58(10) . 2_646 ?
O8 Ca2 O2 136.73(9) . 2_646 ?
O12 Ca2 O5 154.96(10) 2_645 . ?
O2W Ca2 O5 124.52(10) . . ?
O8 Ca2 O5 81.84(10) . . ?
O2 Ca2 O5 77.51(9) 2_646 . ?
O12 Ca2 O6 102.89(10) 2_645 . ?
O2W Ca2 O6 166.39(10) . . ?
O8 Ca2 O6 109.02(9) . . ?
O2 Ca2 O6 87.98(9) 2_646 . ?
O5 Ca2 O6 53.08(8) . . ?
O12 Ca2 O7 81.80(10) 2_645 . ?
O2W Ca2 O7 125.17(10) . . ?
O8 Ca2 O7 51.86(9) . . ?
O2 Ca2 O7 155.25(9) 2_646 . ?
O5 Ca2 O7 82.13(9) . . ?
O6 Ca2 O7 68.43(8) . . ?
O12 Ca2 C27 129.56(11) 2_645 . ?
O2W Ca2 C27 148.82(11) . . ?
O8 Ca2 C27 95.99(10) . . ?
O2 Ca2 C27 81.51(10) 2_646 . ?
O5 Ca2 C27 26.16(9) . . ?
O6 Ca2 C27 26.92(9) . . ?
O7 Ca2 C27 74.05(9) . . ?
O12 Ca2 C40 93.55(11) 2_645 . ?
O2W Ca2 C40 104.58(11) . . ?
O8 Ca2 C40 25.51(10) . . ?
O2 Ca2 C40 154.46(10) 2_646 . ?
O5 Ca2 C40 80.16(10) . . ?
O6 Ca2 C40 88.46(10) . . ?
O7 Ca2 C40 26.39(10) . . ?
C27 Ca2 C40 83.93(11) . . ?
O12 Ca2 C54 19.33(11) 2_645 2_645 ?
O2W Ca2 C54 99.59(11) . 2_645 ?
O8 Ca2 C54 108.33(10) . 2_645 ?
O2 Ca2 C54 113.03(10) 2_646 2_645 ?
O5 Ca2 C54 135.83(10) . 2_645 ?
O6 Ca2 C54 83.62(10) . 2_645 ?
O7 Ca2 C54 73.01(9) . 2_645 ?
C27 Ca2 C54 110.24(11) . 2_645 ?
C40 Ca2 C54 91.67(11) . 2_645 ?
O12 Ca2 Ca3 74.93(8) 2_645 . ?
O2W Ca2 Ca3 152.09(8) . . ?
O8 Ca2 Ca3 89.98(7) . . ?
O2 Ca2 Ca3 122.87(7) 2_646 . ?
O5 Ca2 Ca3 80.53(6) . . ?
O6 Ca2 Ca3 38.54(5) . . ?
O7 Ca2 Ca3 38.51(6) . . ?
C27 Ca2 Ca3 58.56(7) . . ?
C40 Ca2 Ca3 64.53(8) . . ?
C54 Ca2 Ca3 57.28(8) 2_645 . ?
O11 Ca3 O11 180.000(7) 2_645 4_566 ?
O11 Ca3 O7 86.67(10) 2_645 . ?
O11 Ca3 O7 93.33(10) 4_566 . ?
O11 Ca3 O7 93.33(10) 2_645 3_656 ?
O11 Ca3 O7 86.67(10) 4_566 3_656 ?
O7 Ca3 O7 180.0 . 3_656 ?
O11 Ca3 O6 95.44(9) 2_645 3_656 ?
O11 Ca3 O6 84.56(9) 4_566 3_656 ?
O7 Ca3 O6 102.97(9) . 3_656 ?
O7 Ca3 O6 77.03(9) 3_656 3_656 ?
O11 Ca3 O6 84.56(9) 2_645 . ?
O11 Ca3 O6 95.44(9) 4_566 . ?
O7 Ca3 O6 77.03(9) . . ?
O7 Ca3 O6 102.97(9) 3_656 . ?
O6 Ca3 O6 180.0 3_656 . ?
O11 Ca3 Ca2 117.88(7) 2_645 3_656 ?
O11 Ca3 Ca2 62.12(7) 4_566 3_656 ?
O7 Ca3 Ca2 134.92(7) . 3_656 ?
O7 Ca3 Ca2 45.08(7) 3_656 3_656 ?
O6 Ca3 Ca2 42.11(6) 3_656 3_656 ?
O6 Ca3 Ca2 137.89(6) . 3_656 ?
O11 Ca3 Ca2 62.12(7) 2_645 . ?
O11 Ca3 Ca2 117.88(7) 4_566 . ?
O7 Ca3 Ca2 45.08(7) . . ?
O7 Ca3 Ca2 134.92(7) 3_656 . ?
O6 Ca3 Ca2 137.89(6) 3_656 . ?
O6 Ca3 Ca2 42.11(6) . . ?
Ca2 Ca3 Ca2 180.0 3_656 . ?
Ca1 O3W Ca1 104.99(9) 3_767 . ?
C13 O1 Ca1 99.6(2) . . ?
C13 O2 Ca2 136.3(2) . 2_656 ?
C13 O2 Ca1 88.7(2) . . ?
Ca2 O2 Ca1 128.30(10) 2_656 . ?
C20 O3 Ca1 140.2(2) . 1_455 ?
C27 O5 Ca2 96.3(2) . . ?
C27 O6 Ca3 128.1(2) . . ?
C27 O6 Ca2 89.2(2) . . ?
Ca3 O6 Ca2 99.35(9) . . ?
C40 O7 Ca3 168.4(3) . . ?
C40 O7 Ca2 84.5(2) . . ?
Ca3 O7 Ca2 96.41(9) . . ?
C40 O8 Ca2 100.4(2) . . ?
C47 O9 Ca1 90.9(2) . 4_464 ?
C47 O10 Ca1 93.5(2) . 4_464 ?
C54 O11 Ca3 141.2(3) . 2_655 ?
C54 O12 Ca2 123.6(3) . 2_655 ?
C6 C1 C2 118.3(3) . . ?
C6 C1 C7 122.4(3) . . ?
C2 C1 C7 119.2(3) . . ?
C3 C2 C1 121.8(4) . . ?
C4 C3 C2 118.5(3) . . ?
C4 C3 C14 121.9(3) . . ?
C2 C3 C14 119.6(3) . . ?
C3 C4 C5 121.2(3) . . ?
C6 C5 C4 118.8(4) . . ?
C6 C5 C21 121.4(3) . . ?
C4 C5 C21 119.8(3) . . ?
C1 C6 C5 121.4(3) . . ?
C12 C7 C8 118.1(3) . . ?
C12 C7 C1 120.6(3) . . ?
C8 C7 C1 121.3(4) . . ?
C9 C8 C7 120.2(4) . . ?
C10 C9 C8 121.1(4) . . ?
C9 C10 C11 118.4(3) . . ?
C9 C10 C13 122.4(3) . . ?
C11 C10 C13 119.2(3) . . ?
C12 C11 C10 120.8(4) . . ?
C11 C12 C7 121.5(3) . . ?
O2 C13 O1 121.0(3) . . ?
O2 C13 C10 120.0(3) . . ?
O1 C13 C10 119.0(3) . . ?
O2 C13 Ca1 66.09(19) . . ?
O1 C13 Ca1 55.14(19) . . ?
C10 C13 Ca1 172.0(3) . . ?
C19 C14 C15 118.7(3) . . ?
C19 C14 C3 120.8(4) . . ?
C15 C14 C3 120.5(3) . . ?
C16 C15 C14 121.2(4) . . ?
C15 C16 C17 119.4(4) . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 C20 118.9(4) . . ?
C18 C17 C20 121.4(4) . . ?
C19 C18 C17 120.0(4) . . ?
C18 C19 C14 120.8(4) . . ?
O3 C20 O4 123.7(3) . . ?
O3 C20 C17 122.7(3) . . ?
O4 C20 C17 113.6(3) . . ?
C26 C21 C22 118.6(3) . . ?
C26 C21 C5 120.6(3) . . ?
C22 C21 C5 120.8(3) . . ?
C23 C22 C21 120.8(4) . . ?
C22 C23 C24 120.4(3) . . ?
C23 C24 C25 119.3(3) . . ?
C23 C24 C27 119.5(3) . . ?
C25 C24 C27 121.2(3) . . ?
C26 C25 C24 120.2(3) . . ?
C25 C26 C21 120.6(3) . . ?
O5 C27 O6 121.4(3) . . ?
O5 C27 C24 119.1(3) . . ?
O6 C27 C24 119.6(3) . . ?
O5 C27 Ca2 57.49(19) . . ?
O6 C27 Ca2 63.88(19) . . ?
C24 C27 Ca2 175.9(2) . . ?
C29 C28 C33 119.0(4) . . ?
C29 C28 C34 120.0(4) . . ?
C33 C28 C34 121.0(4) . . ?
C28 C29 C30 120.9(4) . . ?
C31 C30 C29 119.0(4) . . ?
C31 C30 C41 118.4(4) . . ?
C29 C30 C41 122.5(4) . . ?
C30 C31 C32 121.8(4) . . ?
C33 C32 C31 118.5(4) . . ?
C33 C32 C48 123.4(4) . . ?
C31 C32 C48 118.0(3) . . ?
C32 C33 C28 120.8(4) . . ?
C35 C34 C39 117.5(4) . . ?
C35 C34 C28 121.5(4) . . ?
C39 C34 C28 121.0(4) . . ?
C36 C35 C34 121.7(4) . . ?
C35 C36 C37 120.4(4) . . ?
C36 C37 C38 118.5(4) . . ?
C36 C37 C40 122.2(3) . . ?
C38 C37 C40 119.3(3) . . ?
C39 C38 C37 120.9(4) . . ?
C38 C39 C34 121.1(4) . . ?
O8 C40 O7 123.1(4) . . ?
O8 C40 C37 118.5(3) . . ?
O7 C40 C37 118.4(3) . . ?
O8 C40 Ca2 54.13(19) . . ?
O7 C40 Ca2 69.1(2) . . ?
C37 C40 Ca2 171.8(3) . . ?
C46 C41 C42 119.0(4) . . ?
C46 C41 C30 119.7(4) . . ?
C42 C41 C30 120.9(4) . . ?
C41 C42 C43 120.1(4) . . ?
C44 C43 C42 120.2(4) . . ?
C45 C44 C43 119.6(4) . . ?
C45 C44 C47 118.9(4) . . ?
C43 C44 C47 121.5(4) . . ?
C44 C45 C46 120.3(4) . . ?
C41 C46 C45 120.6(4) . . ?
O10 C47 O9 121.2(4) . . ?
O10 C47 C44 118.4(4) . . ?
O9 C47 C44 120.4(4) . . ?
O10 C47 Ca1 59.8(2) . 4_464 ?
O9 C47 Ca1 62.3(2) . 4_464 ?
C44 C47 Ca1 171.4(3) . 4_464 ?
C49 C48 C53 119.0(4) . . ?
C49 C48 C32 118.7(4) . . ?
C53 C48 C32 122.2(4) . . ?
C50 C49 C48 121.0(4) . . ?
C49 C50 C51 120.1(4) . . ?
C52 C51 C50 118.9(3) . . ?
C52 C51 C54 121.4(4) . . ?
C50 C51 C54 119.7(4) . . ?
C53 C52 C51 121.0(4) . . ?
C52 C53 C48 119.9(4) . . ?
O12 C54 O11 124.9(4) . . ?
O12 C54 C51 117.1(4) . . ?
O11 C54 C51 118.0(4) . . ?
O12 C54 Ca2 37.11(19) . 2_655 ?
O11 C54 Ca2 88.1(2) . 2_655 ?
C51 C54 Ca2 153.1(3) . 2_655 ?
C1T O1T C4T 110.1(5) . . ?
O1T C1T C2T 103.6(6) . . ?
C3T C2T C1T 107.0(7) . . ?
C2T C3T C4T 104.6(7) . . ?
O1T C4T C3T 108.6(7) . . ?
C8T O2T C5T 103.4(7) . . ?
C6T C5T O2T 107.1(8) . . ?
C5T C6T C7T 104.6(9) . . ?
C8T C7T C6T 99.5(9) . . ?
O2T C8T C7T 103.6(9) . . ?
C12T O3T C9T 106.7(9) . . ?
O3T C9T C10T 106.7(9) . . ?
C11T C10T C9T 108.0(10) . . ?
C12T C11T C10T 104.9(11) . . ?
O3T C12T C11T 112.0(10) . . ?
C13T O4T C16T 108.5(7) . . ?
O4T C13T C14T 104.1(7) . . ?
C15T C14T C13T 106.5(7) . . ?
C14T C15T C16T 100.5(8) . . ?
O4T C16T C15T 104.8(8) . . ?
C20T O5T C17T 105.8(7) . . ?
C18T C17T O5T 105.7(9) . . ?
C17T C18T C19T 99.0(11) . . ?
C20T C19T C18T 109.7(9) . . ?
O5T C20T C19T 106.0(8) . . ?
C24T O6T C21T 109.7(9) . . ?
O6T C21T C22T 104.1(10) . . ?
C21T C22T C23T 103.1(12) . . ?
C24T C23T C22T 103.1(14) . . ?
O6T C24T C23T 104.3(13) . . ?
C24' O6' C21' 108.0(11) . . ?
O6' C21' C22' 104.8(10) . . ?
C23' C22' C21' 101.4(11) . . ?
C24' C23' C22' 101.5(15) . . ?
O6' C24' C23' 103.7(13) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1WA O10 0.8399(11) 2.39(4) 2.692(4) 102(3) 2_655
O1W H1WB O6' 0.8399(11) 2.01(2) 2.723(9) 142(3) .
O1W H1WB O6T 0.8399(11) 2.118(12) 2.819(11) 140.7(9) .
O2W H2WA O9 0.8400(11) 1.888(16) 2.672(4) 155(4) 3
O2W H2WB O2T 0.8399(11) 1.965(10) 2.769(8) 159.8(19) .
O3W H3WA O5 0.8399(11) 1.999(7) 2.745(3) 147.5(11) 4_666
O3W H3WB O4W 0.8400(11) 1.837(5) 2.667(4) 169.4(13) .
O4W H4WA O1T 0.8401(11) 1.953(14) 2.772(6) 165(4) .
O4W H4WB O8 0.8401(12) 2.001(14) 2.815(4) 163(5) 4_666
O4 H4O O1 0.83(2) 1.72(2) 2.540(4) 175(4) 1_455

_diffrn_measured_fraction_theta_max 0.930
_diffrn_reflns_theta_full        28.07
_diffrn_measured_fraction_theta_full 0.930
_refine_diff_density_max         1.047
_refine_diff_density_min         -0.851
_refine_diff_density_rms         0.149
_database_code_depnum_ccdc_archive 'CCDC 986428'
#######################################################################
#
#                 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_ZnCaBTB

#============================================================================== 
_audit_creation_method           SHELXL-97
_chemical_name_systematic        ZnCaBTB
_chemical_name_common            ZnCaBTB
_chemical_melting_point          none
_chemical_formula_moiety         
'C54 H34 Ca1 O14 Zn2, 3(C2.48 H1.86 O0.62), 3(C2.6 O0.65), 3(H0.88 O0.44)'
_chemical_formula_sum            'C69.25 H65.28 Ca O19.14 Zn2'
_chemical_formula_weight         1374.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0020 0.0010 '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 0.0090 0.0050 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.1980 0.2510 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.3480 1.1820 '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 1 c'
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_Int_Tables_number      163

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

_cell_length_a                   16.550(2)
_cell_length_b                   16.550(2)
_cell_length_c                   14.748(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     3498.3(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1428
_exptl_absorpt_coefficient_mu    0.597
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.63000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31148
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0138
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.76
_diffrn_reflns_theta_max         24.83
_reflns_number_total             2894
_reflns_number_gt                2836
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0976P)²+6.0873P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.052(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2894
_refine_ls_number_parameters     193
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0707
_refine_ls_R_factor_gt           0.0701
_refine_ls_wR_factor_ref         0.2010
_refine_ls_wR_factor_gt          0.2006
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_restrained_S_all      1.187
_refine_ls_shift/su_max          0.002
_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
Ca1 Ca 0.3333 0.6667 0.7500 0.0205(3) Uani 1 6 d S . .
Zn1 Zn 0.3333 0.6667 0.50022(4) 0.0298(3) Uani 1 3 d SD . .
O1 O 0.46627(16) 0.74470(17) 0.52074(18) 0.0390(6) Uani 1 1 d . . .
O2 O 0.45175(16) 0.67857(16) 0.65641(17) 0.0352(6) Uani 1 1 d . . .
O1W O 0.3333 0.6667 0.3641(4) 0.0674(17) Uani 1 3 d SD . .
H1W H 0.2780(12) 0.646(7) 0.3468(4) 0.081 Uiso 0.67 1 d PD . .
C1 C 0.4995(2) 0.7326(2) 0.5943(2) 0.0335(7) Uani 1 1 d . . .
C2 C 0.6036(2) 0.7882(2) 0.6036(2) 0.0312(6) Uani 1 1 d . . .
C3 C 0.6508(2) 0.7586(2) 0.6598(2) 0.0321(6) Uani 1 1 d . . .
H3 H 0.6167 0.7032 0.6945 0.068(16) Uiso 1 1 calc R . .
C4 C 0.7475(2) 0.8091(2) 0.6659(2) 0.0306(6) Uani 1 1 d . . .
H4 H 0.7791 0.7866 0.7028 0.037 Uiso 1 1 calc R . .
C5 C 0.7990(2) 0.8930(2) 0.61818(18) 0.0260(6) Uani 1 1 d . . .
C6 C 0.7508(2) 0.9234(2) 0.5634(2) 0.0317(6) Uani 1 1 d . . .
H6 H 0.7842 0.9808 0.5317 0.038 Uiso 1 1 calc R . .
C7 C 0.6540(2) 0.8703(2) 0.5547(2) 0.0358(7) Uani 1 1 d . . .
H7 H 0.6223 0.8905 0.5151 0.043 Uiso 1 1 calc R . .
C8 C 0.9023(2) 0.94773(19) 0.62362(17) 0.0249(6) Uani 1 1 d . . .
C9 C 0.9485(2) 1.0452(2) 0.62407(17) 0.0256(6) Uani 1 1 d . . .
H9 H 0.9131 1.0761 0.6247 0.031 Uiso 1 1 calc R . .
O3 O 0.5468(8) 0.9534(6) 0.1831(6) 0.071(4) Uani 0.310(8) 1 d PG A 1
C10 C 0.5475(8) 1.0391(6) 0.1636(6) 0.061(4) Uani 0.310(8) 1 d PG A 1
H10A H 0.6115 1.0931 0.1695 0.073 Uiso 0.155(4) 1 calc PR A 1
H10B H 0.5061 1.0477 0.2061 0.073 Uiso 0.155(4) 1 calc PR A 1
C11 C 0.5125(8) 1.0311(7) 0.0660(6) 0.049(3) Uani 0.310(8) 1 d PG A 1
H11A H 0.5531 1.0888 0.0317 0.059 Uiso 0.310(8) 1 calc PR A 1
H11B H 0.4480 1.0201 0.0654 0.059 Uiso 0.310(8) 1 calc PR A 1
C12 C 0.5158(8) 0.9474(6) 0.0246(5) 0.057(4) Uani 0.310(8) 1 d PG A 1
H12A H 0.4524 0.8933 0.0160 0.069 Uiso 0.310(8) 1 calc PR A 1
H12B H 0.5492 0.9639 -0.0341 0.069 Uiso 0.310(8) 1 calc PR A 1
C13 C 0.5700(8) 0.9279(7) 0.0975(7) 0.076(6) Uani 0.310(8) 1 d PG A 1
H13A H 0.5516 0.8610 0.0974 0.092 Uiso 0.310(8) 1 calc PR A 1
H13B H 0.6380 0.9654 0.0861 0.092 Uiso 0.310(8) 1 calc PR A 1
O4 O 0.5974(15) 0.7542(17) 0.2371(14) 0.189(19) Uani 0.326(9) 1 d PD . 2
C14 C 0.6081(13) 0.8199(16) 0.1714(10) 0.24(2) Uani 0.651(18) 1 d PD . 2
H14A H 0.5768 0.7895 0.1138 0.290 Uiso 0.651(18) 1 calc PR . 2
H14B H 0.6747 0.8650 0.1594 0.290 Uiso 0.651(18) 1 calc PR . 2
C15 C 0.559(3) 0.867(2) 0.2187(17) 0.26(4) Uani 0.326(9) 1 d PD . 2
H15A H 0.6001 0.9354 0.2216 0.308 Uiso 0.326(9) 1 calc PR . 2
H15B H 0.5005 0.8526 0.1868 0.308 Uiso 0.326(9) 1 calc PR . 2
C16 C 0.538(4) 0.824(5) 0.314(2) 0.27(4) Uani 0.326(9) 1 d PD . 2
H16A H 0.4729 0.7714 0.3181 0.320 Uiso 0.326(9) 1 calc PR . 2
H16B H 0.5473 0.8709 0.3604 0.320 Uiso 0.326(9) 1 calc PR . 2
O2W O 0.1869(10) 0.5934(5) 0.2500 0.25(3) Uani 0.44(3) 2 d SP B 3
H2W H 0.1512 0.5559 0.2892 0.295 Uiso 0.44(3) 1 d P B 3


_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
Ca1 O2 2.323(2) 2_665 ?
Ca1 O2 2.323(2) 5_556 ?
Ca1 O2 2.323(2) 3_565 ?
Ca1 O2 2.323(2) 6_566 ?
Ca1 O2 2.323(2) . ?
Ca1 O2 2.323(2) 4_666 ?
Ca1 Zn1 3.6837(10) . ?
Ca1 Zn1 3.6837(9) 4_666 ?
Zn1 O1 1.939(2) 2_665 ?
Zn1 O1 1.939(2) . ?
Zn1 O1 1.939(2) 3_565 ?
Zn1 O1W 2.008(6) . ?
O1 C1 1.277(4) . ?
O2 C1 1.248(4) . ?
O1W H1W 0.841(5) . ?
C1 C2 1.500(4) . ?
C2 C3 1.386(5) . ?
C2 C7 1.389(5) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.402(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.394(4) . ?
C5 C8 1.484(4) . ?
C6 C7 1.396(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.392(4) 2_765 ?
C8 C9 1.398(4) . ?
C9 C8 1.392(4) 3_675 ?
C9 H9 0.9500 . ?
O3 C10 1.4429 . ?
O3 C13 1.4433 . ?
C10 C11 1.5317 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 C12 1.5388 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C13 1.5350 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
O4 C15 1.11(3) 6_565 ?
O4 C16 1.15(3) 6_565 ?
O4 C14 1.399(16) . ?
O4 C14 1.439(19) 6_565 ?
O4 O4 1.52(5) 6_565 ?
C14 C15 1.547(19) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 C16 1.538(19) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C14 1.55(2) 6_565 ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
O2W H2W 0.837(9) . ?

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
O2 Ca1 O2 86.15(12) 2_665 5_556 ?
O2 Ca1 O2 88.32(9) 2_665 3_565 ?
O2 Ca1 O2 97.85(12) 5_556 3_565 ?
O2 Ca1 O2 97.85(12) 2_665 6_566 ?
O2 Ca1 O2 88.32(9) 5_556 6_566 ?
O2 Ca1 O2 171.58(11) 3_565 6_566 ?
O2 Ca1 O2 88.32(9) 2_665 . ?
O2 Ca1 O2 171.58(12) 5_556 . ?
O2 Ca1 O2 88.32(9) 3_565 . ?
O2 Ca1 O2 86.15(13) 6_566 . ?
O2 Ca1 O2 171.58(12) 2_665 4_666 ?
O2 Ca1 O2 88.32(9) 5_556 4_666 ?
O2 Ca1 O2 86.15(13) 3_565 4_666 ?
O2 Ca1 O2 88.32(9) 6_566 4_666 ?
O2 Ca1 O2 97.85(12) . 4_666 ?
O2 Ca1 Zn1 53.56(7) 2_665 . ?
O2 Ca1 Zn1 126.44(7) 5_556 . ?
O2 Ca1 Zn1 53.56(7) 3_565 . ?
O2 Ca1 Zn1 126.44(7) 6_566 . ?
O2 Ca1 Zn1 53.56(7) . . ?
O2 Ca1 Zn1 126.44(7) 4_666 . ?
O2 Ca1 Zn1 126.44(7) 2_665 4_666 ?
O2 Ca1 Zn1 53.56(7) 5_556 4_666 ?
O2 Ca1 Zn1 126.44(7) 3_565 4_666 ?
O2 Ca1 Zn1 53.56(7) 6_566 4_666 ?
O2 Ca1 Zn1 126.44(7) . 4_666 ?
O2 Ca1 Zn1 53.56(7) 4_666 4_666 ?
Zn1 Ca1 Zn1 180.0 . 4_666 ?
O1 Zn1 O1 117.61(4) 2_665 . ?
O1 Zn1 O1 117.61(4) 2_665 3_565 ?
O1 Zn1 O1 117.61(4) . 3_565 ?
O1 Zn1 O1W 98.98(8) 2_665 . ?
O1 Zn1 O1W 98.98(8) . . ?
O1 Zn1 O1W 98.98(8) 3_565 . ?
O1 Zn1 Ca1 81.02(8) 2_665 . ?
O1 Zn1 Ca1 81.02(8) . . ?
O1 Zn1 Ca1 81.02(8) 3_565 . ?
O1W Zn1 Ca1 180.000(1) . . ?
C1 O1 Zn1 117.6(2) . . ?
C1 O2 Ca1 134.6(2) . . ?
Zn1 O1W H1W 107.6(7) . . ?
O2 C1 O1 124.6(3) . . ?
O2 C1 C2 119.6(3) . . ?
O1 C1 C2 115.7(3) . . ?
C3 C2 C7 119.3(3) . . ?
C3 C2 C1 121.0(3) . . ?
C7 C2 C1 119.7(3) . . ?
C2 C3 C4 120.6(3) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C5 120.7(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C6 C5 C4 118.3(3) . . ?
C6 C5 C8 120.3(3) . . ?
C4 C5 C8 121.4(3) . . ?
C5 C6 C7 120.7(3) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C2 C7 C6 120.4(3) . . ?
C2 C7 H7 119.8 . . ?
C6 C7 H7 119.8 . . ?
C9 C8 C9 119.0(3) 2_765 . ?
C9 C8 C5 120.7(3) 2_765 . ?
C9 C8 C5 120.2(3) . . ?
C8 C9 C8 121.0(3) 3_675 . ?
C8 C9 H9 119.5 3_675 . ?
C8 C9 H9 119.5 . . ?
C10 O3 C13 103.9 . . ?
O3 C10 C11 106.6 . . ?
O3 C10 H10A 110.4 . . ?
C11 C10 H10A 110.4 . . ?
O3 C10 H10B 110.4 . . ?
C11 C10 H10B 110.4 . . ?
H10A C10 H10B 108.6 . . ?
C10 C11 C12 105.6 . . ?
C10 C11 H11A 110.6 . . ?
C12 C11 H11A 110.6 . . ?
C10 C11 H11B 110.6 . . ?
C12 C11 H11B 110.6 . . ?
H11A C11 H11B 108.7 . . ?
C13 C12 C11 101.5 . . ?
C13 C12 H12A 111.5 . . ?
C11 C12 H12A 111.5 . . ?
C13 C12 H12B 111.5 . . ?
C11 C12 H12B 111.5 . . ?
H12A C12 H12B 109.3 . . ?
O3 C13 C12 106.4 . . ?
O3 C13 H13A 110.4 . . ?
C12 C13 H13A 110.4 . . ?
O3 C13 H13B 110.4 . . ?
C12 C13 H13B 110.4 . . ?
H13A C13 H13B 108.6 . . ?
C15 O4 C16 86(2) 6_565 6_565 ?
C15 O4 C14 156(3) 6_565 . ?
C16 O4 C14 74.3(14) 6_565 . ?
C15 O4 C14 73.4(13) 6_565 6_565 ?
C16 O4 C14 138(4) 6_565 6_565 ?
C14 O4 C14 114(2) . 6_565 ?
C15 O4 O4 118(2) 6_565 6_565 ?
C16 O4 O4 108(3) 6_565 6_565 ?
C14 O4 O4 58.9(11) . 6_565 ?
C14 O4 O4 56.3(14) 6_565 6_565 ?
O4 C14 C15 100.6(15) . . ?
O4 C14 H14A 111.6 . . ?
C15 C14 H14A 111.6 . . ?
O4 C14 H14B 111.6 . . ?
C15 C14 H14B 111.6 . . ?
H14A C14 H14B 109.4 . . ?
C16 C15 C14 103.4(13) . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C15 C16 C14 105.4(14) . 6_565 ?
C15 C16 H16A 110.7 . . ?
C14 C16 H16A 110.7 6_565 . ?
C15 C16 H16B 110.7 . . ?
C14 C16 H16B 110.7 6_565 . ?
H16A C16 H16B 108.8 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.83
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.840
_refine_diff_density_min         -0.766
_refine_diff_density_rms         0.158
_chemical_compound_source        'chemical reaction'
_chemical_properties_physical    Moisture-sensitive
_exptl_crystal_preparation       'gas adsorption properties'
_database_code_depnum_ccdc_archive 'CCDC 986349'
