# 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.
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data_Compound-1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H15 Cd3 O19, 2(C4 H9 N O), C2 H8 N'
_chemical_formula_sum            'C42 H41 Cd3 N3 O21'
_chemical_formula_weight         1260.98

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'
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'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   21.9035(6)
_cell_length_b                   14.5496(4)
_cell_length_c                   27.9653(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     8912.2(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5975
_cell_measurement_theta_min      3.0360
_cell_measurement_theta_max      29.1400

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.880
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5008
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.72667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            22819
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0669
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         2.36
_diffrn_reflns_theta_max         25.00
_reflns_number_total             7837
_reflns_number_gt                5904
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.1000P)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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7837
_refine_ls_number_parameters     631
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0492
_refine_ls_wR_factor_ref         0.1608
_refine_ls_wR_factor_gt          0.1372
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_restrained_S_all      0.999
_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
Cd1 Cd 1.05904(2) 0.33788(3) -0.025598(15) 0.02561(16) Uani 1 1 d . . .
Cd2 Cd 0.93467(2) 0.22070(4) -0.219657(14) 0.02530(16) Uani 1 1 d . . .
Cd3 Cd 1.00214(2) 0.18173(3) -0.111209(15) 0.02530(16) Uani 1 1 d . . .
C1 C 1.1599(3) 0.2860(4) -0.1533(2) 0.0227(13) Uani 1 1 d . . .
C2 C 1.1282(3) 0.2661(4) -0.1955(2) 0.0230(13) Uani 1 1 d . . .
C3 C 1.1608(3) 0.2571(4) -0.2374(2) 0.0251(14) Uani 1 1 d . . .
C4 C 1.2235(3) 0.2683(5) -0.2393(2) 0.0342(17) Uani 1 1 d . . .
H4A H 1.2445 0.2620 -0.2680 0.041 Uiso 1 1 calc R . .
C5 C 1.2542(3) 0.2895(6) -0.1969(2) 0.0414(19) Uani 1 1 d . . .
H5A H 1.2962 0.2993 -0.1974 0.050 Uiso 1 1 calc R . .
C6 C 1.2228(3) 0.2961(5) -0.1542(2) 0.0378(18) Uani 1 1 d . . .
H6A H 1.2439 0.3073 -0.1260 0.045 Uiso 1 1 calc R . .
C7 C 1.1279(3) 0.2981(4) -0.1065(2) 0.0269(15) Uani 1 1 d . . .
C8 C 1.0605(3) 0.2557(5) -0.1996(2) 0.0270(15) Uani 1 1 d . . .
C9 C 1.1142(3) 0.2859(4) -0.31388(18) 0.0214(14) Uani 1 1 d . . .
C10 C 1.1034(3) 0.2460(5) -0.35791(19) 0.0259(14) Uani 1 1 d . . .
H10A H 1.1078 0.1830 -0.3622 0.031 Uiso 1 1 calc R . .
C11 C 1.0856(3) 0.3021(5) -0.3956(2) 0.0232(14) Uani 1 1 d . . .
C12 C 1.0778(3) 0.3936(5) -0.3884(2) 0.0253(14) Uani 1 1 d . . .
H12A H 1.0656 0.4307 -0.4138 0.030 Uiso 1 1 calc R . .
C13 C 1.0876(3) 0.4327(4) -0.34376(19) 0.0220(13) Uani 1 1 d . . .
C14 C 1.1064(3) 0.3776(4) -0.30615(19) 0.0247(14) Uani 1 1 d . . .
H14A H 1.1136 0.4028 -0.2761 0.030 Uiso 1 1 calc R . .
C15 C 1.0759(3) 0.2586(5) -0.4436(2) 0.0249(14) Uani 1 1 d . . .
C16 C 1.0785(3) 0.5348(4) -0.3371(2) 0.0239(14) Uani 1 1 d . . .
C17 C 0.8670(3) 0.2941(4) -0.0499(2) 0.0211(13) Uani 1 1 d . . .
C18 C 0.8375(3) 0.2820(4) -0.0942(2) 0.0239(14) Uani 1 1 d . . .
C19 C 0.7748(3) 0.2730(6) -0.0952(2) 0.0399(19) Uani 1 1 d . . .
H19A H 0.7548 0.2685 -0.1244 0.048 Uiso 1 1 calc R . .
C20 C 0.7412(3) 0.2708(6) -0.0535(3) 0.0420(19) Uani 1 1 d . . .
H20A H 0.6990 0.2641 -0.0547 0.050 Uiso 1 1 calc R . .
C21 C 0.7702(3) 0.2784(5) -0.0098(2) 0.0329(16) Uani 1 1 d . . .
H21A H 0.7478 0.2752 0.0185 0.039 Uiso 1 1 calc R . .
C22 C 0.8309(3) 0.2904(4) -0.0084(2) 0.0267(14) Uani 1 1 d . . .
C23 C 0.9351(3) 0.3090(5) -0.0422(2) 0.0213(14) Uani 1 1 d . . .
C24 C 0.8728(3) 0.2769(4) -0.1400(2) 0.0278(15) Uani 1 1 d . . .
C25 C 0.8800(3) 0.2350(4) 0.0619(2) 0.0233(14) Uani 1 1 d . . .
C26 C 0.8926(3) 0.2547(5) 0.1091(2) 0.0280(15) Uani 1 1 d . . .
H26A H 0.8888 0.3146 0.1205 0.034 Uiso 1 1 calc R . .
C27 C 0.9110(3) 0.1848(5) 0.1397(2) 0.0279(15) Uani 1 1 d . . .
C28 C 0.9176(3) 0.0963(5) 0.1225(2) 0.0288(15) Uani 1 1 d . . .
H28A H 0.9288 0.0491 0.1431 0.035 Uiso 1 1 calc R . .
C29 C 0.9076(3) 0.0780(5) 0.0744(2) 0.0284(15) Uani 1 1 d . . .
C30 C 0.8873(3) 0.1473(4) 0.04376(19) 0.0247(14) Uani 1 1 d . . .
H30A H 0.8789 0.1348 0.0118 0.030 Uiso 1 1 calc R . .
C31 C 0.9193(3) 0.2080(5) 0.1919(2) 0.0282(15) Uani 1 1 d . . .
C32 C 0.9162(3) -0.0175(5) 0.0565(2) 0.0329(16) Uani 1 1 d . . .
C33 C 0.7970(4) 0.5173(7) -0.1336(3) 0.061(2) Uani 1 1 d . . .
C34 C 0.7550(7) 0.5138(12) -0.1762(4) 0.135(6) Uani 1 1 d . . .
H34A H 0.7787 0.5045 -0.2048 0.202 Uiso 1 1 calc R . .
H34B H 0.7330 0.5706 -0.1786 0.202 Uiso 1 1 calc R . .
H34C H 0.7267 0.4639 -0.1725 0.202 Uiso 1 1 calc R . .
C35 C 0.7089(4) 0.5304(8) -0.0811(4) 0.087(3) Uani 1 1 d . . .
H35A H 0.6861 0.5278 -0.1104 0.130 Uiso 1 1 calc R . .
H35B H 0.6989 0.5859 -0.0643 0.130 Uiso 1 1 calc R . .
H35C H 0.6987 0.4783 -0.0616 0.130 Uiso 1 1 calc R . .
C36 C 0.8141(4) 0.5322(7) -0.0503(3) 0.065(3) Uani 1 1 d . . .
H36A H 0.8560 0.5316 -0.0605 0.097 Uiso 1 1 calc R . .
H36B H 0.8064 0.4798 -0.0304 0.097 Uiso 1 1 calc R . .
H36C H 0.8063 0.5874 -0.0325 0.097 Uiso 1 1 calc R . .
C37 C 1.2047(5) 0.5263(6) -0.1205(3) 0.053(2) Uani 1 1 d . . .
C38 C 1.2493(5) 0.5218(8) -0.0797(3) 0.079(3) Uani 1 1 d . . .
H38A H 1.2274 0.5150 -0.0501 0.118 Uiso 1 1 calc R . .
H38B H 1.2730 0.5773 -0.0788 0.118 Uiso 1 1 calc R . .
H38C H 1.2760 0.4701 -0.0840 0.118 Uiso 1 1 calc R . .
C39 C 1.1817(4) 0.5334(7) -0.2032(3) 0.067(3) Uani 1 1 d . . .
H39A H 1.1410 0.5346 -0.1906 0.100 Uiso 1 1 calc R . .
H39B H 1.1874 0.4786 -0.2217 0.100 Uiso 1 1 calc R . .
H39C H 1.1881 0.5863 -0.2232 0.100 Uiso 1 1 calc R . .
C40 C 1.2916(4) 0.5350(7) -0.1755(3) 0.065(3) Uani 1 1 d . . .
H40A H 1.3159 0.5365 -0.1469 0.097 Uiso 1 1 calc R . .
H40B H 1.3005 0.5881 -0.1946 0.097 Uiso 1 1 calc R . .
H40C H 1.3010 0.4804 -0.1934 0.097 Uiso 1 1 calc R . .
C41 C 1.0011(4) 0.5116(9) -0.1415(4) 0.085(4) Uani 1 1 d . . .
H41A H 0.9978 0.4721 -0.1141 0.127 Uiso 1 1 calc R . .
H41B H 0.9878 0.5724 -0.1331 0.127 Uiso 1 1 calc R . .
H41C H 1.0428 0.5137 -0.1519 0.127 Uiso 1 1 calc R . .
C42 C 0.9674(5) 0.5344(7) -0.2232(3) 0.078(3) Uani 1 1 d . . .
H42A H 0.9421 0.5092 -0.2481 0.116 Uiso 1 1 calc R . .
H42B H 1.0090 0.5362 -0.2339 0.116 Uiso 1 1 calc R . .
H42C H 0.9540 0.5955 -0.2158 0.116 Uiso 1 1 calc R . .
O1 O 1.1563(2) 0.3068(4) -0.06884(15) 0.0415(13) Uani 1 1 d . . .
O1W O 1.0872(3) 0.4831(4) -0.03270(19) 0.0501(14) Uani 1 1 d D . .
H1WB H 1.079(4) 0.538(3) -0.024(3) 0.075 Uiso 1 1 d D . .
H1WA H 1.107(4) 0.492(6) -0.0584(18) 0.075 Uiso 1 1 d D . .
O2 O 1.0687(2) 0.3005(3) -0.10639(14) 0.0255(10) Uani 1 1 d . . .
O3 O 1.0294(2) 0.3179(4) -0.21725(17) 0.0457(14) Uani 1 1 d . . .
O4 O 1.0369(2) 0.1783(4) -0.18791(16) 0.0387(12) Uani 1 1 d . . .
O5 O 1.1303(2) 0.2245(3) -0.27778(13) 0.0280(10) Uani 1 1 d . . .
O6 O 1.0650(2) 0.1750(3) -0.44570(15) 0.0389(13) Uani 1 1 d . . .
O7 O 1.0798(2) 0.3066(3) -0.48117(15) 0.0371(12) Uani 1 1 d . . .
O8 O 1.0663(2) 0.5789(3) -0.37458(17) 0.0408(13) Uani 1 1 d . . .
O9 O 1.0845(2) 0.5690(3) -0.29639(15) 0.0344(11) Uani 1 1 d . . .
O10 O 0.93020(19) 0.2909(3) -0.13956(15) 0.0275(10) Uani 1 1 d . . .
O11 O 0.8452(2) 0.2542(4) -0.17683(14) 0.0413(13) Uani 1 1 d . . .
O12 O 0.9686(2) 0.2387(3) -0.04221(13) 0.0285(10) Uani 1 1 d . . .
O13 O 0.9543(2) 0.3853(4) -0.03359(17) 0.0387(12) Uani 1 1 d . . .
O14 O 0.8604(2) 0.3088(3) 0.03465(14) 0.0297(11) Uani 1 1 d . . .
O15 O 0.9077(3) -0.0265(4) 0.01062(17) 0.0590(18) Uani 1 1 d . . .
H15 H 0.911(5) -0.088(7) 0.003(3) 0.088 Uiso 1 1 d . . .
O16 O 0.9278(2) -0.0812(4) 0.08272(17) 0.0457(14) Uani 1 1 d . . .
O17 O 0.9134(2) 0.1484(4) 0.22258(15) 0.0448(13) Uani 1 1 d . . .
O18 O 0.9309(3) 0.2909(4) 0.20176(18) 0.0492(15) Uani 1 1 d . . .
O19 O 0.8529(3) 0.5104(5) -0.1393(2) 0.078(2) Uani 1 1 d . . .
O20 O 1.1483(2) 0.5190(4) -0.11396(17) 0.0488(14) Uani 1 1 d . . .
N1 N 0.7744(3) 0.5291(5) -0.0918(3) 0.0573(19) Uani 1 1 d . . .
N2 N 1.2266(3) 0.5348(5) -0.1628(3) 0.059(2) Uani 1 1 d . . .
N3 N 0.9629(3) 0.4760(5) -0.1801(3) 0.061(2) Uani 1 1 d . . .
H3B H 0.9238 0.4740 -0.1702 0.073 Uiso 1 1 calc R . .
H3A H 0.9746 0.4184 -0.1873 0.073 Uiso 1 1 calc R . .


_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
Cd1 O1W 2.210(5) . ?
Cd1 O6 2.246(4) 7_566 ?
Cd1 O2 2.333(4) . ?
Cd1 O13 2.405(5) . ?
Cd1 O7 2.484(5) 7_566 ?
Cd1 O1 2.492(5) . ?
Cd1 O12 2.494(5) . ?
Cd1 C15 2.714(6) 7_566 ?
Cd2 O18 2.205(5) 7_565 ?
Cd2 O9 2.290(5) 3_744 ?
Cd2 O11 2.348(5) . ?
Cd2 O10 2.464(4) . ?
Cd2 O4 2.486(5) . ?
Cd2 O3 2.512(6) . ?
Cd2 O17 2.540(5) 7_565 ?
Cd2 C31 2.702(6) 7_565 ?
Cd2 C24 2.731(6) . ?
Cd2 Cd3 3.4210(6) . ?
Cd3 O8 2.155(5) 3_744 ?
Cd3 O12 2.225(4) . ?
Cd3 O16 2.264(5) 5_755 ?
Cd3 O2 2.265(5) . ?
Cd3 O4 2.276(5) . ?
Cd3 O10 2.374(4) . ?
C1 C6 1.385(9) . ?
C1 C2 1.400(8) . ?
C1 C7 1.494(8) . ?
C2 C3 1.380(8) . ?
C2 C8 1.495(9) . ?
C3 C4 1.384(9) . ?
C3 O5 1.394(7) . ?
C4 C5 1.399(10) . ?
C4 H4A 0.9300 . ?
C5 C6 1.381(9) . ?
C5 H5A 0.9300 . ?
C6 H6A 0.9300 . ?
C7 O1 1.229(7) . ?
C7 O2 1.298(8) . ?
C8 O3 1.236(8) . ?
C8 O4 1.281(8) . ?
C9 C14 1.363(9) . ?
C9 C10 1.381(8) . ?
C9 O5 1.393(7) . ?
C10 C11 1.388(9) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(9) . ?
C11 C15 1.499(8) . ?
C12 C13 1.389(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.385(8) . ?
C13 C16 1.511(9) . ?
C14 H14A 0.9300 . ?
C15 O6 1.241(8) . ?
C15 O7 1.265(8) . ?
C15 Cd1 2.714(6) 7_565 ?
C16 O9 1.249(7) . ?
C16 O8 1.258(7) . ?
C17 C22 1.406(8) . ?
C17 C18 1.407(8) . ?
C17 C23 1.523(8) . ?
C18 C19 1.380(9) . ?
C18 C24 1.500(8) . ?
C19 C20 1.379(9) . ?
C19 H19A 0.9300 . ?
C20 C21 1.382(10) . ?
C20 H20A 0.9300 . ?
C21 C22 1.340(9) . ?
C21 H21A 0.9300 . ?
C22 O14 1.393(7) . ?
C23 O13 1.212(8) . ?
C23 O12 1.258(8) . ?
C24 O11 1.238(7) . ?
C24 O10 1.273(8) . ?
C25 C26 1.380(8) . ?
C25 C30 1.382(9) . ?
C25 O14 1.384(7) . ?
C26 C27 1.388(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.383(9) . ?
C27 C31 1.510(8) . ?
C28 C29 1.388(8) . ?
C28 H28A 0.9300 . ?
C29 C30 1.396(9) . ?
C29 C32 1.489(9) . ?
C30 H30A 0.9300 . ?
C31 O17 1.226(8) . ?
C31 O18 1.262(9) . ?
C31 Cd2 2.702(6) 7_566 ?
C32 O16 1.210(8) . ?
C32 O15 1.302(8) . ?
C33 O19 1.239(10) . ?
C33 N1 1.281(11) . ?
C33 C34 1.506(13) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N1 1.467(11) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 N1 1.451(10) . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 O20 1.254(10) . ?
C37 N2 1.281(10) . ?
C37 C38 1.504(12) . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 N2 1.498(10) . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 N2 1.468(10) . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 N3 1.459(12) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 N3 1.480(11) . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
O1W H1WB 0.85(2) . ?
O1W H1WA 0.84(2) . ?
O6 Cd1 2.246(4) 7_565 ?
O7 Cd1 2.484(5) 7_565 ?
O8 Cd3 2.155(5) 3_754 ?
O9 Cd2 2.290(5) 3_754 ?
O15 H15 0.93(10) . ?
O16 Cd3 2.264(5) 5_755 ?
O17 Cd2 2.540(5) 7_566 ?
O18 Cd2 2.205(5) 7_566 ?
N3 H3B 0.9000 . ?
N3 H3A 0.9000 . ?

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 Cd1 O6 98.79(19) . 7_566 ?
O1W Cd1 O2 96.35(18) . . ?
O6 Cd1 O2 159.80(17) 7_566 . ?
O1W Cd1 O13 89.1(2) . . ?
O6 Cd1 O13 99.90(17) 7_566 . ?
O2 Cd1 O13 93.62(15) . . ?
O1W Cd1 O7 143.4(2) . 7_566 ?
O6 Cd1 O7 54.63(16) 7_566 7_566 ?
O2 Cd1 O7 105.70(15) . 7_566 ?
O13 Cd1 O7 117.62(18) . 7_566 ?
O1W Cd1 O1 83.7(2) . . ?
O6 Cd1 O1 114.69(17) 7_566 . ?
O2 Cd1 O1 53.88(15) . . ?
O13 Cd1 O1 145.33(15) . . ?
O7 Cd1 O1 86.15(16) 7_566 . ?
O1W Cd1 O12 139.3(2) . . ?
O6 Cd1 O12 100.57(16) 7_566 . ?
O2 Cd1 O12 75.92(14) . . ?
O13 Cd1 O12 52.51(16) . . ?
O7 Cd1 O12 75.46(16) 7_566 . ?
O1 Cd1 O12 118.95(15) . . ?
O1W Cd1 C15 122.2(2) . 7_566 ?
O6 Cd1 C15 26.92(18) 7_566 7_566 ?
O2 Cd1 C15 133.26(18) . 7_566 ?
O13 Cd1 C15 110.89(18) . 7_566 ?
O7 Cd1 C15 27.71(17) 7_566 7_566 ?
O1 Cd1 C15 101.53(17) . 7_566 ?
O12 Cd1 C15 88.07(17) . 7_566 ?
O18 Cd2 O9 96.58(18) 7_565 3_744 ?
O18 Cd2 O11 119.51(19) 7_565 . ?
O9 Cd2 O11 86.96(18) 3_744 . ?
O18 Cd2 O10 159.38(18) 7_565 . ?
O9 Cd2 O10 102.37(15) 3_744 . ?
O11 Cd2 O10 54.34(15) . . ?
O18 Cd2 O4 111.78(18) 7_565 . ?
O9 Cd2 O4 81.72(17) 3_744 . ?
O11 Cd2 O4 128.38(15) . . ?
O10 Cd2 O4 79.27(14) . . ?
O18 Cd2 O3 95.79(19) 7_565 . ?
O9 Cd2 O3 133.50(17) 3_744 . ?
O11 Cd2 O3 124.00(18) . . ?
O10 Cd2 O3 77.00(15) . . ?
O4 Cd2 O3 52.13(16) . . ?
O18 Cd2 O17 54.31(18) 7_565 7_565 ?
O9 Cd2 O17 144.42(17) 3_744 7_565 ?
O11 Cd2 O17 90.93(17) . 7_565 ?
O10 Cd2 O17 105.07(15) . 7_565 ?
O4 Cd2 O17 125.30(17) . 7_565 ?
O3 Cd2 O17 75.30(17) . 7_565 ?
O18 Cd2 C31 27.5(2) 7_565 7_565 ?
O9 Cd2 C31 121.76(19) 3_744 7_565 ?
O11 Cd2 C31 106.47(19) . 7_565 ?
O10 Cd2 C31 131.89(19) . 7_565 ?
O4 Cd2 C31 122.27(18) . 7_565 ?
O3 Cd2 C31 84.90(17) . 7_565 ?
O17 Cd2 C31 26.82(18) 7_565 7_565 ?
O18 Cd2 C24 144.7(2) 7_565 . ?
O9 Cd2 C24 92.16(17) 3_744 . ?
O11 Cd2 C24 26.89(17) . . ?
O10 Cd2 C24 27.77(16) . . ?
O4 Cd2 C24 103.28(17) . . ?
O3 Cd2 C24 102.68(18) . . ?
O17 Cd2 C24 101.74(17) 7_565 . ?
C31 Cd2 C24 124.7(2) 7_565 . ?
O18 Cd2 Cd3 152.50(15) 7_565 . ?
O9 Cd2 Cd3 75.27(11) 3_744 . ?
O11 Cd2 Cd3 86.72(11) . . ?
O10 Cd2 Cd3 43.94(10) . . ?
O4 Cd2 Cd3 41.69(10) . . ?
O3 Cd2 Cd3 73.30(10) . . ?
O17 Cd2 Cd3 140.10(12) 7_565 . ?
C31 Cd2 Cd3 158.19(14) 7_565 . ?
C24 Cd2 Cd3 62.68(14) . . ?
O8 Cd3 O12 100.90(17) 3_744 . ?
O8 Cd3 O16 95.0(2) 3_744 5_755 ?
O12 Cd3 O16 99.16(17) . 5_755 ?
O8 Cd3 O2 171.29(17) 3_744 . ?
O12 Cd3 O2 82.89(16) . . ?
O16 Cd3 O2 92.07(18) 5_755 . ?
O8 Cd3 O4 92.50(17) 3_744 . ?
O12 Cd3 O4 159.32(18) . . ?
O16 Cd3 O4 95.23(19) 5_755 . ?
O2 Cd3 O4 81.82(16) . . ?
O8 Cd3 O10 86.63(18) 3_744 . ?
O12 Cd3 O10 79.70(15) . . ?
O16 Cd3 O10 178.15(18) 5_755 . ?
O2 Cd3 O10 86.35(16) . . ?
O4 Cd3 O10 85.50(17) . . ?
O8 Cd3 Cd2 69.58(13) 3_744 . ?
O12 Cd3 Cd2 124.37(11) . . ?
O16 Cd3 Cd2 135.37(13) 5_755 . ?
O2 Cd3 Cd2 101.79(11) . . ?
O4 Cd3 Cd2 46.58(13) . . ?
O10 Cd3 Cd2 46.07(11) . . ?
C6 C1 C2 119.9(6) . . ?
C6 C1 C7 118.1(5) . . ?
C2 C1 C7 122.0(6) . . ?
C3 C2 C1 118.7(6) . . ?
C3 C2 C8 115.9(5) . . ?
C1 C2 C8 125.4(5) . . ?
C2 C3 C4 122.4(6) . . ?
C2 C3 O5 118.2(6) . . ?
C4 C3 O5 118.9(5) . . ?
C3 C4 C5 118.1(6) . . ?
C3 C4 H4A 121.0 . . ?
C5 C4 H4A 121.0 . . ?
C6 C5 C4 120.5(6) . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
C5 C6 C1 120.4(6) . . ?
C5 C6 H6A 119.8 . . ?
C1 C6 H6A 119.8 . . ?
O1 C7 O2 120.1(6) . . ?
O1 C7 C1 121.6(6) . . ?
O2 C7 C1 118.2(5) . . ?
O3 C8 O4 121.5(6) . . ?
O3 C8 C2 120.3(6) . . ?
O4 C8 C2 118.0(6) . . ?
C14 C9 C10 122.1(5) . . ?
C14 C9 O5 123.0(5) . . ?
C10 C9 O5 114.9(5) . . ?
C9 C10 C11 118.6(6) . . ?
C9 C10 H10A 120.7 . . ?
C11 C10 H10A 120.7 . . ?
C12 C11 C10 119.9(5) . . ?
C12 C11 C15 121.9(6) . . ?
C10 C11 C15 118.1(6) . . ?
C11 C12 C13 121.0(6) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C14 C13 C12 119.5(6) . . ?
C14 C13 C16 121.0(5) . . ?
C12 C13 C16 119.5(5) . . ?
C9 C14 C13 118.9(5) . . ?
C9 C14 H14A 120.5 . . ?
C13 C14 H14A 120.5 . . ?
O6 C15 O7 121.0(6) . . ?
O6 C15 C11 118.9(6) . . ?
O7 C15 C11 120.1(6) . . ?
O6 C15 Cd1 55.0(3) . 7_565 ?
O7 C15 Cd1 66.0(3) . 7_565 ?
C11 C15 Cd1 173.8(5) . 7_565 ?
O9 C16 O8 125.3(6) . . ?
O9 C16 C13 119.4(5) . . ?
O8 C16 C13 115.2(5) . . ?
C22 C17 C18 117.6(6) . . ?
C22 C17 C23 116.1(5) . . ?
C18 C17 C23 126.3(5) . . ?
C19 C18 C17 119.1(6) . . ?
C19 C18 C24 119.5(6) . . ?
C17 C18 C24 121.4(6) . . ?
C20 C19 C18 121.0(6) . . ?
C20 C19 H19A 119.5 . . ?
C18 C19 H19A 119.5 . . ?
C19 C20 C21 120.1(6) . . ?
C19 C20 H20A 119.9 . . ?
C21 C20 H20A 119.9 . . ?
C22 C21 C20 119.4(6) . . ?
C22 C21 H21A 120.3 . . ?
C20 C21 H21A 120.3 . . ?
C21 C22 O14 120.7(6) . . ?
C21 C22 C17 122.6(6) . . ?
O14 C22 C17 116.4(6) . . ?
O13 C23 O12 122.7(6) . . ?
O13 C23 C17 119.9(6) . . ?
O12 C23 C17 117.2(6) . . ?
O11 C24 O10 122.3(6) . . ?
O11 C24 C18 118.1(6) . . ?
O10 C24 C18 119.5(5) . . ?
O11 C24 Cd2 59.0(3) . . ?
O10 C24 Cd2 64.4(3) . . ?
C18 C24 Cd2 165.4(4) . . ?
C26 C25 C30 121.3(6) . . ?
C26 C25 O14 115.3(6) . . ?
C30 C25 O14 123.3(5) . . ?
C25 C26 C27 119.7(6) . . ?
C25 C26 H26A 120.1 . . ?
C27 C26 H26A 120.1 . . ?
C28 C27 C26 119.8(6) . . ?
C28 C27 C31 122.2(6) . . ?
C26 C27 C31 117.9(6) . . ?
C27 C28 C29 120.0(6) . . ?
C27 C28 H28A 120.0 . . ?
C29 C28 H28A 120.0 . . ?
C28 C29 C30 120.4(6) . . ?
C28 C29 C32 119.1(6) . . ?
C30 C29 C32 120.5(5) . . ?
C25 C30 C29 118.6(5) . . ?
C25 C30 H30A 120.7 . . ?
C29 C30 H30A 120.7 . . ?
O17 C31 O18 123.0(6) . . ?
O17 C31 C27 120.3(6) . . ?
O18 C31 C27 116.6(6) . . ?
O17 C31 Cd2 69.2(3) . 7_566 ?
O18 C31 Cd2 53.8(3) . 7_566 ?
C27 C31 Cd2 170.3(5) . 7_566 ?
O16 C32 O15 123.4(7) . . ?
O16 C32 C29 122.5(6) . . ?
O15 C32 C29 114.1(6) . . ?
O19 C33 N1 120.6(9) . . ?
O19 C33 C34 119.9(10) . . ?
N1 C33 C34 119.4(10) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 H35A 109.5 . . ?
N1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N1 C36 H36A 109.5 . . ?
N1 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
N1 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
O20 C37 N2 120.8(8) . . ?
O20 C37 C38 121.7(8) . . ?
N2 C37 C38 117.5(9) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
N2 C39 H39A 109.5 . . ?
N2 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
N2 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N2 C40 H40A 109.5 . . ?
N2 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
N2 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
N3 C41 H41A 109.5 . . ?
N3 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
N3 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N3 C42 H42A 109.5 . . ?
N3 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
N3 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C7 O1 Cd1 90.1(4) . . ?
Cd1 O1W H1WB 145(7) . . ?
Cd1 O1W H1WA 111(6) . . ?
H1WB O1W H1WA 101(9) . . ?
C7 O2 Cd3 128.5(4) . . ?
C7 O2 Cd1 95.6(3) . . ?
Cd3 O2 Cd1 100.21(16) . . ?
C8 O3 Cd2 93.1(4) . . ?
C8 O4 Cd3 110.9(4) . . ?
C8 O4 Cd2 93.1(4) . . ?
Cd3 O4 Cd2 91.73(17) . . ?
C9 O5 C3 119.3(5) . . ?
C15 O6 Cd1 98.1(4) . 7_565 ?
C15 O7 Cd1 86.3(4) . 7_565 ?
C16 O8 Cd3 130.9(4) . 3_754 ?
C16 O9 Cd2 122.9(4) . 3_754 ?
C24 O10 Cd3 123.4(4) . . ?
C24 O10 Cd2 87.9(4) . . ?
Cd3 O10 Cd2 89.99(15) . . ?
C24 O11 Cd2 94.1(4) . . ?
C23 O12 Cd3 119.7(4) . . ?
C23 O12 Cd1 89.7(4) . . ?
Cd3 O12 Cd1 96.61(16) . . ?
C23 O13 Cd1 95.0(4) . . ?
C25 O14 C22 118.1(5) . . ?
C32 O15 H15 108(6) . . ?
C32 O16 Cd3 148.4(5) . 5_755 ?
C31 O17 Cd2 84.0(4) . 7_566 ?
C31 O18 Cd2 98.7(4) . 7_566 ?
C33 N1 C36 120.3(8) . . ?
C33 N1 C35 124.4(8) . . ?
C36 N1 C35 115.0(8) . . ?
C37 N2 C40 125.9(8) . . ?
C37 N2 C39 116.7(8) . . ?
C40 N2 C39 116.9(7) . . ?
C41 N3 C42 111.2(8) . . ?
C41 N3 H3B 109.4 . . ?
C42 N3 H3B 109.4 . . ?
C41 N3 H3A 109.4 . . ?
C42 N3 H3A 109.4 . . ?
H3B N3 H3A 108.0 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.690
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.145
_database_code_depnum_ccdc_archive 'CCDC 990734'
#######################################################################
#
#                 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_Compound-2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H6 Cd O9, 2(C4 H9 N O), Ca '
_chemical_formula_sum            'C24 H24 Ca Cd N2 O11'
_chemical_formula_weight         668.93

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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   12.0047(7)
_cell_length_b                   10.9563(7)
_cell_length_c                   21.0767(15)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.389(7)
_cell_angle_gamma                90.00
_cell_volume                     2659.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2896
_cell_measurement_theta_min      2.5607
_cell_measurement_theta_max      29.0305

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Eos'
_diffrn_measurement_method       'multiwire proportional'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            6968
_diffrn_reflns_av_R_equivalents  0.0232
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.00
_reflns_number_total             4683
_reflns_number_gt                3617
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0303P)²+2.7095P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4324
_refine_ls_number_parameters     352
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0868
_refine_ls_wR_factor_gt          0.0804
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_restrained_S_all      1.133
_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
Cd1 Cd 0.63605(2) 1.68064(3) -0.039712(14) 0.02231(11) Uani 1 1 d . . .
Ca2 Ca 0.35622(6) 1.55455(8) -0.12728(4) 0.0217(2) Uani 1 1 d . . .
O1 O 0.6272(2) 1.7688(3) -0.13490(14) 0.0336(8) Uani 1 1 d . . .
O2 O 0.4381(2) 1.7243(3) -0.16496(15) 0.0339(8) Uani 1 1 d . . .
O3 O 0.2204(2) 1.8812(3) -0.40912(15) 0.0345(8) Uani 1 1 d . . .
O4 O 0.3097(2) 1.7736(3) -0.46972(14) 0.0342(8) Uani 1 1 d . . .
O5 O 0.7319(2) 1.8495(3) -0.34110(15) 0.0341(8) Uani 1 1 d . . .
O6 O 0.9634(2) 1.9686(3) -0.39303(16) 0.0413(9) Uani 1 1 d . . .
O7 O 0.7819(3) 2.0004(3) -0.45050(17) 0.0412(8) Uani 1 1 d . . .
O8 O 1.0417(3) 1.6771(3) -0.49329(16) 0.0391(8) Uani 1 1 d . . .
O9 O 0.9441(3) 1.8487(3) -0.52188(15) 0.0329(7) Uani 1 1 d . . .
O10 O 0.3144(3) 1.4925(4) -0.23725(17) 0.0612(11) Uani 1 1 d . . .
O11 O 0.1819(3) 1.6488(4) -0.1385(2) 0.0688(13) Uani 1 1 d . . .
N1 N 0.3842(11) 1.4840(6) -0.3233(4) 0.149(4) Uani 1 1 d . . .
N2 N 0.0087(4) 1.6584(5) -0.1236(3) 0.0718(17) Uani 1 1 d . . .
C1 C 0.5283(3) 1.7624(4) -0.1764(2) 0.0238(9) Uani 1 1 d . . .
C2 C 0.5227(3) 1.7997(4) -0.24616(19) 0.0206(9) Uani 1 1 d . . .
C3 C 0.4188(3) 1.8068(4) -0.2959(2) 0.0228(9) Uani 1 1 d . . .
H3A H 0.3489 1.8005 -0.2854 0.027 Uiso 1 1 calc R . .
C4 C 0.4182(3) 1.8231(4) -0.36094(19) 0.0232(9) Uani 1 1 d . . .
C5 C 0.5231(3) 1.8329(4) -0.3768(2) 0.0274(10) Uani 1 1 d . . .
H5A H 0.5234 1.8399 -0.4207 0.033 Uiso 1 1 calc R . .
C6 C 0.6258(3) 1.8322(4) -0.3272(2) 0.0253(10) Uani 1 1 d . . .
C7 C 0.6273(3) 1.8165(4) -0.2618(2) 0.0243(9) Uani 1 1 d . . .
H7A H 0.6973 1.8170 -0.2286 0.029 Uiso 1 1 calc R . .
C8 C 0.3078(4) 1.8259(4) -0.4170(2) 0.0273(10) Uani 1 1 d . . .
C9 C 0.7656(3) 1.7604(4) -0.3787(2) 0.0286(10) Uani 1 1 d . . .
C10 C 0.8363(3) 1.7986(4) -0.4171(2) 0.0224(9) Uani 1 1 d . . .
C11 C 0.8816(3) 1.7111(4) -0.4507(2) 0.0294(11) Uani 1 1 d . . .
C12 C 0.8574(4) 1.5881(5) -0.4454(3) 0.0438(13) Uani 1 1 d . . .
H12A H 0.8903 1.5298 -0.4667 0.053 Uiso 1 1 calc R . .
C13 C 0.7841(4) 1.5526(5) -0.4083(3) 0.0545(16) Uani 1 1 d . . .
H13A H 0.7657 1.4706 -0.4061 0.065 Uiso 1 1 calc R . .
C14 C 0.7384(4) 1.6383(5) -0.3747(3) 0.0434(13) Uani 1 1 d . . .
H14A H 0.6897 1.6142 -0.3497 0.052 Uiso 1 1 calc R . .
C15 C 0.8628(4) 1.9320(4) -0.4205(2) 0.0268(10) Uani 1 1 d . . .
C16 C 0.9596(4) 1.7470(4) -0.4916(2) 0.0285(10) Uani 1 1 d . . .
C17 C 0.1783(6) 1.5015(8) -0.3491(3) 0.099(3) Uani 1 1 d . . .
H17A H 0.1831 1.4997 -0.3938 0.149 Uiso 1 1 calc RD . .
H17B H 0.1430 1.5767 -0.3415 0.149 Uiso 1 1 calc R . .
H17C H 0.1321 1.4341 -0.3420 0.149 Uiso 1 1 calc R . .
C18 C 0.3141(9) 1.4911(6) -0.2959(5) 0.100(3) Uani 1 1 d . . .
C19 C 0.3899(8) 1.4846(8) -0.3937(4) 0.123(3) Uani 1 1 d . . .
H19A H 0.3127 1.4884 -0.4232 0.184 Uiso 1 1 calc RD . .
H19B H 0.4274 1.4114 -0.4022 0.184 Uiso 1 1 calc R . .
H19C H 0.4334 1.5544 -0.4008 0.184 Uiso 1 1 calc R . .
C20 C 0.5092(6) 1.4786(7) -0.2710(4) 0.085(2) Uani 1 1 d . . .
H20A H 0.5010 1.4788 -0.2270 0.128 Uiso 1 1 calc R . .
H20B H 0.5538 1.5483 -0.2768 0.128 Uiso 1 1 calc R . .
H20C H 0.5483 1.4053 -0.2778 0.128 Uiso 1 1 calc R . .
C21 C 0.0742(5) 1.6518(5) -0.1612(3) 0.0575(16) Uani 1 1 d . . .
C22 C 0.0181(7) 1.6464(7) -0.2357(3) 0.097(3) Uani 1 1 d . . .
H22A H 0.0775 1.6416 -0.2580 0.146 Uiso 1 1 calc R . .
H22B H -0.0276 1.7185 -0.2497 0.146 Uiso 1 1 calc R . .
H22C H -0.0308 1.5757 -0.2462 0.146 Uiso 1 1 calc R . .
C23 C 0.0652(7) 1.6581(8) -0.0503(3) 0.098(3) Uani 1 1 d . . .
H23A H 0.1481 1.6574 -0.0419 0.147 Uiso 1 1 calc R . .
H23B H 0.0413 1.5869 -0.0311 0.147 Uiso 1 1 calc R . .
H23C H 0.0424 1.7300 -0.0310 0.147 Uiso 1 1 calc R . .
C24 C -0.1184(5) 1.6604(7) -0.1447(5) 0.106(3) Uani 1 1 d . . .
H24A H -0.1454 1.6603 -0.1922 0.159 Uiso 1 1 calc R . .
H24B H -0.1456 1.7326 -0.1280 0.159 Uiso 1 1 calc R . .
H24C H -0.1476 1.5895 -0.1279 0.159 Uiso 1 1 calc R . .


_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
Cd1 O1 2.202(3) . ?
Cd1 O7 2.242(3) 2_644 ?
Cd1 O4 2.245(3) 4_696 ?
Cd1 O8 2.301(3) 4_596 ?
Cd1 O9 2.458(3) 4_596 ?
Cd1 C16 2.711(4) 4_596 ?
Cd1 Ca2 3.6195(8) . ?
Ca2 O11 2.285(3) . ?
Ca2 O6 2.289(3) 2_644 ?
Ca2 O10 2.330(4) . ?
Ca2 O3 2.333(3) 2_544 ?
Ca2 O2 2.345(3) . ?
Ca2 O9 2.419(3) 4_596 ?
O1 C1 1.262(5) . ?
O2 C1 1.245(5) . ?
O3 C8 1.262(5) . ?
O3 Ca2 2.333(3) 2_554 ?
O4 C8 1.255(5) . ?
O4 Cd1 2.245(3) 4_595 ?
O5 C9 1.387(5) . ?
O5 C6 1.398(4) . ?
O6 C15 1.248(5) . ?
O6 Ca2 2.289(3) 2_654 ?
O7 C15 1.249(5) . ?
O7 Cd1 2.242(3) 2_654 ?
O8 C16 1.255(5) . ?
O8 Cd1 2.301(3) 4_695 ?
O9 C16 1.271(5) . ?
O9 Ca2 2.419(3) 4_695 ?
O9 Cd1 2.458(3) 4_695 ?
O10 C18 1.234(8) . ?
O11 C21 1.246(6) . ?
N1 C18 1.150(9) . ?
N1 C19 1.506(9) . ?
N1 C20 1.592(12) . ?
N2 C21 1.266(7) . ?
N2 C24 1.465(7) . ?
N2 C23 1.502(8) . ?
C1 C2 1.510(5) . ?
C2 C3 1.387(5) . ?
C2 C7 1.398(5) . ?
C3 C4 1.379(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.395(5) . ?
C4 C8 1.507(5) . ?
C5 C6 1.373(6) . ?
C5 H5A 0.9300 . ?
C6 C7 1.384(6) . ?
C7 H7A 0.9300 . ?
C9 C14 1.385(7) . ?
C9 C10 1.393(6) . ?
C10 C11 1.391(6) . ?
C10 C15 1.502(6) . ?
C11 C12 1.390(6) . ?
C11 C16 1.494(6) . ?
C12 C13 1.388(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.379(7) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C16 Cd1 2.711(4) 4_695 ?
C17 C18 1.703(11) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 C22 1.524(9) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?

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
O1 Cd1 O7 102.22(12) . 2_644 ?
O1 Cd1 O4 107.33(11) . 4_696 ?
O7 Cd1 O4 84.63(12) 2_644 4_696 ?
O1 Cd1 O8 100.82(12) . 4_596 ?
O7 Cd1 O8 156.55(12) 2_644 4_596 ?
O4 Cd1 O8 92.68(12) 4_696 4_596 ?
O1 Cd1 O9 112.99(10) . 4_596 ?
O7 Cd1 O9 110.74(11) 2_644 4_596 ?
O4 Cd1 O9 131.73(10) 4_696 4_596 ?
O8 Cd1 O9 55.13(10) 4_596 4_596 ?
O1 Cd1 C16 111.75(12) . 4_596 ?
O7 Cd1 C16 134.57(13) 2_644 4_596 ?
O4 Cd1 C16 111.57(12) 4_696 4_596 ?
O8 Cd1 C16 27.48(12) 4_596 4_596 ?
O9 Cd1 C16 27.92(12) 4_596 4_596 ?
O1 Cd1 Ca2 84.47(8) . . ?
O7 Cd1 Ca2 89.18(8) 2_644 . ?
O4 Cd1 Ca2 167.59(8) 4_696 . ?
O8 Cd1 Ca2 88.73(8) 4_596 . ?
O9 Cd1 Ca2 41.66(7) 4_596 . ?
C16 Cd1 Ca2 65.90(10) 4_596 . ?
O11 Ca2 O6 174.86(15) . 2_644 ?
O11 Ca2 O10 95.44(16) . . ?
O6 Ca2 O10 89.58(14) 2_644 . ?
O11 Ca2 O3 88.13(13) . 2_544 ?
O6 Ca2 O3 92.49(12) 2_644 2_544 ?
O10 Ca2 O3 95.47(13) . 2_544 ?
O11 Ca2 O2 93.79(13) . . ?
O6 Ca2 O2 85.67(12) 2_644 . ?
O10 Ca2 O2 83.55(13) . . ?
O3 Ca2 O2 177.92(12) 2_544 . ?
O11 Ca2 O9 92.68(14) . 4_596 ?
O6 Ca2 O9 82.19(11) 2_644 4_596 ?
O10 Ca2 O9 163.18(12) . 4_596 ?
O3 Ca2 O9 99.50(11) 2_544 4_596 ?
O2 Ca2 O9 81.23(11) . 4_596 ?
O11 Ca2 Cd1 124.86(11) . . ?
O6 Ca2 Cd1 50.85(9) 2_644 . ?
O10 Ca2 Cd1 121.80(10) . . ?
O3 Ca2 Cd1 122.58(7) 2_544 . ?
O2 Ca2 Cd1 56.79(7) . . ?
O9 Ca2 Cd1 42.50(7) 4_596 . ?
C1 O1 Cd1 113.6(3) . . ?
C1 O2 Ca2 143.3(3) . . ?
C8 O3 Ca2 148.6(3) . 2_554 ?
C8 O4 Cd1 103.5(2) . 4_595 ?
C9 O5 C6 117.0(3) . . ?
C15 O6 Ca2 163.6(3) . 2_654 ?
C15 O7 Cd1 106.0(3) . 2_654 ?
C16 O8 Cd1 94.8(3) . 4_695 ?
C16 O9 Ca2 144.0(3) . 4_695 ?
C16 O9 Cd1 87.2(2) . 4_695 ?
Ca2 O9 Cd1 95.84(10) 4_695 4_695 ?
C18 O10 Ca2 159.7(5) . . ?
C21 O11 Ca2 150.8(4) . . ?
C18 N1 C19 137.6(13) . . ?
C18 N1 C20 109.6(9) . . ?
C19 N1 C20 112.7(8) . . ?
C21 N2 C24 126.1(7) . . ?
C21 N2 C23 117.6(5) . . ?
C24 N2 C23 116.2(6) . . ?
O2 C1 O1 125.8(4) . . ?
O2 C1 C2 118.4(4) . . ?
O1 C1 C2 115.7(4) . . ?
C3 C2 C7 119.3(4) . . ?
C3 C2 C1 122.4(4) . . ?
C7 C2 C1 118.0(3) . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C3 C4 C5 119.7(4) . . ?
C3 C4 C8 122.6(4) . . ?
C5 C4 C8 117.7(4) . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5A 120.2 . . ?
C4 C5 H5A 120.2 . . ?
C5 C6 C7 121.0(4) . . ?
C5 C6 O5 121.1(4) . . ?
C7 C6 O5 117.9(4) . . ?
C6 C7 C2 119.4(4) . . ?
C6 C7 H7A 120.3 . . ?
C2 C7 H7A 120.3 . . ?
O4 C8 O3 124.0(4) . . ?
O4 C8 C4 116.9(4) . . ?
O3 C8 C4 119.1(4) . . ?
C14 C9 O5 122.3(4) . . ?
C14 C9 C10 121.2(4) . . ?
O5 C9 C10 116.4(4) . . ?
C11 C10 C9 118.7(4) . . ?
C11 C10 C15 121.8(4) . . ?
C9 C10 C15 119.5(4) . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 C16 118.7(4) . . ?
C10 C11 C16 120.8(4) . . ?
C13 C12 C11 119.8(5) . . ?
C13 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
C14 C13 C12 120.4(5) . . ?
C14 C13 H13A 119.8 . . ?
C12 C13 H13A 119.8 . . ?
C13 C14 C9 119.5(4) . . ?
C13 C14 H14A 120.3 . . ?
C9 C14 H14A 120.3 . . ?
O6 C15 O7 123.7(4) . . ?
O6 C15 C10 118.7(4) . . ?
O7 C15 C10 117.5(4) . . ?
O8 C16 O9 121.7(4) . . ?
O8 C16 C11 118.7(4) . . ?
O9 C16 C11 119.5(4) . . ?
O8 C16 Cd1 57.8(2) . 4_695 ?
O9 C16 Cd1 64.9(2) . 4_695 ?
C11 C16 Cd1 167.3(3) . 4_695 ?
C18 C17 H17A 109.5 . . ?
C18 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C18 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 O10 135.0(12) . . ?
N1 C18 C17 112.0(10) . . ?
O10 C18 C17 113.0(7) . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O11 C21 N2 121.4(6) . . ?
O11 C21 C22 120.2(6) . . ?
N2 C21 C22 118.4(6) . . ?
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 . . ?
N2 C23 H23A 109.5 . . ?
N2 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
N2 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 H24A 109.5 . . ?
N2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.924
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.085
_database_code_depnum_ccdc_archive 'CCDC 990735'
#######################################################################
#
#                 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_Compound-3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H6 Cd O9, C4 H9 N O, 2(H2 O), Ca '
_chemical_formula_sum            'C20 H19 Ca Cd N O12'
_chemical_formula_weight         617.84

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'
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'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   9.9912(3)
_cell_length_b                   21.7677(9)
_cell_length_c                   10.2461(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.975(3)
_cell_angle_gamma                90.00
_cell_volume                     2227.05(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3113
_cell_measurement_theta_min      2.7256
_cell_measurement_theta_max      29.0946

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.843
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1240
_exptl_absorpt_coefficient_mu    1.279
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.83162
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, Eos'
_diffrn_measurement_method       'multiwire proportional'
_diffrn_detector_area_resol_mean 16.2083
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            7986
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3918
_reflns_number_gt                3390
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0260P)²+2.1849P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3918
_refine_ls_number_parameters     328
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0728
_refine_ls_wR_factor_gt          0.0680
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.049
_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
Cd1 Cd 0.87855(2) 0.560335(12) 0.74593(2) 0.02189(9) Uani 1 1 d . . .
O1 O 0.9110(3) 0.46117(12) 0.7958(3) 0.0359(6) Uani 1 1 d . . .
O1W O 1.1467(3) 0.41251(18) 0.6730(3) 0.0569(9) Uani 1 1 d D . .
H1WA H 1.0679(18) 0.421(2) 0.646(4) 0.085 Uiso 1 1 d D . .
H1WB H 1.192(4) 0.410(3) 0.604(3) 0.085 Uiso 1 1 d D . .
O2 O 0.7703(2) 0.46638(12) 0.9599(2) 0.0313(6) Uani 1 1 d . . .
O2W O 1.4485(3) 0.47659(16) 0.8614(4) 0.0578(9) Uani 1 1 d D . .
H2WA H 1.482(4) 0.4408(8) 0.865(6) 0.087 Uiso 1 1 d D . .
H2WB H 1.5095(15) 0.4991(15) 0.831(5) 0.087 Uiso 1 1 d D . .
O3 O 0.6362(2) 0.37107(13) 0.7587(2) 0.0323(6) Uani 1 1 d . . .
O4 O 0.9757(2) 0.42243(15) 0.4150(3) 0.0436(8) Uani 1 1 d . . .
O5 O 0.8515(2) 0.45299(13) 0.2458(2) 0.0366(7) Uani 1 1 d . . .
O6 O 0.3590(2) 0.44869(15) 0.2618(3) 0.0459(8) Uani 1 1 d . . .
O7 O 0.2640(2) 0.41314(15) 0.4330(3) 0.0441(8) Uani 1 1 d . . .
O8 O 1.0577(3) 0.33903(14) 1.1637(3) 0.0437(7) Uani 1 1 d . . .
O9 O 1.0678(2) 0.41835(12) 1.0310(3) 0.0334(6) Uani 1 1 d . . .
O10 O 1.3208(4) 0.36660(16) 0.9180(4) 0.0741(11) Uani 1 1 d . . .
N1 N 1.4509(5) 0.2920(2) 0.9999(5) 0.0686(13) Uani 1 1 d . . .
C1 C 0.8403(3) 0.43762(17) 0.8838(3) 0.0241(8) Uani 1 1 d . . .
C2 C 0.8413(3) 0.36821(16) 0.8874(3) 0.0202(7) Uani 1 1 d . . .
C3 C 0.9323(3) 0.33339(17) 0.9623(3) 0.0247(8) Uani 1 1 d . . .
C4 C 0.9273(4) 0.26980(18) 0.9557(4) 0.0359(9) Uani 1 1 d . . .
H4A H 0.9864 0.2465 1.0074 0.043 Uiso 1 1 calc R . .
C5 C 0.8355(4) 0.24076(19) 0.8732(4) 0.0455(11) Uani 1 1 d . . .
H5A H 0.8368 0.1982 0.8655 0.055 Uiso 1 1 calc R . .
C6 C 0.7425(4) 0.27432(19) 0.8026(4) 0.0360(9) Uani 1 1 d . . .
H6A H 0.6788 0.2548 0.7488 0.043 Uiso 1 1 calc R . .
C7 C 0.7445(3) 0.33727(18) 0.8123(3) 0.0247(8) Uani 1 1 d . . .
C8 C 0.6358(3) 0.38774(17) 0.6285(3) 0.0236(8) Uani 1 1 d . . .
C9 C 0.5104(3) 0.39750(17) 0.5697(3) 0.0249(8) Uani 1 1 d . . .
H9A H 0.4334 0.3908 0.6161 0.030 Uiso 1 1 calc R . .
C10 C 0.7513(3) 0.39789(17) 0.5613(3) 0.0250(8) Uani 1 1 d . . .
H10A H 0.8349 0.3912 0.6016 0.030 Uiso 1 1 calc R . .
C11 C 0.7413(3) 0.41813(17) 0.4331(3) 0.0236(8) Uani 1 1 d . . .
C12 C 0.6160(3) 0.42713(17) 0.3737(3) 0.0274(8) Uani 1 1 d . . .
H12A H 0.6095 0.4399 0.2871 0.033 Uiso 1 1 calc R . .
C13 C 0.5010(3) 0.41742(17) 0.4410(3) 0.0238(8) Uani 1 1 d . . .
C14 C 0.3662(3) 0.42774(17) 0.3752(4) 0.0283(8) Uani 1 1 d . . .
C15 C 0.8642(3) 0.43209(18) 0.3597(4) 0.0292(9) Uani 1 1 d . . .
C16 C 1.0269(3) 0.36452(18) 1.0582(4) 0.0285(8) Uani 1 1 d . . .
C17 C 1.3581(5) 0.3121(3) 0.9213(6) 0.0628(15) Uani 1 1 d . . .
C18 C 1.2901(6) 0.2653(3) 0.8266(7) 0.095(2) Uani 1 1 d . . .
H18A H 1.2229 0.2858 0.7733 0.142 Uiso 1 1 calc R . .
H18B H 1.2491 0.2333 0.8759 0.142 Uiso 1 1 calc R . .
H18C H 1.3561 0.2477 0.7717 0.142 Uiso 1 1 calc R . .
C19 C 1.5180(6) 0.3362(3) 1.0891(6) 0.0872(19) Uani 1 1 d . . .
H19A H 1.4831 0.3766 1.0724 0.131 Uiso 1 1 calc R . .
H19B H 1.6126 0.3359 1.0752 0.131 Uiso 1 1 calc R . .
H19C H 1.5022 0.3248 1.1778 0.131 Uiso 1 1 calc R . .
C20 C 1.4917(5) 0.2274(2) 1.0102(6) 0.0769(18) Uani 1 1 d . . .
H20A H 1.4413 0.2035 0.9469 0.115 Uiso 1 1 calc R . .
H20B H 1.4751 0.2125 1.0963 0.115 Uiso 1 1 calc R . .
H20C H 1.5855 0.2240 0.9940 0.115 Uiso 1 1 calc R . .
Ca1 Ca 1.20996(9) 0.46020(4) 0.87577(7) 0.0351(2) Uani 1 1 d D . .


_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
Cd1 O1 2.239(3) . ?
Cd1 O4 2.268(2) 3_766 ?
Cd1 O7 2.354(2) 3_666 ?
Cd1 O9 2.375(3) 3_767 ?
Cd1 O6 2.380(2) 3_666 ?
Cd1 O8 2.454(3) 3_767 ?
Cd1 C14 2.717(3) 3_666 ?
Cd1 C16 2.732(4) 3_767 ?
O1 C1 1.272(4) . ?
O1 Ca1 3.070(3) . ?
O1W Ca1 2.388(3) . ?
O1W H1WA 0.846(10) . ?
O1W H1WB 0.852(10) . ?
O2 C1 1.235(4) . ?
O2 Ca1 2.325(3) 3_767 ?
O2W Ca1 2.420(3) . ?
O2W H2WA 0.848(10) . ?
O2W H2WB 0.850(9) . ?
O3 C8 1.382(4) . ?
O3 C7 1.404(4) . ?
O4 C15 1.250(4) . ?
O4 Cd1 2.268(2) 3_766 ?
O5 C15 1.255(4) . ?
O5 Ca1 2.334(3) 3_766 ?
O6 C14 1.248(4) . ?
O6 Cd1 2.380(2) 3_666 ?
O7 C14 1.240(4) . ?
O7 Cd1 2.354(2) 3_666 ?
O8 C16 1.245(4) . ?
O8 Cd1 2.454(3) 3_767 ?
O9 C16 1.275(4) . ?
O9 Ca1 2.352(3) . ?
O9 Cd1 2.375(3) 3_767 ?
O10 C17 1.243(6) . ?
O10 Ca1 2.352(3) . ?
N1 C17 1.284(6) . ?
N1 C20 1.467(6) . ?
N1 C19 1.472(7) . ?
C1 C2 1.511(5) . ?
C2 C7 1.389(5) . ?
C2 C3 1.394(5) . ?
C3 C4 1.387(5) . ?
C3 C16 1.501(5) . ?
C4 C5 1.379(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.369(5) . ?
C5 H5A 0.9300 . ?
C6 C7 1.374(5) . ?
C6 H6A 0.9300 . ?
C8 C10 1.382(4) . ?
C8 C9 1.388(4) . ?
C9 C13 1.388(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.385(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.387(4) . ?
C11 C15 1.492(5) . ?
C12 C13 1.377(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.502(4) . ?
C14 Cd1 2.717(3) 3_666 ?
C16 Cd1 2.732(4) 3_767 ?
C17 C18 1.548(8) . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
Ca1 O2 2.325(3) 3_767 ?
Ca1 O5 2.334(3) 3_766 ?
Ca1 H2WA 2.76(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O4 103.52(10) . 3_766 ?
O1 Cd1 O7 119.55(11) . 3_666 ?
O4 Cd1 O7 77.27(9) 3_766 3_666 ?
O1 Cd1 O9 86.70(10) . 3_767 ?
O4 Cd1 O9 122.55(9) 3_766 3_767 ?
O7 Cd1 O9 144.26(10) 3_666 3_767 ?
O1 Cd1 O6 93.69(10) . 3_666 ?
O4 Cd1 O6 130.84(9) 3_766 3_666 ?
O7 Cd1 O6 54.45(9) 3_666 3_666 ?
O9 Cd1 O6 103.86(9) 3_767 3_666 ?
O1 Cd1 O8 137.81(9) . 3_767 ?
O4 Cd1 O8 87.81(11) 3_766 3_767 ?
O7 Cd1 O8 102.52(10) 3_666 3_767 ?
O9 Cd1 O8 54.25(9) 3_767 3_767 ?
O6 Cd1 O8 109.37(10) 3_666 3_767 ?
O1 Cd1 C14 108.51(11) . 3_666 ?
O4 Cd1 C14 104.03(10) 3_766 3_666 ?
O7 Cd1 C14 27.11(10) 3_666 3_666 ?
O9 Cd1 C14 126.20(10) 3_767 3_666 ?
O6 Cd1 C14 27.34(10) 3_666 3_666 ?
O8 Cd1 C14 107.75(10) 3_767 3_666 ?
O1 Cd1 C16 111.45(11) . 3_767 ?
O4 Cd1 C16 102.75(11) 3_766 3_767 ?
O7 Cd1 C16 127.57(11) 3_666 3_767 ?
O9 Cd1 C16 27.80(10) 3_767 3_767 ?
O6 Cd1 C16 113.13(10) 3_666 3_767 ?
O8 Cd1 C16 27.10(10) 3_767 3_767 ?
C14 Cd1 C16 124.15(10) 3_666 3_767 ?
C1 O1 Cd1 118.1(2) . . ?
C1 O1 Ca1 111.5(2) . . ?
Cd1 O1 Ca1 101.51(9) . . ?
Ca1 O1W H1WA 114(3) . . ?
Ca1 O1W H1WB 128(3) . . ?
H1WA O1W H1WB 104.8(16) . . ?
C1 O2 Ca1 140.3(2) . 3_767 ?
Ca1 O2W H2WA 104(3) . . ?
Ca1 O2W H2WB 145.8(18) . . ?
H2WA O2W H2WB 105.2(16) . . ?
C8 O3 C7 119.5(2) . . ?
C15 O4 Cd1 103.2(2) . 3_766 ?
C15 O5 Ca1 143.7(3) . 3_766 ?
C14 O6 Cd1 91.5(2) . 3_666 ?
C14 O7 Cd1 92.9(2) . 3_666 ?
C16 O8 Cd1 89.0(2) . 3_767 ?
C16 O9 Ca1 135.2(2) . . ?
C16 O9 Cd1 91.9(2) . 3_767 ?
Ca1 O9 Cd1 116.97(10) . 3_767 ?
C17 O10 Ca1 166.0(4) . . ?
C17 N1 C20 124.3(5) . . ?
C17 N1 C19 118.1(5) . . ?
C20 N1 C19 117.5(5) . . ?
O2 C1 O1 125.7(3) . . ?
O2 C1 C2 119.6(3) . . ?
O1 C1 C2 114.6(3) . . ?
C7 C2 C3 118.0(3) . . ?
C7 C2 C1 117.9(3) . . ?
C3 C2 C1 124.1(3) . . ?
C4 C3 C2 119.6(3) . . ?
C4 C3 C16 120.2(3) . . ?
C2 C3 C16 119.9(3) . . ?
C5 C4 C3 120.7(4) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C6 C5 C4 120.3(4) . . ?
C6 C5 H5A 119.9 . . ?
C4 C5 H5A 119.9 . . ?
C5 C6 C7 119.1(3) . . ?
C5 C6 H6A 120.5 . . ?
C7 C6 H6A 120.5 . . ?
C6 C7 C2 122.1(3) . . ?
C6 C7 O3 119.0(3) . . ?
C2 C7 O3 118.4(3) . . ?
C10 C8 O3 123.3(3) . . ?
C10 C8 C9 121.0(3) . . ?
O3 C8 C9 115.6(3) . . ?
C8 C9 C13 119.4(3) . . ?
C8 C9 H9A 120.3 . . ?
C13 C9 H9A 120.3 . . ?
C8 C10 C11 119.3(3) . . ?
C8 C10 H10A 120.4 . . ?
C11 C10 H10A 120.4 . . ?
C12 C11 C10 119.7(3) . . ?
C12 C11 C15 119.7(3) . . ?
C10 C11 C15 120.6(3) . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C9 119.6(3) . . ?
C12 C13 C14 120.2(3) . . ?
C9 C13 C14 120.2(3) . . ?
O7 C14 O6 121.1(3) . . ?
O7 C14 C13 119.2(3) . . ?
O6 C14 C13 119.7(3) . . ?
O7 C14 Cd1 59.94(18) . 3_666 ?
O6 C14 Cd1 61.14(18) . 3_666 ?
C13 C14 Cd1 176.9(3) . 3_666 ?
O4 C15 O5 122.8(3) . . ?
O4 C15 C11 118.3(3) . . ?
O5 C15 C11 118.9(3) . . ?
O8 C16 O9 121.9(3) . . ?
O8 C16 C3 119.9(4) . . ?
O9 C16 C3 118.1(3) . . ?
O8 C16 Cd1 63.9(2) . 3_767 ?
O9 C16 Cd1 60.33(19) . 3_767 ?
C3 C16 Cd1 160.9(2) . 3_767 ?
O10 C17 N1 123.4(6) . . ?
O10 C17 C18 119.1(5) . . ?
N1 C17 C18 117.5(5) . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 H20A 109.5 . . ?
N1 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
N1 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O2 Ca1 O5 81.03(10) 3_767 3_766 ?
O2 Ca1 O10 115.77(12) 3_767 . ?
O5 Ca1 O10 155.94(11) 3_766 . ?
O2 Ca1 O9 79.32(9) 3_767 . ?
O5 Ca1 O9 121.37(9) 3_766 . ?
O10 Ca1 O9 80.30(11) . . ?
O2 Ca1 O1W 160.41(11) 3_767 . ?
O5 Ca1 O1W 80.25(12) 3_766 . ?
O10 Ca1 O1W 83.81(13) . . ?
O9 Ca1 O1W 105.79(11) . . ?
O2 Ca1 O2W 83.33(11) 3_767 . ?
O5 Ca1 O2W 95.15(10) 3_766 . ?
O10 Ca1 O2W 71.36(12) . . ?
O9 Ca1 O2W 135.84(11) . . ?
O1W Ca1 O2W 104.04(12) . . ?
O2 Ca1 O1 104.23(8) 3_767 . ?
O5 Ca1 O1 67.43(8) 3_766 . ?
O10 Ca1 O1 120.18(11) . . ?
O9 Ca1 O1 65.07(8) . . ?
O1W Ca1 O1 62.93(9) . . ?
O2W Ca1 O1 159.09(10) . . ?
O2 Ca1 H2WA 94.3(11) 3_767 . ?
O5 Ca1 H2WA 110.2(7) 3_766 . ?
O10 Ca1 H2WA 54.2(4) . . ?
O9 Ca1 H2WA 125.9(9) . . ?
O1W Ca1 H2WA 97.5(12) . . ?
O2W Ca1 H2WA 17.4(4) . . ?
O1 Ca1 H2WA 160.4(12) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.080
_database_code_depnum_ccdc_archive 'CCDC 990736'
#######################################################################
#
#                 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_Compound-4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C16 H7 O9, C16 H8 O9, C4 H9 N O, 2(H2 O), O, 2(Ba)'
_chemical_formula_sum            'C36 H28 Ba2 N O22 Zn0'
_chemical_formula_weight         1101.27

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'
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'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.2726(4)
_cell_length_b                   13.3346(5)
_cell_length_c                   15.2745(6)
_cell_angle_alpha                100.554(4)
_cell_angle_beta                 107.524(4)
_cell_angle_gamma                99.341(3)
_cell_volume                     1907.96(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5781
_cell_measurement_theta_min      2.3481
_cell_measurement_theta_max      29.2386

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.917
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1078
_exptl_absorpt_coefficient_mu    2.145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.90426
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12651
_diffrn_reflns_av_R_equivalents  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0489
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.35
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6721
_reflns_number_gt                5671
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0356P)²+1.4157P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6721
_refine_ls_number_parameters     566
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0824
_refine_ls_wR_factor_gt          0.0769
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.047
_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
Ba1 Ba 1.52788(3) 0.820198(19) 0.490161(17) 0.01845(8) Uani 1 1 d . . .
Ba2 Ba 1.08845(3) 0.92503(2) 0.391523(17) 0.02126(9) Uani 1 1 d . . .
C1 C 1.3534(6) 0.6828(5) 0.6406(5) 0.062(2) Uani 1 1 d D . .
C2 C 1.3630(7) 0.7458(5) 0.7394(4) 0.0647(18) Uani 1 1 d D . .
H2A H 1.3755 0.8190 0.7407 0.097 Uiso 1 1 d R . .
H2B H 1.2781 0.7220 0.7513 0.097 Uiso 1 1 d R . .
H2C H 1.4413 0.7353 0.7872 0.097 Uiso 1 1 d R . .
C3 C 1.3272(8) 0.5283(6) 0.7071(5) 0.081(3) Uani 1 1 d D . .
H3A H 1.3319 0.5797 0.7616 0.122 Uiso 1 1 calc R . .
H3B H 1.4042 0.4949 0.7236 0.122 Uiso 1 1 calc R . .
H3C H 1.2403 0.4766 0.6858 0.122 Uiso 1 1 calc R . .
C4 C 1.3306(9) 0.5186(6) 0.5389(5) 0.089(3) Uani 1 1 d D . .
H4A H 1.3384 0.5644 0.4981 0.133 Uiso 1 1 calc R . .
H4B H 1.2433 0.4670 0.5101 0.133 Uiso 1 1 calc R . .
H4C H 1.4071 0.4841 0.5485 0.133 Uiso 1 1 calc R . .
C17 C 0.7827(4) 0.6179(3) -0.0770(3) 0.0183(9) Uani 1 1 d . . .
C20 C 1.1533(4) 0.7599(3) -0.0200(3) 0.0209(9) Uani 1 1 d . . .
C22 C 0.7596(4) 0.6957(3) -0.1241(3) 0.0204(9) Uani 1 1 d . . .
H22B H 0.7682 0.7637 -0.0910 0.024 Uiso 1 1 calc R . .
C23 C 1.0948(4) 0.7363(3) -0.1188(3) 0.0195(9) Uani 1 1 d . . .
C24 C 0.7234(4) 0.6706(3) -0.2220(3) 0.0191(9) Uani 1 1 d . . .
C25 C 0.7732(4) 0.5176(3) -0.1244(3) 0.0200(9) Uani 1 1 d . . .
H25A H 0.7930 0.4670 -0.0910 0.024 Uiso 1 1 calc R . .
C26 C 1.1367(4) 0.9396(3) -0.0136(3) 0.0194(9) Uani 1 1 d . . .
H26A H 1.1509 1.0075 0.0220 0.023 Uiso 1 1 calc R . .
C28 C 0.7340(4) 0.4920(3) -0.2222(3) 0.0196(9) Uani 1 1 d . . .
C29 C 1.0569(4) 0.8146(3) -0.1635(3) 0.0200(9) Uani 1 1 d . . .
H29A H 1.0184 0.7990 -0.2292 0.024 Uiso 1 1 calc R . .
C30 C 1.0761(4) 0.9153(3) -0.1110(3) 0.0174(9) Uani 1 1 d . . .
C32 C 1.1757(4) 0.8625(3) 0.0302(3) 0.0190(9) Uani 1 1 d . . .
C33 C 0.9146(4) 0.7025(3) 0.2103(3) 0.0182(9) Uani 1 1 d . . .
C34 C 0.7096(4) 0.5693(3) -0.2704(3) 0.0213(9) Uani 1 1 d . . .
H34A H 0.6837 0.5527 -0.3361 0.026 Uiso 1 1 calc R . .
C35 C 1.4588(4) 0.9506(3) 0.2541(3) 0.0170(9) Uani 1 1 d . . .
C36 C 1.0748(4) 0.6297(3) -0.1793(3) 0.0248(10) Uani 1 1 d . . .
C37 C 0.5762(5) 0.6330(4) 0.0039(3) 0.0285(11) Uani 1 1 d . . .
H37A H 0.5479 0.6084 -0.0615 0.034 Uiso 1 1 calc R . .
C38 C 1.3696(4) 0.9502(3) 0.3167(3) 0.0152(9) Uani 1 1 d . . .
C39 C 0.7156(4) 0.6551(3) 0.0581(3) 0.0196(9) Uani 1 1 d . . .
C40 C 0.7155(4) 0.3828(3) -0.2761(3) 0.0224(10) Uani 1 1 d . . .
C41 C 0.6621(4) 0.7066(3) 0.2000(3) 0.0205(9) Uani 1 1 d . . .
C42 C 0.7610(4) 0.6898(3) 0.1566(3) 0.0171(9) Uani 1 1 d . . .
C43 C 0.7038(5) 0.7513(3) 0.3052(3) 0.0234(10) Uani 1 1 d . . .
C44 C 1.3893(4) 0.9208(3) 0.1568(3) 0.0180(9) Uani 1 1 d . . .
C45 C 0.6993(4) 0.7509(3) -0.2775(3) 0.0229(10) Uani 1 1 d . . .
C46 C 1.4621(5) 0.9224(4) 0.0938(3) 0.0280(11) Uani 1 1 d . . .
H46A H 1.4141 0.9029 0.0289 0.034 Uiso 1 1 calc R . .
C48 C 1.0369(4) 0.9973(3) -0.1627(3) 0.0211(9) Uani 1 1 d . . .
C49 C 1.6908(5) 1.0103(3) 0.3927(3) 0.0243(10) Uani 1 1 d . . .
C50 C 1.6058(4) 0.9804(3) 0.2888(3) 0.0202(9) Uani 1 1 d . . .
C51 C 1.6773(5) 0.9807(4) 0.2248(3) 0.0296(11) Uani 1 1 d . . .
H51A H 1.7748 0.9998 0.2472 0.036 Uiso 1 1 calc R . .
C53 C 0.5211(5) 0.6848(4) 0.1443(3) 0.0301(11) Uani 1 1 d . . .
H53A H 0.4546 0.6955 0.1728 0.036 Uiso 1 1 calc R . .
C54 C 1.6061(5) 0.9532(4) 0.1287(3) 0.0353(12) Uani 1 1 d . . .
H54A H 1.6558 0.9554 0.0870 0.042 Uiso 1 1 calc R . .
C56 C 0.4786(5) 0.6476(4) 0.0472(3) 0.0309(11) Uani 1 1 d . . .
H56A H 0.3839 0.6324 0.0110 0.037 Uiso 1 1 calc R . .
O1 O 1.0729(3) 1.0919(2) -0.1090(2) 0.0267(8) Uani 1 1 d . . .
H1 H 1.051(6) 1.128(4) -0.142(4) 0.051(19) Uiso 1 1 d . . .
O1W O 1.1076(4) 0.7300(3) 0.4371(3) 0.0454(10) Uani 1 1 d . . .
H1WA H 1.0655 0.6807 0.3875 0.068 Uiso 1 1 d R . .
H1WB H 1.1958 0.7426 0.4648 0.068 Uiso 1 1 d R . .
O2 O 0.9782(3) 0.9740(2) -0.2481(2) 0.0269(7) Uani 1 1 d . . .
O2W O 1.8267(3) 0.8595(2) 0.5310(2) 0.0280(7) Uani 1 1 d . . .
H2WA H 1.8436 0.8417 0.4799 0.042 Uiso 1 1 d R . .
H2WB H 1.8688 0.8226 0.5649 0.042 Uiso 1 1 d R . .
O3 O 0.6692(4) 0.7312(3) -0.3627(2) 0.0325(8) Uani 1 1 d . . .
O3W O 1.9765(6) 0.7114(4) 0.5821(4) 0.0859(18) Uani 1 1 d . . .
O4 O 0.7129(4) 0.8442(3) -0.2251(2) 0.0321(8) Uani 1 1 d . . .
H4 H 0.687(8) 0.880(6) -0.261(5) 0.09(3) Uiso 1 1 d . . .
O5 O 0.7510(4) 0.3199(3) -0.2213(2) 0.0270(8) Uani 1 1 d . . .
H5 H 0.738(7) 0.269(5) -0.249(5) 0.06(2) Uiso 1 1 d . . .
O6 O 0.6704(4) 0.3567(2) -0.3621(2) 0.0314(8) Uani 1 1 d . . .
O7 O 0.8213(3) 0.6414(2) 0.0214(2) 0.0240(7) Uani 1 1 d . . .
O9 O 0.8311(3) 0.7919(2) 0.3511(2) 0.0292(7) Uani 1 1 d . . .
O10 O 0.6087(3) 0.7468(3) 0.3405(2) 0.0365(8) Uani 1 1 d . . .
O11 O 0.9507(3) 0.6284(2) 0.2427(2) 0.0252(7) Uani 1 1 d . . .
O12 O 0.9978(3) 0.7864(2) 0.2171(2) 0.0208(6) Uani 1 1 d . . .
O13 O 1.2445(3) 0.8894(2) 0.12827(19) 0.0206(6) Uani 1 1 d . . .
O14 O 1.1130(4) 0.5612(3) -0.1306(3) 0.0361(9) Uani 1 1 d . . .
H14 H 1.093(6) 0.501(5) -0.174(4) 0.052(18) Uiso 1 1 d . . .
O15 O 1.0299(4) 0.6091(3) -0.2647(2) 0.0388(9) Uani 1 1 d . . .
O16 O 1.3324(3) 0.8679(2) 0.3407(2) 0.0190(6) Uani 1 1 d . . .
O17 O 1.6257(3) 1.0139(2) 0.4520(2) 0.0248(7) Uani 1 1 d . . .
O18 O 1.8217(3) 1.0279(3) 0.4157(2) 0.0356(8) Uani 1 1 d . . .
O20 O 1.3287(3) 1.0319(2) 0.3391(2) 0.0209(7) Uani 1 1 d . . .
O21 O 1.3603(4) 0.7245(3) 0.5770(3) 0.0464(10) Uani 1 1 d . . .
N1 N 1.3354(6) 0.5801(5) 0.6306(4) 0.080(2) Uani 1 1 d D . .


_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
Ba1 O10 2.731(3) 1_655 ?
Ba1 O21 2.763(3) . ?
Ba1 O20 2.779(3) 2_876 ?
Ba1 O16 2.799(3) . ?
Ba1 O6 2.809(3) 2_765 ?
Ba1 O17 2.843(3) . ?
Ba1 O3 2.853(3) 1_656 ?
Ba1 O2W 2.880(3) . ?
Ba1 O17 3.069(3) 2_876 ?
Ba1 Ba2 4.4109(4) 2_876 ?
Ba1 Ba2 4.8297(4) . ?
Ba2 O18 2.722(3) 2_876 ?
Ba2 O12 2.743(3) . ?
Ba2 O2 2.749(3) 2_775 ?
Ba2 O9 2.759(3) . ?
Ba2 O2W 2.781(3) 2_876 ?
Ba2 O1W 2.834(3) . ?
Ba2 O16 3.006(3) . ?
Ba2 O20 3.038(3) . ?
Ba2 O17 3.046(3) 2_876 ?
Ba2 C49 3.252(4) 2_876 ?
Ba2 C38 3.402(4) . ?
Ba2 Ba1 4.4109(4) 2_876 ?
C1 O21 1.217(7) . ?
C1 N1 1.326(6) . ?
C1 C2 1.553(7) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 N1 1.478(6) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.471(7) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C17 C25 1.372(6) . ?
C17 C22 1.379(5) . ?
C17 O7 1.394(5) . ?
C20 C32 1.385(6) . ?
C20 C23 1.399(6) . ?
C22 C24 1.388(6) . ?
C22 H22B 0.9300 . ?
C23 C29 1.393(6) . ?
C23 C36 1.492(6) . ?
C24 C34 1.379(6) . ?
C24 C45 1.489(6) . ?
C25 C28 1.385(6) . ?
C25 H25A 0.9300 . ?
C26 C32 1.375(5) . ?
C26 C30 1.380(6) . ?
C26 H26A 0.9300 . ?
C28 C34 1.385(6) . ?
C28 C40 1.487(6) . ?
C29 C30 1.382(6) . ?
C29 H29A 0.9300 . ?
C30 C48 1.499(6) . ?
C32 O13 1.398(5) . ?
C33 O11 1.243(5) . ?
C33 O12 1.260(5) . ?
C33 C42 1.508(6) . ?
C34 H34A 0.9300 . ?
C35 C44 1.389(6) . ?
C35 C50 1.402(6) . ?
C35 C38 1.510(6) . ?
C36 O15 1.205(5) . ?
C36 O14 1.317(5) . ?
C37 C39 1.371(6) . ?
C37 C56 1.378(6) . ?
C37 H37A 0.9300 . ?
C38 O16 1.256(5) . ?
C38 O20 1.258(4) . ?
C39 O7 1.386(5) . ?
C39 C42 1.396(6) . ?
C40 O6 1.214(5) . ?
C40 O5 1.307(5) . ?
C41 C53 1.392(6) . ?
C41 C42 1.394(6) . ?
C41 C43 1.509(6) . ?
C43 O10 1.248(5) . ?
C43 O9 1.255(5) . ?
C44 C46 1.385(6) . ?
C44 O13 1.385(5) . ?
C45 O3 1.210(5) . ?
C45 O4 1.311(5) . ?
C46 C54 1.375(6) . ?
C46 H46A 0.9300 . ?
C48 O2 1.217(5) . ?
C48 O1 1.299(5) . ?
C49 O18 1.253(5) . ?
C49 O17 1.277(5) . ?
C49 C50 1.503(6) . ?
C49 Ba2 3.252(4) 2_876 ?
C50 C51 1.389(6) . ?
C51 C54 1.376(6) . ?
C51 H51A 0.9300 . ?
C53 C56 1.380(6) . ?
C53 H53A 0.9300 . ?
C54 H54A 0.9300 . ?
C56 H56A 0.9300 . ?
O1 H1 0.77(5) . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8500 . ?
O2 Ba2 2.749(3) 2_775 ?
O2W Ba2 2.781(3) 2_876 ?
O2W H2WA 0.8500 . ?
O2W H2WB 0.8501 . ?
O3 Ba1 2.853(3) 1_454 ?
O4 H4 0.80(7) . ?
O5 H5 0.70(6) . ?
O6 Ba1 2.809(3) 2_765 ?
O10 Ba1 2.731(3) 1_455 ?
O14 H14 0.89(6) . ?
O17 Ba2 3.046(3) 2_876 ?
O17 Ba1 3.069(3) 2_876 ?
O18 Ba2 2.722(3) 2_876 ?
O20 Ba1 2.779(3) 2_876 ?

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
O10 Ba1 O21 132.81(11) 1_655 . ?
O10 Ba1 O20 131.67(9) 1_655 2_876 ?
O21 Ba1 O20 88.82(10) . 2_876 ?
O10 Ba1 O16 78.14(9) 1_655 . ?
O21 Ba1 O16 102.64(9) . . ?
O20 Ba1 O16 121.45(8) 2_876 . ?
O10 Ba1 O6 68.32(10) 1_655 2_765 ?
O21 Ba1 O6 69.22(11) . 2_765 ?
O20 Ba1 O6 158.03(9) 2_876 2_765 ?
O16 Ba1 O6 66.33(8) . 2_765 ?
O10 Ba1 O17 80.63(10) 1_655 . ?
O21 Ba1 O17 143.77(10) . . ?
O20 Ba1 O17 71.08(8) 2_876 . ?
O16 Ba1 O17 66.45(8) . . ?
O6 Ba1 O17 127.42(8) 2_765 . ?
O10 Ba1 O3 105.16(10) 1_655 1_656 ?
O21 Ba1 O3 64.73(10) . 1_656 ?
O20 Ba1 O3 66.99(8) 2_876 1_656 ?
O16 Ba1 O3 165.74(9) . 1_656 ?
O6 Ba1 O3 101.61(9) 2_765 1_656 ?
O17 Ba1 O3 127.57(9) . 1_656 ?
O10 Ba1 O2W 65.09(9) 1_655 . ?
O21 Ba1 O2W 131.06(9) . . ?
O20 Ba1 O2W 68.64(8) 2_876 . ?
O16 Ba1 O2W 126.27(8) . . ?
O6 Ba1 O2W 125.63(9) 2_765 . ?
O17 Ba1 O2W 69.91(8) . . ?
O3 Ba1 O2W 66.49(9) 1_656 . ?
O10 Ba1 O17 138.35(9) 1_655 2_876 ?
O21 Ba1 O17 75.57(10) . 2_876 ?
O20 Ba1 O17 63.64(8) 2_876 2_876 ?
O16 Ba1 O17 64.37(8) . 2_876 ?
O6 Ba1 O17 109.08(9) 2_765 2_876 ?
O17 Ba1 O17 68.56(10) . 2_876 ?
O3 Ba1 O17 115.68(8) 1_656 2_876 ?
O2W Ba1 O17 124.14(8) . 2_876 ?
O10 Ba1 Ba2 90.04(7) 1_655 2_876 ?
O21 Ba1 Ba2 131.01(8) . 2_876 ?
O20 Ba1 Ba2 42.94(6) 2_876 2_876 ?
O16 Ba1 Ba2 109.72(6) . 2_876 ?
O6 Ba1 Ba2 158.35(7) 2_765 2_876 ?
O17 Ba1 Ba2 43.28(6) . 2_876 ?
O3 Ba1 Ba2 84.31(7) 1_656 2_876 ?
O2W Ba1 Ba2 38.02(6) . 2_876 ?
O17 Ba1 Ba2 86.29(6) 2_876 2_876 ?
O10 Ba1 Ba2 112.23(7) 1_655 . ?
O21 Ba1 Ba2 73.57(7) . . ?
O20 Ba1 Ba2 101.28(5) 2_876 . ?
O16 Ba1 Ba2 35.09(6) . . ?
O6 Ba1 Ba2 73.53(7) 2_765 . ?
O17 Ba1 Ba2 81.02(6) . . ?
O3 Ba1 Ba2 136.46(7) 1_656 . ?
O2W Ba1 Ba2 150.91(6) . . ?
O17 Ba1 Ba2 37.67(5) 2_876 . ?
Ba2 Ba1 Ba2 116.338(7) 2_876 . ?
O18 Ba2 O12 152.48(9) 2_876 . ?
O18 Ba2 O2 138.74(10) 2_876 2_775 ?
O12 Ba2 O2 68.73(8) . 2_775 ?
O18 Ba2 O9 99.91(9) 2_876 . ?
O12 Ba2 O9 67.02(9) . . ?
O2 Ba2 O9 99.70(9) 2_775 . ?
O18 Ba2 O2W 68.42(9) 2_876 2_876 ?
O12 Ba2 O2W 138.84(8) . 2_876 ?
O2 Ba2 O2W 71.00(9) 2_775 2_876 ?
O9 Ba2 O2W 129.07(9) . 2_876 ?
O18 Ba2 O1W 75.57(10) 2_876 . ?
O12 Ba2 O1W 76.96(9) . . ?
O2 Ba2 O1W 145.68(10) 2_775 . ?
O9 Ba2 O1W 66.40(10) . . ?
O2W Ba2 O1W 142.54(10) 2_876 . ?
O18 Ba2 O16 104.84(9) 2_876 . ?
O12 Ba2 O16 69.13(8) . . ?
O2 Ba2 O16 92.05(8) 2_775 . ?
O9 Ba2 O16 126.13(8) . . ?
O2W Ba2 O16 104.54(8) 2_876 . ?
O1W Ba2 O16 74.60(9) . . ?
O18 Ba2 O20 106.09(9) 2_876 . ?
O12 Ba2 O20 87.68(8) . . ?
O2 Ba2 O20 62.66(8) 2_775 . ?
O9 Ba2 O20 153.71(8) . . ?
O2W Ba2 O20 66.34(8) 2_876 . ?
O1W Ba2 O20 116.31(9) . . ?
O16 Ba2 O20 42.65(7) . . ?
O18 Ba2 O17 45.09(8) 2_876 2_876 ?
O12 Ba2 O17 129.98(8) . 2_876 ?
O2 Ba2 O17 122.78(8) 2_775 2_876 ?
O9 Ba2 O17 137.22(8) . 2_876 ?
O2W Ba2 O17 68.30(8) 2_876 2_876 ?
O1W Ba2 O17 79.22(9) . 2_876 ?
O16 Ba2 O17 62.37(8) . 2_876 ?
O20 Ba2 O17 64.98(7) . 2_876 ?
O18 Ba2 C49 21.99(10) 2_876 2_876 ?
O12 Ba2 C49 146.01(10) . 2_876 ?
O2 Ba2 C49 134.86(10) 2_775 2_876 ?
O9 Ba2 C49 118.78(10) . 2_876 ?
O2W Ba2 C49 66.70(9) 2_876 2_876 ?
O1W Ba2 C49 76.07(11) . 2_876 ?
O16 Ba2 C49 83.99(10) . 2_876 ?
O20 Ba2 C49 86.07(10) . 2_876 ?
O17 Ba2 C49 23.10(9) 2_876 2_876 ?
O18 Ba2 C38 109.70(9) 2_876 . ?
O12 Ba2 C38 74.93(9) . . ?
O2 Ba2 C38 74.70(9) 2_775 . ?
O9 Ba2 C38 140.63(9) . . ?
O2W Ba2 C38 86.76(9) 2_876 . ?
O1W Ba2 C38 96.04(10) . . ?
O16 Ba2 C38 21.49(8) . . ?
O20 Ba2 C38 21.58(8) . . ?
O17 Ba2 C38 64.64(8) 2_876 . ?
C49 Ba2 C38 87.74(10) 2_876 . ?
O18 Ba2 Ba1 69.80(7) 2_876 2_876 ?
O12 Ba2 Ba1 126.10(6) . 2_876 ?
O2 Ba2 Ba1 83.75(7) 2_775 2_876 ?
O9 Ba2 Ba1 166.39(6) . 2_876 ?
O2W Ba2 Ba1 39.62(6) 2_876 2_876 ?
O1W Ba2 Ba1 117.39(7) . 2_876 ?
O16 Ba2 Ba1 66.51(5) . 2_876 ?
O20 Ba2 Ba1 38.54(5) . 2_876 ?
O17 Ba2 Ba1 39.78(5) 2_876 2_876 ?
C49 Ba2 Ba1 53.47(8) 2_876 2_876 ?
C38 Ba2 Ba1 52.98(7) . 2_876 ?
O21 C1 N1 122.7(6) . . ?
O21 C1 C2 122.6(6) . . ?
N1 C1 C2 114.7(6) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.4 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C25 C17 C22 121.6(4) . . ?
C25 C17 O7 118.6(4) . . ?
C22 C17 O7 119.8(4) . . ?
C32 C20 C23 118.2(4) . . ?
C17 C22 C24 118.7(4) . . ?
C17 C22 H22B 120.7 . . ?
C24 C22 H22B 120.7 . . ?
C29 C23 C20 119.7(4) . . ?
C29 C23 C36 118.1(4) . . ?
C20 C23 C36 122.1(4) . . ?
C34 C24 C22 120.1(4) . . ?
C34 C24 C45 118.2(4) . . ?
C22 C24 C45 121.7(4) . . ?
C17 C25 C28 119.7(4) . . ?
C17 C25 H25A 120.2 . . ?
C28 C25 H25A 120.2 . . ?
C32 C26 C30 119.3(4) . . ?
C32 C26 H26A 120.3 . . ?
C30 C26 H26A 120.3 . . ?
C25 C28 C34 119.2(4) . . ?
C25 C28 C40 121.0(4) . . ?
C34 C28 C40 119.7(4) . . ?
C30 C29 C23 120.6(4) . . ?
C30 C29 H29A 119.7 . . ?
C23 C29 H29A 119.7 . . ?
C26 C30 C29 120.0(4) . . ?
C26 C30 C48 121.5(4) . . ?
C29 C30 C48 118.4(4) . . ?
C26 C32 C20 122.1(4) . . ?
C26 C32 O13 118.8(4) . . ?
C20 C32 O13 119.0(4) . . ?
O11 C33 O12 124.6(4) . . ?
O11 C33 C42 117.7(4) . . ?
O12 C33 C42 117.7(3) . . ?
C24 C34 C28 120.7(4) . . ?
C24 C34 H34A 119.7 . . ?
C28 C34 H34A 119.7 . . ?
C44 C35 C50 119.0(4) . . ?
C44 C35 C38 117.3(3) . . ?
C50 C35 C38 123.7(4) . . ?
O15 C36 O14 123.5(4) . . ?
O15 C36 C23 123.0(4) . . ?
O14 C36 C23 113.5(4) . . ?
C39 C37 C56 119.4(4) . . ?
C39 C37 H37A 120.3 . . ?
C56 C37 H37A 120.3 . . ?
O16 C38 O20 122.0(4) . . ?
O16 C38 C35 119.9(3) . . ?
O20 C38 C35 118.0(3) . . ?
O16 C38 Ba2 61.2(2) . . ?
O20 C38 Ba2 62.7(2) . . ?
C35 C38 Ba2 162.3(2) . . ?
C37 C39 O7 123.7(4) . . ?
C37 C39 C42 121.6(4) . . ?
O7 C39 C42 114.6(3) . . ?
O6 C40 O5 124.8(4) . . ?
O6 C40 C28 122.2(4) . . ?
O5 C40 C28 113.0(4) . . ?
C53 C41 C42 119.2(4) . . ?
C53 C41 C43 118.8(4) . . ?
C42 C41 C43 122.0(4) . . ?
C41 C42 C39 118.7(4) . . ?
C41 C42 C33 123.8(4) . . ?
C39 C42 C33 117.4(4) . . ?
O10 C43 O9 124.4(4) . . ?
O10 C43 C41 117.6(4) . . ?
O9 C43 C41 117.9(4) . . ?
C46 C44 O13 123.2(4) . . ?
C46 C44 C35 121.4(4) . . ?
O13 C44 C35 115.4(4) . . ?
O3 C45 O4 123.6(4) . . ?
O3 C45 C24 123.0(4) . . ?
O4 C45 C24 113.4(4) . . ?
C54 C46 C44 119.2(4) . . ?
C54 C46 H46A 120.4 . . ?
C44 C46 H46A 120.4 . . ?
O2 C48 O1 124.7(4) . . ?
O2 C48 C30 120.9(4) . . ?
O1 C48 C30 114.4(4) . . ?
O18 C49 O17 123.8(4) . . ?
O18 C49 C50 117.8(4) . . ?
O17 C49 C50 118.3(4) . . ?
O18 C49 Ba2 54.5(2) . 2_876 ?
O17 C49 Ba2 69.4(2) . 2_876 ?
C50 C49 Ba2 172.3(3) . 2_876 ?
C51 C50 C35 118.9(4) . . ?
C51 C50 C49 118.0(4) . . ?
C35 C50 C49 123.1(4) . . ?
C54 C51 C50 121.1(4) . . ?
C54 C51 H51A 119.5 . . ?
C50 C51 H51A 119.5 . . ?
C56 C53 C41 120.9(4) . . ?
C56 C53 H53A 119.6 . . ?
C41 C53 H53A 119.6 . . ?
C46 C54 C51 120.5(4) . . ?
C46 C54 H54A 119.8 . . ?
C51 C54 H54A 119.8 . . ?
C37 C56 C53 120.1(4) . . ?
C37 C56 H56A 119.9 . . ?
C53 C56 H56A 119.9 . . ?
C48 O1 H1 107(4) . . ?
Ba2 O1W H1WA 109.3 . . ?
Ba2 O1W H1WB 99.0 . . ?
H1WA O1W H1WB 121.6 . . ?
C48 O2 Ba2 137.9(3) . 2_775 ?
Ba2 O2W Ba1 102.36(9) 2_876 . ?
Ba2 O2W H2WA 112.2 2_876 . ?
Ba1 O2W H2WA 109.4 . . ?
Ba2 O2W H2WB 115.3 2_876 . ?
Ba1 O2W H2WB 115.4 . . ?
H2WA O2W H2WB 102.3 . . ?
C45 O3 Ba1 135.4(3) . 1_454 ?
C45 O4 H4 106(5) . . ?
C40 O5 H5 109(5) . . ?
C40 O6 Ba1 131.8(3) . 2_765 ?
C39 O7 C17 116.3(3) . . ?
C43 O9 Ba2 155.6(3) . . ?
C43 O10 Ba1 147.2(3) . 1_455 ?
C33 O12 Ba2 114.3(3) . . ?
C44 O13 C32 114.8(3) . . ?
C36 O14 H14 105(3) . . ?
C38 O16 Ba1 117.6(2) . . ?
C38 O16 Ba2 97.3(2) . . ?
Ba1 O16 Ba2 112.54(9) . . ?
C49 O17 Ba1 116.5(3) . . ?
C49 O17 Ba2 87.5(2) . 2_876 ?
Ba1 O17 Ba2 96.94(8) . 2_876 ?
C49 O17 Ba1 128.6(2) . 2_876 ?
Ba1 O17 Ba1 111.44(10) . 2_876 ?
Ba2 O17 Ba1 104.33(9) 2_876 2_876 ?
C49 O18 Ba2 103.5(3) . 2_876 ?
C38 O20 Ba1 121.6(2) . 2_876 ?
C38 O20 Ba2 95.7(2) . . ?
Ba1 O20 Ba2 98.53(8) 2_876 . ?
C1 O21 Ba1 147.7(4) . . ?
C1 N1 C4 116.0(6) . . ?
C1 N1 C3 123.5(6) . . ?
C4 N1 C3 120.5(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.498
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 990737'
#######################################################################
#
#                 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_Compound-5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C16 H8 O9), C2 H3 N O, 3(H2 O), C H3, 2(Ba)'
_chemical_formula_sum            'C35 H28 Ba2 N O22'
_chemical_formula_weight         1089.24

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'
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.2724(6)
_cell_length_b                   13.3126(7)
_cell_length_c                   15.2949(10)
_cell_angle_alpha                100.307(5)
_cell_angle_beta                 107.572(6)
_cell_angle_gamma                100.414(5)
_cell_volume                     1899.38(19)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3243
_cell_measurement_theta_min      2.5630
_cell_measurement_theta_max      27.8490

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1066
_exptl_absorpt_coefficient_mu    2.154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78736
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         none
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            12322
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.41
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6692
_reflns_number_gt                5010
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_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)+(0.0433P)²+0.3965P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6692
_refine_ls_number_parameters     548
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1102
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.006
_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
Ba1 Ba -0.47357(4) -0.17964(3) -0.01184(3) 0.01880(12) Uani 1 1 d . . .
Ba2 Ba -0.08678(4) 0.07525(3) 0.10966(3) 0.02184(12) Uani 1 1 d . . .
C1 C 0.3455(6) 0.2927(5) 0.3033(4) 0.0182(14) Uani 1 1 d . . .
C2 C 0.4854(7) 0.3128(5) 0.3598(5) 0.0285(16) Uani 1 1 d . . .
H2A H 0.5516 0.2998 0.3319 0.034 Uiso 1 1 calc R . .
C3 C 0.5290(7) 0.3515(5) 0.4563(5) 0.0323(17) Uani 1 1 d . . .
H3A H 0.6242 0.3671 0.4926 0.039 Uiso 1 1 calc R . .
C4 C 0.4319(7) 0.3674(5) 0.4995(5) 0.0273(16) Uani 1 1 d . . .
H4A H 0.4605 0.3923 0.5649 0.033 Uiso 1 1 calc R . .
C5 C 0.2912(7) 0.3457(5) 0.4441(4) 0.0211(15) Uani 1 1 d . . .
C6 C 0.2463(6) 0.3115(4) 0.3467(4) 0.0171(14) Uani 1 1 d . . .
C7 C 0.3033(7) 0.2472(5) 0.1985(4) 0.0210(14) Uani 1 1 d . . .
C8 C 0.0928(7) 0.2980(5) 0.2919(4) 0.0181(14) Uani 1 1 d . . .
C9 C 0.2227(7) 0.3820(5) 0.5784(4) 0.0209(14) Uani 1 1 d . . .
C10 C 0.2472(7) 0.3053(5) 0.6260(4) 0.0225(15) Uani 1 1 d . . .
H10A H 0.2408 0.2377 0.5931 0.027 Uiso 1 1 calc R . .
C11 C 0.2814(6) 0.3295(5) 0.7236(4) 0.0198(14) Uani 1 1 d . . .
C12 C 0.2910(6) 0.4303(5) 0.7721(4) 0.0195(14) Uani 1 1 d . . .
H12A H 0.3158 0.4470 0.8377 0.023 Uiso 1 1 calc R . .
C13 C 0.2637(7) 0.5068(5) 0.7227(4) 0.0192(14) Uani 1 1 d . . .
C14 C 0.2278(7) 0.4821(5) 0.6246(4) 0.0219(15) Uani 1 1 d . . .
H14A H 0.2077 0.5323 0.5909 0.026 Uiso 1 1 calc R . .
C15 C 0.3062(7) 0.2494(5) 0.7784(5) 0.0238(15) Uani 1 1 d . . .
C16 C 0.2787(7) 0.6153(5) 0.7772(5) 0.0241(16) Uani 1 1 d . . .
C17 C -0.3943(7) -0.0115(5) -0.2096(4) 0.0238(15) Uani 1 1 d . . .
C18 C -0.3225(7) -0.0062(6) -0.2723(5) 0.038(2) Uani 1 1 d . . .
H18A H -0.2247 0.0176 -0.2495 0.046 Uiso 1 1 calc R . .
C19 C -0.3948(7) -0.0360(6) -0.3688(5) 0.042(2) Uani 1 1 d . . .
H19A H -0.3447 -0.0318 -0.4101 0.050 Uiso 1 1 calc R . .
C20 C -0.5376(7) -0.0713(5) -0.4046(4) 0.0300(17) Uani 1 1 d . . .
H20A H -0.5851 -0.0921 -0.4697 0.036 Uiso 1 1 calc R . .
C21 C -0.6118(6) -0.0759(5) -0.3419(4) 0.0191(14) Uani 1 1 d . . .
C22 C -0.5417(6) -0.0463(4) -0.2450(4) 0.0143(13) Uani 1 1 d . . .
C23 C -0.3103(7) 0.0150(5) -0.1059(5) 0.0239(15) Uani 1 1 d . . .
C24 C -0.6323(6) -0.0494(4) -0.1832(4) 0.0148(13) Uani 1 1 d . . .
C25 C -0.8259(6) -0.1382(5) -0.4692(4) 0.0200(14) Uani 1 1 d . . .
C26 C -0.8644(6) -0.0600(5) -0.5132(4) 0.0174(14) Uani 1 1 d . . .
H26A H -0.8495 0.0080 -0.4775 0.021 Uiso 1 1 calc R . .
C27 C -0.9254(6) -0.0847(5) -0.6115(4) 0.0167(13) Uani 1 1 d . . .
C28 C -0.9446(6) -0.1865(5) -0.6641(4) 0.0207(14) Uani 1 1 d . . .
H28A H -0.9835 -0.2029 -0.7298 0.025 Uiso 1 1 calc R . .
C29 C -0.9061(6) -0.2635(5) -0.6189(4) 0.0213(14) Uani 1 1 d . . .
C30 C -0.8488(6) -0.2398(5) -0.5212(4) 0.0221(15) Uani 1 1 d . . .
H30A H -0.8258 -0.2920 -0.4907 0.027 Uiso 1 1 calc R . .
C31 C -0.9635(6) -0.0026(5) -0.6626(5) 0.0205(14) Uani 1 1 d . . .
C32 C -0.9238(7) -0.3698(5) -0.6792(5) 0.0249(15) Uani 1 1 d . . .
C33 C -0.6545(11) -0.3265(12) 0.1338(10) 0.107(5) Uani 1 1 d . . .
C34 C -0.6703(11) -0.4587(9) 0.2093(8) 0.093(4) Uani 1 1 d . . .
H34A H -0.6590 -0.4227 0.2723 0.139 Uiso 1 1 calc R . .
H34B H -0.5974 -0.4953 0.2115 0.139 Uiso 1 1 calc R . .
H34C H -0.7608 -0.5085 0.1813 0.139 Uiso 1 1 calc R . .
C35 C -0.677(3) -0.478(3) 0.0472(13) 0.51(4) Uani 1 1 d . . .
H35A H -0.6726 -0.4379 0.0012 0.759 Uiso 1 1 calc R . .
H35B H -0.7661 -0.5293 0.0240 0.759 Uiso 1 1 calc R . .
H35C H -0.6018 -0.5122 0.0584 0.759 Uiso 1 1 calc R . .
O1 O 0.1746(5) 0.2059(3) 0.1516(3) 0.0304(11) Uani 1 1 d . . .
O1W O -0.0939(5) 0.2733(4) 0.0663(3) 0.0420(13) Uani 1 1 d . . .
H1WA H -0.0812 0.3021 0.1235 0.063 Uiso 1 1 d R . .
H1WB H -0.1766 0.2793 0.0392 0.063 Uiso 1 1 d R . .
O2 O 0.3984(5) 0.2529(4) 0.1635(3) 0.0361(12) Uani 1 1 d . . .
O2W O -0.1737(5) -0.1402(3) 0.0285(3) 0.0287(11) Uani 1 1 d D . .
H2WA H -0.179(7) -0.171(5) -0.0265(19) 0.043 Uiso 1 1 d D . .
H2WB H -0.132(7) -0.174(5) 0.064(3) 0.043 Uiso 1 1 d D . .
O3 O 0.0598(5) 0.3726(3) 0.2589(3) 0.0240(10) Uani 1 1 d . . .
O3W O -0.0368(9) -0.2921(7) 0.0781(7) 0.102(3) Uiso 1 1 d D . .
H3WA H -0.044(11) -0.356(2) 0.075(8) 0.153 Uiso 1 1 d D . .
H3WB H 0.044(6) -0.258(7) 0.114(7) 0.153 Uiso 1 1 d D . .
O4 O 0.0055(4) 0.2138(3) 0.2842(3) 0.0212(10) Uani 1 1 d . . .
O5 O 0.1859(5) 0.3604(3) 0.4801(3) 0.0244(10) Uani 1 1 d . . .
O6 O 0.2958(5) 0.1565(3) 0.7258(3) 0.0362(13) Uani 1 1 d . . .
H6 H 0.3097 0.1119 0.7588 0.054 Uiso 1 1 d R . .
O7 O 0.3359(5) 0.2691(3) 0.8638(3) 0.0329(12) Uani 1 1 d . . .
O8 O 0.3205(5) 0.6417(3) 0.8625(3) 0.0332(12) Uani 1 1 d . . .
O9 O 0.2420(5) 0.6774(3) 0.7203(3) 0.0293(11) Uani 1 1 d . . .
H9 H 0.2567 0.7356 0.7598 0.044 Uiso 1 1 d R . .
O10 O -0.1780(5) 0.0328(4) -0.0830(3) 0.0373(13) Uani 1 1 d . . .
O11 O -0.3749(5) 0.0158(3) -0.0473(3) 0.0259(11) Uani 1 1 d . . .
O12 O -0.6703(4) -0.1325(3) -0.1598(3) 0.0184(9) Uani 1 1 d . . .
O13 O -0.6723(5) 0.0320(3) -0.1602(3) 0.0222(10) Uani 1 1 d . . .
O14 O -0.7576(4) -0.1119(3) -0.3713(3) 0.0222(10) Uani 1 1 d . . .
O15 O -0.9266(5) 0.0923(3) -0.6083(3) 0.0270(11) Uani 1 1 d . . .
H15A H -0.9461 0.1461 -0.6338 0.032 Uiso 1 1 d R . .
O16 O -1.0204(5) -0.0256(3) -0.7474(3) 0.0286(11) Uani 1 1 d . . .
O17 O -0.9659(6) -0.3894(4) -0.7648(3) 0.0421(13) Uani 1 1 d . . .
O18 O -0.8887(5) -0.4386(3) -0.6310(3) 0.0377(13) Uani 1 1 d . . .
H18 H -0.8896 -0.4897 -0.6736 0.057 Uiso 1 1 d R . .
O19 O -0.6465(5) -0.2700(4) 0.0744(4) 0.0467(14) Uani 1 1 d . . .
N1 N -0.6615(12) -0.3889(18) 0.1574(16) 0.322(17) Uani 1 1 d . . .


_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
Ba1 O2 2.733(4) 2 ?
Ba1 O19 2.749(5) . ?
Ba1 O13 2.782(4) 2_455 ?
Ba1 O12 2.793(4) . ?
Ba1 O8 2.814(4) 1_444 ?
Ba1 O11 2.824(4) . ?
Ba1 O7 2.861(5) 2_556 ?
Ba1 O2W 2.880(5) . ?
Ba1 O11 3.061(4) 2_455 ?
Ba1 Ba2 4.3779(6) . ?
Ba2 O10 2.725(4) . ?
Ba2 O4 2.740(4) . ?
Ba2 O1 2.741(4) . ?
Ba2 O16 2.745(4) 1_656 ?
Ba2 O2W 2.774(4) . ?
Ba2 O1W 2.840(5) . ?
Ba2 O12 3.005(4) 2_455 ?
Ba2 O13 3.006(4) 2_455 ?
Ba2 O11 3.055(4) . ?
Ba2 C23 3.256(7) . ?
Ba2 C24 3.384(6) 2_455 ?
Ba2 H1WA 2.9782 . ?
C1 C2 1.383(8) . ?
C1 C6 1.409(8) . ?
C1 C7 1.503(8) . ?
C2 C3 1.375(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.378(9) . ?
C3 H3A 0.9300 . ?
C4 C5 1.382(9) . ?
C4 H4A 0.9300 . ?
C5 C6 1.381(8) . ?
C5 O5 1.382(7) . ?
C6 C8 1.506(8) . ?
C7 O2 1.246(7) . ?
C7 O1 1.260(7) . ?
C8 O3 1.245(7) . ?
C8 O4 1.265(7) . ?
C9 C10 1.373(8) . ?
C9 C14 1.375(8) . ?
C9 O5 1.395(7) . ?
C10 C11 1.388(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.383(8) . ?
C11 C15 1.481(8) . ?
C12 C13 1.392(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.394(8) . ?
C13 C16 1.488(8) . ?
C14 H14A 0.9300 . ?
C15 O7 1.215(7) . ?
C15 O6 1.317(7) . ?
C16 O8 1.205(7) . ?
C16 O9 1.325(7) . ?
C17 C18 1.379(8) . ?
C17 C22 1.401(8) . ?
C17 C23 1.500(8) . ?
C18 C19 1.382(9) . ?
C18 H18A 0.9300 . ?
C19 C20 1.359(9) . ?
C19 H19A 0.9300 . ?
C20 C21 1.397(8) . ?
C20 H20A 0.9300 . ?
C21 C22 1.383(8) . ?
C21 O14 1.390(7) . ?
C22 C24 1.514(8) . ?
C23 O10 1.262(8) . ?
C23 O11 1.266(7) . ?
C24 O12 1.255(6) . ?
C24 O13 1.257(6) . ?
C24 Ba2 3.384(6) 2_455 ?
C25 C30 1.380(8) . ?
C25 C26 1.390(8) . ?
C25 O14 1.395(7) . ?
C26 C27 1.392(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.393(8) . ?
C27 C31 1.494(8) . ?
C28 C29 1.385(8) . ?
C28 H28A 0.9300 . ?
C29 C30 1.383(8) . ?
C29 C32 1.491(9) . ?
C30 H30A 0.9300 . ?
C31 O16 1.205(7) . ?
C31 O15 1.301(7) . ?
C32 O17 1.210(7) . ?
C32 O18 1.309(7) . ?
C33 N1 0.962(15) . ?
C33 O19 1.290(13) . ?
C34 N1 1.335(11) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 N1 1.82(4) . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
O1W H1WA 0.8500 . ?
O1W H1WB 0.8501 . ?
O2 Ba1 2.733(4) 2 ?
O2W H2WA 0.848(19) . ?
O2W H2WB 0.835(19) . ?
O3W H3WA 0.83(2) . ?
O3W H3WB 0.84(2) . ?
O6 H6 0.8499 . ?
O7 Ba1 2.861(5) 2_556 ?
O8 Ba1 2.814(4) 1_666 ?
O9 H9 0.8500 . ?
O11 Ba1 3.061(4) 2_455 ?
O12 Ba2 3.005(4) 2_455 ?
O13 Ba1 2.782(4) 2_455 ?
O13 Ba2 3.006(4) 2_455 ?
O15 H15A 0.8999 . ?
O16 Ba2 2.745(4) 1_454 ?
O18 H18 0.8500 . ?

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 Ba1 O19 134.05(16) 2 . ?
O2 Ba1 O13 132.78(13) 2 2_455 ?
O19 Ba1 O13 87.59(14) . 2_455 ?
O2 Ba1 O12 77.84(13) 2 . ?
O19 Ba1 O12 100.75(14) . . ?
O13 Ba1 O12 121.62(11) 2_455 . ?
O2 Ba1 O8 69.07(13) 2 1_444 ?
O19 Ba1 O8 68.61(15) . 1_444 ?
O13 Ba1 O8 156.18(12) 2_455 1_444 ?
O12 Ba1 O8 66.48(12) . 1_444 ?
O2 Ba1 O11 81.52(13) 2 . ?
O19 Ba1 O11 140.81(15) . . ?
O13 Ba1 O11 71.10(12) 2_455 . ?
O12 Ba1 O11 66.68(12) . . ?
O8 Ba1 O11 128.58(13) 1_444 . ?
O2 Ba1 O7 106.47(14) 2 2_556 ?
O19 Ba1 O7 65.56(15) . 2_556 ?
O13 Ba1 O7 66.49(12) 2_455 2_556 ?
O12 Ba1 O7 164.80(13) . 2_556 ?
O8 Ba1 O7 100.99(13) 1_444 2_556 ?
O11 Ba1 O7 127.98(13) . 2_556 ?
O2 Ba1 O2W 65.67(13) 2 . ?
O19 Ba1 O2W 132.39(14) . . ?
O13 Ba1 O2W 69.21(12) 2_455 . ?
O12 Ba1 O2W 126.86(12) . . ?
O8 Ba1 O2W 126.33(13) 1_444 . ?
O11 Ba1 O2W 70.72(13) . . ?
O7 Ba1 O2W 67.10(13) 2_556 . ?
O2 Ba1 O11 138.28(13) 2 2_455 ?
O19 Ba1 O11 72.85(14) . 2_455 ?
O13 Ba1 O11 63.65(12) 2_455 2_455 ?
O12 Ba1 O11 64.28(11) . 2_455 ?
O8 Ba1 O11 107.99(13) 1_444 2_455 ?
O11 Ba1 O11 68.28(13) . 2_455 ?
O7 Ba1 O11 114.68(12) 2_556 2_455 ?
O2W Ba1 O11 124.83(12) . 2_455 ?
O2 Ba1 Ba2 91.17(10) 2 . ?
O19 Ba1 Ba2 129.92(12) . . ?
O13 Ba1 Ba2 42.81(8) 2_455 . ?
O12 Ba1 Ba2 110.61(8) . . ?
O8 Ba1 Ba2 160.24(9) 1_444 . ?
O11 Ba1 Ba2 43.93(9) . . ?
O7 Ba1 Ba2 84.11(10) 2_556 . ?
O2W Ba1 Ba2 38.40(9) . . ?
O11 Ba1 Ba2 86.58(8) 2_455 . ?
O10 Ba2 O4 151.27(13) . . ?
O10 Ba2 O1 99.77(13) . . ?
O4 Ba2 O1 67.43(12) . . ?
O10 Ba2 O16 140.18(14) . 1_656 ?
O4 Ba2 O16 68.51(12) . 1_656 ?
O1 Ba2 O16 98.37(13) . 1_656 ?
O10 Ba2 O2W 68.64(14) . . ?
O4 Ba2 O2W 139.82(12) . . ?
O1 Ba2 O2W 127.36(13) . . ?
O16 Ba2 O2W 72.14(13) 1_656 . ?
O10 Ba2 O1W 74.68(14) . . ?
O4 Ba2 O1W 76.60(13) . . ?
O1 Ba2 O1W 66.04(14) . . ?
O16 Ba2 O1W 145.09(13) 1_656 . ?
O2W Ba2 O1W 142.47(14) . . ?
O10 Ba2 O12 104.15(13) . 2_455 ?
O4 Ba2 O12 68.90(11) . 2_455 ?
O1 Ba2 O12 126.77(12) . 2_455 ?
O16 Ba2 O12 92.58(12) 1_656 2_455 ?
O2W Ba2 O12 105.63(12) . 2_455 ?
O1W Ba2 O12 75.56(12) . 2_455 ?
O10 Ba2 O13 106.36(13) . 2_455 ?
O4 Ba2 O13 87.53(11) . 2_455 ?
O1 Ba2 O13 153.64(12) . 2_455 ?
O16 Ba2 O13 63.21(12) 1_656 2_455 ?
O2W Ba2 O13 67.48(12) . 2_455 ?
O1W Ba2 O13 117.57(12) . 2_455 ?
O12 Ba2 O13 42.85(10) 2_455 2_455 ?
O10 Ba2 O11 45.02(12) . . ?
O4 Ba2 O11 129.37(12) . . ?
O1 Ba2 O11 137.67(12) . . ?
O16 Ba2 O11 123.64(12) 1_656 . ?
O2W Ba2 O11 68.79(12) . . ?
O1W Ba2 O11 79.93(12) . . ?
O12 Ba2 O11 62.03(11) 2_455 . ?
O13 Ba2 O11 65.06(11) 2_455 . ?
O10 Ba2 C23 22.17(14) . . ?
O4 Ba2 C23 144.80(14) . . ?
O1 Ba2 C23 119.01(14) . . ?
O16 Ba2 C23 136.11(14) 1_656 . ?
O2W Ba2 C23 67.18(14) . . ?
O1W Ba2 C23 75.90(14) . . ?
O12 Ba2 C23 83.23(14) 2_455 . ?
O13 Ba2 C23 86.09(14) 2_455 . ?
O11 Ba2 C23 22.85(13) . . ?
O10 Ba2 C24 109.56(14) . 2_455 ?
O4 Ba2 C24 74.67(13) . 2_455 ?
O1 Ba2 C24 141.03(13) . 2_455 ?
O16 Ba2 C24 75.18(14) 1_656 2_455 ?
O2W Ba2 C24 87.93(13) . 2_455 ?
O1W Ba2 C24 97.16(14) . 2_455 ?
O12 Ba2 C24 21.62(11) 2_455 2_455 ?
O13 Ba2 C24 21.66(11) 2_455 2_455 ?
O11 Ba2 C24 64.56(12) . 2_455 ?
C23 Ba2 C24 87.41(15) . 2_455 ?
O10 Ba2 Ba1 69.92(10) . . ?
O4 Ba2 Ba1 126.37(8) . . ?
O1 Ba2 Ba1 165.52(9) . . ?
O16 Ba2 Ba1 84.62(10) 1_656 . ?
O2W Ba2 Ba1 40.15(10) . . ?
O1W Ba2 Ba1 118.53(10) . . ?
O12 Ba2 Ba1 66.91(7) 2_455 . ?
O13 Ba2 Ba1 38.97(8) 2_455 . ?
O11 Ba2 Ba1 39.89(7) . . ?
C23 Ba2 Ba1 53.52(11) . . ?
C24 Ba2 Ba1 53.44(9) 2_455 . ?
O10 Ba2 H1WA 91.0 . . ?
O4 Ba2 H1WA 60.4 . . ?
O1 Ba2 H1WA 64.9 . . ?
O16 Ba2 H1WA 128.8 1_656 . ?
O2W Ba2 H1WA 156.9 . . ?
O1W Ba2 H1WA 16.6 . . ?
O12 Ba2 H1WA 67.8 2_455 . ?
O13 Ba2 H1WA 110.6 2_455 . ?
O11 Ba2 H1WA 89.3 . . ?
C23 Ba2 H1WA 89.8 . . ?
C24 Ba2 H1WA 89.0 2_455 . ?
Ba1 Ba2 H1WA 123.8 . . ?
C2 C1 C6 118.5(6) . . ?
C2 C1 C7 119.2(5) . . ?
C6 C1 C7 122.2(5) . . ?
C3 C2 C1 121.5(6) . . ?
C3 C2 H2A 119.2 . . ?
C1 C2 H2A 119.2 . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 C5 119.0(6) . . ?
C3 C4 H4A 120.5 . . ?
C5 C4 H4A 120.5 . . ?
C6 C5 O5 114.7(6) . . ?
C6 C5 C4 121.7(6) . . ?
O5 C5 C4 123.6(5) . . ?
C5 C6 C1 119.0(6) . . ?
C5 C6 C8 117.8(5) . . ?
C1 C6 C8 123.2(5) . . ?
O2 C7 O1 124.1(6) . . ?
O2 C7 C1 117.6(6) . . ?
O1 C7 C1 118.3(5) . . ?
O3 C8 O4 124.2(6) . . ?
O3 C8 C6 117.2(5) . . ?
O4 C8 C6 118.5(5) . . ?
C10 C9 C14 121.7(6) . . ?
C10 C9 O5 121.2(5) . . ?
C14 C9 O5 117.1(5) . . ?
C9 C10 C11 119.5(6) . . ?
C9 C10 H10A 120.3 . . ?
C11 C10 H10A 120.3 . . ?
C12 C11 C10 119.9(6) . . ?
C12 C11 C15 118.2(5) . . ?
C10 C11 C15 121.8(5) . . ?
C11 C12 C13 119.9(6) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C12 C13 C14 120.0(5) . . ?
C12 C13 C16 118.6(6) . . ?
C14 C13 C16 121.4(6) . . ?
C9 C14 C13 118.9(6) . . ?
C9 C14 H14A 120.6 . . ?
C13 C14 H14A 120.6 . . ?
O7 C15 O6 124.0(6) . . ?
O7 C15 C11 122.7(6) . . ?
O6 C15 C11 113.4(5) . . ?
O8 C16 O9 125.4(6) . . ?
O8 C16 C13 123.1(6) . . ?
O9 C16 C13 111.5(5) . . ?
C18 C17 C22 119.1(6) . . ?
C18 C17 C23 118.3(6) . . ?
C22 C17 C23 122.5(5) . . ?
C17 C18 C19 120.5(6) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C20 C19 C18 121.3(6) . . ?
C20 C19 H19A 119.4 . . ?
C18 C19 H19A 119.4 . . ?
C19 C20 C21 118.8(6) . . ?
C19 C20 H20A 120.6 . . ?
C21 C20 H20A 120.6 . . ?
C22 C21 O14 115.9(5) . . ?
C22 C21 C20 120.9(6) . . ?
O14 C21 C20 123.2(5) . . ?
C21 C22 C17 119.4(5) . . ?
C21 C22 C24 116.7(5) . . ?
C17 C22 C24 123.9(5) . . ?
O10 C23 O11 124.2(6) . . ?
O10 C23 C17 116.9(6) . . ?
O11 C23 C17 118.9(6) . . ?
O10 C23 Ba2 54.6(3) . . ?
O11 C23 Ba2 69.6(3) . . ?
C17 C23 Ba2 171.5(4) . . ?
O12 C24 O13 121.8(5) . . ?
O12 C24 C22 120.4(5) . . ?
O13 C24 C22 117.7(5) . . ?
O12 C24 Ba2 61.9(3) . 2_455 ?
O13 C24 Ba2 62.0(3) . 2_455 ?
C22 C24 Ba2 162.6(4) . 2_455 ?
C30 C25 C26 121.0(6) . . ?
C30 C25 O14 119.8(5) . . ?
C26 C25 O14 119.2(5) . . ?
C25 C26 C27 119.3(5) . . ?
C25 C26 H26A 120.4 . . ?
C27 C26 H26A 120.4 . . ?
C26 C27 C28 119.6(5) . . ?
C26 C27 C31 121.4(5) . . ?
C28 C27 C31 118.9(5) . . ?
C29 C28 C27 120.3(6) . . ?
C29 C28 H28A 119.9 . . ?
C27 C28 H28A 119.9 . . ?
C30 C29 C28 120.1(6) . . ?
C30 C29 C32 122.1(6) . . ?
C28 C29 C32 117.8(6) . . ?
C25 C30 C29 119.6(6) . . ?
C25 C30 H30A 120.2 . . ?
C29 C30 H30A 120.2 . . ?
O16 C31 O15 124.9(6) . . ?
O16 C31 C27 120.8(6) . . ?
O15 C31 C27 114.3(5) . . ?
O17 C32 O18 123.7(6) . . ?
O17 C32 C29 122.5(6) . . ?
O18 C32 C29 113.9(6) . . ?
N1 C33 O19 158(3) . . ?
N1 C34 H34A 109.5 . . ?
N1 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
N1 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C35 H35A 109.5 . . ?
N1 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N1 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C7 O1 Ba2 156.2(4) . . ?
Ba2 O1W H1WA 91.0 . . ?
Ba2 O1W H1WB 113.9 . . ?
H1WA O1W H1WB 100.3 . . ?
C7 O2 Ba1 146.3(4) . 2 ?
Ba2 O2W Ba1 101.45(13) . . ?
Ba2 O2W H2WA 126(5) . . ?
Ba1 O2W H2WA 96(5) . . ?
Ba2 O2W H2WB 112(5) . . ?
Ba1 O2W H2WB 115(5) . . ?
H2WA O2W H2WB 105(3) . . ?
H3WA O3W H3WB 109(4) . . ?
C8 O4 Ba2 114.0(3) . . ?
C5 O5 C9 116.6(5) . . ?
C15 O6 H6 111.5 . . ?
C15 O7 Ba1 135.5(4) . 2_556 ?
C16 O8 Ba1 129.8(4) . 1_666 ?
C16 O9 H9 101.6 . . ?
C23 O10 Ba2 103.3(4) . . ?
C23 O11 Ba1 116.9(4) . . ?
C23 O11 Ba2 87.5(4) . . ?
Ba1 O11 Ba2 96.17(12) . . ?
C23 O11 Ba1 128.0(4) . 2_455 ?
Ba1 O11 Ba1 111.72(13) . 2_455 ?
Ba2 O11 Ba1 104.86(12) . 2_455 ?
C24 O12 Ba1 117.4(4) . . ?
C24 O12 Ba2 96.5(3) . 2_455 ?
Ba1 O12 Ba2 113.41(13) . 2_455 ?
C24 O13 Ba1 121.5(4) . 2_455 ?
C24 O13 Ba2 96.4(3) . 2_455 ?
Ba1 O13 Ba2 98.22(12) 2_455 2_455 ?
C21 O14 C25 114.6(4) . . ?
C31 O15 H15A 119.6 . . ?
C31 O16 Ba2 138.2(4) . 1_454 ?
C32 O18 H18 102.4 . . ?
C33 O19 Ba1 144.4(6) . . ?
C33 N1 C34 166(3) . . ?
C33 N1 C35 95(2) . . ?
C34 N1 C35 99(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.146

#=========================END
_database_code_depnum_ccdc_archive 'CCDC 990738'
