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


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#                                CCDC 
# 
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# 
#  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 
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#  except for the purpose of generating routine backup copies 
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data_sun3
_database_code_depnum_ccdc_archive 'CCDC 888794'
#TrackingRef 'web_deposit_cif_file_0_LeiHan_1344431600.Ca.cif'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21 H19 Ca N3 O8, C3 H7 N O '
_chemical_formula_sum            'C24 H26 Ca N4 O9'
_chemical_formula_weight         554.57

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'
Ca Ca 0.2262 0.3064 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/a'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'

_cell_length_a                   28.2810(8)
_cell_length_b                   28.2810(8)
_cell_length_c                   13.5488(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     10836.5(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4640
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_T_max  0.944
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      298(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  ?
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            37248
_diffrn_reflns_av_R_equivalents  0.1336
_diffrn_reflns_av_sigmaI/netI    0.1610
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.67
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5502
_reflns_number_gt                2657
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2005)'
_computing_cell_refinement       'SMART '
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5502
_refine_ls_number_parameters     317
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1529
_refine_ls_wR_factor_gt          0.1387
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.887
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.19023(3) -0.00490(4) 0.62304(9) 0.0280(2) Uani 1 1 d . . .
O1 O 0.20341(12) 0.00244(13) 0.4239(3) 0.0404(10) Uani 1 1 d . . .
O2 O 0.16589(13) 0.05590(14) 0.5102(3) 0.0475(11) Uani 1 1 d . . .
O3 O 0.24182(13) 0.04691(12) 0.0685(2) 0.0344(9) Uani 1 1 d . . .
O4 O 0.18158(13) 0.07738(14) -0.0121(3) 0.0453(10) Uani 1 1 d . . .
O5 O 0.14404(17) 0.21669(14) 0.2600(4) 0.0748(15) Uani 1 1 d . . .
O6 O 0.02956(15) 0.10554(17) 0.2595(4) 0.0839(17) Uani 1 1 d . . .
O7 O 0.13003(16) -0.05118(18) 0.5376(3) 0.0701(14) Uani 1 1 d . . .
O8 O 0.12285(17) 0.03137(18) 0.7040(3) 0.0736(15) Uani 1 1 d . . .
N1 N 0.08709(17) 0.16164(17) 0.2550(4) 0.0376(10) Uani 1 1 d . . .
N2 N 0.0877(3) -0.0330(3) 0.3959(6) 0.123(3) Uani 1 1 d . . .
N3 N 0.0778(2) 0.0117(2) 0.8382(4) 0.0665(16) Uani 1 1 d . . .
C1 C 0.18026(18) 0.04020(19) 0.4305(4) 0.0335(13) Uani 1 1 d . . .
C2 C 0.20148(18) 0.06617(17) 0.0652(4) 0.0284(12) Uani 1 1 d . . .
C3 C 0.16854(17) 0.06609(18) 0.3382(4) 0.0295(12) Uani 1 1 d . . .
C4 C 0.19091(18) 0.05451(17) 0.2482(4) 0.0292(11) Uani 1 1 d . . .
H4A H 0.2148 0.0309 0.2468 0.035 Uiso 1 1 calc R . .
C5 C 0.17798(18) 0.07755(17) 0.1613(4) 0.0310(13) Uani 1 1 d . . .
C6 C 0.14273(19) 0.11169(19) 0.1648(4) 0.0361(14) Uani 1 1 d . . .
H6A H 0.1323 0.1265 0.1058 0.043 Uiso 1 1 calc R . .
C7 C 0.12284(19) 0.1241(2) 0.2545(4) 0.0374(13) Uani 1 1 d . . .
C8 C 0.13483(19) 0.10175(18) 0.3402(4) 0.0337(13) Uani 1 1 d . . .
H8A H 0.1202 0.1105 0.4006 0.040 Uiso 1 1 calc R . .
C9 C 0.1024(2) 0.2078(2) 0.2582(4) 0.0401(15) Uani 1 1 d . . .
C10 C 0.0394(2) 0.1466(2) 0.2586(5) 0.0468(17) Uani 1 1 d . . .
C11 C -0.0439(2) 0.1731(2) 0.2612(5) 0.0591(19) Uani 1 1 d . . .
H11A H -0.0535 0.1410 0.2645 0.071 Uiso 1 1 calc R . .
C12 C 0.00357(19) 0.18476(19) 0.2587(4) 0.0390(15) Uani 1 1 d . . .
C13 C 0.0777(2) 0.2909(2) 0.2587(5) 0.0582(19) Uani 1 1 d . . .
H13A H 0.1102 0.2992 0.2572 0.070 Uiso 1 1 calc R . .
C14 C 0.0658(2) 0.2441(2) 0.2584(4) 0.0412(16) Uani 1 1 d . . .
C15 C 0.0181(2) 0.2321(2) 0.2575(4) 0.0347(12) Uani 1 1 d . . .
C16 C 0.1219(3) -0.0569(3) 0.4493(7) 0.089(2) Uani 1 1 d . . .
H16A H 0.1405 -0.0796 0.4150 0.107 Uiso 1 1 calc R . .
C17 C 0.0576(3) 0.0019(4) 0.4409(8) 0.144(5) Uani 1 1 d . . .
H17A H 0.0643 0.0035 0.5118 0.216 Uiso 1 1 calc R . .
H17B H 0.0245 -0.0069 0.4307 0.216 Uiso 1 1 calc R . .
H17C H 0.0636 0.0329 0.4109 0.216 Uiso 1 1 calc R . .
C18 C 0.0812(4) -0.0377(4) 0.2893(6) 0.141(5) Uani 1 1 d . . .
H18A H 0.0546 -0.0179 0.2681 0.211 Uiso 1 1 calc R . .
H18B H 0.0745 -0.0709 0.2732 0.211 Uiso 1 1 calc R . .
H18C H 0.1100 -0.0277 0.2552 0.211 Uiso 1 1 calc R . .
C19 C 0.1116(3) 0.0358(2) 0.7910(6) 0.067(2) Uani 1 1 d . . .
H19A H 0.1286 0.0585 0.8285 0.081 Uiso 1 1 calc R . .
C20 C 0.0521(3) -0.0235(3) 0.7874(7) 0.118(4) Uani 1 1 d . . .
H20A H 0.0681 -0.0309 0.7251 0.177 Uiso 1 1 calc R . .
H20B H 0.0201 -0.0119 0.7737 0.177 Uiso 1 1 calc R . .
H20C H 0.0503 -0.0520 0.8282 0.177 Uiso 1 1 calc R . .
C21 C 0.0676(2) 0.0209(3) 0.9414(4) 0.109(3) Uani 1 1 d . . .
H21A H 0.0917 0.0422 0.9685 0.163 Uiso 1 1 calc R . .
H21B H 0.0680 -0.0090 0.9781 0.163 Uiso 1 1 calc R . .
H21C H 0.0364 0.0356 0.9473 0.163 Uiso 1 1 calc R . .
O31 O 0.0583(2) 0.1882(3) 0.4755(4) 0.280(7) Uani 1 1 d R . .
N31 N 0.0530(2) 0.1523(3) 0.6232(4) 0.478(16) Uani 1 1 d RDU . .
C31 C 0.0447(2) 0.1052(3) 0.5862(4) 0.432(10) Uani 1 1 d RU . .
H31A H 0.0384 0.0838 0.6416 0.648 Uiso 1 1 calc R . .
H31B H 0.0726 0.0943 0.5501 0.648 Uiso 1 1 calc R . .
H31C H 0.0173 0.1056 0.5417 0.648 Uiso 1 1 calc R . .
C32 C 0.0598(2) 0.1610(3) 0.7264(4) 0.432(10) Uani 1 1 d RD . .
H32A H 0.0521 0.1323 0.7638 0.648 Uiso 1 1 calc R . .
H32B H 0.0393 0.1869 0.7476 0.648 Uiso 1 1 calc R . .
H32C H 0.0929 0.1695 0.7384 0.648 Uiso 1 1 calc R . .
C33 C 0.0622(2) 0.1877(3) 0.5659(4) 0.432(10) Uani 1 1 d R . .
H33 H 0.0729 0.2160 0.5965 0.518 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ca1 0.0264(6) 0.0303(6) 0.0274(4) 0.0056(5) 0.0009(5) 0.0008(6)
O1 0.037(2) 0.038(2) 0.046(2) 0.017(2) 0.0020(17) 0.0144(18)
O2 0.061(3) 0.055(3) 0.027(2) 0.001(2) 0.0042(19) 0.021(2)
O3 0.035(2) 0.032(2) 0.036(2) 0.0004(16) 0.0053(18) 0.0071(18)
O4 0.043(3) 0.068(3) 0.025(2) 0.0067(19) 0.0004(19) 0.011(2)
O5 0.038(3) 0.046(3) 0.141(5) 0.014(3) 0.022(3) 0.022(2)
O6 0.042(3) 0.037(3) 0.173(5) -0.028(3) -0.016(3) 0.018(2)
O7 0.074(3) 0.093(4) 0.044(3) -0.002(3) -0.009(2) -0.029(3)
O8 0.061(3) 0.110(4) 0.050(3) 0.006(3) 0.019(3) 0.038(3)
N1 0.035(3) 0.040(3) 0.038(2) 0.001(2) 0.002(2) 0.025(2)
N2 0.060(5) 0.197(9) 0.112(7) -0.020(6) -0.016(5) 0.010(5)
N3 0.051(4) 0.075(4) 0.073(4) 0.011(3) 0.010(3) -0.011(3)
C1 0.028(3) 0.036(3) 0.037(3) 0.006(3) 0.001(3) 0.006(3)
C2 0.033(3) 0.023(3) 0.030(3) 0.001(2) 0.009(3) 0.008(3)
C3 0.032(3) 0.028(3) 0.028(3) 0.008(2) 0.003(2) 0.011(3)
C4 0.026(3) 0.028(3) 0.033(2) -0.001(2) -0.001(2) 0.012(2)
C5 0.027(3) 0.033(3) 0.033(3) 0.001(2) 0.003(2) 0.008(2)
C6 0.040(3) 0.039(3) 0.029(3) 0.006(3) 0.001(3) 0.013(3)
C7 0.036(3) 0.050(4) 0.027(3) -0.003(3) 0.005(3) 0.024(2)
C8 0.040(3) 0.034(3) 0.028(3) -0.005(2) 0.004(2) 0.017(3)
C9 0.033(4) 0.035(4) 0.053(4) 0.011(3) 0.010(3) 0.024(3)
C10 0.047(4) 0.028(4) 0.065(4) -0.010(3) -0.004(3) 0.015(3)
C11 0.058(5) 0.035(4) 0.084(5) -0.011(4) -0.016(4) 0.009(3)
C12 0.027(3) 0.037(4) 0.054(4) -0.011(3) -0.015(3) 0.015(3)
C13 0.030(4) 0.058(5) 0.087(5) 0.011(4) 0.014(3) 0.020(3)
C14 0.035(4) 0.038(4) 0.050(4) 0.008(3) 0.004(3) 0.016(3)
C15 0.039(4) 0.030(3) 0.035(3) 0.001(3) -0.006(3) 0.018(2)
C16 0.050(5) 0.110(7) 0.108(7) -0.013(6) -0.004(5) -0.014(5)
C17 0.077(7) 0.189(12) 0.166(10) -0.039(9) 0.025(7) 0.046(8)
C18 0.135(9) 0.220(14) 0.067(6) -0.034(7) -0.029(6) -0.021(8)
C19 0.047(5) 0.064(5) 0.091(6) 0.003(5) -0.016(4) 0.016(4)
C20 0.095(7) 0.097(7) 0.162(9) -0.016(6) -0.051(7) -0.017(6)
C21 0.111(8) 0.124(8) 0.092(7) 0.019(6) 0.059(6) 0.015(6)
O31 0.422(18) 0.320(15) 0.097(6) 0.015(7) 0.036(8) 0.134(14)
N31 0.486(18) 0.476(18) 0.473(18) 0.020(10) 0.009(10) 0.018(10)
C31 0.452(13) 0.424(13) 0.419(13) 0.009(9) 0.011(9) 0.035(9)
C32 0.452(13) 0.424(13) 0.419(13) 0.009(9) 0.011(9) 0.035(9)
C33 0.452(13) 0.424(13) 0.419(13) 0.009(9) 0.011(9) 0.035(9)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O3 2.377(4) 7_545 ?
Ca1 O1 2.385(4) 4 ?
Ca1 O2 2.402(4) . ?
Ca1 O8 2.426(4) . ?
Ca1 O4 2.428(4) 6_445 ?
Ca1 O7 2.439(5) . ?
Ca1 O3 2.675(3) 6_445 ?
Ca1 O1 2.732(4) . ?
Ca1 C2 2.887(5) 6_445 ?
Ca1 C1 2.917(5) . ?
Ca1 Ca1 4.1505(8) 4 ?
Ca1 Ca1 4.1505(8) 6_444 ?
O1 C1 1.256(6) . ?
O1 Ca1 2.385(4) 6_444 ?
O2 C1 1.236(6) . ?
O3 C2 1.265(6) . ?
O3 Ca1 2.377(4) 7_544 ?
O3 Ca1 2.675(3) 4_554 ?
O4 C2 1.230(6) . ?
O4 Ca1 2.428(4) 4_554 ?
O5 C9 1.204(7) . ?
O6 C10 1.193(7) . ?
O7 C16 1.230(9) . ?
O8 C19 1.228(8) . ?
N1 C9 1.375(7) . ?
N1 C10 1.416(7) . ?
N1 C7 1.467(6) . ?
N2 C16 1.385(11) . ?
N2 C17 1.438(11) . ?
N2 C18 1.462(10) . ?
N3 C19 1.337(9) . ?
N3 C20 1.411(9) . ?
N3 C21 1.451(8) . ?
C1 C3 1.487(7) . ?
C2 C5 1.497(6) . ?
C2 Ca1 2.887(5) 4_554 ?
C3 C8 1.388(7) . ?
C3 C4 1.413(6) . ?
C4 C5 1.395(6) . ?
C5 C6 1.389(7) . ?
C6 C7 1.383(7) . ?
C7 C8 1.364(7) . ?
C9 C14 1.459(8) . ?
C10 C12 1.481(8) . ?
C11 C12 1.384(9) . ?
C11 C13 1.396(8) 3 ?
C12 C15 1.400(8) . ?
C13 C14 1.365(8) . ?
C13 C11 1.396(8) 3 ?
C14 C15 1.391(8) . ?
C15 C15 1.438(9) 3 ?
O31 C33 1.2302 . ?
N31 C33 1.2933 . ?
N31 C32 1.4327 . ?
N31 C31 1.4425 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ca1 O1 78.38(10) 7_545 4 ?
O3 Ca1 O2 113.06(12) 7_545 . ?
O1 Ca1 O2 87.60(13) 4 . ?
O3 Ca1 O8 170.67(14) 7_545 . ?
O1 Ca1 O8 101.00(15) 4 . ?
O2 Ca1 O8 76.11(14) . . ?
O3 Ca1 O4 89.72(13) 7_545 6_445 ?
O1 Ca1 O4 114.70(13) 4 6_445 ?
O2 Ca1 O4 151.50(13) . 6_445 ?
O8 Ca1 O4 82.07(16) . 6_445 ?
O3 Ca1 O7 98.55(15) 7_545 . ?
O1 Ca1 O7 168.31(14) 4 . ?
O2 Ca1 O7 83.23(16) . . ?
O8 Ca1 O7 83.86(16) . . ?
O4 Ca1 O7 76.34(14) 6_445 . ?
O3 Ca1 O3 100.39(11) 7_545 6_445 ?
O1 Ca1 O3 68.59(11) 4 6_445 ?
O2 Ca1 O3 133.96(13) . 6_445 ?
O8 Ca1 O3 70.97(13) . 6_445 ?
O4 Ca1 O3 50.79(12) 6_445 6_445 ?
O7 Ca1 O3 123.09(13) . 6_445 ?
O3 Ca1 O1 67.71(10) 7_545 . ?
O1 Ca1 O1 97.94(11) 4 . ?
O2 Ca1 O1 49.90(11) . . ?
O8 Ca1 O1 121.44(13) . . ?
O4 Ca1 O1 135.82(13) 6_445 . ?
O7 Ca1 O1 70.58(12) . . ?
O3 Ca1 O1 164.16(9) 6_445 . ?
O3 Ca1 C2 96.74(13) 7_545 6_445 ?
O1 Ca1 C2 92.68(14) 4 6_445 ?
O2 Ca1 C2 149.56(14) . 6_445 ?
O8 Ca1 C2 73.96(15) . 6_445 ?
O4 Ca1 C2 24.91(12) 6_445 6_445 ?
O7 Ca1 C2 98.90(15) . 6_445 ?
O3 Ca1 C2 25.94(12) 6_445 6_445 ?
O1 Ca1 C2 158.72(14) . 6_445 ?
O3 Ca1 C1 91.07(14) 7_545 . ?
O1 Ca1 C1 93.59(14) 4 . ?
O2 Ca1 C1 24.51(12) . . ?
O8 Ca1 C1 98.25(16) . . ?
O4 Ca1 C1 151.23(15) 6_445 . ?
O7 Ca1 C1 75.10(15) . . ?
O3 Ca1 C1 156.01(14) 6_445 . ?
O1 Ca1 C1 25.41(12) . . ?
C2 Ca1 C1 170.83(13) 6_445 . ?
O3 Ca1 Ca1 99.88(9) 7_545 4 ?
O1 Ca1 Ca1 38.71(9) 4 4 ?
O2 Ca1 Ca1 108.14(10) . 4 ?
O8 Ca1 Ca1 74.84(12) . 4 ?
O4 Ca1 Ca1 83.09(9) 6_445 4 ?
O7 Ca1 Ca1 152.19(11) . 4 ?
O3 Ca1 Ca1 32.48(8) 6_445 4 ?
O1 Ca1 Ca1 136.19(8) . 4 ?
C2 Ca1 Ca1 58.38(11) 6_445 4 ?
C1 Ca1 Ca1 124.98(11) . 4 ?
O3 Ca1 Ca1 37.18(9) 7_545 6_444 ?
O1 Ca1 Ca1 97.98(8) 4 6_444 ?
O2 Ca1 Ca1 82.79(9) . 6_444 ?
O8 Ca1 Ca1 150.82(12) . 6_444 ?
O4 Ca1 Ca1 109.67(11) 6_445 6_444 ?
O7 Ca1 Ca1 73.73(11) . 6_444 ?
O3 Ca1 Ca1 137.32(8) 6_445 6_444 ?
O1 Ca1 Ca1 33.09(8) . 6_444 ?
C2 Ca1 Ca1 127.15(11) 6_445 6_444 ?
C1 Ca1 Ca1 58.42(11) . 6_444 ?
Ca1 Ca1 Ca1 131.761(19) 4 6_444 ?
C1 O1 Ca1 165.0(3) . 6_444 ?
C1 O1 Ca1 85.6(3) . . ?
Ca1 O1 Ca1 108.20(13) 6_444 . ?
C1 O2 Ca1 101.8(3) . . ?
C2 O3 Ca1 162.8(3) . 7_544 ?
C2 O3 Ca1 86.4(3) . 4_554 ?
Ca1 O3 Ca1 110.34(13) 7_544 4_554 ?
C2 O4 Ca1 98.9(3) . 4_554 ?
C16 O7 Ca1 131.5(5) . . ?
C19 O8 Ca1 132.9(4) . . ?
C9 N1 C10 125.8(4) . . ?
C9 N1 C7 118.1(5) . . ?
C10 N1 C7 116.0(5) . . ?
C16 N2 C17 121.8(8) . . ?
C16 N2 C18 124.0(9) . . ?
C17 N2 C18 114.1(9) . . ?
C19 N3 C20 119.7(7) . . ?
C19 N3 C21 120.7(7) . . ?
C20 N3 C21 119.6(7) . . ?
O2 C1 O1 122.6(5) . . ?
O2 C1 C3 119.0(5) . . ?
O1 C1 C3 118.4(5) . . ?
O2 C1 Ca1 53.7(3) . . ?
O1 C1 Ca1 69.0(3) . . ?
C3 C1 Ca1 171.5(4) . . ?
O4 C2 O3 123.6(4) . . ?
O4 C2 C5 118.8(4) . . ?
O3 C2 C5 117.5(4) . . ?
O4 C2 Ca1 56.2(2) . 4_554 ?
O3 C2 Ca1 67.6(3) . 4_554 ?
C5 C2 Ca1 171.0(3) . 4_554 ?
C8 C3 C4 119.5(4) . . ?
C8 C3 C1 119.7(5) . . ?
C4 C3 C1 120.8(4) . . ?
C5 C4 C3 120.2(4) . . ?
C6 C5 C4 118.9(5) . . ?
C6 C5 C2 119.9(5) . . ?
C4 C5 C2 121.2(4) . . ?
C7 C6 C5 119.9(5) . . ?
C8 C7 C6 122.0(4) . . ?
C8 C7 N1 120.2(5) . . ?
C6 C7 N1 117.9(5) . . ?
C7 C8 C3 119.4(5) . . ?
O5 C9 N1 120.5(5) . . ?
O5 C9 C14 123.1(6) . . ?
N1 C9 C14 116.4(5) . . ?
O6 C10 N1 121.0(5) . . ?
O6 C10 C12 123.4(6) . . ?
N1 C10 C12 115.6(5) . . ?
C12 C11 C13 119.3(7) . 3 ?
C11 C12 C15 120.8(5) . . ?
C11 C12 C10 119.4(5) . . ?
C15 C12 C10 119.8(5) . . ?
C14 C13 C11 122.7(6) . 3 ?
C13 C14 C15 118.3(5) . . ?
C13 C14 C9 120.5(6) . . ?
C15 C14 C9 121.1(5) . . ?
C14 C15 C12 121.1(4) . . ?
C14 C15 C15 121.2(7) . 3 ?
C12 C15 C15 117.7(7) . 3 ?
O7 C16 N2 125.0(9) . . ?
O8 C19 N3 126.3(7) . . ?
C33 N31 C32 115.2 . . ?
C33 N31 C31 122.6 . . ?
C32 N31 C31 121.2 . . ?
O31 C33 N31 126.1 . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.368
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.067