Supplementary Material (ESI) for Chemical Communications
This journal is (C) The Royal Society of Chemistry 2001

data_global

_journal_coden_Cambridge      182

loop_
_publ_author_name
'Blake, Alexander J.'
'Devillanova, F. A.'
'Garau, Alessandra'
'Lippolis, Vito'
'Schroder, Martin'
'Tei, Lorenzo'
'Wilson, Claire'


_publ_contact_author_name     	'Prof Martin Schroder'  
_publ_contact_author_address 
;
School of Chemistry
University of Nottingham
University Park
Nottingham
NG7 2RD
UNITED KINGDOM
;

_publ_contact_author_phone          '0115 951 3488/3047'
_publ_contact_author_fax                 '0115 951 3563'
_publ_contact_author_email            'M.SCHRODER@NOTTINGHAM.AC.UK'
_publ_requested_journal                  'Chemical Communications'

_publ_section_title
;
A new co-facial dinucleating macropolycycle: segregated versus encapsulated 
complexation
;


data_(4)

_database_code_CSD	171456

# Code CDCAGE

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum            'C40 H64 Cd2 N12 O10'
_chemical_formula_weight          1097.83

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            Monoclinic
_symmetry_space_group_name_H-M    C2/c

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

_cell_length_a                    29.371(2)
_cell_length_b                    10.3258(8)
_cell_length_c                    14.6576(11)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.1880(10)
_cell_angle_gamma                 90.00
_cell_volume                      4419.5(6)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     3499
_cell_measurement_theta_min       2.45
_cell_measurement_theta_max       27.35

_exptl_crystal_description        tablet
_exptl_crystal_colour             Yellow
_exptl_crystal_size_max           0.17
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.07
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.650
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              2256
_exptl_absorpt_coefficient_mu     1.034
_exptl_absorpt_correction_type    Multi-scan
_exptl_absorpt_correction_T_min   0.641
_exptl_absorpt_correction_T_max   0.690
_exptl_absorpt_process_details   '(Saint v6.02a; SHELXTL v5.10)'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type  'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method        omega
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         '<1% (uncorrected)'
_diffrn_reflns_number             13410
_diffrn_reflns_av_R_equivalents   0.0451
_diffrn_reflns_av_sigmaI/netI     0.0729
_diffrn_reflns_limit_h_min        -24
_diffrn_reflns_limit_h_max        38
_diffrn_reflns_limit_k_min        -12
_diffrn_reflns_limit_k_max        13
_diffrn_reflns_limit_l_min        -19
_diffrn_reflns_limit_l_max        19
_diffrn_reflns_theta_min          1.39
_diffrn_reflns_theta_max          28.74
_reflns_number_total              5125
_reflns_number_gt                 3569
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection      'Bruker SMART version 5.054 (Bruker, 1998)'
_computing_cell_refinement      'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction       
'Bruker SAINT; Bruker SHELXTL (Bruker,1997)'
_computing_structure_solution   'Bruker SHELXTL'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics   'Bruker SHELXTL'
_computing_publication_material 'SHELXL-97; PLATON (Spek, 2000)'

_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^)+(0.0272P)^2^+4.0376P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      'Direct methods'
_atom_sites_solution_secondary    'Difference Fourier map'
_atom_sites_solution_hydrogens    
'DeltaF synthesis for MeOH H, others placed geometrically'
_refine_ls_hydrogen_treatment     
'rotating rigid body for MeOH, others riding on parent atom'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5125
_refine_ls_number_parameters      293
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0584
_refine_ls_R_factor_gt            0.0342
_refine_ls_wR_factor_ref          0.0811
_refine_ls_wR_factor_gt           0.0672
_refine_ls_goodness_of_fit_ref    0.964
_refine_ls_restrained_S_all       0.964
_refine_ls_shift/su_max           0.017
_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_symetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd Cd 0.616512(9) 0.45986(2) 0.333665(17) 0.01621(8) Uani 1 1 d . . .
N1 N 0.68644(10) 0.3851(3) 0.41683(18) 0.0180(7) Uani 1 1 d . . .
C2 C 0.69190(12) 0.4593(4) 0.5041(2) 0.0213(8) Uani 1 1 d . . .
H2A H 0.7211 0.4341 0.5397 0.026 Uiso 1 1 calc R . .
H2B H 0.6667 0.4363 0.5408 0.026 Uiso 1 1 calc R . .
C3 C 0.69174(12) 0.6052(4) 0.4888(2) 0.0227(8) Uani 1 1 d . . .
H3A H 0.6924 0.6500 0.5487 0.027 Uiso 1 1 calc R . .
H3B H 0.7196 0.6306 0.4606 0.027 Uiso 1 1 calc R . .
N4 N 0.65035(10) 0.6460(3) 0.42813(19) 0.0202(7) Uani 1 1 d . . .
C5 C 0.66224(13) 0.7401(4) 0.3586(3) 0.0240(9) Uani 1 1 d . . .
H5A H 0.6791 0.8134 0.3899 0.029 Uiso 1 1 calc R . .
H5B H 0.6337 0.7748 0.3253 0.029 Uiso 1 1 calc R . .
C6 C 0.69157(13) 0.6798(4) 0.2895(3) 0.0261(9) Uani 1 1 d . . .
H6A H 0.6926 0.7397 0.2370 0.031 Uiso 1 1 calc R . .
H6B H 0.7232 0.6686 0.3191 0.031 Uiso 1 1 calc R . .
N7 N 0.67376(10) 0.5529(3) 0.25505(19) 0.0224(7) Uani 1 1 d . . .
H7 H 0.6621 0.5628 0.1939 0.027 Uiso 1 1 calc R . .
C8 C 0.70856(12) 0.4474(4) 0.2605(2) 0.0243(8) Uani 1 1 d . . .
H8A H 0.7354 0.4766 0.2306 0.029 Uiso 1 1 calc R . .
H8B H 0.6954 0.3708 0.2265 0.029 Uiso 1 1 calc R . .
C9 C 0.72425(12) 0.4083(4) 0.3603(2) 0.0228(8) Uani 1 1 d . . .
H9A H 0.7429 0.3285 0.3599 0.027 Uiso 1 1 calc R . .
H9B H 0.7441 0.4776 0.3894 0.027 Uiso 1 1 calc R . .
C11 C 0.67889(13) 0.2472(3) 0.4346(2) 0.0218(8) Uani 1 1 d . . .
H11A H 0.6557 0.2384 0.4784 0.026 Uiso 1 1 calc R . .
H11B H 0.7078 0.2080 0.4630 0.026 Uiso 1 1 calc R . .
C12 C 0.66273(12) 0.1749(3) 0.3464(2) 0.0216(8) Uani 1 1 d . . .
H12A H 0.6878 0.1709 0.3064 0.026 Uiso 1 1 calc R . .
H12B H 0.6541 0.0852 0.3610 0.026 Uiso 1 1 calc R . .
N13 N 0.62288(10) 0.2428(3) 0.29837(19) 0.0186(7) Uani 1 1 d . . .
C14 C 0.59644(12) 0.1757(3) 0.2414(2) 0.0192(8) Uani 1 1 d . . .
H14A H 0.6049 0.0879 0.2336 0.023 Uiso 1 1 calc R . .
C15 C 0.55466(12) 0.2198(3) 0.1873(2) 0.0170(8) Uani 1 1 d . . .
C16 C 0.54236(12) 0.3519(3) 0.1716(2) 0.0157(7) Uani 1 1 d . . .
O17 O 0.56884(8) 0.4493(2) 0.20013(15) 0.0196(5) Uani 1 1 d . . .
C41 C 0.61409(12) 0.6932(3) 0.4817(2) 0.0218(8) Uani 1 1 d . . .
H41A H 0.6204 0.7845 0.4994 0.026 Uiso 1 1 calc R . .
H41B H 0.6145 0.6416 0.5388 0.026 Uiso 1 1 calc R . .
C42 C 0.56707(12) 0.6839(3) 0.4283(2) 0.0202(8) Uani 1 1 d . . .
H42A H 0.5437 0.7155 0.4667 0.024 Uiso 1 1 calc R . .
H42B H 0.5659 0.7393 0.3730 0.024 Uiso 1 1 calc R . .
N43 N 0.55693(10) 0.5492(3) 0.40086(18) 0.0173(6) Uani 1 1 d . . .
C44 C 0.51550(12) 0.5099(3) 0.3968(2) 0.0166(8) Uani 1 1 d . . .
H44A H 0.4924 0.5711 0.4069 0.020 Uiso 1 1 calc R . .
C45 C 0.50157(12) 0.3752(3) 0.3774(2) 0.0156(7) Uani 1 1 d . . .
C46 C 0.53051(12) 0.2744(3) 0.4093(2) 0.0170(8) Uani 1 1 d . . .
H46A H 0.5596 0.2942 0.4412 0.020 Uiso 1 1 calc R . .
C47 C 0.51795(12) 0.1457(3) 0.3957(2) 0.0189(8) Uani 1 1 d . . .
C48 C 0.47527(12) 0.1224(3) 0.3479(2) 0.0195(8) Uani 1 1 d . . .
H48 H 0.4659 0.0349 0.3387 0.023 Uiso 1 1 calc R . .
C49 C 0.54994(12) 0.0358(4) 0.4275(2) 0.0250(8) Uani 1 1 d . . .
H49A H 0.5772 0.0708 0.4637 0.038 Uiso 1 1 calc R . .
H49B H 0.5591 -0.0103 0.3740 0.038 Uiso 1 1 calc R . .
H49C H 0.5342 -0.0242 0.4653 0.038 Uiso 1 1 calc R . .
N1S N 0.67412(11) 0.0378(3) 0.1154(2) 0.0317(8) Uani 1 1 d . . .
O1 O 0.69419(10) 0.1421(3) 0.1333(2) 0.0406(8) Uani 1 1 d . . .
O2 O 0.67009(11) -0.0392(3) 0.1805(2) 0.0537(9) Uani 1 1 d . . .
O3 O 0.65979(17) 0.0103(3) 0.0381(2) 0.0960(18) Uani 1 1 d . . .
C1M C 0.57775(16) 0.7627(4) 0.1426(3) 0.0405(12) Uani 1 1 d . . .
H1M1 H 0.5704 0.7453 0.2051 0.061 Uiso 1 1 calc R . .
H1M2 H 0.5497 0.7849 0.1034 0.061 Uiso 1 1 calc R . .
H1M3 H 0.5994 0.8351 0.1436 0.061 Uiso 1 1 calc R . .
O1M O 0.59779(11) 0.6509(3) 0.1073(2) 0.0449(8) Uani 1 1 d . . .
H1M H 0.5898(14) 0.574(4) 0.143(3) 0.067 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
Cd 0.01514(13) 0.01576(13) 0.01757(13) -0.00091(12) 0.00097(9) 0.00088(12)
N1 0.0170(16) 0.0210(16) 0.0157(14) 0.0010(13) 0.0002(13) 0.0006(13)
C2 0.0198(19) 0.027(2) 0.0160(16) 0.0010(17) -0.0012(15) 0.0018(18)
C3 0.021(2) 0.024(2) 0.0216(19) -0.0043(16) -0.0008(16) -0.0021(17)
N4 0.0163(16) 0.0221(17) 0.0222(16) -0.0021(13) 0.0016(13) -0.0012(13)
C5 0.018(2) 0.021(2) 0.033(2) 0.0021(17) 0.0011(17) -0.0031(16)
C6 0.018(2) 0.028(2) 0.033(2) 0.0083(18) 0.0045(17) -0.0040(17)
N7 0.0209(16) 0.0278(18) 0.0187(15) 0.0052(14) 0.0026(13) 0.0011(15)
C8 0.022(2) 0.031(2) 0.0216(18) 0.0003(17) 0.0058(16) 0.0038(18)
C9 0.017(2) 0.028(2) 0.0231(19) -0.0003(16) 0.0032(16) 0.0035(17)
C11 0.022(2) 0.0184(19) 0.0247(19) 0.0047(16) -0.0013(17) 0.0041(16)
C12 0.019(2) 0.019(2) 0.0250(19) 0.0010(16) -0.0025(16) 0.0059(16)
N13 0.0199(17) 0.0182(16) 0.0175(15) 0.0004(13) 0.0018(13) 0.0034(13)
C14 0.022(2) 0.0152(18) 0.0202(18) -0.0003(15) 0.0027(16) 0.0038(15)
C15 0.0189(19) 0.0149(18) 0.0175(17) -0.0007(14) 0.0037(15) 0.0007(15)
C16 0.0184(19) 0.0168(19) 0.0127(16) -0.0003(14) 0.0051(15) -0.0003(15)
O17 0.0201(13) 0.0164(13) 0.0211(12) 0.0017(11) -0.0025(10) -0.0024(11)
C41 0.023(2) 0.0190(19) 0.0238(19) -0.0064(16) 0.0017(17) -0.0020(16)
C42 0.021(2) 0.0142(18) 0.0255(19) -0.0030(15) 0.0033(16) 0.0012(16)
N43 0.0180(16) 0.0146(15) 0.0188(14) 0.0001(13) -0.0007(12) 0.0008(13)
C44 0.0195(19) 0.0167(18) 0.0135(16) 0.0012(14) 0.0015(15) 0.0036(15)
C45 0.0169(19) 0.0166(18) 0.0139(16) 0.0002(14) 0.0038(14) -0.0008(15)
C46 0.0153(19) 0.0215(19) 0.0146(17) -0.0001(15) 0.0033(15) 0.0009(15)
C47 0.023(2) 0.0184(19) 0.0154(17) 0.0022(14) 0.0042(16) 0.0027(16)
C48 0.027(2) 0.0131(18) 0.0193(18) 0.0000(15) 0.0046(16) -0.0032(16)
C49 0.026(2) 0.022(2) 0.0261(19) 0.0017(17) 0.0006(16) 0.0050(18)
N1S 0.0290(19) 0.0254(19) 0.039(2) -0.0026(18) -0.0037(16) 0.0147(17)
O1 0.0353(18) 0.0234(16) 0.061(2) 0.0041(14) -0.0058(16) -0.0053(14)
O2 0.059(2) 0.0306(17) 0.077(2) 0.0106(18) 0.0309(19) 0.0045(17)
O3 0.161(5) 0.047(2) 0.063(2) -0.0243(19) -0.066(3) 0.038(3)
C1M 0.055(3) 0.025(2) 0.037(2) -0.0003(19) -0.011(2) -0.005(2)
O1M 0.045(2) 0.049(2) 0.0406(18) 0.0163(15) 0.0049(16) 0.0089(17)

_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
Cd O17 2.283(2) . y
Cd N43 2.293(3) . y
Cd N13 2.312(3) . y
Cd N7 2.344(3) . y
Cd N1 2.400(3) . y
Cd N4 2.510(3) . y
N1 C11 1.469(4) . ?
N1 C9 1.474(4) . ?
N1 C2 1.484(4) . ?
C2 C3 1.523(5) . ?
C3 N4 1.488(4) . ?
N4 C41 1.473(4) . ?
N4 C5 1.477(4) . ?
C5 C6 1.530(5) . ?
C6 N7 1.480(4) . ?
N7 C8 1.490(4) . ?
C8 C9 1.540(5) . ?
C11 C12 1.523(5) . ?
C12 N13 1.476(4) . ?
N13 C14 1.281(4) . ?
C14 C15 1.460(5) . ?
C15 C48 1.398(5) 2_655 ?
C15 C16 1.424(5) . ?
C16 O17 1.312(4) . ?
C16 C45 1.428(5) 2_655 ?
C41 C42 1.516(5) . ?
C42 N43 1.469(4) . ?
N43 C44 1.278(4) . ?
C44 C45 1.468(5) . ?
C45 C46 1.393(4) . ?
C45 C16 1.428(5) 2_655 ?
C46 C47 1.387(5) . ?
C47 C48 1.389(5) . ?
C47 C49 1.515(5) . ?
C48 C15 1.398(5) 2_655 ?
N1S O3 1.199(4) . ?
N1S O1 1.242(4) . ?
N1S O2 1.257(4) . ?
C1M O1M 1.418(5) . ?

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
O17 Cd N43 87.80(9) . . y
O17 Cd N13 79.56(9) . . y
N43 Cd N13 124.76(10) . . y
O17 Cd N7 90.25(9) . . y
N43 Cd N7 131.88(10) . . y
N13 Cd N7 101.97(10) . . y
O17 Cd N1 146.32(9) . . y
N43 Cd N1 124.22(9) . . y
N13 Cd N1 73.53(10) . . y
N7 Cd N1 76.20(10) . . y
O17 Cd N4 132.79(9) . . y
N43 Cd N4 74.34(10) . . y
N13 Cd N4 145.96(10) . . y
N7 Cd N4 72.25(10) . . y
N1 Cd N4 72.53(9) . . y
C11 N1 C9 113.2(3) . . ?
C11 N1 C2 110.6(3) . . ?
C9 N1 C2 112.4(3) . . ?
C11 N1 Cd 105.3(2) . . ?
C9 N1 Cd 108.52(19) . . ?
C2 N1 Cd 106.2(2) . . ?
N1 C2 C3 112.7(3) . . ?
N4 C3 C2 110.9(3) . . ?
C41 N4 C5 112.9(3) . . ?
C41 N4 C3 111.5(3) . . ?
C5 N4 C3 111.1(3) . . ?
C41 N4 Cd 106.4(2) . . ?
C5 N4 Cd 103.4(2) . . ?
C3 N4 Cd 111.3(2) . . ?
N4 C5 C6 112.4(3) . . ?
N7 C6 C5 112.5(3) . . ?
C6 N7 C8 114.5(3) . . ?
C6 N7 Cd 116.2(2) . . ?
C8 N7 Cd 101.4(2) . . ?
N7 C8 C9 112.1(3) . . ?
N1 C9 C8 114.2(3) . . ?
N1 C11 C12 111.3(3) . . ?
N13 C12 C11 109.3(3) . . ?
C14 N13 C12 116.6(3) . . ?
C14 N13 Cd 127.8(2) . . ?
C12 N13 Cd 115.6(2) . . ?
N13 C14 C15 126.9(3) . . ?
C48 C15 C16 119.4(3) 2_655 . ?
C48 C15 C14 115.7(3) 2_655 . ?
C16 C15 C14 124.8(3) . . ?
O17 C16 C15 123.5(3) . . ?
O17 C16 C45 120.2(3) . 2_655 ?
C15 C16 C45 116.3(3) . 2_655 ?
C16 O17 Cd 126.7(2) . . ?
N4 C41 C42 112.0(3) . . ?
N43 C42 C41 110.4(3) . . ?
C44 N43 C42 118.5(3) . . ?
C44 N43 Cd 128.2(2) . . ?
C42 N43 Cd 110.9(2) . . ?
N43 C44 C45 123.6(3) . . ?
C46 C45 C16 121.9(3) . 2_655 ?
C46 C45 C44 119.7(3) . . ?
C16 C45 C44 118.4(3) 2_655 . ?
C47 C46 C45 121.6(3) . . ?
C46 C47 C48 116.8(3) . . ?
C46 C47 C49 121.8(3) . . ?
C48 C47 C49 121.4(3) . . ?
C47 C48 C15 124.0(3) . 2_655 ?
O3 N1S O1 121.0(4) . . ?
O3 N1S O2 121.0(4) . . ?
O1 N1S O2 117.9(3) . . ?

_diffrn_measured_fraction_theta_max    0.896
_diffrn_reflns_theta_full              27.50
_diffrn_measured_fraction_theta_full   0.978
_refine_diff_density_max    1.01
_refine_diff_density_min   -0.71
_refine_diff_density_rms    0.10

#===END


data_(5)

_database_code_CSD	171457

# Code YPHON3

_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum             'C42 H73 N16 O25 Y3'
_chemical_formula_weight          1468.89

_refine_special_details
;
One nitrate oxygen was modelled over two sites, 0.55:0.45 with
distance restraints applied and isotropic adps. Two other non-H atoms were
refined with isotropic adps - the MeO coordinated to Y2, which refined
with unacceptably large anistropic adps and for which no alternative
sites could be located. There are a number of significant systematically
absent reflections in the data set, however, solution and partial refinement
in a lower symmetry space group - e.g. C2 shows considerable correlation
between independent atoms and an over 90% fit to C2/c.
Generally poor anistropic adps, however, no improvement through use of
XABS or tighter application of DELU restraints.
;

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'
'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'
'Y'  'Y'  -2.7962   3.5667
'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            'Monoclinic'
_symmetry_space_group_name_H-M    'C2/c'

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

_cell_length_a                    21.414(5)
_cell_length_b                    17.830(3)
_cell_length_c                    18.622(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  123.285(3)
_cell_angle_gamma                 90.00
_cell_volume                      5944(2)
_cell_formula_units_Z             4
_cell_measurement_temperature     150(2)
_cell_measurement_reflns_used     2539
_cell_measurement_theta_min       2.3
_cell_measurement_theta_max       22.75

_exptl_crystal_description        'rectangular tablet'
_exptl_crystal_colour             'yellow'
_exptl_crystal_size_max           0.30
_exptl_crystal_size_mid           0.16
_exptl_crystal_size_min           0.04
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.642
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              3016
_exptl_absorpt_coefficient_mu     2.998
_exptl_absorpt_correction_type    'multi-scan'
_exptl_absorpt_correction_T_min   0.635
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    'Bruker SADABS v.2 (2001)'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       150(2)
_diffrn_radiation_wavelength      0.71073
_diffrn_radiation_type            MoK\a
_diffrn_radiation_source          'fine-focus sealed tube'
_diffrn_radiation_monochromator   graphite
_diffrn_measurement_device_type   'Bruker SMART1000 CCD area detector'
_diffrn_measurement_method        omega
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             16196
_diffrn_reflns_av_R_equivalents   0.074
_diffrn_reflns_av_sigmaI/netI     0.1018
_diffrn_reflns_limit_h_min        -24
_diffrn_reflns_limit_h_max        27
_diffrn_reflns_limit_k_min        -14
_diffrn_reflns_limit_k_max        23
_diffrn_reflns_limit_l_min        -23
_diffrn_reflns_limit_l_max        15
_diffrn_reflns_theta_min          1.64
_diffrn_reflns_theta_max          26.00
_reflns_number_total              6981
_reflns_number_gt                 3733
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection      'Bruker SMART version 5.624 (Bruker, 2001)'
_computing_cell_refinement      'Bruker SAINT version 6.02a (Bruker, 2000)'
_computing_data_reduction      
'Bruker SAINT; Bruker SHELXTL (Bruker,1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     ?
_computing_publication_material   ?

_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^)+(0.0001P)^2^+164.1717P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      Patterson
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    'geometrically placed, MeOH from delta-F'
_refine_ls_hydrogen_treatment     'riding model, MeOH rotating rigid group'
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          5802
_refine_ls_number_parameters      383
_refine_ls_number_restraints      113
_refine_ls_R_factor_all           0.1491
_refine_ls_R_factor_gt            0.0983
_refine_ls_wR_factor_ref          0.2476
_refine_ls_wR_factor_gt           0.2238
_refine_ls_goodness_of_fit_ref    1.191
_refine_ls_restrained_S_all       1.182
_refine_ls_shift/su_max           0.012
_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_symetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Y1 Y 0.42800(5) 0.20660(6) 0.76530(7) 0.0344(3) Uani 1 1 d U . .
Y2 Y 0.5000 0.30660(10) 0.2500 0.0546(5) Uani 1 2 d SU . .
O1 O 0.5000 0.1228(6) 0.7500 0.069(4) Uani 1 2 d SU . .
N1 N 0.7019(4) 0.2382(5) 0.7550(5) 0.0354(19) Uani 1 1 d U . .
C2 C 0.6989(6) 0.1943(7) 0.6845(7) 0.041(2) Uani 1 1 d U . .
H2A H 0.6590 0.2154 0.6285 0.049 Uiso 1 1 calc R . .
H2B H 0.7469 0.2008 0.6891 0.049 Uiso 1 1 calc R . .
C3 C 0.6850(6) 0.1132(7) 0.6851(8) 0.047(3) Uani 1 1 d U . .
H3A H 0.7304 0.0896 0.7340 0.057 Uiso 1 1 calc R . .
H3B H 0.6758 0.0904 0.6316 0.057 Uiso 1 1 calc R . .
N4 N 0.6196(6) 0.0958(6) 0.6922(9) 0.063(3) Uani 1 1 d U . .
C5 C 0.6410(9) 0.0381(8) 0.7596(13) 0.082(4) Uani 1 1 d U . .
H5A H 0.5959 0.0214 0.7574 0.099 Uiso 1 1 calc R . .
H5B H 0.6625 -0.0059 0.7482 0.099 Uiso 1 1 calc R . .
C6 C 0.6958(10) 0.0677(8) 0.8456(12) 0.084(4) Uani 1 1 d U . .
H6A H 0.7454 0.0702 0.8535 0.101 Uiso 1 1 calc R . .
H6B H 0.6997 0.0330 0.8893 0.101 Uiso 1 1 calc R . .
N7 N 0.6755(6) 0.1428(6) 0.8590(7) 0.056(3) Uani 1 1 d U . .
H7 H 0.6611 0.1365 0.8976 0.067 Uiso 1 1 calc R . .
C8 C 0.7388(6) 0.1962(8) 0.8999(7) 0.053(3) Uani 1 1 d U . .
H8A H 0.7804 0.1749 0.9547 0.064 Uiso 1 1 calc R . .
H8B H 0.7229 0.2436 0.9129 0.064 Uiso 1 1 calc R . .
C9 C 0.7657(6) 0.2122(7) 0.8410(6) 0.045(3) Uani 1 1 d U . .
H9A H 0.8049 0.2514 0.8669 0.054 Uiso 1 1 calc R . .
H9B H 0.7877 0.1662 0.8340 0.054 Uiso 1 1 calc R . .
C41 C 0.5552(8) 0.0704(9) 0.6061(13) 0.091(5) Uani 1 1 d U . .
H41A H 0.5717 0.0285 0.5854 0.109 Uiso 1 1 calc R . .
H41B H 0.5148 0.0516 0.6120 0.109 Uiso 1 1 calc R . .
C42 C 0.5264(8) 0.1305(10) 0.5432(11) 0.085(5) Uani 1 1 d U . .
H42B H 0.4796 0.1139 0.4902 0.102 Uiso 1 1 calc R . .
H42A H 0.5631 0.1425 0.5283 0.102 Uiso 1 1 calc R . .
C11 C 0.7094(6) 0.3196(6) 0.7434(7) 0.038(2) Uani 1 1 d U . .
H11B H 0.7313 0.3262 0.7088 0.046 Uiso 1 1 calc R . .
H11A H 0.7431 0.3435 0.8000 0.046 Uiso 1 1 calc R . .
C12 C 0.6338(6) 0.3563(6) 0.6986(6) 0.037(2) Uani 1 1 d U . .
H12A H 0.6386 0.4113 0.6954 0.044 Uiso 1 1 calc R . .
H12B H 0.6012 0.3366 0.6394 0.044 Uiso 1 1 calc R . .
N13 N 0.6022(4) 0.3388(5) 0.7493(5) 0.0311(18) Uani 1 1 d U . .
C14 C 0.6061(6) 0.3905(6) 0.7977(7) 0.033(2) Uani 1 1 d U . .
H14A H 0.6202 0.4387 0.7895 0.040 Uiso 1 1 calc R . .
C15 C 0.5907(5) 0.3840(6) 0.8667(6) 0.033(2) Uani 1 1 d U . .
C16 C 0.6010(6) 0.4474(7) 0.9143(7) 0.042(2) Uani 1 1 d U . .
H16A H 0.6154 0.4926 0.9003 0.050 Uiso 1 1 calc R . .
C17 C 0.5909(6) 0.4477(8) 0.9827(7) 0.051(3) Uani 1 1 d U . .
C18 C 0.5704(6) 0.3798(8) 1.0013(6) 0.048(2) Uani 1 1 d U . .
H18A H 0.5668 0.3772 1.0499 0.057 Uiso 1 1 calc R . .
C19 C 0.5548(5) 0.3154(7) 0.9513(6) 0.041(2) Uani 1 1 d U . .
C20 C 0.5658(5) 0.3165(6) 0.8821(6) 0.0313(19) Uani 1 1 d U . .
O21 O 0.5526(3) 0.2546(4) 0.8369(4) 0.0335(15) Uani 1 1 d U . .
C22 C 0.6028(8) 0.5188(8) 1.0323(8) 0.069(4) Uani 1 1 d U . .
H22A H 0.5930 0.5093 1.0771 0.104 Uiso 1 1 calc R . .
H22B H 0.5687 0.5577 0.9932 0.104 Uiso 1 1 calc R . .
H22C H 0.6546 0.5357 1.0590 0.104 Uiso 1 1 calc R . .
C23 C 0.5321(6) 0.2475(8) 0.9740(7) 0.050(3) Uani 1 1 d U . .
H23A H 0.5522 0.2393 1.0332 0.060 Uiso 1 1 calc R . .
N24 N 0.4886(5) 0.1989(6) 0.9225(6) 0.048(2) Uani 1 1 d U . .
N1N N 0.3405(6) 0.0724(6) 0.4764(6) 0.061(3) Uani 1 1 d DU . .
O1N O 0.3222(7) 0.1380(6) 0.4749(6) 0.082(3) Uani 1 1 d DU A .
O2N O 0.3762(5) 0.0368(6) 0.5453(6) 0.079(3) Uani 1 1 d DU A .
O3N O 0.3413(14) 0.0586(13) 0.4115(11) 0.085(10) Uiso 0.58(5) 1 d PDU A 1
O3N' O 0.3044(18) 0.0319(15) 0.4117(15) 0.110(16) Uiso 0.47(5) 1 d PDU A 2
N2N N 0.5878(8) 0.3072(9) 0.4344(10) 0.087(4) Uani 1 1 d U . .
O4N O 0.3872(5) 0.3285(5) 0.2555(7) 0.065(2) Uani 1 1 d U . .
O5N O 0.4601(5) 0.4211(5) 0.2851(6) 0.060(2) Uani 1 1 d U . .
O6N O 0.3592(5) 0.4378(5) 0.2831(6) 0.061(2) Uani 1 1 d U . .
N3N N 0.4010(5) 0.3966(6) 0.2749(6) 0.041(2) Uani 1 1 d U . .
O7N O 0.5267(7) 0.2695(7) 0.3899(8) 0.093(3) Uani 1 1 d U . .
O8N O 0.6068(5) 0.3442(7) 0.3927(6) 0.083(3) Uani 1 1 d U . .
O9N O 0.6260(8) 0.3023(8) 0.5122(8) 0.120(4) Uani 1 1 d U . .
C1S C 0.7186(9) 0.1302(11) 0.4971(14) 0.111(7) Uani 1 1 d U . .
H1S1 H 0.7366 0.1366 0.4592 0.166 Uiso 1 1 calc R . .
H1S2 H 0.7443 0.0877 0.5357 0.166 Uiso 1 1 calc R . .
H1S3 H 0.7287 0.1759 0.5311 0.166 Uiso 1 1 calc R . .
O1S O 0.6384(6) 0.1159(7) 0.4456(9) 0.100(4) Uani 1 1 d U . .
H1S H 0.6301 0.0716 0.4535 0.150 Uiso 1 1 calc R . .
O2S O 0.4198(7) 0.1990(7) 0.1991(8) 0.102(4) Uiso 1 1 d U . .
C2S C 0.4034(14) 0.1592(15) 0.2513(17) 0.157(10) Uiso 1 1 d U . .
H2S1 H 0.4464 0.1281 0.2917 0.236 Uiso 1 1 calc R . .
H2S2 H 0.3599 0.1271 0.2156 0.236 Uiso 1 1 calc R . .
H2S3 H 0.3926 0.1945 0.2835 0.236 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
Y1 0.0316(5) 0.0423(6) 0.0374(5) 0.0026(5) 0.0241(4) -0.0003(5)
Y2 0.0504(10) 0.0526(11) 0.0830(13) 0.000 0.0506(10) 0.000
O1 0.076(9) 0.044(6) 0.142(12) 0.000 0.096(10) 0.000
N1 0.025(4) 0.058(5) 0.025(4) 0.000(4) 0.015(4) 0.003(4)
C2 0.031(5) 0.064(6) 0.035(5) -0.010(5) 0.022(5) 0.002(5)
C3 0.038(5) 0.070(6) 0.044(7) -0.013(6) 0.029(5) 0.004(5)
N4 0.055(6) 0.043(6) 0.114(7) -0.017(5) 0.060(6) -0.003(5)
C5 0.089(10) 0.039(7) 0.167(11) 0.002(6) 0.101(9) 0.006(6)
C6 0.110(12) 0.058(7) 0.132(9) 0.031(7) 0.095(9) 0.032(7)
N7 0.061(6) 0.065(6) 0.066(7) 0.026(5) 0.051(6) 0.025(5)
C8 0.042(6) 0.089(8) 0.028(5) 0.017(6) 0.019(5) 0.024(5)
C9 0.032(5) 0.078(8) 0.030(5) 0.005(5) 0.019(4) 0.010(5)
C41 0.056(8) 0.074(10) 0.149(11) -0.067(7) 0.060(8) -0.023(7)
C42 0.041(7) 0.113(12) 0.090(9) -0.074(7) 0.030(7) -0.011(7)
C11 0.040(5) 0.059(6) 0.032(6) -0.008(4) 0.031(5) -0.007(5)
C12 0.046(6) 0.049(6) 0.020(5) 0.003(4) 0.021(5) -0.003(5)
N13 0.021(4) 0.044(5) 0.028(4) 0.007(4) 0.013(4) 0.005(4)
C14 0.039(6) 0.038(6) 0.038(6) 0.004(4) 0.030(5) 0.005(5)
C15 0.028(5) 0.053(5) 0.021(5) 0.003(4) 0.015(4) 0.004(4)
C16 0.038(6) 0.060(6) 0.026(5) -0.001(4) 0.017(5) 0.008(5)
C17 0.043(6) 0.080(7) 0.031(6) -0.008(5) 0.020(5) 0.013(6)
C18 0.036(6) 0.097(7) 0.015(5) -0.006(5) 0.017(5) 0.011(6)
C19 0.027(5) 0.078(6) 0.024(5) 0.004(4) 0.017(4) 0.006(5)
C20 0.025(4) 0.056(5) 0.015(4) 0.006(4) 0.013(4) 0.007(4)
O21 0.028(3) 0.054(4) 0.024(3) 0.007(3) 0.017(3) 0.004(3)
C22 0.073(9) 0.094(9) 0.041(7) -0.020(7) 0.032(7) 0.012(8)
C23 0.029(5) 0.106(8) 0.018(5) 0.029(5) 0.015(4) 0.007(5)
N24 0.026(4) 0.080(7) 0.038(4) 0.036(4) 0.017(4) 0.013(4)
N1N 0.066(7) 0.083(8) 0.039(6) -0.011(5) 0.033(6) 0.005(6)
O1N 0.138(10) 0.075(6) 0.057(6) 0.004(5) 0.069(7) 0.015(6)
O2N 0.061(6) 0.103(8) 0.063(6) 0.017(5) 0.028(5) 0.009(5)
N2N 0.089(7) 0.109(11) 0.085(5) 0.037(7) 0.062(5) 0.029(6)
O4N 0.068(5) 0.063(5) 0.100(7) -0.005(5) 0.069(5) -0.006(4)
O5N 0.048(4) 0.069(5) 0.077(6) -0.008(4) 0.042(5) -0.008(3)
O6N 0.060(5) 0.073(6) 0.072(6) -0.003(5) 0.051(5) 0.005(4)
N3N 0.050(5) 0.057(5) 0.035(5) 0.002(4) 0.035(4) -0.005(4)
O7N 0.098(6) 0.102(8) 0.113(7) 0.040(6) 0.080(6) 0.023(5)
O8N 0.059(4) 0.135(10) 0.058(5) 0.026(5) 0.034(4) 0.006(5)
O9N 0.139(10) 0.150(12) 0.082(5) 0.060(7) 0.068(6) 0.059(9)
C1S 0.071(9) 0.124(16) 0.16(2) -0.022(14) 0.075(12) -0.007(11)
O1S 0.070(6) 0.102(9) 0.118(10) 0.011(8) 0.045(7) 0.004(6)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Y1 O1 2.274(8) . y
Y1 O21 2.324(7) 2_656 y
Y1 O21 2.392(7) . y
Y1 N13 2.420(9) 2_656 y
Y1 N7 2.436(10) 2_656 y
Y1 N24 2.470(9) . y
Y1 N4 2.541(10) 2_656 y
Y1 N1 2.653(8) 2_656 y
Y1 Y1 3.429(2) 2_656 y
Y2 O2S 2.396(13) . y
Y2 O2S 2.396(13) 2_655 ?
Y2 O7N 2.433(11) 2_655 ?
Y2 O7N 2.433(11) . y
Y2 O5N 2.437(9) 2_655 ?
Y2 O5N 2.437(9) . y
Y2 O8N 2.464(10) . y
Y2 O8N 2.464(10) 2_655 ?
Y2 O4N 2.504(8) 2_655 ?
Y2 O4N 2.504(8) . y
Y2 N2N 2.871(15) 2_655 ?
Y2 N2N 2.871(15) . ?
O1 Y1 2.274(8) 2_656 ?
N1 C11 1.490(14) . ?
N1 C9 1.498(12) . ?
N1 C2 1.501(13) . ?
N1 Y1 2.653(8) 2_656 ?
C2 C3 1.477(16) . ?
C3 N4 1.508(14) . ?
N4 C5 1.49(2) . ?
N4 C41 1.501(19) . ?
N4 Y1 2.541(10) 2_656 ?
C5 C6 1.47(2) . ?
C6 N7 1.470(17) . ?
N7 C8 1.482(16) . ?
N7 Y1 2.436(10) 2_656 ?
C8 C9 1.520(14) . ?
C41 C42 1.45(2) . ?
C42 N24 1.491(15) 2_656 ?
C11 C12 1.504(14) . ?
C12 N13 1.466(12) . ?
N13 C14 1.260(13) . ?
N13 Y1 2.420(9) 2_656 ?
C14 C15 1.495(13) . ?
C15 C16 1.378(15) . ?
C15 C20 1.408(14) . ?
C16 C17 1.402(15) . ?
C17 C18 1.397(18) . ?
C17 C22 1.507(17) . ?
C18 C19 1.398(16) . ?
C19 C20 1.433(13) . ?
C19 C23 1.451(16) . ?
C20 O21 1.320(12) . ?
O21 Y1 2.324(7) 2_656 ?
C23 N24 1.247(15) . ?
N24 C42 1.491(15) 2_656 ?
N1N O1N 1.230(8) . ?
N1N O3N 1.242(9) . ?
N1N O3N' 1.243(10) . ?
N1N O2N 1.249(8) . ?
N2N O9N 1.214(17) . ?
N2N O8N 1.246(15) . ?
N2N O7N 1.289(18) . ?
O4N N3N 1.256(12) . ?
O5N N3N 1.252(11) . ?
O6N N3N 1.229(12) . ?
C1S O1S 1.458(18) . ?
O2S C2S 1.39(3) . ?

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 Y1 O21 72.6(2) . 2_656 y
O1 Y1 O21 71.3(2) . . y
O21 Y1 O21 71.3(3) 2_656 . y
O1 Y1 N13 141.6(3) . 2_656 y
O21 Y1 N13 72.9(3) 2_656 2_656 y
O21 Y1 N13 82.0(2) . 2_656 y
O1 Y1 N7 84.2(3) . 2_656 y
O21 Y1 N7 82.7(3) 2_656 2_656 y
O21 Y1 N7 148.4(3) . 2_656 y
N13 Y1 N7 107.5(3) 2_656 2_656 y
O1 Y1 N24 99.2(2) . . y
O21 Y1 N24 141.0(3) 2_656 . y
O21 Y1 N24 70.1(3) . . y
N13 Y1 N24 97.0(3) 2_656 . y
N7 Y1 N24 135.4(3) 2_656 . y
O1 Y1 N4 86.8(3) . 2_656 y
O21 Y1 N4 145.5(3) 2_656 2_656 y
O21 Y1 N4 128.3(3) . 2_656 y
N13 Y1 N4 131.6(3) 2_656 2_656 y
N7 Y1 N4 67.7(4) 2_656 2_656 y
N24 Y1 N4 68.1(4) . 2_656 y
O1 Y1 N1 148.3(3) . 2_656 y
O21 Y1 N1 116.7(2) 2_656 2_656 y
O21 Y1 N1 139.8(3) . 2_656 y
N13 Y1 N1 65.3(3) 2_656 2_656 y
N7 Y1 N1 68.2(3) 2_656 2_656 y
N24 Y1 N1 90.5(3) . 2_656 y
N4 Y1 N1 69.0(3) 2_656 2_656 y
O1 Y1 Y1 41.1(2) . 2_656 ?
O21 Y1 Y1 44.13(16) 2_656 2_656 ?
O21 Y1 Y1 42.57(16) . 2_656 ?
N13 Y1 Y1 100.99(18) 2_656 2_656 ?
N7 Y1 Y1 105.9(2) 2_656 2_656 ?
N24 Y1 Y1 105.1(2) . 2_656 ?
N4 Y1 Y1 127.1(2) 2_656 2_656 ?
N1 Y1 Y1 160.72(19) 2_656 2_656 ?
O2S Y2 O2S 73.6(6) . 2_655 ?
O2S Y2 O7N 70.3(4) . 2_655 ?
O2S Y2 O7N 84.3(4) 2_655 2_655 ?
O2S Y2 O7N 84.3(4) . . ?
O2S Y2 O7N 70.3(4) 2_655 . ?
O7N Y2 O7N 148.4(6) 2_655 . ?
O2S Y2 O5N 147.7(4) . 2_655 ?
O2S Y2 O5N 119.7(4) 2_655 2_655 ?
O7N Y2 O5N 81.5(4) 2_655 2_655 ?
O7N Y2 O5N 127.2(4) . 2_655 ?
O2S Y2 O5N 119.7(3) . . ?
O2S Y2 O5N 147.7(4) 2_655 . ?
O7N Y2 O5N 127.2(4) 2_655 . ?
O7N Y2 O5N 81.5(4) . . ?
O5N Y2 O5N 66.2(4) 2_655 . ?
O2S Y2 O8N 133.2(4) . . ?
O2S Y2 O8N 75.6(4) 2_655 . ?
O7N Y2 O8N 139.7(4) 2_655 . ?
O7N Y2 O8N 52.1(4) . . ?
O5N Y2 O8N 78.8(3) 2_655 . ?
O5N Y2 O8N 74.8(3) . . ?
O2S Y2 O8N 75.6(4) . 2_655 ?
O2S Y2 O8N 133.2(4) 2_655 2_655 ?
O7N Y2 O8N 52.1(4) 2_655 2_655 ?
O7N Y2 O8N 139.7(4) . 2_655 ?
O5N Y2 O8N 74.8(3) 2_655 2_655 ?
O5N Y2 O8N 78.8(3) . 2_655 ?
O8N Y2 O8N 148.4(6) . 2_655 ?
O2S Y2 O4N 127.4(4) . 2_655 ?
O2S Y2 O4N 69.0(4) 2_655 2_655 ?
O7N Y2 O4N 70.3(4) 2_655 2_655 ?
O7N Y2 O4N 114.9(4) . 2_655 ?
O5N Y2 O4N 51.0(3) 2_655 2_655 ?
O5N Y2 O4N 111.6(3) . 2_655 ?
O8N Y2 O4N 69.9(3) . 2_655 ?
O8N Y2 O4N 105.0(3) 2_655 2_655 ?
O2S Y2 O4N 69.0(4) . . ?
O2S Y2 O4N 127.4(4) 2_655 . ?
O7N Y2 O4N 114.9(4) 2_655 . ?
O7N Y2 O4N 70.3(4) . . ?
O5N Y2 O4N 111.6(3) 2_655 . ?
O5N Y2 O4N 51.0(3) . . ?
O8N Y2 O4N 105.0(3) . . ?
O8N Y2 O4N 69.9(3) 2_655 . ?
O4N Y2 O4N 162.1(4) 2_655 . ?
O2S Y2 N2N 70.9(4) . 2_655 ?
O2S Y2 N2N 109.4(4) 2_655 2_655 ?
O7N Y2 N2N 26.5(4) 2_655 2_655 ?
O7N Y2 N2N 153.7(4) . 2_655 ?
O5N Y2 N2N 76.8(4) 2_655 2_655 ?
O5N Y2 N2N 102.8(4) . 2_655 ?
O8N Y2 N2N 154.2(4) . 2_655 ?
O8N Y2 N2N 25.6(4) 2_655 2_655 ?
O4N Y2 N2N 87.9(4) 2_655 2_655 ?
O4N Y2 N2N 92.0(4) . 2_655 ?
O2S Y2 N2N 109.4(4) . . ?
O2S Y2 N2N 70.9(4) 2_655 . ?
O7N Y2 N2N 153.7(4) 2_655 . ?
O7N Y2 N2N 26.5(4) . . ?
O5N Y2 N2N 102.8(4) 2_655 . ?
O5N Y2 N2N 76.8(4) . . ?
O8N Y2 N2N 25.6(4) . . ?
O8N Y2 N2N 154.2(4) 2_655 . ?
O4N Y2 N2N 92.0(4) 2_655 . ?
O4N Y2 N2N 87.9(4) . . ?
N2N Y2 N2N 179.6(6) 2_655 . ?
Y1 O1 Y1 97.9(4) 2_656 . y
C11 N1 C9 110.4(9) . . ?
C11 N1 C2 109.7(8) . . ?
C9 N1 C2 110.5(8) . . ?
C11 N1 Y1 112.0(6) . 2_656 ?
C9 N1 Y1 111.0(6) . 2_656 ?
C2 N1 Y1 103.1(6) . 2_656 ?
C3 C2 N1 114.5(9) . . ?
C2 C3 N4 113.8(9) . . ?
C5 N4 C41 111.8(12) . . ?
C5 N4 C3 110.2(10) . . ?
C41 N4 C3 108.7(11) . . ?
C5 N4 Y1 105.4(8) . 2_656 ?
C41 N4 Y1 106.1(8) . 2_656 ?
C3 N4 Y1 114.7(7) . 2_656 ?
C6 C5 N4 111.3(12) . . ?
C5 C6 N7 112.2(13) . . ?
C6 N7 C8 113.5(11) . . ?
C6 N7 Y1 117.7(10) . 2_656 ?
C8 N7 Y1 106.7(7) . 2_656 ?
N7 C8 C9 110.6(10) . . ?
N1 C9 C8 110.1(8) . . ?
C42 C41 N4 112.0(12) . . ?
C41 C42 N24 110.8(13) . 2_656 ?
N1 C11 C12 109.6(8) . . ?
N13 C12 C11 106.6(8) . . ?
C14 N13 C12 115.6(9) . . ?
C14 N13 Y1 134.6(7) . 2_656 ?
C12 N13 Y1 109.0(6) . 2_656 ?
N13 C14 C15 126.8(10) . . ?
C16 C15 C20 120.9(9) . . ?
C16 C15 C14 117.2(10) . . ?
C20 C15 C14 121.9(9) . . ?
C15 C16 C17 122.6(12) . . ?
C18 C17 C16 116.6(11) . . ?
C18 C17 C22 123.2(11) . . ?
C16 C17 C22 120.2(13) . . ?
C17 C18 C19 122.6(10) . . ?
C18 C19 C20 119.4(10) . . ?
C18 C19 C23 119.1(10) . . ?
C20 C19 C23 121.3(10) . . ?
O21 C20 C15 123.9(8) . . ?
O21 C20 C19 118.5(9) . . ?
C15 C20 C19 117.6(10) . . ?
C20 O21 Y1 139.2(6) . 2_656 ?
C20 O21 Y1 116.0(5) . . ?
Y1 O21 Y1 93.3(2) 2_656 . y
N24 C23 C19 125.7(9) . . ?
C23 N24 C42 119.0(11) . 2_656 ?
C23 N24 Y1 123.9(7) . . ?
C42 N24 Y1 117.1(9) 2_656 . ?
O1N N1N O3N 109.9(13) . . ?
O1N N1N O3N' 120.6(16) . . ?
O1N N1N O2N 121.0(11) . . ?
O3N N1N O2N 124.9(13) . . ?
O3N' N1N O2N 113.9(18) . . ?
O9N N2N O8N 123.0(17) . . ?
O9N N2N O7N 120.8(15) . . ?
O8N N2N O7N 116.1(14) . . ?
O9N N2N Y2 175.5(13) . . ?
O8N N2N Y2 58.6(8) . . ?
O7N N2N Y2 57.4(8) . . ?
N3N O4N Y2 94.8(6) . . ?
N3N O5N Y2 98.2(7) . . ?
O6N N3N O5N 121.1(10) . . ?
O6N N3N O4N 122.8(9) . . ?
O5N N3N O4N 116.0(9) . . ?
O6N N3N Y2 176.6(7) . . ?
O5N N3N Y2 56.5(6) . . ?
O4N N3N Y2 59.6(5) . . ?
N2N O7N Y2 96.1(8) . . ?
N2N O8N Y2 95.8(10) . . ?
C2S O2S Y2 122.1(14) . . ?

_diffrn_measured_fraction_theta_max    0.994
_diffrn_reflns_theta_full              26.00
_diffrn_measured_fraction_theta_full   0.994
_refine_diff_density_max    0.87
_refine_diff_density_min   -0.94
_refine_diff_density_rms    0.13

#===END