# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350

_publ_contact_author_name        'Prof. Wei-guang, Zhang'
_publ_contact_author_address     
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;

_publ_contact_author_phone       '86 20 39347768'
_publ_contact_author_fax         '86 20 39347768'
_publ_contact_author_email       wgzhang@scnu.edu.cn
_publ_requested_category         ?
_publ_requested_coeditor_name    ?

_publ_contact_letter             
;
dear sir
Please consider this CIF submission for publication in CrystEngComm
All authors have seen and approved this submission.
Yours sincerely,
Wei-guang Zhang
;

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
?
;

loop_
_publ_author_name
_publ_author_address

'Jun Fan'
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;
'Zhi-Hong Wang'
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;
'Xia Yin'
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;
'Wei-Guang Zhang'
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;
'Ming Yang'
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;
;
Zhuo-fen Huang
;
;
School of Chemistry and Environment,
South China Normal University,
Guangzhou 510006, P.R. China
;

data_hzf
_database_code_depnum_ccdc_archive 'CCDC 717618'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Eu N2 O8, N O3, H2 O'
_chemical_formula_sum            'C22 H22 Eu N3 O12'
_chemical_formula_weight         672.39

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'
Eu Eu -0.1578 3.6682 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   18.724(4)
_cell_length_b                   15.086(3)
_cell_length_c                   8.6362(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.97(3)
_cell_angle_gamma                90.00
_cell_volume                     2433.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    4396
_cell_measurement_theta_min      1.09
_cell_measurement_theta_max      25.24

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    2.649
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4575
_exptl_absorpt_correction_T_max  0.5962
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21076
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.09
_diffrn_reflns_theta_max         25.24
_reflns_number_total             4396
_reflns_number_gt                3534
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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)+(0.0650P)²+0.8000P] where P=(Fo²+2Fc²)/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         4396
_refine_ls_number_parameters     344
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0908
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.6057(4) 0.4620(4) 0.7411(7) 0.0542(16) Uani 1 1 d . . .
H1 H 0.6444 0.4240 0.7602 0.065 Uiso 1 1 calc R . .
C2 C 0.5409(4) 0.4386(5) 0.7974(9) 0.0618(19) Uani 1 1 d . . .
H2 H 0.5375 0.3861 0.8528 0.074 Uiso 1 1 calc R . .
C3 C 0.4822(4) 0.4906(5) 0.7734(8) 0.0626(19) Uani 1 1 d . . .
H3 H 0.4391 0.4752 0.8137 0.075 Uiso 1 1 calc R . .
C4 C 0.4881(3) 0.5681(4) 0.6865(7) 0.0486(16) Uani 1 1 d . . .
C5 C 0.4299(4) 0.6252(5) 0.6474(8) 0.0625(19) Uani 1 1 d . . .
H5 H 0.3851 0.6123 0.6820 0.075 Uiso 1 1 calc R . .
C6 C 0.4383(3) 0.6981(5) 0.5605(8) 0.0611(18) Uani 1 1 d . . .
H6 H 0.3990 0.7343 0.5356 0.073 Uiso 1 1 calc R . .
C7 C 0.5049(3) 0.7209(4) 0.5065(7) 0.0501(15) Uani 1 1 d . . .
H7 H 0.5095 0.7712 0.4458 0.060 Uiso 1 1 calc R . .
C8 C 0.5634(3) 0.6680(4) 0.5446(6) 0.0375(13) Uani 1 1 d . . .
C9 C 0.5563(3) 0.5892(3) 0.6327(6) 0.0365(13) Uani 1 1 d . . .
C10 C 0.6418(3) 0.7559(4) 0.4025(6) 0.0427(13) Uani 1 1 d . . .
H10A H 0.6242 0.8108 0.4441 0.051 Uiso 1 1 calc R . .
H10B H 0.6153 0.7442 0.3041 0.051 Uiso 1 1 calc R . .
C11 C 0.7208(3) 0.7642(4) 0.3784(6) 0.0402(13) Uani 1 1 d . . .
C12 C 0.8999(4) 0.6330(4) 0.7870(7) 0.0543(16) Uani 1 1 d . . .
H12 H 0.8673 0.6341 0.8636 0.065 Uiso 1 1 calc R . .
C13 C 0.9698(4) 0.6567(5) 0.8292(8) 0.0625(18) Uani 1 1 d . . .
H13 H 0.9829 0.6745 0.9303 0.075 Uiso 1 1 calc R . .
C14 C 1.0190(4) 0.6537(5) 0.7213(9) 0.0668(19) Uani 1 1 d . . .
H14 H 1.0667 0.6676 0.7485 0.080 Uiso 1 1 calc R . .
C15 C 0.9977(3) 0.6296(4) 0.5694(7) 0.0487(15) Uani 1 1 d . . .
C16 C 1.0455(4) 0.6259(5) 0.4467(9) 0.0624(19) Uani 1 1 d . . .
H16 H 1.0936 0.6400 0.4670 0.075 Uiso 1 1 calc R . .
C17 C 1.0212(4) 0.6025(5) 0.3038(9) 0.0602(18) Uani 1 1 d . . .
H17 H 1.0530 0.6006 0.2258 0.072 Uiso 1 1 calc R . .
C18 C 0.9498(4) 0.5809(4) 0.2680(8) 0.0558(18) Uani 1 1 d . . .
H18 H 0.9346 0.5649 0.1671 0.067 Uiso 1 1 calc R . .
C19 C 0.9015(3) 0.5831(3) 0.3810(6) 0.0383(13) Uani 1 1 d . . .
C20 C 0.9249(3) 0.6083(4) 0.5345(7) 0.0402(13) Uani 1 1 d . . .
C21 C 0.8011(3) 0.5617(4) 0.2014(6) 0.0477(15) Uani 1 1 d . . .
H21A H 0.8201 0.5118 0.1463 0.057 Uiso 1 1 calc R . .
H21B H 0.8143 0.6157 0.1497 0.057 Uiso 1 1 calc R . .
C22 C 0.7203(3) 0.5547(4) 0.1988(6) 0.0428(14) Uani 1 1 d . . .
Eu1 Eu 0.740989(14) 0.581314(16) 0.57730(3) 0.02887(12) Uani 1 1 d . . .
N1 N 0.6156(2) 0.5357(3) 0.6615(5) 0.0387(11) Uani 1 1 d . . .
N2 N 0.8758(3) 0.6089(3) 0.6457(5) 0.0414(11) Uani 1 1 d . . .
N3 N 0.7639(5) 0.2774(6) 0.2353(9) 0.092(2) Uani 1 1 d . . .
O1 O 0.63169(19) 0.6850(2) 0.5078(4) 0.0389(9) Uani 1 1 d . . .
O2 O 0.7647(2) 0.7188(3) 0.4565(4) 0.0461(10) Uani 1 1 d . . .
O3 O 0.7352(2) 0.8215(3) 0.2807(4) 0.0528(11) Uani 1 1 d . . .
O4 O 0.8309(2) 0.5621(3) 0.3587(4) 0.0415(9) Uani 1 1 d . . .
O5 O 0.6917(2) 0.5529(3) 0.3255(4) 0.0442(9) Uani 1 1 d . . .
O6 O 0.6883(2) 0.5482(3) 0.0680(4) 0.0594(12) Uani 1 1 d . . .
O7 O 0.7196(6) 0.2325(7) 0.280(2) 0.264(9) Uani 1 1 d . . .
O8 O 0.7739(6) 0.3517(5) 0.2481(9) 0.158(4) Uani 1 1 d . . .
O9 O 0.8099(5) 0.2299(6) 0.1808(12) 0.167(4) Uani 1 1 d . . .
O1W O 0.8484(4) 0.1302(6) 0.4471(9) 0.154(3) Uani 1 1 d . . .
H1W H 0.8222 0.1658 0.3892 0.230 Uiso 1 1 d R . .
H2W H 0.8636 0.1584 0.5283 0.230 Uiso 1 1 d R . .
O2W O 0.7553(3) 0.4243(2) 0.5343(5) 0.0554(12) Uani 1 1 d . . .
H4W H 0.7631 0.4075 0.4449 0.083 Uiso 1 1 d R . .
H3W H 0.7814 0.3959 0.5990 0.083 Uiso 1 1 d R . .
O3W O 0.7648(2) 0.5033(3) 0.8258(4) 0.0517(11) Uani 1 1 d . . .
H5W H 0.7501 0.5248 0.9089 0.078 Uiso 1 1 d R . .
H6W H 0.7901 0.4578 0.8504 0.078 Uiso 1 1 d 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
C1 N1 1.327(7) . ?
C1 C2 1.384(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.354(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.398(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.411(10) . ?
C4 C9 1.425(8) . ?
C5 C6 1.348(10) . ?
C5 H5 0.9300 . ?
C6 C7 1.404(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.377(8) . ?
C7 H7 0.9300 . ?
C8 O1 1.363(6) . ?
C8 C9 1.422(7) . ?
C9 N1 1.382(7) . ?
C10 O1 1.426(6) . ?
C10 C11 1.512(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O2 1.234(7) . ?
C11 O3 1.250(6) . ?
C12 N2 1.322(7) . ?
C12 C13 1.381(9) . ?
C12 H12 0.9300 . ?
C13 C14 1.357(10) . ?
C13 H13 0.9300 . ?
C14 C15 1.393(9) . ?
C14 H14 0.9300 . ?
C15 C20 1.412(8) . ?
C15 C16 1.435(9) . ?
C16 C17 1.332(10) . ?
C16 H16 0.9300 . ?
C17 C18 1.390(10) . ?
C17 H17 0.9300 . ?
C18 C19 1.376(8) . ?
C18 H18 0.9300 . ?
C19 O4 1.359(7) . ?
C19 C20 1.419(8) . ?
C20 N2 1.374(7) . ?
C21 O4 1.432(7) . ?
C21 C22 1.516(9) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O6 1.245(7) . ?
C22 O5 1.251(7) . ?
Eu1 O3 2.297(4) 4_576 ?
Eu1 O5 2.343(4) . ?
Eu1 O2 2.377(4) . ?
Eu1 O2W 2.415(4) . ?
Eu1 O3W 2.461(4) . ?
Eu1 N2 2.586(5) . ?
Eu1 N1 2.597(4) . ?
Eu1 O1 2.612(4) . ?
Eu1 O4 2.631(4) . ?
N3 O8 1.140(9) . ?
N3 O7 1.159(11) . ?
N3 O9 1.238(9) . ?
O3 Eu1 2.297(4) 4_575 ?
O1W H1W 0.8632 . ?
O1W H2W 0.8530 . ?
O2W H4W 0.8353 . ?
O2W H3W 0.8346 . ?
O3W H5W 0.8506 . ?
O3W H6W 0.8529 . ?

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
N1 C1 C2 123.6(7) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 121.3(6) . . ?
C3 C2 H2 119.3 . . ?
C1 C2 H2 119.3 . . ?
C2 C3 C4 118.3(6) . . ?
C2 C3 H3 120.9 . . ?
C4 C3 H3 120.9 . . ?
C3 C4 C5 123.4(6) . . ?
C3 C4 C9 117.9(6) . . ?
C5 C4 C9 118.7(6) . . ?
C6 C5 C4 120.9(6) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C7 121.7(6) . . ?
C5 C6 H6 119.1 . . ?
C7 C6 H6 119.1 . . ?
C8 C7 C6 119.2(6) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
O1 C8 C7 125.3(5) . . ?
O1 C8 C9 114.0(5) . . ?
C7 C8 C9 120.7(5) . . ?
N1 C9 C8 118.7(5) . . ?
N1 C9 C4 122.6(5) . . ?
C8 C9 C4 118.7(5) . . ?
O1 C10 C11 108.9(4) . . ?
O1 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
O1 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O2 C11 O3 125.8(6) . . ?
O2 C11 C10 120.0(5) . . ?
O3 C11 C10 114.1(5) . . ?
N2 C12 C13 124.8(6) . . ?
N2 C12 H12 117.6 . . ?
C13 C12 H12 117.6 . . ?
C14 C13 C12 119.1(6) . . ?
C14 C13 H13 120.4 . . ?
C12 C13 H13 120.4 . . ?
C13 C14 C15 119.4(6) . . ?
C13 C14 H14 120.3 . . ?
C15 C14 H14 120.3 . . ?
C14 C15 C20 118.1(6) . . ?
C14 C15 C16 123.5(6) . . ?
C20 C15 C16 118.5(6) . . ?
C17 C16 C15 120.2(6) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 121.9(6) . . ?
C16 C17 H17 119.0 . . ?
C18 C17 H17 119.0 . . ?
C19 C18 C17 120.4(7) . . ?
C19 C18 H18 119.8 . . ?
C17 C18 H18 119.8 . . ?
O4 C19 C18 125.1(6) . . ?
O4 C19 C20 115.4(5) . . ?
C18 C19 C20 119.5(6) . . ?
N2 C20 C15 122.1(5) . . ?
N2 C20 C19 118.5(5) . . ?
C15 C20 C19 119.4(5) . . ?
O4 C21 C22 109.7(4) . . ?
O4 C21 H21A 109.7 . . ?
C22 C21 H21A 109.7 . . ?
O4 C21 H21B 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O6 C22 O5 125.8(6) . . ?
O6 C22 C21 115.8(5) . . ?
O5 C22 C21 118.4(5) . . ?
O3 Eu1 O5 142.23(15) 4_576 . ?
O3 Eu1 O2 78.40(14) 4_576 . ?
O5 Eu1 O2 79.96(14) . . ?
O3 Eu1 O2W 139.07(15) 4_576 . ?
O5 Eu1 O2W 73.65(15) . . ?
O2 Eu1 O2W 139.64(15) . . ?
O3 Eu1 O3W 69.73(15) 4_576 . ?
O5 Eu1 O3W 139.29(14) . . ?
O2 Eu1 O3W 140.53(14) . . ?
O2W Eu1 O3W 69.51(14) . . ?
O3 Eu1 N2 79.61(15) 4_576 . ?
O5 Eu1 N2 123.86(14) . . ?
O2 Eu1 N2 75.58(14) . . ?
O2W Eu1 N2 94.36(16) . . ?
O3W Eu1 N2 76.29(15) . . ?
O3 Eu1 N1 82.14(15) 4_576 . ?
O5 Eu1 N1 84.61(14) . . ?
O2 Eu1 N1 123.61(14) . . ?
O2W Eu1 N1 84.00(16) . . ?
O3W Eu1 N1 75.03(14) . . ?
N2 Eu1 N1 149.91(14) . . ?
O3 Eu1 O1 73.48(14) 4_576 . ?
O5 Eu1 O1 69.16(13) . . ?
O2 Eu1 O1 62.87(12) . . ?
O2W Eu1 O1 130.18(14) . . ?
O3W Eu1 O1 125.31(13) . . ?
N2 Eu1 O1 133.87(13) . . ?
N1 Eu1 O1 60.92(13) . . ?
O3 Eu1 O4 133.28(14) 4_576 . ?
O5 Eu1 O4 62.89(13) . . ?
O2 Eu1 O4 68.45(13) . . ?
O2W Eu1 O4 72.46(15) . . ?
O3W Eu1 O4 119.15(13) . . ?
N2 Eu1 O4 61.23(13) . . ?
N1 Eu1 O4 143.84(13) . . ?
O1 Eu1 O4 115.54(11) . . ?
C1 N1 C9 116.3(5) . . ?
C1 N1 Eu1 121.9(4) . . ?
C9 N1 Eu1 121.7(3) . . ?
C12 N2 C20 116.4(5) . . ?
C12 N2 Eu1 121.3(4) . . ?
C20 N2 Eu1 121.9(4) . . ?
O8 N3 O7 131.3(10) . . ?
O8 N3 O9 119.4(10) . . ?
O7 N3 O9 108.7(10) . . ?
C8 O1 C10 117.3(4) . . ?
C8 O1 Eu1 124.5(3) . . ?
C10 O1 Eu1 117.3(3) . . ?
C11 O2 Eu1 125.9(4) . . ?
C11 O3 Eu1 168.9(4) . 4_575 ?
C19 O4 C21 116.5(4) . . ?
C19 O4 Eu1 122.5(3) . . ?
C21 O4 Eu1 117.0(3) . . ?
C22 O5 Eu1 130.0(4) . . ?
H1W O1W H2W 108.1 . . ?
Eu1 O2W H4W 117.9 . . ?
Eu1 O2W H3W 117.8 . . ?
H4W O2W H3W 109.4 . . ?
Eu1 O3W H5W 120.3 . . ?
Eu1 O3W H6W 131.7 . . ?
H5W O3W H6W 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.3(11) . . . . ?
C1 C2 C3 C4 1.6(11) . . . . ?
C2 C3 C4 C5 176.8(7) . . . . ?
C2 C3 C4 C9 -2.1(9) . . . . ?
C3 C4 C5 C6 -178.6(6) . . . . ?
C9 C4 C5 C6 0.2(9) . . . . ?
C4 C5 C6 C7 -0.6(10) . . . . ?
C5 C6 C7 C8 -0.7(10) . . . . ?
C6 C7 C8 O1 -176.0(5) . . . . ?
C6 C7 C8 C9 2.3(8) . . . . ?
O1 C8 C9 N1 -4.8(6) . . . . ?
C7 C8 C9 N1 176.8(5) . . . . ?
O1 C8 C9 C4 175.8(5) . . . . ?
C7 C8 C9 C4 -2.6(7) . . . . ?
C3 C4 C9 N1 0.9(8) . . . . ?
C5 C4 C9 N1 -178.0(5) . . . . ?
C3 C4 C9 C8 -179.8(5) . . . . ?
C5 C4 C9 C8 1.3(8) . . . . ?
O1 C10 C11 O2 -6.4(7) . . . . ?
O1 C10 C11 O3 176.1(4) . . . . ?
N2 C12 C13 C14 -1.7(11) . . . . ?
C12 C13 C14 C15 2.1(11) . . . . ?
C13 C14 C15 C20 -0.5(10) . . . . ?
C13 C14 C15 C16 178.9(7) . . . . ?
C14 C15 C16 C17 -179.8(7) . . . . ?
C20 C15 C16 C17 -0.4(10) . . . . ?
C15 C16 C17 C18 -0.1(11) . . . . ?
C16 C17 C18 C19 -0.1(10) . . . . ?
C17 C18 C19 O4 -179.1(5) . . . . ?
C17 C18 C19 C20 0.6(9) . . . . ?
C14 C15 C20 N2 -1.5(9) . . . . ?
C16 C15 C20 N2 179.0(6) . . . . ?
C14 C15 C20 C19 -179.7(6) . . . . ?
C16 C15 C20 C19 0.9(8) . . . . ?
O4 C19 C20 N2 0.5(7) . . . . ?
C18 C19 C20 N2 -179.2(5) . . . . ?
O4 C19 C20 C15 178.8(5) . . . . ?
C18 C19 C20 C15 -1.0(8) . . . . ?
O4 C21 C22 O6 -175.8(5) . . . . ?
O4 C21 C22 O5 1.9(8) . . . . ?
C2 C1 N1 C9 -1.5(9) . . . . ?
C2 C1 N1 Eu1 175.3(5) . . . . ?
C8 C9 N1 C1 -178.5(5) . . . . ?
C4 C9 N1 C1 0.9(7) . . . . ?
C8 C9 N1 Eu1 4.7(6) . . . . ?
C4 C9 N1 Eu1 -175.9(4) . . . . ?
O3 Eu1 N1 C1 -103.4(4) 4_576 . . . ?
O5 Eu1 N1 C1 112.0(4) . . . . ?
O2 Eu1 N1 C1 -173.8(4) . . . . ?
O2W Eu1 N1 C1 38.0(4) . . . . ?
O3W Eu1 N1 C1 -32.4(4) . . . . ?
N2 Eu1 N1 C1 -50.4(6) . . . . ?
O1 Eu1 N1 C1 -178.8(5) . . . . ?
O4 Eu1 N1 C1 86.9(5) . . . . ?
O3 Eu1 N1 C9 73.2(4) 4_576 . . . ?
O5 Eu1 N1 C9 -71.3(4) . . . . ?
O2 Eu1 N1 C9 2.8(4) . . . . ?
O2W Eu1 N1 C9 -145.4(4) . . . . ?
O3W Eu1 N1 C9 144.2(4) . . . . ?
N2 Eu1 N1 C9 126.3(4) . . . . ?
O1 Eu1 N1 C9 -2.2(3) . . . . ?
O4 Eu1 N1 C9 -96.5(4) . . . . ?
C13 C12 N2 C20 -0.3(9) . . . . ?
C13 C12 N2 Eu1 -173.8(5) . . . . ?
C15 C20 N2 C12 2.0(8) . . . . ?
C19 C20 N2 C12 -179.9(5) . . . . ?
C15 C20 N2 Eu1 175.4(4) . . . . ?
C19 C20 N2 Eu1 -6.4(7) . . . . ?
O3 Eu1 N2 C12 25.8(5) 4_576 . . . ?
O5 Eu1 N2 C12 173.4(4) . . . . ?
O2 Eu1 N2 C12 106.3(5) . . . . ?
O2W Eu1 N2 C12 -113.4(5) . . . . ?
O3W Eu1 N2 C12 -45.7(5) . . . . ?
N1 Eu1 N2 C12 -27.8(6) . . . . ?
O1 Eu1 N2 C12 80.5(5) . . . . ?
O4 Eu1 N2 C12 179.4(5) . . . . ?
O3 Eu1 N2 C20 -147.3(4) 4_576 . . . ?
O5 Eu1 N2 C20 0.3(5) . . . . ?
O2 Eu1 N2 C20 -66.8(4) . . . . ?
O2W Eu1 N2 C20 73.5(4) . . . . ?
O3W Eu1 N2 C20 141.2(4) . . . . ?
N1 Eu1 N2 C20 159.1(4) . . . . ?
O1 Eu1 N2 C20 -92.6(4) . . . . ?
O4 Eu1 N2 C20 6.3(4) . . . . ?
C7 C8 O1 C10 -9.8(7) . . . . ?
C9 C8 O1 C10 171.8(4) . . . . ?
C7 C8 O1 Eu1 -178.7(4) . . . . ?
C9 C8 O1 Eu1 2.9(6) . . . . ?
C11 C10 O1 C8 179.5(4) . . . . ?
C11 C10 O1 Eu1 -10.8(5) . . . . ?
O3 Eu1 O1 C8 -90.6(4) 4_576 . . . ?
O5 Eu1 O1 C8 95.0(4) . . . . ?
O2 Eu1 O1 C8 -175.8(4) . . . . ?
O2W Eu1 O1 C8 50.7(4) . . . . ?
O3W Eu1 O1 C8 -41.4(4) . . . . ?
N2 Eu1 O1 C8 -147.5(3) . . . . ?
N1 Eu1 O1 C8 -0.5(3) . . . . ?
O4 Eu1 O1 C8 138.8(3) . . . . ?
O3 Eu1 O1 C10 100.5(4) 4_576 . . . ?
O5 Eu1 O1 C10 -73.9(3) . . . . ?
O2 Eu1 O1 C10 15.3(3) . . . . ?
O2W Eu1 O1 C10 -118.2(3) . . . . ?
O3W Eu1 O1 C10 149.7(3) . . . . ?
N2 Eu1 O1 C10 43.6(4) . . . . ?
N1 Eu1 O1 C10 -169.4(4) . . . . ?
O4 Eu1 O1 C10 -30.1(4) . . . . ?
O3 C11 O2 Eu1 -158.6(4) . . . . ?
C10 C11 O2 Eu1 24.3(7) . . . . ?
O3 Eu1 O2 C11 -98.4(5) 4_576 . . . ?
O5 Eu1 O2 C11 50.4(4) . . . . ?
O2W Eu1 O2 C11 99.9(5) . . . . ?
O3W Eu1 O2 C11 -134.7(4) . . . . ?
N2 Eu1 O2 C11 179.5(5) . . . . ?
N1 Eu1 O2 C11 -26.1(5) . . . . ?
O1 Eu1 O2 C11 -21.2(4) . . . . ?
O4 Eu1 O2 C11 115.1(5) . . . . ?
O2 C11 O3 Eu1 148.5(17) . . . 4_575 ?
C10 C11 O3 Eu1 -34(2) . . . 4_575 ?
C18 C19 O4 C21 -17.9(8) . . . . ?
C20 C19 O4 C21 162.4(5) . . . . ?
C18 C19 O4 Eu1 -174.8(4) . . . . ?
C20 C19 O4 Eu1 5.5(6) . . . . ?
C22 C21 O4 C19 -169.2(5) . . . . ?
C22 C21 O4 Eu1 -11.1(6) . . . . ?
O3 Eu1 O4 C19 30.8(4) 4_576 . . . ?
O5 Eu1 O4 C19 168.3(4) . . . . ?
O2 Eu1 O4 C19 78.8(4) . . . . ?
O2W Eu1 O4 C19 -111.5(4) . . . . ?
O3W Eu1 O4 C19 -58.1(4) . . . . ?
N2 Eu1 O4 C19 -6.1(3) . . . . ?
N1 Eu1 O4 C19 -163.3(3) . . . . ?
O1 Eu1 O4 C19 121.8(4) . . . . ?
O3 Eu1 O4 C21 -126.0(4) 4_576 . . . ?
O5 Eu1 O4 C21 11.5(4) . . . . ?
O2 Eu1 O4 C21 -78.0(4) . . . . ?
O2W Eu1 O4 C21 91.8(4) . . . . ?
O3W Eu1 O4 C21 145.1(4) . . . . ?
N2 Eu1 O4 C21 -162.9(4) . . . . ?
N1 Eu1 O4 C21 40.0(5) . . . . ?
O1 Eu1 O4 C21 -35.0(4) . . . . ?
O6 C22 O5 Eu1 -171.5(5) . . . . ?
C21 C22 O5 Eu1 11.0(8) . . . . ?
O3 Eu1 O5 C22 114.2(5) 4_576 . . . ?
O2 Eu1 O5 C22 58.4(5) . . . . ?
O2W Eu1 O5 C22 -90.7(5) . . . . ?
O3W Eu1 O5 C22 -116.5(5) . . . . ?
N2 Eu1 O5 C22 -6.5(6) . . . . ?
N1 Eu1 O5 C22 -176.0(5) . . . . ?
O1 Eu1 O5 C22 123.1(5) . . . . ?
O4 Eu1 O5 C22 -12.4(5) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H1W O9 0.86 2.04 2.800(14) 146.0 .
O1W H2W O9 0.85 2.40 3.042(13) 132.3 4_566
O1W H1W O7 0.86 2.31 3.129(17) 158.5 .
O2W H4W O8 0.84 1.92 2.748(8) 170.9 .
O2W H3W O9 0.83 2.08 2.806(10) 145.0 4_566
O3W H5W O6 0.85 1.89 2.701(6) 159.2 1_556
O3W H6W O1W 0.85 1.88 2.716(8) 167.5 4_566

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.24
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.101

#===END

data_a
_database_code_depnum_ccdc_archive 'CCDC 717619'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H20 Gd N2 O8, N O3, H2 O'
_chemical_formula_sum            'C22 H22 Gd N3 O12'
_chemical_formula_weight         677.68

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'
Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   18.7397(7)
_cell_length_b                   15.1331(6)
_cell_length_c                   8.6165(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.999(2)
_cell_angle_gamma                90.00
_cell_volume                     2437.60(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    5713
_cell_measurement_theta_min      1.09
_cell_measurement_theta_max      27.97

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1340
_exptl_absorpt_coefficient_mu    2.792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4868
_exptl_absorpt_correction_T_max  0.6645
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21452
_diffrn_reflns_av_R_equivalents  0.0983
_diffrn_reflns_av_sigmaI/netI    0.0990
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.09
_diffrn_reflns_theta_max         25.25
_reflns_number_total             4398
_reflns_number_gt                2797
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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)+(0.0390P)²+0.4130P] where P=(Fo²+2Fc²)/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         4398
_refine_ls_number_parameters     343
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0978
_refine_ls_R_factor_gt           0.0490
_refine_ls_wR_factor_ref         0.1073
_refine_ls_wR_factor_gt          0.0864
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_restrained_S_all      1.079
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.3919(5) -0.0369(7) 0.2606(11) 0.051(3) Uani 1 1 d . . .
H1 H 0.3527 -0.0739 0.2415 0.061 Uiso 1 1 calc R . .
C2 C 0.4582(6) -0.0617(7) 0.2031(12) 0.063(3) Uani 1 1 d . . .
H2 H 0.4615 -0.1145 0.1489 0.076 Uiso 1 1 calc R . .
C3 C 0.5161(6) -0.0101(7) 0.2260(12) 0.059(3) Uani 1 1 d . . .
H3 H 0.5589 -0.0256 0.1846 0.070 Uiso 1 1 calc R . .
C4 C 0.5113(5) 0.0677(6) 0.3133(10) 0.043(2) Uani 1 1 d . . .
C5 C 0.5709(5) 0.1241(7) 0.3481(13) 0.063(3) Uani 1 1 d . . .
H5 H 0.6151 0.1112 0.3109 0.076 Uiso 1 1 calc R . .
C6 C 0.5623(5) 0.1970(7) 0.4366(13) 0.064(3) Uani 1 1 d . . .
H6 H 0.6013 0.2334 0.4622 0.077 Uiso 1 1 calc R . .
C7 C 0.4939(5) 0.2187(6) 0.4914(10) 0.047(2) Uani 1 1 d . . .
H7 H 0.4890 0.2680 0.5542 0.057 Uiso 1 1 calc R . .
C8 C 0.4361(4) 0.1670(6) 0.4513(9) 0.035(2) Uani 1 1 d . . .
C9 C 0.4428(4) 0.0886(6) 0.3658(9) 0.0294(19) Uani 1 1 d . . .
C10 C 0.3575(4) 0.2553(6) 0.5964(9) 0.040(2) Uani 1 1 d . . .
H10A H 0.3751 0.3100 0.5547 0.048 Uiso 1 1 calc R . .
H10B H 0.3841 0.2436 0.6949 0.048 Uiso 1 1 calc R . .
C11 C 0.2789(5) 0.2645(6) 0.6221(10) 0.040(2) Uani 1 1 d . . .
C12 C 0.1004(5) 0.1337(7) 0.2115(11) 0.055(3) Uani 1 1 d . . .
H12 H 0.1331 0.1350 0.1352 0.066 Uiso 1 1 calc R . .
C13 C 0.0309(6) 0.1572(7) 0.1670(13) 0.065(3) Uani 1 1 d . . .
H13 H 0.0172 0.1741 0.0655 0.078 Uiso 1 1 calc R . .
C14 C -0.0165(5) 0.1545(7) 0.2789(13) 0.061(3) Uani 1 1 d . . .
H14 H -0.0638 0.1703 0.2531 0.073 Uiso 1 1 calc R . .
C15 C 0.0032(5) 0.1289(6) 0.4311(12) 0.045(2) Uani 1 1 d . . .
C16 C -0.0435(5) 0.1259(7) 0.5515(14) 0.061(3) Uani 1 1 d . . .
H16 H -0.0913 0.1414 0.5312 0.073 Uiso 1 1 calc R . .
C17 C -0.0202(5) 0.1011(7) 0.6950(14) 0.065(3) Uani 1 1 d . . .
H17 H -0.0523 0.0978 0.7723 0.078 Uiso 1 1 calc R . .
C18 C 0.0515(5) 0.0801(6) 0.7306(11) 0.053(3) Uani 1 1 d . . .
H18 H 0.0673 0.0641 0.8314 0.064 Uiso 1 1 calc R . .
C19 C 0.0977(4) 0.0831(6) 0.6172(10) 0.039(2) Uani 1 1 d . . .
C20 C 0.0750(5) 0.1085(5) 0.4640(11) 0.038(2) Uani 1 1 d . . .
C21 C 0.1980(5) 0.0631(7) 0.8005(9) 0.051(3) Uani 1 1 d . . .
H21A H 0.1786 0.0140 0.8564 0.062 Uiso 1 1 calc R . .
H21B H 0.1855 0.1177 0.8511 0.062 Uiso 1 1 calc R . .
C22 C 0.2798(5) 0.0545(6) 0.7995(11) 0.042(2) Uani 1 1 d . . .
Gd1 Gd 0.25945(2) 0.08215(3) 0.42226(5) 0.02776(14) Uani 1 1 d . . .
N1 N 0.3838(4) 0.0360(5) 0.3394(8) 0.0371(18) Uani 1 1 d . . .
N2 N 0.1246(4) 0.1097(5) 0.3520(8) 0.0380(18) Uani 1 1 d . . .
N3 N 0.2329(7) 0.7230(9) 0.2677(15) 0.108(4) Uani 1 1 d . . .
O1 O 0.3678(3) 0.1851(4) 0.4911(6) 0.0383(15) Uani 1 1 d . . .
O2 O 0.2356(3) 0.2178(4) 0.5429(6) 0.0445(17) Uani 1 1 d . . .
O3 O 0.2647(3) 0.3209(4) 0.7208(6) 0.0521(18) Uani 1 1 d . . .
O4 O 0.1698(3) 0.0629(4) 0.6410(6) 0.0371(15) Uani 1 1 d . . .
O5 O 0.3090(3) 0.0531(4) 0.6731(6) 0.0435(16) Uani 1 1 d . . .
O6 O 0.3129(3) 0.0493(4) 0.9306(7) 0.0571(19) Uani 1 1 d . . .
O7 O 0.2273(6) 0.6452(7) 0.2533(12) 0.150(5) Uani 1 1 d . . .
O8 O 0.2784(7) 0.7650(8) 0.2141(19) 0.213(7) Uani 1 1 d . . .
O9 O 0.1886(5) 0.7705(8) 0.3204(14) 0.166(5) Uani 1 1 d . . .
O1W O 0.1505(5) 0.8743(7) 0.0527(11) 0.141(4) Uani 1 1 d . . .
H1W H 0.1171 0.8371 0.0665 0.211 Uiso 1 1 d R . .
H2W H 0.1685 0.8616 -0.0334 0.211 Uiso 1 1 d R . .
O2W O 0.2449(3) -0.0757(4) 0.4647(7) 0.0526(17) Uani 1 1 d . . .
H3W H 0.2085 -0.0844 0.4021 0.079 Uiso 1 1 d R . .
H4W H 0.2302 -0.0747 0.5645 0.079 Uiso 1 1 d R . .
O3W O 0.2347(3) 0.0049(4) 0.1735(6) 0.0519(17) Uani 1 1 d . . .
H5W H 0.2523 0.0326 0.0993 0.078 Uiso 1 1 d R . .
H6W H 0.1966 -0.0208 0.1370 0.078 Uiso 1 1 d 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
C1 N1 1.311(10) . ?
C1 C2 1.419(12) . ?
C1 H1 0.9300 . ?
C2 C3 1.340(13) . ?
C2 H2 0.9300 . ?
C3 C4 1.402(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.421(13) . ?
C4 C9 1.427(11) . ?
C5 C6 1.357(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.434(12) . ?
C6 H6 0.9300 . ?
C7 C8 1.361(11) . ?
C7 H7 0.9300 . ?
C8 O1 1.376(9) . ?
C8 C9 1.406(11) . ?
C9 N1 1.367(10) . ?
C10 O1 1.420(8) . ?
C10 C11 1.511(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O2 1.243(9) . ?
C11 O3 1.246(9) . ?
C12 N2 1.314(10) . ?
C12 C13 1.378(12) . ?
C12 H12 0.9300 . ?
C13 C14 1.356(13) . ?
C13 H13 0.9300 . ?
C14 C15 1.392(12) . ?
C14 H14 0.9300 . ?
C15 C20 1.390(11) . ?
C15 C16 1.405(12) . ?
C16 C17 1.336(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.394(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.350(11) . ?
C18 H18 0.9300 . ?
C19 O4 1.387(9) . ?
C19 C20 1.411(11) . ?
C20 N2 1.387(10) . ?
C21 O4 1.438(9) . ?
C21 C22 1.539(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O6 1.252(9) . ?
C22 O5 1.253(10) . ?
Gd1 O3 2.281(6) 4_565 ?
Gd1 O5 2.334(5) . ?
Gd1 O2 2.357(5) . ?
Gd1 O2W 2.435(6) . ?
Gd1 O3W 2.457(5) . ?
Gd1 N1 2.581(7) . ?
Gd1 N2 2.590(7) . ?
Gd1 O1 2.595(5) . ?
Gd1 O4 2.627(5) . ?
N3 O8 1.184(13) . ?
N3 O7 1.187(12) . ?
N3 O9 1.210(13) . ?
O3 Gd1 2.281(6) 4_566 ?
O1W H1W 0.8557 . ?
O1W H2W 0.8580 . ?
O2W H3W 0.8496 . ?
O2W H4W 0.9213 . ?
O3W H5W 0.8504 . ?
O3W H6W 0.8537 . ?

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
N1 C1 C2 122.6(9) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 120.9(9) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 119.1(9) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C3 C4 C5 122.6(9) . . ?
C3 C4 C9 116.7(9) . . ?
C5 C4 C9 120.7(9) . . ?
C6 C5 C4 119.0(9) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C5 C6 C7 120.9(10) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 119.9(9) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C7 C8 O1 124.0(8) . . ?
C7 C8 C9 121.3(8) . . ?
O1 C8 C9 114.6(7) . . ?
N1 C9 C8 118.5(7) . . ?
N1 C9 C4 123.6(8) . . ?
C8 C9 C4 117.9(8) . . ?
O1 C10 C11 109.9(7) . . ?
O1 C10 H10A 109.7 . . ?
C11 C10 H10A 109.7 . . ?
O1 C10 H10B 109.7 . . ?
C11 C10 H10B 109.7 . . ?
H10A C10 H10B 108.2 . . ?
O2 C11 O3 127.0(8) . . ?
O2 C11 C10 118.2(8) . . ?
O3 C11 C10 114.8(8) . . ?
N2 C12 C13 125.9(10) . . ?
N2 C12 H12 117.0 . . ?
C13 C12 H12 117.0 . . ?
C14 C13 C12 116.6(10) . . ?
C14 C13 H13 121.7 . . ?
C12 C13 H13 121.7 . . ?
C13 C14 C15 122.3(10) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C20 C15 C14 116.3(9) . . ?
C20 C15 C16 119.1(9) . . ?
C14 C15 C16 124.5(10) . . ?
C17 C16 C15 120.8(10) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 121.1(10) . . ?
C16 C17 H17 119.5 . . ?
C18 C17 H17 119.5 . . ?
C19 C18 C17 119.3(9) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 O4 123.5(8) . . ?
C18 C19 C20 121.3(8) . . ?
O4 C19 C20 115.1(7) . . ?
N2 C20 C15 122.8(8) . . ?
N2 C20 C19 118.8(8) . . ?
C15 C20 C19 118.4(8) . . ?
O4 C21 C22 107.1(7) . . ?
O4 C21 H21A 110.3 . . ?
C22 C21 H21A 110.3 . . ?
O4 C21 H21B 110.3 . . ?
C22 C21 H21B 110.3 . . ?
H21A C21 H21B 108.5 . . ?
O6 C22 O5 124.4(9) . . ?
O6 C22 C21 115.5(8) . . ?
O5 C22 C21 120.1(8) . . ?
O3 Gd1 O5 142.3(2) 4_565 . ?
O3 Gd1 O2 78.2(2) 4_565 . ?
O5 Gd1 O2 80.2(2) . . ?
O3 Gd1 O2W 139.2(2) 4_565 . ?
O5 Gd1 O2W 73.6(2) . . ?
O2 Gd1 O2W 139.59(19) . . ?
O3 Gd1 O3W 70.0(2) 4_565 . ?
O5 Gd1 O3W 139.2(2) . . ?
O2 Gd1 O3W 140.25(19) . . ?
O2W Gd1 O3W 69.39(19) . . ?
O3 Gd1 N1 82.9(2) 4_565 . ?
O5 Gd1 N1 84.1(2) . . ?
O2 Gd1 N1 124.0(2) . . ?
O2W Gd1 N1 83.6(2) . . ?
O3W Gd1 N1 75.5(2) . . ?
O3 Gd1 N2 79.1(2) 4_565 . ?
O5 Gd1 N2 124.4(2) . . ?
O2 Gd1 N2 75.6(2) . . ?
O2W Gd1 N2 94.3(2) . . ?
O3W Gd1 N2 75.6(2) . . ?
N1 Gd1 N2 149.7(2) . . ?
O3 Gd1 O1 73.35(19) 4_565 . ?
O5 Gd1 O1 69.31(19) . . ?
O2 Gd1 O1 62.98(18) . . ?
O2W Gd1 O1 130.43(19) . . ?
O3W Gd1 O1 125.62(18) . . ?
N1 Gd1 O1 61.20(19) . . ?
N2 Gd1 O1 133.78(19) . . ?
O3 Gd1 O4 132.92(19) 4_565 . ?
O5 Gd1 O4 63.10(18) . . ?
O2 Gd1 O4 68.29(18) . . ?
O2W Gd1 O4 72.51(18) . . ?
O3W Gd1 O4 118.79(18) . . ?
N1 Gd1 O4 143.47(19) . . ?
N2 Gd1 O4 61.5(2) . . ?
O1 Gd1 O4 115.59(16) . . ?
C1 N1 C9 117.0(8) . . ?
C1 N1 Gd1 120.7(6) . . ?
C9 N1 Gd1 122.1(5) . . ?
C12 N2 C20 116.1(8) . . ?
C12 N2 Gd1 121.9(6) . . ?
C20 N2 Gd1 121.7(5) . . ?
O8 N3 O7 123.6(15) . . ?
O8 N3 O9 111.0(14) . . ?
O7 N3 O9 124.8(15) . . ?
C8 O1 C10 118.7(6) . . ?
C8 O1 Gd1 123.4(5) . . ?
C10 O1 Gd1 117.1(4) . . ?
C11 O2 Gd1 127.0(6) . . ?
C11 O3 Gd1 169.2(6) . 4_566 ?
C19 O4 C21 115.5(6) . . ?
C19 O4 Gd1 122.3(5) . . ?
C21 O4 Gd1 118.3(4) . . ?
C22 O5 Gd1 129.3(6) . . ?
H1W O1W H2W 108.0 . . ?
Gd1 O2W H3W 98.6 . . ?
Gd1 O2W H4W 99.7 . . ?
H3W O2W H4W 108.4 . . ?
Gd1 O3W H5W 111.2 . . ?
Gd1 O3W H6W 129.8 . . ?
H5W O3W H6W 107.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.8(16) . . . . ?
C1 C2 C3 C4 2.5(16) . . . . ?
C2 C3 C4 C5 177.4(10) . . . . ?
C2 C3 C4 C9 -3.0(14) . . . . ?
C3 C4 C5 C6 -178.3(9) . . . . ?
C9 C4 C5 C6 2.1(14) . . . . ?
C4 C5 C6 C7 -1.6(15) . . . . ?
C5 C6 C7 C8 -1.7(14) . . . . ?
C6 C7 C8 O1 -176.3(8) . . . . ?
C6 C7 C8 C9 4.5(13) . . . . ?
C7 C8 C9 N1 175.1(8) . . . . ?
O1 C8 C9 N1 -4.2(10) . . . . ?
C7 C8 C9 C4 -4.0(12) . . . . ?
O1 C8 C9 C4 176.8(7) . . . . ?
C3 C4 C9 N1 2.1(12) . . . . ?
C5 C4 C9 N1 -178.3(8) . . . . ?
C3 C4 C9 C8 -179.0(8) . . . . ?
C5 C4 C9 C8 0.6(12) . . . . ?
O1 C10 C11 O2 -5.7(11) . . . . ?
O1 C10 C11 O3 175.6(7) . . . . ?
N2 C12 C13 C14 -0.5(16) . . . . ?
C12 C13 C14 C15 -0.4(16) . . . . ?
C13 C14 C15 C20 1.9(15) . . . . ?
C13 C14 C15 C16 179.2(10) . . . . ?
C20 C15 C16 C17 -2.2(15) . . . . ?
C14 C15 C16 C17 -179.5(10) . . . . ?
C15 C16 C17 C18 2.0(16) . . . . ?
C16 C17 C18 C19 -1.4(16) . . . . ?
C17 C18 C19 O4 -179.6(8) . . . . ?
C17 C18 C19 C20 1.0(14) . . . . ?
C14 C15 C20 N2 -2.6(13) . . . . ?
C16 C15 C20 N2 179.9(8) . . . . ?
C14 C15 C20 C19 179.3(9) . . . . ?
C16 C15 C20 C19 1.8(13) . . . . ?
C18 C19 C20 N2 -179.4(8) . . . . ?
O4 C19 C20 N2 1.2(12) . . . . ?
C18 C19 C20 C15 -1.2(13) . . . . ?
O4 C19 C20 C15 179.3(7) . . . . ?
O4 C21 C22 O6 -176.7(8) . . . . ?
O4 C21 C22 O5 3.4(12) . . . . ?
C2 C1 N1 C9 -0.3(13) . . . . ?
C2 C1 N1 Gd1 175.4(7) . . . . ?
C8 C9 N1 C1 -179.4(7) . . . . ?
C4 C9 N1 C1 -0.4(12) . . . . ?
C8 C9 N1 Gd1 5.0(9) . . . . ?
C4 C9 N1 Gd1 -176.1(6) . . . . ?
O3 Gd1 N1 C1 -103.4(6) 4_565 . . . ?
O5 Gd1 N1 C1 112.1(6) . . . . ?
O2 Gd1 N1 C1 -173.9(6) . . . . ?
O2W Gd1 N1 C1 37.9(6) . . . . ?
O3W Gd1 N1 C1 -32.4(6) . . . . ?
N2 Gd1 N1 C1 -49.7(8) . . . . ?
O1 Gd1 N1 C1 -178.3(7) . . . . ?
O4 Gd1 N1 C1 86.7(7) . . . . ?
O3 Gd1 N1 C9 72.1(6) 4_565 . . . ?
O5 Gd1 N1 C9 -72.4(6) . . . . ?
O2 Gd1 N1 C9 1.6(7) . . . . ?
O2W Gd1 N1 C9 -146.5(6) . . . . ?
O3W Gd1 N1 C9 143.2(6) . . . . ?
N2 Gd1 N1 C9 125.8(6) . . . . ?
O1 Gd1 N1 C9 -2.8(5) . . . . ?
O4 Gd1 N1 C9 -97.7(6) . . . . ?
C13 C12 N2 C20 -0.2(14) . . . . ?
C13 C12 N2 Gd1 -173.9(8) . . . . ?
C15 C20 N2 C12 1.8(12) . . . . ?
C19 C20 N2 C12 179.9(8) . . . . ?
C15 C20 N2 Gd1 175.6(6) . . . . ?
C19 C20 N2 Gd1 -6.3(10) . . . . ?
O3 Gd1 N2 C12 26.0(7) 4_565 . . . ?
O5 Gd1 N2 C12 173.6(6) . . . . ?
O2 Gd1 N2 C12 106.4(7) . . . . ?
O2W Gd1 N2 C12 -113.3(7) . . . . ?
O3W Gd1 N2 C12 -45.9(7) . . . . ?
N1 Gd1 N2 C12 -28.6(9) . . . . ?
O1 Gd1 N2 C12 80.0(7) . . . . ?
O4 Gd1 N2 C12 179.2(8) . . . . ?
O3 Gd1 N2 C20 -147.4(6) 4_565 . . . ?
O5 Gd1 N2 C20 0.2(7) . . . . ?
O2 Gd1 N2 C20 -67.0(6) . . . . ?
O2W Gd1 N2 C20 73.3(6) . . . . ?
O3W Gd1 N2 C20 140.7(6) . . . . ?
N1 Gd1 N2 C20 158.0(5) . . . . ?
O1 Gd1 N2 C20 -93.4(6) . . . . ?
O4 Gd1 N2 C20 5.8(5) . . . . ?
C7 C8 O1 C10 -8.3(12) . . . . ?
C9 C8 O1 C10 170.9(7) . . . . ?
C7 C8 O1 Gd1 -177.6(6) . . . . ?
C9 C8 O1 Gd1 1.6(9) . . . . ?
C11 C10 O1 C8 179.2(7) . . . . ?
C11 C10 O1 Gd1 -10.9(8) . . . . ?
O3 Gd1 O1 C8 -90.5(6) 4_565 . . . ?
O5 Gd1 O1 C8 95.2(6) . . . . ?
O2 Gd1 O1 C8 -175.4(6) . . . . ?
O2W Gd1 O1 C8 51.1(6) . . . . ?
O3W Gd1 O1 C8 -41.3(6) . . . . ?
N1 Gd1 O1 C8 0.5(5) . . . . ?
N2 Gd1 O1 C8 -146.4(5) . . . . ?
O4 Gd1 O1 C8 139.4(5) . . . . ?
O3 Gd1 O1 C10 100.2(5) 4_565 . . . ?
O5 Gd1 O1 C10 -74.2(5) . . . . ?
O2 Gd1 O1 C10 15.2(5) . . . . ?
O2W Gd1 O1 C10 -118.3(5) . . . . ?
O3W Gd1 O1 C10 149.3(5) . . . . ?
N1 Gd1 O1 C10 -168.9(6) . . . . ?
N2 Gd1 O1 C10 44.2(6) . . . . ?
O4 Gd1 O1 C10 -30.0(5) . . . . ?
O3 C11 O2 Gd1 -157.8(6) . . . . ?
C10 C11 O2 Gd1 23.7(11) . . . . ?
O3 Gd1 O2 C11 -98.4(7) 4_565 . . . ?
O5 Gd1 O2 C11 50.5(7) . . . . ?
O2W Gd1 O2 C11 100.4(7) . . . . ?
O3W Gd1 O2 C11 -135.3(6) . . . . ?
N1 Gd1 O2 C11 -25.5(7) . . . . ?
N2 Gd1 O2 C11 180.0(7) . . . . ?
O1 Gd1 O2 C11 -21.2(6) . . . . ?
O4 Gd1 O2 C11 115.3(7) . . . . ?
O2 C11 O3 Gd1 152(3) . . . 4_566 ?
C10 C11 O3 Gd1 -29(3) . . . 4_566 ?
C18 C19 O4 C21 -17.4(12) . . . . ?
C20 C19 O4 C21 162.0(7) . . . . ?
C18 C19 O4 Gd1 -175.0(7) . . . . ?
C20 C19 O4 Gd1 4.5(10) . . . . ?
C22 C21 O4 C19 -170.9(7) . . . . ?
C22 C21 O4 Gd1 -12.4(9) . . . . ?
O3 Gd1 O4 C19 31.8(6) 4_565 . . . ?
O5 Gd1 O4 C19 169.5(6) . . . . ?
O2 Gd1 O4 C19 79.6(6) . . . . ?
O2W Gd1 O4 C19 -110.4(6) . . . . ?
O3W Gd1 O4 C19 -56.9(6) . . . . ?
N1 Gd1 O4 C19 -162.1(5) . . . . ?
N2 Gd1 O4 C19 -5.3(5) . . . . ?
O1 Gd1 O4 C19 122.5(6) . . . . ?
O3 Gd1 O4 C21 -125.1(6) 4_565 . . . ?
O5 Gd1 O4 C21 12.6(6) . . . . ?
O2 Gd1 O4 C21 -77.3(6) . . . . ?
O2W Gd1 O4 C21 92.7(6) . . . . ?
O3W Gd1 O4 C21 146.2(6) . . . . ?
N1 Gd1 O4 C21 41.0(7) . . . . ?
N2 Gd1 O4 C21 -162.2(6) . . . . ?
O1 Gd1 O4 C21 -34.4(6) . . . . ?
O6 C22 O5 Gd1 -170.2(6) . . . . ?
C21 C22 O5 Gd1 9.8(12) . . . . ?
O3 Gd1 O5 C22 114.4(7) 4_565 . . . ?
O2 Gd1 O5 C22 58.6(7) . . . . ?
O2W Gd1 O5 C22 -90.3(7) . . . . ?
O3W Gd1 O5 C22 -115.7(7) . . . . ?
N1 Gd1 O5 C22 -175.4(7) . . . . ?
N2 Gd1 O5 C22 -6.4(8) . . . . ?
O1 Gd1 O5 C22 123.2(8) . . . . ?
O4 Gd1 O5 C22 -11.9(7) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1W H2W O7 0.86 2.21 3.055(13) 168.1 4_575
O1W H2W O9 0.86 2.41 3.085(15) 136.4 4_575
O2W H4W O7 0.92 1.95 2.741(11) 143.0 4_566
O2W H3W O9 0.85 2.33 2.809(12) 116.3 1_545
O3W H5W O6 0.85 1.92 2.721(8) 156.0 1_554
O3W H6W O1W 0.85 1.93 2.693(10) 149.0 1_545

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.155

#===END
data_a1
_database_code_depnum_ccdc_archive 'CCDC 717620'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H34 N4 O17 Pr2, 3(H2 O)'
_chemical_formula_sum            'C46 H40 N4 O20 Pr2'
_chemical_formula_weight         1250.64

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'
Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   19.268(4)
_cell_length_b                   16.070(3)
_cell_length_c                   15.592(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.38(3)
_cell_angle_gamma                90.00
_cell_volume                     4748.8(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    8597
_cell_measurement_theta_min      1.07
_cell_measurement_theta_max      25.25

_exptl_crystal_description       block
_exptl_crystal_colour            light-green
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2488
_exptl_absorpt_coefficient_mu    2.113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6158
_exptl_absorpt_correction_T_max  0.7216
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            50762
_diffrn_reflns_av_R_equivalents  0.0972
_diffrn_reflns_av_sigmaI/netI    0.0818
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         25.25
_reflns_number_total             8595
_reflns_number_gt                5649
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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)+(0.0800P)²+0.2200P] where P=(Fo²+2Fc²)/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         8595
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1012
_refine_ls_R_factor_gt           0.0538
_refine_ls_wR_factor_ref         0.1482
_refine_ls_wR_factor_gt          0.1215
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1085(5) 0.9090(6) 0.6302(6) 0.053(3) Uani 1 1 d . . .
H1 H 0.1434 0.9158 0.6793 0.064 Uiso 1 1 calc R . .
C2 C 0.0402(5) 0.8941(7) 0.6435(7) 0.064(3) Uani 1 1 d . . .
H2 H 0.0311 0.8912 0.7000 0.077 Uiso 1 1 calc R . .
C3 C -0.0123(5) 0.8838(6) 0.5758(7) 0.053(3) Uani 1 1 d . . .
H3 H -0.0581 0.8742 0.5845 0.063 Uiso 1 1 calc R . .
C4 C 0.0031(5) 0.8877(5) 0.4907(6) 0.042(2) Uani 1 1 d . . .
C5 C -0.0484(5) 0.8781(6) 0.4146(7) 0.058(3) Uani 1 1 d . . .
H5 H -0.0955 0.8703 0.4188 0.069 Uiso 1 1 calc R . .
C6 C -0.0288(5) 0.8804(8) 0.3360(7) 0.066(3) Uani 1 1 d . . .
H6 H -0.0624 0.8714 0.2860 0.080 Uiso 1 1 calc R . .
C7 C 0.0419(5) 0.8961(7) 0.3283(6) 0.057(3) Uani 1 1 d . . .
H7 H 0.0541 0.8987 0.2733 0.068 Uiso 1 1 calc R . .
C8 C 0.0913(4) 0.9072(5) 0.3987(6) 0.037(2) Uani 1 1 d . . .
C9 C 0.0745(4) 0.9035(5) 0.4841(5) 0.035(2) Uani 1 1 d . . .
C10 C 0.1822(4) 0.9293(6) 0.3151(5) 0.043(2) Uani 1 1 d . . .
H10A H 0.1526 0.9693 0.2790 0.052 Uiso 1 1 calc R . .
H10B H 0.1754 0.8754 0.2868 0.052 Uiso 1 1 calc R . .
C11 C 0.2572(4) 0.9545(5) 0.3236(5) 0.0298(19) Uani 1 1 d . . .
C12 C 0.4257(5) 0.9034(6) 0.6545(6) 0.049(2) Uani 1 1 d . . .
H12 H 0.3983 0.8592 0.6677 0.059 Uiso 1 1 calc R . .
C13 C 0.4986(6) 0.8992(7) 0.6844(7) 0.064(3) Uani 1 1 d . . .
H13 H 0.5187 0.8551 0.7188 0.077 Uiso 1 1 calc R . .
C14 C 0.5394(5) 0.9622(7) 0.6613(7) 0.056(3) Uani 1 1 d . . .
H14 H 0.5881 0.9607 0.6793 0.067 Uiso 1 1 calc R . .
C15 C 0.5082(4) 1.0286(6) 0.6107(6) 0.041(2) Uani 1 1 d . . .
C16 C 0.5466(5) 1.0962(6) 0.5847(6) 0.048(2) Uani 1 1 d . . .
H16 H 0.5957 1.0956 0.5974 0.058 Uiso 1 1 calc R . .
C17 C 0.5131(5) 1.1610(7) 0.5422(7) 0.058(3) Uani 1 1 d . . .
H17 H 0.5394 1.2044 0.5251 0.070 Uiso 1 1 calc R . .
C18 C 0.4390(5) 1.1649(6) 0.5227(7) 0.053(3) Uani 1 1 d . . .
H18 H 0.4164 1.2112 0.4947 0.063 Uiso 1 1 calc R . .
C19 C 0.4001(4) 1.0983(6) 0.5460(5) 0.038(2) Uani 1 1 d . . .
C20 C 0.4331(4) 1.0289(6) 0.5899(5) 0.039(2) Uani 1 1 d . . .
C21 C 0.2899(4) 1.1682(5) 0.4860(6) 0.044(2) Uani 1 1 d . . .
H21A H 0.3017 1.1744 0.4284 0.052 Uiso 1 1 calc R . .
H21B H 0.3037 1.2186 0.5188 0.052 Uiso 1 1 calc R . .
C22 C 0.2122(5) 1.1543(7) 0.4784(7) 0.052(3) Uani 1 1 d . . .
C23 C 0.4168(5) 0.8474(6) 0.1976(7) 0.059(3) Uani 1 1 d . . .
H23 H 0.3882 0.8391 0.2389 0.071 Uiso 1 1 calc R . .
C24 C 0.4890(5) 0.8279(7) 0.2195(7) 0.063(3) Uani 1 1 d . . .
H24 H 0.5077 0.8090 0.2752 0.076 Uiso 1 1 calc R . .
C25 C 0.5312(5) 0.8368(6) 0.1591(7) 0.059(3) Uani 1 1 d . . .
H25 H 0.5788 0.8234 0.1734 0.071 Uiso 1 1 calc R . .
C26 C 0.5033(5) 0.8658(6) 0.0760(7) 0.050(3) Uani 1 1 d . . .
C27 C 0.5435(5) 0.8759(6) 0.0092(8) 0.061(3) Uani 1 1 d . . .
H27 H 0.5915 0.8642 0.0199 0.073 Uiso 1 1 calc R . .
C28 C 0.5120(5) 0.9025(7) -0.0696(8) 0.063(3) Uani 1 1 d . . .
H28 H 0.5388 0.9086 -0.1132 0.076 Uiso 1 1 calc R . .
C29 C 0.4401(5) 0.9215(6) -0.0884(8) 0.058(3) Uani 1 1 d . . .
H29 H 0.4195 0.9375 -0.1446 0.069 Uiso 1 1 calc R . .
C30 C 0.4001(4) 0.9166(5) -0.0249(6) 0.039(2) Uani 1 1 d . . .
C31 C 0.4303(4) 0.8857(5) 0.0573(6) 0.043(2) Uani 1 1 d . . .
C32 C 0.2967(5) 0.9654(6) -0.1182(6) 0.047(2) Uani 1 1 d . . .
H32A H 0.2946 0.9200 -0.1596 0.057 Uiso 1 1 calc R . .
H32B H 0.3233 1.0106 -0.1379 0.057 Uiso 1 1 calc R . .
C33 C 0.2228(4) 0.9946(6) -0.1136(6) 0.040(2) Uani 1 1 d . . .
C34 C 0.0825(4) 0.8560(6) 0.0868(6) 0.045(2) Uani 1 1 d . . .
H34 H 0.1067 0.8076 0.0778 0.055 Uiso 1 1 calc R . .
C35 C 0.0097(5) 0.8504(6) 0.0844(6) 0.046(2) Uani 1 1 d . . .
H35 H -0.0131 0.7992 0.0762 0.056 Uiso 1 1 calc R . .
C36 C -0.0272(5) 0.9208(6) 0.0943(6) 0.046(2) Uani 1 1 d . . .
H36 H -0.0759 0.9184 0.0907 0.055 Uiso 1 1 calc R . .
C37 C 0.0086(4) 0.9976(6) 0.1103(5) 0.038(2) Uani 1 1 d . . .
C38 C -0.0259(5) 1.0716(7) 0.1238(6) 0.052(3) Uani 1 1 d . . .
H38 H -0.0744 1.0714 0.1225 0.062 Uiso 1 1 calc R . .
C39 C 0.0105(5) 1.1430(7) 0.1387(6) 0.051(3) Uani 1 1 d . . .
H39 H -0.0132 1.1919 0.1472 0.061 Uiso 1 1 calc R . .
C40 C 0.0841(4) 1.1451(6) 0.1417(6) 0.045(2) Uani 1 1 d . . .
H40 H 0.1087 1.1948 0.1533 0.054 Uiso 1 1 calc R . .
C41 C 0.1194(4) 1.0736(5) 0.1276(5) 0.0315(19) Uani 1 1 d . . .
C42 C 0.0820(4) 0.9974(6) 0.1126(5) 0.033(2) Uani 1 1 d . . .
C43 C 0.2306(4) 1.1433(6) 0.1475(7) 0.050(2) Uani 1 1 d . . .
H43A H 0.2279 1.1625 0.2058 0.061 Uiso 1 1 calc R . .
H43B H 0.2109 1.1862 0.1064 0.061 Uiso 1 1 calc R . .
C44 C 0.3076(5) 1.1278(7) 0.1403(6) 0.047(2) Uani 1 1 d . . .
C45 C 0.2575(4) 0.7288(6) 0.1233(5) 0.034(2) Uani 1 1 d . . .
C46 C 0.2556(5) 0.7412(6) 0.0240(6) 0.043(2) Uani 1 1 d . . .
N1 N 0.1271(3) 0.9142(4) 0.5546(4) 0.0384(18) Uani 1 1 d . . .
N2 N 0.3935(3) 0.9650(5) 0.6096(4) 0.0374(17) Uani 1 1 d . . .
N3 N 0.3883(4) 0.8772(5) 0.1199(5) 0.0434(19) Uani 1 1 d . . .
N4 N 0.1189(3) 0.9256(5) 0.1009(4) 0.0355(17) Uani 1 1 d . . .
O1 O 0.1618(3) 0.9248(4) 0.3984(4) 0.0409(15) Uani 1 1 d . . .
O2 O 0.2913(3) 0.9762(4) 0.3961(4) 0.0396(15) Uani 1 1 d . . .
O3 O 0.2812(3) 0.9546(4) 0.2529(4) 0.0432(15) Uani 1 1 d . . .
O4 O 0.3271(3) 1.0975(4) 0.5300(4) 0.0396(14) Uani 1 1 d . . .
O5 O 0.1912(3) 1.0833(4) 0.4924(4) 0.0453(16) Uani 1 1 d . . .
O6 O 0.1749(4) 1.2161(5) 0.4562(6) 0.080(3) Uani 1 1 d . . .
O7 O 0.3310(3) 0.9380(4) -0.0337(4) 0.0446(16) Uani 1 1 d . . .
O8 O 0.2009(3) 0.9914(4) -0.0421(4) 0.0427(15) Uani 1 1 d . . .
O9 O 0.1869(3) 1.0206(4) -0.1838(4) 0.0472(16) Uani 1 1 d . . .
O10 O 0.1906(3) 1.0687(3) 0.1294(4) 0.0376(14) Uani 1 1 d . . .
O11 O 0.3233(3) 1.0584(4) 0.1130(4) 0.0475(16) Uani 1 1 d . . .
O12 O 0.3486(3) 1.1859(4) 0.1623(6) 0.078(3) Uani 1 1 d . . .
O13 O 0.2658(3) 0.6556(4) 0.1503(4) 0.0425(15) Uani 1 1 d . . .
O14 O 0.2715(4) 0.6806(4) -0.0170(4) 0.0532(18) Uani 1 1 d . . .
O15 O 0.2496(3) 0.7923(4) 0.1665(4) 0.0414(15) Uani 1 1 d . . .
O16 O 0.2374(4) 0.8135(4) -0.0045(4) 0.0517(17) Uani 1 1 d . . .
O1W O 0.2545(3) 1.0292(4) 0.6783(4) 0.0484(17) Uani 1 1 d . . .
H1W H 0.2372 1.0173 0.7234 0.073 Uiso 1 1 d R . .
H2W H 0.2443 1.0799 0.6658 0.073 Uiso 1 1 d R . .
O4W O 0.1707(7) 0.7061(8) 0.3077(7) 0.175(6) Uani 1 1 d . . .
H8W H 0.1367 0.6742 0.2855 0.262 Uiso 1 1 d R . .
H7W H 0.1747 0.7011 0.3630 0.262 Uiso 1 1 d R . .
Pr1 Pr 0.25554(2) 0.96012(3) 0.53853(3) 0.03157(15) Uani 1 1 d . . .
Pr2 Pr 0.25711(2) 0.93328(3) 0.09493(3) 0.03240(15) Uani 1 1 d . . .
O2W O 0.6959(4) 0.8231(4) 0.2612(5) 0.073(2) Uani 1 1 d . . .
H3W H 0.7371 0.8070 0.2627 0.109 Uiso 1 1 d R . .
H4W H 0.6719 0.7849 0.2753 0.109 Uiso 1 1 d R . .
O3W O 0.8181(4) 0.8005(5) 0.1946(5) 0.091(3) Uani 1 1 d . . .
H5W H 0.8484 0.8364 0.1950 0.136 Uiso 1 1 d R . .
H6W H 0.7878 0.8065 0.1507 0.136 Uiso 1 1 d 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
C1 N1 1.296(11) . ?
C1 C2 1.388(13) . ?
C1 H1 0.9300 . ?
C2 C3 1.334(14) . ?
C2 H2 0.9300 . ?
C3 C4 1.412(13) . ?
C3 H3 0.9300 . ?
C4 C5 1.410(13) . ?
C4 C9 1.422(11) . ?
C5 C6 1.347(13) . ?
C5 H5 0.9300 . ?
C6 C7 1.412(13) . ?
C6 H6 0.9300 . ?
C7 C8 1.329(11) . ?
C7 H7 0.9300 . ?
C8 O1 1.388(9) . ?
C8 C9 1.428(11) . ?
C9 N1 1.364(10) . ?
C10 O1 1.425(9) . ?
C10 C11 1.483(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O2 1.251(9) . ?
C11 O3 1.270(8) . ?
C12 N2 1.303(11) . ?
C12 C13 1.399(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.369(14) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.415(13) . ?
C15 C20 1.425(11) . ?
C16 C17 1.335(13) . ?
C16 H16 0.9300 . ?
C17 C18 1.408(13) . ?
C17 H17 0.9300 . ?
C18 C19 1.390(12) . ?
C18 H18 0.9300 . ?
C19 O4 1.383(9) . ?
C19 C20 1.400(12) . ?
C20 N2 1.347(11) . ?
C21 O4 1.448(9) . ?
C21 C22 1.498(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O6 1.238(11) . ?
C22 O5 1.242(11) . ?
C23 N3 1.327(11) . ?
C23 C24 1.405(13) . ?
C23 H23 0.9300 . ?
C24 C25 1.358(14) . ?
C24 H24 0.9300 . ?
C25 C26 1.391(14) . ?
C25 H25 0.9300 . ?
C26 C27 1.415(14) . ?
C26 C31 1.420(12) . ?
C27 C28 1.339(15) . ?
C27 H27 0.9300 . ?
C28 C29 1.396(14) . ?
C28 H28 0.9300 . ?
C29 C30 1.364(12) . ?
C29 H29 0.9300 . ?
C30 O7 1.357(10) . ?
C30 C31 1.399(12) . ?
C31 N3 1.383(11) . ?
C32 O7 1.433(10) . ?
C32 C33 1.514(12) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 O9 1.257(10) . ?
C33 O8 1.261(10) . ?
C34 N4 1.318(11) . ?
C34 C35 1.400(11) . ?
C34 H34 0.9300 . ?
C35 C36 1.360(12) . ?
C35 H35 0.9300 . ?
C36 C37 1.415(13) . ?
C36 H36 0.9300 . ?
C37 C38 1.396(13) . ?
C37 C42 1.408(11) . ?
C38 C39 1.343(13) . ?
C38 H38 0.9300 . ?
C39 C40 1.412(12) . ?
C39 H39 0.9300 . ?
C40 C41 1.372(11) . ?
C40 H40 0.9300 . ?
C41 O10 1.370(9) . ?
C41 C42 1.418(11) . ?
C42 N4 1.385(11) . ?
C43 O10 1.425(10) . ?
C43 C44 1.528(12) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O12 1.230(11) . ?
C44 O11 1.251(11) . ?
C45 O15 1.247(10) . ?
C45 O13 1.249(10) . ?
C45 C46 1.555(11) . ?
C46 O14 1.233(10) . ?
C46 O16 1.271(11) . ?
N1 Pr1 2.638(6) . ?
N2 Pr1 2.691(6) . ?
N3 Pr2 2.645(7) . ?
N4 Pr2 2.684(6) . ?
O1 Pr1 2.633(5) . ?
O2 Pr1 2.454(5) . ?
O3 Pr2 2.447(6) . ?
O4 Pr1 2.619(6) . ?
O5 Pr1 2.378(6) . ?
O7 Pr2 2.662(6) . ?
O8 Pr2 2.403(6) . ?
O10 Pr2 2.629(6) . ?
O11 Pr2 2.371(6) . ?
O13 Pr1 2.532(6) 4_575 ?
O14 Pr1 2.461(6) 4_575 ?
O15 Pr2 2.542(6) . ?
O16 Pr2 2.458(6) . ?
O1W Pr1 2.449(5) . ?
O1W H1W 0.8524 . ?
O1W H2W 0.8518 . ?
O4W H8W 0.8540 . ?
O4W H7W 0.8543 . ?
Pr1 O14 2.461(6) 4_576 ?
Pr1 O13 2.532(6) 4_576 ?
O2W H3W 0.8306 . ?
O2W H4W 0.8213 . ?
O3W H5W 0.8210 . ?
O3W H6W 0.8215 . ?

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
N1 C1 C2 124.9(9) . . ?
N1 C1 H1 117.6 . . ?
C2 C1 H1 117.6 . . ?
C3 C2 C1 120.4(10) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C2 C3 C4 118.8(9) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C5 C4 C3 123.4(8) . . ?
C5 C4 C9 120.2(8) . . ?
C3 C4 C9 116.4(9) . . ?
C6 C5 C4 119.5(9) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C7 121.0(9) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 120.8(9) . . ?
C8 C7 H7 119.6 . . ?
C6 C7 H7 119.6 . . ?
C7 C8 O1 125.5(8) . . ?
C7 C8 C9 121.1(8) . . ?
O1 C8 C9 113.4(7) . . ?
N1 C9 C4 123.6(8) . . ?
N1 C9 C8 119.1(7) . . ?
C4 C9 C8 117.4(8) . . ?
O1 C10 C11 110.9(7) . . ?
O1 C10 H10A 109.5 . . ?
C11 C10 H10A 109.5 . . ?
O1 C10 H10B 109.5 . . ?
C11 C10 H10B 109.5 . . ?
H10A C10 H10B 108.1 . . ?
O2 C11 O3 124.7(7) . . ?
O2 C11 C10 120.1(7) . . ?
O3 C11 C10 115.1(7) . . ?
N2 C12 C13 124.6(9) . . ?
N2 C12 H12 117.7 . . ?
C13 C12 H12 117.7 . . ?
C14 C13 C12 117.7(10) . . ?
C14 C13 H13 121.1 . . ?
C12 C13 H13 121.1 . . ?
C13 C14 C15 120.3(9) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C14 C15 C16 123.7(8) . . ?
C14 C15 C20 116.6(9) . . ?
C16 C15 C20 119.6(8) . . ?
C17 C16 C15 120.6(9) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 121.5(9) . . ?
C16 C17 H17 119.2 . . ?
C18 C17 H17 119.2 . . ?
C19 C18 C17 118.9(9) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
O4 C19 C18 122.6(8) . . ?
O4 C19 C20 115.9(8) . . ?
C18 C19 C20 121.5(8) . . ?
N2 C20 C19 119.6(7) . . ?
N2 C20 C15 122.6(8) . . ?
C19 C20 C15 117.8(8) . . ?
O4 C21 C22 108.8(7) . . ?
O4 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
O4 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
O6 C22 O5 126.5(9) . . ?
O6 C22 C21 115.1(9) . . ?
O5 C22 C21 118.4(8) . . ?
N3 C23 C24 122.2(10) . . ?
N3 C23 H23 118.9 . . ?
C24 C23 H23 118.9 . . ?
C25 C24 C23 119.8(10) . . ?
C25 C24 H24 120.1 . . ?
C23 C24 H24 120.1 . . ?
C24 C25 C26 120.2(9) . . ?
C24 C25 H25 119.9 . . ?
C26 C25 H25 119.9 . . ?
C25 C26 C27 123.7(9) . . ?
C25 C26 C31 117.9(9) . . ?
C27 C26 C31 118.4(10) . . ?
C28 C27 C26 119.7(9) . . ?
C28 C27 H27 120.2 . . ?
C26 C27 H27 120.2 . . ?
C27 C28 C29 122.1(11) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C30 C29 C28 120.3(11) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
O7 C30 C29 125.8(9) . . ?
O7 C30 C31 115.0(7) . . ?
C29 C30 C31 119.2(9) . . ?
N3 C31 C30 118.7(8) . . ?
N3 C31 C26 121.2(9) . . ?
C30 C31 C26 120.1(9) . . ?
O7 C32 C33 109.5(7) . . ?
O7 C32 H32A 109.8 . . ?
C33 C32 H32A 109.8 . . ?
O7 C32 H32B 109.8 . . ?
C33 C32 H32B 109.8 . . ?
H32A C32 H32B 108.2 . . ?
O9 C33 O8 124.4(8) . . ?
O9 C33 C32 115.9(8) . . ?
O8 C33 C32 119.7(8) . . ?
N4 C34 C35 124.0(9) . . ?
N4 C34 H34 118.0 . . ?
C35 C34 H34 118.0 . . ?
C36 C35 C34 119.1(9) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C37 119.8(8) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C38 C37 C42 120.1(9) . . ?
C38 C37 C36 122.6(8) . . ?
C42 C37 C36 117.3(8) . . ?
C39 C38 C37 120.3(9) . . ?
C39 C38 H38 119.8 . . ?
C37 C38 H38 119.8 . . ?
C38 C39 C40 121.1(9) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 H39 119.4 . . ?
C41 C40 C39 119.9(9) . . ?
C41 C40 H40 120.0 . . ?
C39 C40 H40 120.0 . . ?
O10 C41 C40 124.7(8) . . ?
O10 C41 C42 115.5(7) . . ?
C40 C41 C42 119.8(7) . . ?
N4 C42 C37 122.4(8) . . ?
N4 C42 C41 118.9(7) . . ?
C37 C42 C41 118.7(8) . . ?
O10 C43 C44 110.2(8) . . ?
O10 C43 H43A 109.6 . . ?
C44 C43 H43A 109.6 . . ?
O10 C43 H43B 109.6 . . ?
C44 C43 H43B 109.6 . . ?
H43A C43 H43B 108.1 . . ?
O12 C44 O11 126.0(9) . . ?
O12 C44 C43 116.1(9) . . ?
O11 C44 C43 117.9(8) . . ?
O15 C45 O13 127.5(8) . . ?
O15 C45 C46 116.8(8) . . ?
O13 C45 C46 115.7(8) . . ?
O14 C46 O16 128.3(8) . . ?
O14 C46 C45 116.8(8) . . ?
O16 C46 C45 114.9(8) . . ?
C1 N1 C9 116.0(7) . . ?
C1 N1 Pr1 121.5(6) . . ?
C9 N1 Pr1 122.2(5) . . ?
C12 N2 C20 117.9(7) . . ?
C12 N2 Pr1 122.6(6) . . ?
C20 N2 Pr1 119.0(5) . . ?
C23 N3 C31 118.7(8) . . ?
C23 N3 Pr2 119.0(6) . . ?
C31 N3 Pr2 121.9(6) . . ?
C34 N4 C42 117.3(7) . . ?
C34 N4 Pr2 122.3(6) . . ?
C42 N4 Pr2 120.2(5) . . ?
C8 O1 C10 116.3(6) . . ?
C8 O1 Pr1 124.5(5) . . ?
C10 O1 Pr1 119.0(5) . . ?
C11 O2 Pr1 126.9(5) . . ?
C11 O3 Pr2 147.2(5) . . ?
C19 O4 C21 118.6(6) . . ?
C19 O4 Pr1 121.8(5) . . ?
C21 O4 Pr1 117.7(4) . . ?
C22 O5 Pr1 130.4(6) . . ?
C30 O7 C32 117.0(7) . . ?
C30 O7 Pr2 124.4(5) . . ?
C32 O7 Pr2 118.7(5) . . ?
C33 O8 Pr2 129.3(6) . . ?
C41 O10 C43 117.3(6) . . ?
C41 O10 Pr2 124.6(5) . . ?
C43 O10 Pr2 118.1(5) . . ?
C44 O11 Pr2 129.7(6) . . ?
C45 O13 Pr1 118.1(5) . 4_575 ?
C46 O14 Pr1 119.0(5) . 4_575 ?
C45 O15 Pr2 118.0(5) . . ?
C46 O16 Pr2 119.6(5) . . ?
Pr1 O1W H1W 134.4 . . ?
Pr1 O1W H2W 105.7 . . ?
H1W O1W H2W 107.1 . . ?
H8W O4W H7W 105.9 . . ?
O5 Pr1 O1W 78.7(2) . . ?
O5 Pr1 O2 81.6(2) . . ?
O1W Pr1 O2 143.7(2) . . ?
O5 Pr1 O14 138.6(2) . 4_576 ?
O1W Pr1 O14 138.7(2) . 4_576 ?
O2 Pr1 O14 72.9(2) . 4_576 ?
O5 Pr1 O13 142.4(2) . 4_576 ?
O1W Pr1 O13 74.5(2) . 4_576 ?
O2 Pr1 O13 134.4(2) . 4_576 ?
O14 Pr1 O13 64.37(19) 4_576 4_576 ?
O5 Pr1 O4 62.20(19) . . ?
O1W Pr1 O4 75.65(19) . . ?
O2 Pr1 O4 68.21(18) . . ?
O14 Pr1 O4 131.0(2) 4_576 . ?
O13 Pr1 O4 132.67(18) 4_576 . ?
O5 Pr1 O1 71.7(2) . . ?
O1W Pr1 O1 136.16(19) . . ?
O2 Pr1 O1 62.26(17) . . ?
O14 Pr1 O1 67.7(2) 4_576 . ?
O13 Pr1 O1 111.68(19) 4_576 . ?
O4 Pr1 O1 115.34(17) . . ?
O5 Pr1 N1 79.3(2) . . ?
O1W Pr1 N1 83.4(2) . . ?
O2 Pr1 N1 122.43(19) . . ?
O14 Pr1 N1 87.4(2) 4_576 . ?
O13 Pr1 N1 71.8(2) 4_576 . ?
O4 Pr1 N1 138.8(2) . . ?
O1 Pr1 N1 60.21(19) . . ?
O5 Pr1 N2 121.5(2) . . ?
O1W Pr1 N2 77.7(2) . . ?
O2 Pr1 N2 87.2(2) . . ?
O14 Pr1 N2 89.7(2) 4_576 . ?
O13 Pr1 N2 77.8(2) 4_576 . ?
O4 Pr1 N2 60.4(2) . . ?
O1 Pr1 N2 145.79(19) . . ?
N1 Pr1 N2 147.5(2) . . ?
O11 Pr2 O8 85.5(2) . . ?
O11 Pr2 O3 76.2(2) . . ?
O8 Pr2 O3 144.5(2) . . ?
O11 Pr2 O16 139.3(2) . . ?
O8 Pr2 O16 75.5(2) . . ?
O3 Pr2 O16 136.4(2) . . ?
O11 Pr2 O15 140.9(2) . . ?
O8 Pr2 O15 133.24(19) . . ?
O3 Pr2 O15 72.43(19) . . ?
O16 Pr2 O15 64.19(19) . . ?
O11 Pr2 O10 62.96(18) . . ?
O8 Pr2 O10 72.66(19) . . ?
O3 Pr2 O10 71.91(19) . . ?
O16 Pr2 O10 138.7(2) . . ?
O15 Pr2 O10 125.44(18) . . ?
O11 Pr2 N3 78.0(2) . . ?
O8 Pr2 N3 121.9(2) . . ?
O3 Pr2 N3 84.1(2) . . ?
O16 Pr2 N3 82.0(2) . . ?
O15 Pr2 N3 76.1(2) . . ?
O10 Pr2 N3 137.72(19) . . ?
O11 Pr2 O7 73.5(2) . . ?
O8 Pr2 O7 62.32(18) . . ?
O3 Pr2 O7 136.40(19) . . ?
O16 Pr2 O7 65.8(2) . . ?
O15 Pr2 O7 115.89(18) . . ?
O10 Pr2 O7 118.49(18) . . ?
N3 Pr2 O7 59.6(2) . . ?
O11 Pr2 N4 123.4(2) . . ?
O8 Pr2 N4 76.0(2) . . ?
O3 Pr2 N4 88.91(19) . . ?
O16 Pr2 N4 86.8(2) . . ?
O15 Pr2 N4 79.0(2) . . ?
O10 Pr2 N4 60.50(19) . . ?
N3 Pr2 N4 155.1(2) . . ?
O7 Pr2 N4 134.13(19) . . ?
H3W O2W H4W 110.0 . . ?
H5W O3W H6W 108.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.1(18) . . . . ?
C1 C2 C3 C4 0.6(17) . . . . ?
C2 C3 C4 C5 -179.7(10) . . . . ?
C2 C3 C4 C9 -0.7(14) . . . . ?
C3 C4 C5 C6 -178.1(10) . . . . ?
C9 C4 C5 C6 3.0(15) . . . . ?
C4 C5 C6 C7 -3.0(18) . . . . ?
C5 C6 C7 C8 1.5(18) . . . . ?
C6 C7 C8 O1 -178.4(10) . . . . ?
C6 C7 C8 C9 0.1(16) . . . . ?
C5 C4 C9 N1 179.4(9) . . . . ?
C3 C4 C9 N1 0.4(13) . . . . ?
C5 C4 C9 C8 -1.4(13) . . . . ?
C3 C4 C9 C8 179.7(8) . . . . ?
C7 C8 C9 N1 179.1(9) . . . . ?
O1 C8 C9 N1 -2.2(11) . . . . ?
C7 C8 C9 C4 -0.1(13) . . . . ?
O1 C8 C9 C4 178.6(7) . . . . ?
O1 C10 C11 O2 -6.8(12) . . . . ?
O1 C10 C11 O3 175.4(7) . . . . ?
N2 C12 C13 C14 -3.3(16) . . . . ?
C12 C13 C14 C15 1.0(15) . . . . ?
C13 C14 C15 C16 179.5(10) . . . . ?
C13 C14 C15 C20 3.5(14) . . . . ?
C14 C15 C16 C17 -174.7(10) . . . . ?
C20 C15 C16 C17 1.1(14) . . . . ?
C15 C16 C17 C18 0.8(16) . . . . ?
C16 C17 C18 C19 -2.1(16) . . . . ?
C17 C18 C19 O4 179.4(8) . . . . ?
C17 C18 C19 C20 1.4(14) . . . . ?
O4 C19 C20 N2 3.3(12) . . . . ?
C18 C19 C20 N2 -178.6(8) . . . . ?
O4 C19 C20 C15 -177.6(7) . . . . ?
C18 C19 C20 C15 0.5(13) . . . . ?
C14 C15 C20 N2 -6.6(13) . . . . ?
C16 C15 C20 N2 177.3(8) . . . . ?
C14 C15 C20 C19 174.4(8) . . . . ?
C16 C15 C20 C19 -1.8(12) . . . . ?
O4 C21 C22 O6 167.7(9) . . . . ?
O4 C21 C22 O5 -14.1(13) . . . . ?
N3 C23 C24 C25 -2.3(16) . . . . ?
C23 C24 C25 C26 0.6(16) . . . . ?
C24 C25 C26 C27 -179.3(10) . . . . ?
C24 C25 C26 C31 0.2(15) . . . . ?
C25 C26 C27 C28 178.5(10) . . . . ?
C31 C26 C27 C28 -0.9(15) . . . . ?
C26 C27 C28 C29 0.4(17) . . . . ?
C27 C28 C29 C30 2.8(16) . . . . ?
C28 C29 C30 O7 175.9(9) . . . . ?
C28 C29 C30 C31 -5.4(14) . . . . ?
O7 C30 C31 N3 1.9(12) . . . . ?
C29 C30 C31 N3 -176.9(8) . . . . ?
O7 C30 C31 C26 -176.3(8) . . . . ?
C29 C30 C31 C26 4.9(13) . . . . ?
C25 C26 C31 N3 0.6(13) . . . . ?
C27 C26 C31 N3 -179.9(8) . . . . ?
C25 C26 C31 C30 178.8(9) . . . . ?
C27 C26 C31 C30 -1.8(13) . . . . ?
O7 C32 C33 O9 179.8(7) . . . . ?
O7 C32 C33 O8 -0.5(12) . . . . ?
N4 C34 C35 C36 2.3(14) . . . . ?
C34 C35 C36 C37 -2.5(13) . . . . ?
C35 C36 C37 C38 -177.9(9) . . . . ?
C35 C36 C37 C42 1.8(12) . . . . ?
C42 C37 C38 C39 0.3(14) . . . . ?
C36 C37 C38 C39 180.0(9) . . . . ?
C37 C38 C39 C40 -0.5(15) . . . . ?
C38 C39 C40 C41 1.3(14) . . . . ?
C39 C40 C41 O10 -179.8(8) . . . . ?
C39 C40 C41 C42 -1.8(13) . . . . ?
C38 C37 C42 N4 179.0(8) . . . . ?
C36 C37 C42 N4 -0.7(11) . . . . ?
C38 C37 C42 C41 -0.9(12) . . . . ?
C36 C37 C42 C41 179.4(7) . . . . ?
O10 C41 C42 N4 -0.1(10) . . . . ?
C40 C41 C42 N4 -178.2(7) . . . . ?
O10 C41 C42 C37 179.8(7) . . . . ?
C40 C41 C42 C37 1.6(12) . . . . ?
O10 C43 C44 O12 -173.6(9) . . . . ?
O10 C43 C44 O11 6.5(13) . . . . ?
O15 C45 C46 O14 171.7(8) . . . . ?
O13 C45 C46 O14 -9.3(12) . . . . ?
O15 C45 C46 O16 -8.4(12) . . . . ?
O13 C45 C46 O16 170.6(8) . . . . ?
C2 C1 N1 C9 -0.2(15) . . . . ?
C2 C1 N1 Pr1 172.8(8) . . . . ?
C4 C9 N1 C1 0.0(13) . . . . ?
C8 C9 N1 C1 -179.2(9) . . . . ?
C4 C9 N1 Pr1 -172.9(6) . . . . ?
C8 C9 N1 Pr1 7.9(11) . . . . ?
C13 C12 N2 C20 0.5(14) . . . . ?
C13 C12 N2 Pr1 172.6(8) . . . . ?
C19 C20 N2 C12 -176.4(8) . . . . ?
C15 C20 N2 C12 4.6(12) . . . . ?
C19 C20 N2 Pr1 11.3(10) . . . . ?
C15 C20 N2 Pr1 -167.8(6) . . . . ?
C24 C23 N3 C31 3.0(14) . . . . ?
C24 C23 N3 Pr2 -170.5(7) . . . . ?
C30 C31 N3 C23 179.6(8) . . . . ?
C26 C31 N3 C23 -2.2(13) . . . . ?
C30 C31 N3 Pr2 -7.0(11) . . . . ?
C26 C31 N3 Pr2 171.2(6) . . . . ?
C35 C34 N4 C42 -1.1(13) . . . . ?
C35 C34 N4 Pr2 -176.2(7) . . . . ?
C37 C42 N4 C34 0.4(11) . . . . ?
C41 C42 N4 C34 -179.8(7) . . . . ?
C37 C42 N4 Pr2 175.6(5) . . . . ?
C41 C42 N4 Pr2 -4.6(9) . . . . ?
C7 C8 O1 C10 -1.5(13) . . . . ?
C9 C8 O1 C10 179.9(8) . . . . ?
C7 C8 O1 Pr1 174.1(8) . . . . ?
C9 C8 O1 Pr1 -4.6(10) . . . . ?
C11 C10 O1 C8 175.9(7) . . . . ?
C11 C10 O1 Pr1 0.1(9) . . . . ?
O3 C11 O2 Pr1 -170.9(6) . . . . ?
C10 C11 O2 Pr1 11.6(11) . . . . ?
O2 C11 O3 Pr2 -175.2(6) . . . . ?
C10 C11 O3 Pr2 2.4(14) . . . . ?
C18 C19 O4 C21 1.0(12) . . . . ?
C20 C19 O4 C21 179.1(7) . . . . ?
C18 C19 O4 Pr1 164.8(7) . . . . ?
C20 C19 O4 Pr1 -17.2(9) . . . . ?
C22 C21 O4 C19 -178.3(7) . . . . ?
C22 C21 O4 Pr1 17.3(9) . . . . ?
O6 C22 O5 Pr1 -178.3(8) . . . . ?
C21 C22 O5 Pr1 3.8(14) . . . . ?
C29 C30 O7 C32 2.2(13) . . . . ?
C31 C30 O7 C32 -176.4(8) . . . . ?
C29 C30 O7 Pr2 -177.2(7) . . . . ?
C31 C30 O7 Pr2 4.1(10) . . . . ?
C33 C32 O7 C30 -174.3(7) . . . . ?
C33 C32 O7 Pr2 5.2(9) . . . . ?
O9 C33 O8 Pr2 174.1(6) . . . . ?
C32 C33 O8 Pr2 -5.6(12) . . . . ?
C40 C41 O10 C43 0.3(12) . . . . ?
C42 C41 O10 C43 -177.8(7) . . . . ?
C40 C41 O10 Pr2 -176.9(6) . . . . ?
C42 C41 O10 Pr2 5.0(9) . . . . ?
C44 C43 O10 C41 -175.9(7) . . . . ?
C44 C43 O10 Pr2 1.4(10) . . . . ?
O12 C44 O11 Pr2 166.5(8) . . . . ?
C43 C44 O11 Pr2 -13.6(13) . . . . ?
O15 C45 O13 Pr1 168.0(7) . . . 4_575 ?
C46 C45 O13 Pr1 -11.0(9) . . . 4_575 ?
O16 C46 O14 Pr1 -154.4(8) . . . 4_575 ?
C45 C46 O14 Pr1 25.5(10) . . . 4_575 ?
O13 C45 O15 Pr2 168.8(7) . . . . ?
C46 C45 O15 Pr2 -12.3(9) . . . . ?
O14 C46 O16 Pr2 -154.2(8) . . . . ?
C45 C46 O16 Pr2 26.0(10) . . . . ?
C22 O5 Pr1 O1W 84.0(9) . . . . ?
C22 O5 Pr1 O2 -65.3(8) . . . . ?
C22 O5 Pr1 O14 -117.2(8) . . . 4_576 ?
C22 O5 Pr1 O13 129.2(8) . . . 4_576 ?
C22 O5 Pr1 O4 4.4(8) . . . . ?
C22 O5 Pr1 O1 -128.8(9) . . . . ?
C22 O5 Pr1 N1 169.3(9) . . . . ?
C22 O5 Pr1 N2 16.2(9) . . . . ?
C11 O2 Pr1 O5 -81.7(7) . . . . ?
C11 O2 Pr1 O1W -139.4(6) . . . . ?
C11 O2 Pr1 O14 65.4(7) . . . 4_576 ?
C11 O2 Pr1 O13 85.9(7) . . . 4_576 ?
C11 O2 Pr1 O4 -145.0(7) . . . . ?
C11 O2 Pr1 O1 -8.0(6) . . . . ?
C11 O2 Pr1 N1 -10.0(7) . . . . ?
C11 O2 Pr1 N2 155.9(7) . . . . ?
C19 O4 Pr1 O5 -175.8(6) . . . . ?
C21 O4 Pr1 O5 -11.9(5) . . . . ?
C19 O4 Pr1 O1W 99.5(6) . . . . ?
C21 O4 Pr1 O1W -96.6(6) . . . . ?
C19 O4 Pr1 O2 -83.9(6) . . . . ?
C21 O4 Pr1 O2 80.0(6) . . . . ?
C19 O4 Pr1 O14 -44.1(6) . . . 4_576 ?
C21 O4 Pr1 O14 119.8(6) . . . 4_576 ?
C19 O4 Pr1 O13 47.2(6) . . . 4_576 ?
C21 O4 Pr1 O13 -148.9(5) . . . 4_576 ?
C19 O4 Pr1 O1 -125.8(5) . . . . ?
C21 O4 Pr1 O1 38.1(6) . . . . ?
C19 O4 Pr1 N1 161.3(5) . . . . ?
C21 O4 Pr1 N1 -34.9(7) . . . . ?
C19 O4 Pr1 N2 15.8(5) . . . . ?
C21 O4 Pr1 N2 179.6(6) . . . . ?
C8 O1 Pr1 O5 -82.0(6) . . . . ?
C10 O1 Pr1 O5 93.4(6) . . . . ?
C8 O1 Pr1 O1W -32.0(7) . . . . ?
C10 O1 Pr1 O1W 143.4(6) . . . . ?
C8 O1 Pr1 O2 -172.1(7) . . . . ?
C10 O1 Pr1 O2 3.3(6) . . . . ?
C8 O1 Pr1 O14 106.2(6) . . . 4_576 ?
C10 O1 Pr1 O14 -78.4(6) . . . 4_576 ?
C8 O1 Pr1 O13 58.0(6) . . . 4_576 ?
C10 O1 Pr1 O13 -126.6(6) . . . 4_576 ?
C8 O1 Pr1 O4 -127.6(6) . . . . ?
C10 O1 Pr1 O4 47.8(6) . . . . ?
C8 O1 Pr1 N1 5.9(6) . . . . ?
C10 O1 Pr1 N1 -178.7(7) . . . . ?
C8 O1 Pr1 N2 158.4(6) . . . . ?
C10 O1 Pr1 N2 -26.2(8) . . . . ?
C1 N1 Pr1 O5 -104.6(8) . . . . ?
C9 N1 Pr1 O5 68.0(6) . . . . ?
C1 N1 Pr1 O1W -24.8(7) . . . . ?
C9 N1 Pr1 O1W 147.7(7) . . . . ?
C1 N1 Pr1 O2 -177.4(7) . . . . ?
C9 N1 Pr1 O2 -4.8(7) . . . . ?
C1 N1 Pr1 O14 114.8(8) . . . 4_576 ?
C9 N1 Pr1 O14 -72.6(6) . . . 4_576 ?
C1 N1 Pr1 O13 51.0(7) . . . 4_576 ?
C9 N1 Pr1 O13 -136.4(7) . . . 4_576 ?
C1 N1 Pr1 O4 -84.0(8) . . . . ?
C9 N1 Pr1 O4 88.5(7) . . . . ?
C1 N1 Pr1 O1 -179.5(8) . . . . ?
C9 N1 Pr1 O1 -6.9(6) . . . . ?
C1 N1 Pr1 N2 29.5(10) . . . . ?
C9 N1 Pr1 N2 -157.9(6) . . . . ?
C12 N2 Pr1 O5 162.5(7) . . . . ?
C20 N2 Pr1 O5 -25.5(7) . . . . ?
C12 N2 Pr1 O1W 94.2(7) . . . . ?
C20 N2 Pr1 O1W -93.8(6) . . . . ?
C12 N2 Pr1 O2 -119.0(7) . . . . ?
C20 N2 Pr1 O2 52.9(6) . . . . ?
C12 N2 Pr1 O14 -46.2(7) . . . 4_576 ?
C20 N2 Pr1 O14 125.8(6) . . . 4_576 ?
C12 N2 Pr1 O13 17.6(7) . . . 4_576 ?
C20 N2 Pr1 O13 -170.4(6) . . . 4_576 ?
C12 N2 Pr1 O4 174.5(8) . . . . ?
C20 N2 Pr1 O4 -13.5(5) . . . . ?
C12 N2 Pr1 O1 -93.2(8) . . . . ?
C20 N2 Pr1 O1 78.8(7) . . . . ?
C12 N2 Pr1 N1 38.5(9) . . . . ?
C20 N2 Pr1 N1 -149.5(6) . . . . ?
C44 O11 Pr2 O8 83.1(8) . . . . ?
C44 O11 Pr2 O3 -66.2(8) . . . . ?
C44 O11 Pr2 O16 144.8(7) . . . . ?
C44 O11 Pr2 O15 -103.5(8) . . . . ?
C44 O11 Pr2 O10 10.3(8) . . . . ?
C44 O11 Pr2 N3 -152.9(8) . . . . ?
C44 O11 Pr2 O7 145.6(8) . . . . ?
C44 O11 Pr2 N4 13.1(9) . . . . ?
C33 O8 Pr2 O11 79.6(7) . . . . ?
C33 O8 Pr2 O3 138.2(7) . . . . ?
C33 O8 Pr2 O16 -64.0(7) . . . . ?
C33 O8 Pr2 O15 -94.6(7) . . . . ?
C33 O8 Pr2 O10 142.7(8) . . . . ?
C33 O8 Pr2 N3 6.8(8) . . . . ?
C33 O8 Pr2 O7 6.0(7) . . . . ?
C33 O8 Pr2 N4 -154.3(8) . . . . ?
C11 O3 Pr2 O11 134.9(10) . . . . ?
C11 O3 Pr2 O8 73.7(11) . . . . ?
C11 O3 Pr2 O16 -74.2(11) . . . . ?
C11 O3 Pr2 O15 -68.8(10) . . . . ?
C11 O3 Pr2 O10 69.2(10) . . . . ?
C11 O3 Pr2 N3 -146.0(10) . . . . ?
C11 O3 Pr2 O7 -178.1(9) . . . . ?
C11 O3 Pr2 N4 10.0(10) . . . . ?
C46 O16 Pr2 O11 116.3(7) . . . . ?
C46 O16 Pr2 O8 -178.7(7) . . . . ?
C46 O16 Pr2 O3 -17.3(8) . . . . ?
C46 O16 Pr2 O15 -23.1(6) . . . . ?
C46 O16 Pr2 O10 -138.3(6) . . . . ?
C46 O16 Pr2 N3 55.3(7) . . . . ?
C46 O16 Pr2 O7 115.5(7) . . . . ?
C46 O16 Pr2 N4 -102.4(7) . . . . ?
C45 O15 Pr2 O11 -120.0(6) . . . . ?
C45 O15 Pr2 O8 50.9(7) . . . . ?
C45 O15 Pr2 O3 -158.2(6) . . . . ?
C45 O15 Pr2 O16 17.7(6) . . . . ?
C45 O15 Pr2 O10 150.5(5) . . . . ?
C45 O15 Pr2 N3 -70.1(6) . . . . ?
C45 O15 Pr2 O7 -24.5(6) . . . . ?
C45 O15 Pr2 N4 109.5(6) . . . . ?
C41 O10 Pr2 O11 172.2(6) . . . . ?
C43 O10 Pr2 O11 -5.0(6) . . . . ?
C41 O10 Pr2 O8 78.3(6) . . . . ?
C43 O10 Pr2 O8 -98.9(6) . . . . ?
C41 O10 Pr2 O3 -104.5(6) . . . . ?
C43 O10 Pr2 O3 78.4(6) . . . . ?
C41 O10 Pr2 O16 37.1(7) . . . . ?
C43 O10 Pr2 O16 -140.1(6) . . . . ?
C41 O10 Pr2 O15 -52.9(6) . . . . ?
C43 O10 Pr2 O15 129.9(6) . . . . ?
C41 O10 Pr2 N3 -163.1(5) . . . . ?
C43 O10 Pr2 N3 19.8(7) . . . . ?
C41 O10 Pr2 O7 122.0(6) . . . . ?
C43 O10 Pr2 O7 -55.2(6) . . . . ?
C41 O10 Pr2 N4 -5.1(5) . . . . ?
C43 O10 Pr2 N4 177.7(7) . . . . ?
C23 N3 Pr2 O11 101.7(7) . . . . ?
C31 N3 Pr2 O11 -71.7(6) . . . . ?
C23 N3 Pr2 O8 178.6(7) . . . . ?
C31 N3 Pr2 O8 5.3(7) . . . . ?
C23 N3 Pr2 O3 24.6(7) . . . . ?
C31 N3 Pr2 O3 -148.8(7) . . . . ?
C23 N3 Pr2 O16 -114.0(7) . . . . ?
C31 N3 Pr2 O16 72.6(6) . . . . ?
C23 N3 Pr2 O15 -48.8(7) . . . . ?
C31 N3 Pr2 O15 137.9(7) . . . . ?
C23 N3 Pr2 O10 79.3(8) . . . . ?
C31 N3 Pr2 O10 -94.1(7) . . . . ?
C23 N3 Pr2 O7 179.4(8) . . . . ?
C31 N3 Pr2 O7 6.1(6) . . . . ?
C23 N3 Pr2 N4 -49.8(9) . . . . ?
C31 N3 Pr2 N4 136.8(6) . . . . ?
C30 O7 Pr2 O11 80.3(6) . . . . ?
C32 O7 Pr2 O11 -99.2(6) . . . . ?
C30 O7 Pr2 O8 173.9(7) . . . . ?
C32 O7 Pr2 O8 -5.5(6) . . . . ?
C30 O7 Pr2 O3 32.5(7) . . . . ?
C32 O7 Pr2 O3 -147.0(6) . . . . ?
C30 O7 Pr2 O16 -100.3(6) . . . . ?
C32 O7 Pr2 O16 80.2(6) . . . . ?
C30 O7 Pr2 O15 -58.8(6) . . . . ?
C32 O7 Pr2 O15 121.7(6) . . . . ?
C30 O7 Pr2 O10 125.8(6) . . . . ?
C32 O7 Pr2 O10 -53.7(6) . . . . ?
C30 O7 Pr2 N3 -5.3(6) . . . . ?
C32 O7 Pr2 N3 175.2(6) . . . . ?
C30 O7 Pr2 N4 -158.9(6) . . . . ?
C32 O7 Pr2 N4 21.6(7) . . . . ?
C34 N4 Pr2 O11 176.9(6) . . . . ?
C42 N4 Pr2 O11 1.9(6) . . . . ?
C34 N4 Pr2 O8 102.0(7) . . . . ?
C42 N4 Pr2 O8 -73.0(5) . . . . ?
C34 N4 Pr2 O3 -110.5(7) . . . . ?
C42 N4 Pr2 O3 74.5(5) . . . . ?
C34 N4 Pr2 O16 26.1(7) . . . . ?
C42 N4 Pr2 O16 -148.9(6) . . . . ?
C34 N4 Pr2 O15 -38.2(6) . . . . ?
C42 N4 Pr2 O15 146.8(6) . . . . ?
C34 N4 Pr2 O10 179.7(7) . . . . ?
C42 N4 Pr2 O10 4.7(5) . . . . ?
C34 N4 Pr2 N3 -37.1(9) . . . . ?
C42 N4 Pr2 N3 147.9(6) . . . . ?
C34 N4 Pr2 O7 77.3(7) . . . . ?
C42 N4 Pr2 O7 -97.7(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.399
_refine_diff_density_min         -0.886
_refine_diff_density_rms         0.145

#===END

data_er4
_database_code_depnum_ccdc_archive 'CCDC 717621'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C46 H34 Er2 N4 O17, 3(H2 O)'
_chemical_formula_sum            'C46 H40 Er2 N4 O20'
_chemical_formula_weight         1303.34

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'
Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   19.266(4)
_cell_length_b                   16.039(3)
_cell_length_c                   15.551(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.41(3)
_cell_angle_gamma                90.00
_cell_volume                     4726.3(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    11209
_cell_measurement_theta_min      1.07
_cell_measurement_theta_max      27.97

_exptl_crystal_description       block
_exptl_crystal_colour            pale-orange
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2560
_exptl_absorpt_coefficient_mu    3.612
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4125
_exptl_absorpt_correction_T_max  0.5912
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41762
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_sigmaI/netI    0.0876
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.07
_diffrn_reflns_theta_max         25.25
_reflns_number_total             8506
_reflns_number_gt                5529
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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+0.0200P] where P=(Fo²+2Fc²)/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         8506
_refine_ls_number_parameters     649
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0596
_refine_ls_wR_factor_ref         0.1786
_refine_ls_wR_factor_gt          0.1513
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1105(6) 0.5894(7) 0.6317(8) 0.044(3) Uani 1 1 d . . .
H1 H 0.1456 0.5820 0.6807 0.052 Uiso 1 1 calc R . .
C2 C 0.0400(6) 0.6044(8) 0.6440(8) 0.046(3) Uani 1 1 d . . .
H2 H 0.0299 0.6073 0.7002 0.055 Uiso 1 1 calc R . .
C3 C -0.0114(6) 0.6144(7) 0.5753(8) 0.038(3) Uani 1 1 d . . .
H3 H -0.0575 0.6233 0.5835 0.046 Uiso 1 1 calc R . .
C4 C 0.0034(5) 0.6114(6) 0.4916(7) 0.030(2) Uani 1 1 d . . .
C5 C -0.0462(6) 0.6232(7) 0.4145(8) 0.042(3) Uani 1 1 d . . .
H5 H -0.0931 0.6331 0.4186 0.051 Uiso 1 1 calc R . .
C6 C -0.0284(6) 0.6208(8) 0.3364(7) 0.049(3) Uani 1 1 d . . .
H6 H -0.0627 0.6291 0.2868 0.059 Uiso 1 1 calc R . .
C7 C 0.0429(6) 0.6055(8) 0.3270(7) 0.046(3) Uani 1 1 d . . .
H7 H 0.0552 0.6040 0.2719 0.056 Uiso 1 1 calc R . .
C8 C 0.0921(5) 0.5933(6) 0.3996(7) 0.030(3) Uani 1 1 d . . .
C9 C 0.0751(5) 0.5970(6) 0.4838(7) 0.024(2) Uani 1 1 d . . .
C10 C 0.1824(5) 0.5725(7) 0.3139(7) 0.035(3) Uani 1 1 d . . .
H10A H 0.1760 0.6268 0.2861 0.042 Uiso 1 1 calc R . .
H10B H 0.1524 0.5330 0.2773 0.042 Uiso 1 1 calc R . .
C11 C 0.2582(5) 0.5461(6) 0.3224(6) 0.022(2) Uani 1 1 d . . .
C12 C 0.4249(6) 0.5977(7) 0.6550(8) 0.038(3) Uani 1 1 d . . .
H12 H 0.3978 0.6422 0.6685 0.045 Uiso 1 1 calc R . .
C13 C 0.4974(6) 0.6007(7) 0.6833(8) 0.047(3) Uani 1 1 d . . .
H13 H 0.5174 0.6454 0.7171 0.057 Uiso 1 1 calc R . .
C14 C 0.5400(6) 0.5378(7) 0.6615(8) 0.044(3) Uani 1 1 d . . .
H14 H 0.5887 0.5394 0.6798 0.053 Uiso 1 1 calc R . .
C15 C 0.5075(5) 0.4718(7) 0.6111(7) 0.031(3) Uani 1 1 d . . .
C16 C 0.5453(5) 0.4039(7) 0.5853(7) 0.036(3) Uani 1 1 d . . .
H16 H 0.5943 0.4037 0.5994 0.043 Uiso 1 1 calc R . .
C17 C 0.5122(5) 0.3398(8) 0.5409(8) 0.042(3) Uani 1 1 d . . .
H17 H 0.5384 0.2968 0.5225 0.050 Uiso 1 1 calc R . .
C18 C 0.4380(6) 0.3366(7) 0.5218(7) 0.038(3) Uani 1 1 d . . .
H18 H 0.4156 0.2903 0.4933 0.046 Uiso 1 1 calc R . .
C19 C 0.3988(5) 0.4006(6) 0.5445(6) 0.026(2) Uani 1 1 d . . .
C20 C 0.4320(5) 0.4717(6) 0.5897(6) 0.028(2) Uani 1 1 d . . .
C21 C 0.2889(5) 0.3338(6) 0.4840(8) 0.034(3) Uani 1 1 d . . .
H21A H 0.3026 0.2826 0.5158 0.041 Uiso 1 1 calc R . .
H21B H 0.3009 0.3289 0.4263 0.041 Uiso 1 1 calc R . .
C22 C 0.2096(6) 0.3472(8) 0.4758(7) 0.038(3) Uani 1 1 d . . .
C23 C 0.4165(6) 0.6532(7) 0.1976(8) 0.046(3) Uani 1 1 d . . .
H23 H 0.3881 0.6612 0.2393 0.056 Uiso 1 1 calc R . .
C24 C 0.4893(7) 0.6732(8) 0.2196(9) 0.058(4) Uani 1 1 d . . .
H24 H 0.5082 0.6932 0.2750 0.070 Uiso 1 1 calc R . .
C25 C 0.5293(7) 0.6635(8) 0.1613(10) 0.053(4) Uani 1 1 d . . .
H25 H 0.5770 0.6763 0.1766 0.064 Uiso 1 1 calc R . .
C26 C 0.5034(6) 0.6344(7) 0.0761(8) 0.039(3) Uani 1 1 d . . .
C27 C 0.5425(6) 0.6232(7) 0.0088(9) 0.046(3) Uani 1 1 d . . .
H27 H 0.5907 0.6342 0.0199 0.055 Uiso 1 1 calc R . .
C28 C 0.5121(6) 0.5973(7) -0.0707(9) 0.043(3) Uani 1 1 d . . .
H28 H 0.5387 0.5916 -0.1146 0.052 Uiso 1 1 calc R . .
C29 C 0.4389(6) 0.5784(7) -0.0881(9) 0.043(3) Uani 1 1 d . . .
H29 H 0.4176 0.5616 -0.1439 0.052 Uiso 1 1 calc R . .
C30 C 0.3998(5) 0.5846(6) -0.0247(7) 0.032(3) Uani 1 1 d . . .
C31 C 0.4301(5) 0.6146(6) 0.0599(7) 0.031(3) Uani 1 1 d . . .
C32 C 0.2957(6) 0.5357(7) -0.1181(7) 0.037(3) Uani 1 1 d . . .
H32A H 0.3223 0.4917 -0.1403 0.044 Uiso 1 1 calc R . .
H32B H 0.2927 0.5826 -0.1580 0.044 Uiso 1 1 calc R . .
C33 C 0.2218(5) 0.5045(6) -0.1132(7) 0.025(2) Uani 1 1 d . . .
C34 C 0.0845(5) 0.6457(7) 0.0871(7) 0.037(3) Uani 1 1 d . . .
H34 H 0.1091 0.6940 0.0787 0.045 Uiso 1 1 calc R . .
C35 C 0.0108(6) 0.6515(7) 0.0847(7) 0.042(3) Uani 1 1 d . . .
H35 H -0.0118 0.7029 0.0765 0.051 Uiso 1 1 calc R . .
C36 C -0.0261(6) 0.5820(7) 0.0943(7) 0.034(3) Uani 1 1 d . . .
H36 H -0.0747 0.5847 0.0910 0.041 Uiso 1 1 calc R . .
C37 C 0.0094(5) 0.5050(6) 0.1094(6) 0.026(2) Uani 1 1 d . . .
C38 C -0.0252(6) 0.4308(8) 0.1226(7) 0.038(3) Uani 1 1 d . . .
H38 H -0.0738 0.4311 0.1199 0.045 Uiso 1 1 calc R . .
C39 C 0.0112(5) 0.3581(8) 0.1394(7) 0.040(3) Uani 1 1 d . . .
H39 H -0.0125 0.3095 0.1492 0.048 Uiso 1 1 calc R . .
C40 C 0.0846(5) 0.3562(7) 0.1421(7) 0.033(3) Uani 1 1 d . . .
H40 H 0.1096 0.3066 0.1534 0.040 Uiso 1 1 calc R . .
C41 C 0.1186(5) 0.4277(6) 0.1279(6) 0.023(2) Uani 1 1 d . . .
C42 C 0.0824(4) 0.5047(6) 0.1118(6) 0.020(2) Uani 1 1 d . . .
C43 C 0.2311(5) 0.3585(7) 0.1454(8) 0.041(3) Uani 1 1 d . . .
H43A H 0.2113 0.3170 0.1025 0.050 Uiso 1 1 calc R . .
H43B H 0.2277 0.3373 0.2029 0.050 Uiso 1 1 calc R . .
C44 C 0.3085(5) 0.3731(7) 0.1400(7) 0.031(2) Uani 1 1 d . . .
C45 C 0.2574(5) 0.7719(7) 0.1257(6) 0.029(2) Uani 1 1 d . . .
C46 C 0.2559(6) 0.7608(7) 0.0240(7) 0.037(3) Uani 1 1 d . . .
Er1 Er 0.25542(3) 0.54039(3) 0.53821(3) 0.03444(18) Uani 1 1 d . . .
Er2 Er 0.25754(3) 0.56711(3) 0.09497(3) 0.03553(18) Uani 1 1 d . . .
N1 N 0.1274(4) 0.5857(5) 0.5561(5) 0.0270(19) Uani 1 1 d . . .
N2 N 0.3927(4) 0.5354(5) 0.6102(5) 0.0270(19) Uani 1 1 d . . .
N3 N 0.3879(5) 0.6239(5) 0.1210(6) 0.035(2) Uani 1 1 d . . .
N4 N 0.1197(4) 0.5755(5) 0.1008(5) 0.0233(18) Uani 1 1 d . . .
O1 O 0.1626(3) 0.5763(4) 0.3981(4) 0.0292(16) Uani 1 1 d . . .
O2 O 0.2909(3) 0.5247(4) 0.3968(4) 0.0280(16) Uani 1 1 d . . .
O3 O 0.2818(3) 0.5455(4) 0.2537(4) 0.0284(16) Uani 1 1 d . . .
O4 O 0.3258(3) 0.4031(4) 0.5295(4) 0.0257(15) Uani 1 1 d . . .
O5 O 0.1893(4) 0.4179(4) 0.4907(5) 0.0359(18) Uani 1 1 d . . .
O6 O 0.1728(4) 0.2849(5) 0.4558(7) 0.066(3) Uani 1 1 d . . .
O7 O 0.3316(4) 0.5609(4) -0.0323(5) 0.0328(17) Uani 1 1 d . . .
O8 O 0.2017(3) 0.5086(4) -0.0426(4) 0.0302(16) Uani 1 1 d . . .
O9 O 0.1866(4) 0.4796(5) -0.1838(5) 0.0374(18) Uani 1 1 d . . .
O10 O 0.1919(3) 0.4334(4) 0.1297(4) 0.0263(16) Uani 1 1 d . . .
O11 O 0.3239(3) 0.4424(4) 0.1128(5) 0.0317(17) Uani 1 1 d . . .
O12 O 0.3492(4) 0.3157(5) 0.1620(7) 0.061(3) Uani 1 1 d . . .
O13 O 0.2495(4) 0.7081(4) 0.1674(4) 0.0293(16) Uani 1 1 d . . .
O14 O 0.2379(4) 0.6869(4) -0.0049(5) 0.0403(19) Uani 1 1 d . . .
O15 O 0.2655(4) 0.8450(4) 0.1503(4) 0.0289(16) Uani 1 1 d . . .
O16 O 0.2727(4) 0.8204(4) -0.0174(4) 0.0365(18) Uani 1 1 d . . .
O2W O 0.1835(5) 0.1988(6) 0.3055(7) 0.070(3) Uani 1 1 d . . .
H4W H 0.1849 0.1492 0.3246 0.106 Uiso 1 1 d R . .
H3W H 0.1589 0.2282 0.3341 0.106 Uiso 1 1 d R . .
O3W O 0.3049(4) 0.3228(5) 0.7371(6) 0.053(2) Uani 1 1 d . . .
H5W H 0.2654 0.3093 0.7506 0.080 Uiso 1 1 d R . .
H6W H 0.3084 0.2985 0.6896 0.080 Uiso 1 1 d R . .
O4W O 0.1671(8) 0.7055(9) 0.8087(8) 0.136(6) Uani 1 1 d . . .
H7W H 0.1341 0.6987 0.8378 0.204 Uiso 1 1 d R . .
H8W H 0.2056 0.7036 0.8455 0.204 Uiso 1 1 d R . .
O1W O 0.2543(4) 0.4708(4) 0.6765(4) 0.0356(18) Uani 1 1 d . . .
H2W H 0.2270 0.4624 0.7130 0.053 Uiso 1 1 d R . .
H1W H 0.2684 0.4228 0.6648 0.053 Uiso 1 1 d 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
C1 N1 1.276(14) . ?
C1 C2 1.427(16) . ?
C1 H1 0.9300 . ?
C2 C3 1.328(16) . ?
C2 H2 0.9300 . ?
C3 C4 1.383(16) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(15) . ?
C4 C9 1.426(14) . ?
C5 C6 1.322(16) . ?
C5 H5 0.9300 . ?
C6 C7 1.428(16) . ?
C6 H6 0.9300 . ?
C7 C8 1.351(14) . ?
C7 H7 0.9300 . ?
C8 O1 1.389(11) . ?
C8 C9 1.408(15) . ?
C9 N1 1.380(12) . ?
C10 O1 1.430(12) . ?
C10 C11 1.503(13) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O3 1.235(11) . ?
C11 O2 1.260(11) . ?
C12 N2 1.309(12) . ?
C12 C13 1.387(15) . ?
C12 H12 0.9300 . ?
C13 C14 1.381(17) . ?
C13 H13 0.9300 . ?
C14 C15 1.397(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.408(15) . ?
C15 C20 1.432(14) . ?
C16 C17 1.334(16) . ?
C16 H16 0.9300 . ?
C17 C18 1.408(15) . ?
C17 H17 0.9300 . ?
C18 C19 1.357(14) . ?
C18 H18 0.9300 . ?
C19 O4 1.384(11) . ?
C19 C20 1.429(14) . ?
C20 N2 1.344(13) . ?
C21 O4 1.436(11) . ?
C21 C22 1.524(15) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O6 1.232(13) . ?
C22 O5 1.235(13) . ?
C23 N3 1.306(14) . ?
C23 C24 1.418(17) . ?
C23 H23 0.9300 . ?
C24 C25 1.300(19) . ?
C24 H24 0.9300 . ?
C25 C26 1.409(18) . ?
C25 H25 0.9300 . ?
C26 C27 1.407(17) . ?
C26 C31 1.425(14) . ?
C27 C28 1.336(18) . ?
C27 H27 0.9300 . ?
C28 C29 1.419(16) . ?
C28 H28 0.9300 . ?
C29 C30 1.348(16) . ?
C29 H29 0.9300 . ?
C30 O7 1.352(12) . ?
C30 C31 1.423(15) . ?
C31 N3 1.366(14) . ?
C32 O7 1.445(12) . ?
C32 C33 1.524(14) . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C33 O8 1.231(12) . ?
C33 O9 1.247(12) . ?
C34 N4 1.313(13) . ?
C34 C35 1.416(15) . ?
C34 H34 0.9300 . ?
C35 C36 1.345(16) . ?
C35 H35 0.9300 . ?
C36 C37 1.412(15) . ?
C36 H36 0.9300 . ?
C37 C38 1.397(15) . ?
C37 C42 1.399(12) . ?
C38 C39 1.361(16) . ?
C38 H38 0.9300 . ?
C39 C40 1.408(14) . ?
C39 H39 0.9300 . ?
C40 C41 1.358(14) . ?
C40 H40 0.9300 . ?
C41 O10 1.411(11) . ?
C41 C42 1.418(13) . ?
C42 N4 1.371(12) . ?
C43 O10 1.416(12) . ?
C43 C44 1.528(14) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 O12 1.217(12) . ?
C44 O11 1.245(12) . ?
C45 O15 1.235(12) . ?
C45 O13 1.235(12) . ?
C45 C46 1.586(14) . ?
C46 O16 1.229(13) . ?
C46 O14 1.292(13) . ?
Er1 O5 2.385(7) . ?
Er1 O1W 2.426(7) . ?
Er1 O2 2.431(7) . ?
Er1 O16 2.438(7) 4_576 ?
Er1 O15 2.516(7) 4_576 ?
Er1 O4 2.602(6) . ?
Er1 O1 2.622(6) . ?
Er1 N1 2.633(8) . ?
Er1 N2 2.680(8) . ?
Er2 O11 2.363(7) . ?
Er2 O8 2.405(7) . ?
Er2 O3 2.453(7) . ?
Er2 O14 2.456(7) . ?
Er2 O13 2.544(7) . ?
Er2 O10 2.596(6) . ?
Er2 N3 2.633(9) . ?
Er2 O7 2.643(7) . ?
Er2 N4 2.677(8) . ?
O15 Er1 2.516(7) 4_575 ?
O16 Er1 2.438(7) 4_575 ?
O2W H4W 0.8487 . ?
O2W H3W 0.8491 . ?
O3W H5W 0.8516 . ?
O3W H6W 0.8488 . ?
O4W H7W 0.8519 . ?
O4W H8W 0.8518 . ?
O1W H2W 0.8510 . ?
O1W H1W 0.8472 . ?

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
N1 C1 C2 122.6(10) . . ?
N1 C1 H1 118.7 . . ?
C2 C1 H1 118.7 . . ?
C3 C2 C1 120.1(11) . . ?
C3 C2 H2 119.9 . . ?
C1 C2 H2 119.9 . . ?
C2 C3 C4 120.1(10) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C3 C4 C5 125.0(10) . . ?
C3 C4 C9 117.0(9) . . ?
C5 C4 C9 118.0(10) . . ?
C6 C5 C4 122.0(10) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C7 120.9(10) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 118.9(11) . . ?
C8 C7 H7 120.6 . . ?
C6 C7 H7 120.6 . . ?
C7 C8 O1 123.7(10) . . ?
C7 C8 C9 121.7(10) . . ?
O1 C8 C9 114.6(8) . . ?
N1 C9 C8 119.5(9) . . ?
N1 C9 C4 121.9(9) . . ?
C8 C9 C4 118.5(9) . . ?
O1 C10 C11 110.3(8) . . ?
O1 C10 H10A 109.6 . . ?
C11 C10 H10A 109.6 . . ?
O1 C10 H10B 109.6 . . ?
C11 C10 H10B 109.6 . . ?
H10A C10 H10B 108.1 . . ?
O3 C11 O2 126.2(9) . . ?
O3 C11 C10 115.5(9) . . ?
O2 C11 C10 118.3(9) . . ?
N2 C12 C13 123.3(10) . . ?
N2 C12 H12 118.4 . . ?
C13 C12 H12 118.4 . . ?
C14 C13 C12 120.4(10) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 117.7(10) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C14 C15 C16 122.9(10) . . ?
C14 C15 C20 117.7(10) . . ?
C16 C15 C20 119.3(10) . . ?
C17 C16 C15 121.3(10) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 120.7(11) . . ?
C16 C17 H17 119.7 . . ?
C18 C17 H17 119.7 . . ?
C19 C18 C17 120.5(10) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 O4 125.0(9) . . ?
C18 C19 C20 120.7(9) . . ?
O4 C19 C20 114.2(8) . . ?
N2 C20 C19 120.1(9) . . ?
N2 C20 C15 122.5(9) . . ?
C19 C20 C15 117.4(9) . . ?
O4 C21 C22 109.4(8) . . ?
O4 C21 H21A 109.8 . . ?
C22 C21 H21A 109.8 . . ?
O4 C21 H21B 109.8 . . ?
C22 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
O6 C22 O5 127.2(10) . . ?
O6 C22 C21 115.5(10) . . ?
O5 C22 C21 117.4(9) . . ?
N3 C23 C24 122.5(13) . . ?
N3 C23 H23 118.7 . . ?
C24 C23 H23 118.7 . . ?
C25 C24 C23 119.3(13) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 122.9(12) . . ?
C24 C25 H25 118.6 . . ?
C26 C25 H25 118.6 . . ?
C27 C26 C25 126.6(12) . . ?
C27 C26 C31 119.2(11) . . ?
C25 C26 C31 114.2(11) . . ?
C28 C27 C26 121.5(11) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C27 C28 C29 119.9(12) . . ?
C27 C28 H28 120.1 . . ?
C29 C28 H28 120.1 . . ?
C30 C29 C28 120.8(12) . . ?
C30 C29 H29 119.6 . . ?
C28 C29 H29 119.6 . . ?
C29 C30 O7 125.3(11) . . ?
C29 C30 C31 120.7(10) . . ?
O7 C30 C31 114.0(9) . . ?
N3 C31 C30 118.9(9) . . ?
N3 C31 C26 123.3(10) . . ?
C30 C31 C26 117.9(10) . . ?
O7 C32 C33 109.9(8) . . ?
O7 C32 H32A 109.7 . . ?
C33 C32 H32A 109.7 . . ?
O7 C32 H32B 109.7 . . ?
C33 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
O8 C33 O9 126.4(10) . . ?
O8 C33 C32 118.4(9) . . ?
O9 C33 C32 115.2(9) . . ?
N4 C34 C35 123.2(10) . . ?
N4 C34 H34 118.4 . . ?
C35 C34 H34 118.4 . . ?
C36 C35 C34 119.3(10) . . ?
C36 C35 H35 120.3 . . ?
C34 C35 H35 120.3 . . ?
C35 C36 C37 119.6(10) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C38 C37 C42 119.8(9) . . ?
C38 C37 C36 122.7(9) . . ?
C42 C37 C36 117.5(9) . . ?
C39 C38 C37 121.0(10) . . ?
C39 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C38 C39 C40 120.3(11) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C41 C40 C39 119.2(10) . . ?
C41 C40 H40 120.4 . . ?
C39 C40 H40 120.4 . . ?
C40 C41 O10 124.1(9) . . ?
C40 C41 C42 121.9(9) . . ?
O10 C41 C42 114.0(8) . . ?
N4 C42 C37 122.8(9) . . ?
N4 C42 C41 119.4(8) . . ?
C37 C42 C41 117.9(9) . . ?
O10 C43 C44 110.9(8) . . ?
O10 C43 H43A 109.5 . . ?
C44 C43 H43A 109.5 . . ?
O10 C43 H43B 109.5 . . ?
C44 C43 H43B 109.5 . . ?
H43A C43 H43B 108.1 . . ?
O12 C44 O11 126.2(10) . . ?
O12 C44 C43 117.0(10) . . ?
O11 C44 C43 116.8(9) . . ?
O15 C45 O13 130.1(9) . . ?
O15 C45 C46 113.2(9) . . ?
O13 C45 C46 116.7(10) . . ?
O16 C46 O14 127.7(10) . . ?
O16 C46 C45 118.4(10) . . ?
O14 C46 C45 113.9(10) . . ?
O5 Er1 O1W 78.8(3) . . ?
O5 Er1 O2 81.7(2) . . ?
O1W Er1 O2 143.4(2) . . ?
O5 Er1 O16 138.1(3) . 4_576 ?
O1W Er1 O16 139.4(2) . 4_576 ?
O2 Er1 O16 72.3(2) . 4_576 ?
O5 Er1 O15 141.9(2) . 4_576 ?
O1W Er1 O15 74.6(2) . 4_576 ?
O2 Er1 O15 134.7(2) . 4_576 ?
O16 Er1 O15 65.1(2) 4_576 4_576 ?
O5 Er1 O4 62.7(2) . . ?
O1W Er1 O4 75.2(2) . . ?
O2 Er1 O4 68.4(2) . . ?
O16 Er1 O4 130.6(2) 4_576 . ?
O15 Er1 O4 132.7(2) 4_576 . ?
O5 Er1 O1 71.2(2) . . ?
O1W Er1 O1 136.4(2) . . ?
O2 Er1 O1 62.1(2) . . ?
O16 Er1 O1 67.7(2) 4_576 . ?
O15 Er1 O1 111.8(2) 4_576 . ?
O4 Er1 O1 115.3(2) . . ?
O5 Er1 N1 78.6(3) . . ?
O1W Er1 N1 82.8(2) . . ?
O2 Er1 N1 123.1(2) . . ?
O16 Er1 N1 88.6(3) 4_576 . ?
O15 Er1 N1 71.5(2) 4_576 . ?
O4 Er1 N1 138.2(2) . . ?
O1 Er1 N1 61.0(2) . . ?
O5 Er1 N2 122.4(2) . . ?
O1W Er1 N2 77.4(2) . . ?
O2 Er1 N2 87.6(2) . . ?
O16 Er1 N2 89.3(3) 4_576 . ?
O15 Er1 N2 77.6(2) 4_576 . ?
O4 Er1 N2 60.8(2) . . ?
O1 Er1 N2 145.9(2) . . ?
N1 Er1 N2 146.7(3) . . ?
O11 Er2 O8 85.4(2) . . ?
O11 Er2 O3 76.2(2) . . ?
O8 Er2 O3 144.4(2) . . ?
O11 Er2 O14 139.0(3) . . ?
O8 Er2 O14 75.5(2) . . ?
O3 Er2 O14 136.6(2) . . ?
O11 Er2 O13 140.8(2) . . ?
O8 Er2 O13 133.5(2) . . ?
O3 Er2 O13 72.3(2) . . ?
O14 Er2 O13 64.5(2) . . ?
O11 Er2 O10 63.3(2) . . ?
O8 Er2 O10 72.9(2) . . ?
O3 Er2 O10 71.7(2) . . ?
O14 Er2 O10 138.8(2) . . ?
O13 Er2 O10 124.9(2) . . ?
O11 Er2 N3 78.1(2) . . ?
O8 Er2 N3 122.2(3) . . ?
O3 Er2 N3 83.7(2) . . ?
O14 Er2 N3 82.0(3) . . ?
O13 Er2 N3 75.9(3) . . ?
O10 Er2 N3 137.8(2) . . ?
O11 Er2 O7 72.7(2) . . ?
O8 Er2 O7 62.3(2) . . ?
O3 Er2 O7 135.9(2) . . ?
O14 Er2 O7 66.3(2) . . ?
O13 Er2 O7 116.7(2) . . ?
O10 Er2 O7 118.3(2) . . ?
N3 Er2 O7 59.9(2) . . ?
O11 Er2 N4 123.9(2) . . ?
O8 Er2 N4 76.3(2) . . ?
O3 Er2 N4 89.0(2) . . ?
O14 Er2 N4 86.7(3) . . ?
O13 Er2 N4 78.5(2) . . ?
O10 Er2 N4 60.7(2) . . ?
N3 Er2 N4 154.4(3) . . ?
O7 Er2 N4 134.5(2) . . ?
C1 N1 C9 118.2(9) . . ?
C1 N1 Er1 120.7(7) . . ?
C9 N1 Er1 120.7(6) . . ?
C12 N2 C20 118.2(9) . . ?
C12 N2 Er1 122.4(7) . . ?
C20 N2 Er1 118.7(6) . . ?
C23 N3 C31 117.9(10) . . ?
C23 N3 Er2 119.9(8) . . ?
C31 N3 Er2 121.8(7) . . ?
C34 N4 C42 117.6(8) . . ?
C34 N4 Er2 121.6(7) . . ?
C42 N4 Er2 120.6(6) . . ?
C8 O1 C10 116.6(7) . . ?
C8 O1 Er1 123.5(6) . . ?
C10 O1 Er1 119.8(5) . . ?
C11 O2 Er1 128.8(6) . . ?
C11 O3 Er2 146.8(6) . . ?
C19 O4 C21 117.3(7) . . ?
C19 O4 Er1 122.7(5) . . ?
C21 O4 Er1 117.6(5) . . ?
C22 O5 Er1 130.2(7) . . ?
C30 O7 C32 117.0(8) . . ?
C30 O7 Er2 124.9(6) . . ?
C32 O7 Er2 118.0(6) . . ?
C33 O8 Er2 130.7(6) . . ?
C41 O10 C43 116.7(7) . . ?
C41 O10 Er2 124.9(5) . . ?
C43 O10 Er2 118.2(6) . . ?
C44 O11 Er2 129.7(6) . . ?
C45 O13 Er2 118.7(6) . . ?
C46 O14 Er2 119.8(6) . . ?
C45 O15 Er1 119.3(6) . 4_575 ?
C46 O16 Er1 117.5(7) . 4_575 ?
H4W O2W H3W 108.9 . . ?
H5W O3W H6W 108.3 . . ?
H7W O4W H8W 106.3 . . ?
Er1 O1W H2W 140.3 . . ?
Er1 O1W H1W 100.0 . . ?
H2W O1W H1W 105.1 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1(2) . . . . ?
C1 C2 C3 C4 -1.0(19) . . . . ?
C2 C3 C4 C5 -178.2(12) . . . . ?
C2 C3 C4 C9 0.4(16) . . . . ?
C3 C4 C5 C6 179.0(12) . . . . ?
C9 C4 C5 C6 0.5(17) . . . . ?
C4 C5 C6 C7 0(2) . . . . ?
C5 C6 C7 C8 0(2) . . . . ?
C6 C7 C8 O1 178.7(10) . . . . ?
C6 C7 C8 C9 -1.4(18) . . . . ?
C7 C8 C9 N1 -178.7(10) . . . . ?
O1 C8 C9 N1 1.2(13) . . . . ?
C7 C8 C9 C4 2.0(15) . . . . ?
O1 C8 C9 C4 -178.0(8) . . . . ?
C3 C4 C9 N1 0.6(14) . . . . ?
C5 C4 C9 N1 179.3(10) . . . . ?
C3 C4 C9 C8 179.8(9) . . . . ?
C5 C4 C9 C8 -1.5(14) . . . . ?
O1 C10 C11 O3 -176.0(8) . . . . ?
O1 C10 C11 O2 6.0(13) . . . . ?
N2 C12 C13 C14 2.8(19) . . . . ?
C12 C13 C14 C15 -0.4(18) . . . . ?
C13 C14 C15 C16 -179.6(11) . . . . ?
C13 C14 C15 C20 -3.3(16) . . . . ?
C14 C15 C16 C17 176.5(11) . . . . ?
C20 C15 C16 C17 0.3(16) . . . . ?
C15 C16 C17 C18 -2.7(18) . . . . ?
C16 C17 C18 C19 3.1(18) . . . . ?
C17 C18 C19 O4 -179.3(10) . . . . ?
C17 C18 C19 C20 -1.1(17) . . . . ?
C18 C19 C20 N2 178.7(10) . . . . ?
O4 C19 C20 N2 -2.9(13) . . . . ?
C18 C19 C20 C15 -1.2(15) . . . . ?
O4 C19 C20 C15 177.2(8) . . . . ?
C14 C15 C20 N2 5.3(15) . . . . ?
C16 C15 C20 N2 -178.2(9) . . . . ?
C14 C15 C20 C19 -174.8(9) . . . . ?
C16 C15 C20 C19 1.7(14) . . . . ?
O4 C21 C22 O6 -164.6(10) . . . . ?
O4 C21 C22 O5 14.6(14) . . . . ?
N3 C23 C24 C25 1.0(19) . . . . ?
C23 C24 C25 C26 1(2) . . . . ?
C24 C25 C26 C27 178.9(12) . . . . ?
C24 C25 C26 C31 -1.5(17) . . . . ?
C25 C26 C27 C28 -178.1(11) . . . . ?
C31 C26 C27 C28 2.3(17) . . . . ?
C26 C27 C28 C29 -1.5(18) . . . . ?
C27 C28 C29 C30 -1.5(17) . . . . ?
C28 C29 C30 O7 -173.6(10) . . . . ?
C28 C29 C30 C31 3.4(16) . . . . ?
C29 C30 C31 N3 176.7(10) . . . . ?
O7 C30 C31 N3 -5.9(13) . . . . ?
C29 C30 C31 C26 -2.5(15) . . . . ?
O7 C30 C31 C26 174.8(8) . . . . ?
C27 C26 C31 N3 -179.5(10) . . . . ?
C25 C26 C31 N3 0.9(14) . . . . ?
C27 C26 C31 C30 -0.3(14) . . . . ?
C25 C26 C31 C30 -180.0(10) . . . . ?
O7 C32 C33 O8 3.6(13) . . . . ?
O7 C32 C33 O9 -178.7(8) . . . . ?
N4 C34 C35 C36 -1.9(17) . . . . ?
C34 C35 C36 C37 2.0(16) . . . . ?
C35 C36 C37 C38 178.0(10) . . . . ?
C35 C36 C37 C42 -1.3(14) . . . . ?
C42 C37 C38 C39 1.2(16) . . . . ?
C36 C37 C38 C39 -178.1(10) . . . . ?
C37 C38 C39 C40 -1.3(17) . . . . ?
C38 C39 C40 C41 0.2(16) . . . . ?
C39 C40 C41 O10 179.4(9) . . . . ?
C39 C40 C41 C42 1.0(15) . . . . ?
C38 C37 C42 N4 -178.9(9) . . . . ?
C36 C37 C42 N4 0.5(13) . . . . ?
C38 C37 C42 C41 0.0(13) . . . . ?
C36 C37 C42 C41 179.3(9) . . . . ?
C40 C41 C42 N4 177.8(9) . . . . ?
O10 C41 C42 N4 -0.7(12) . . . . ?
C40 C41 C42 C37 -1.1(14) . . . . ?
O10 C41 C42 C37 -179.6(8) . . . . ?
O10 C43 C44 O12 171.8(10) . . . . ?
O10 C43 C44 O11 -8.6(15) . . . . ?
O15 C45 C46 O16 10.4(14) . . . . ?
O13 C45 C46 O16 -170.6(9) . . . . ?
O15 C45 C46 O14 -171.0(9) . . . . ?
O13 C45 C46 O14 8.0(13) . . . . ?
C2 C1 N1 C9 0.2(17) . . . . ?
C2 C1 N1 Er1 -172.8(9) . . . . ?
C8 C9 N1 C1 180.0(10) . . . . ?
C4 C9 N1 C1 -0.8(15) . . . . ?
C8 C9 N1 Er1 -7.0(12) . . . . ?
C4 C9 N1 Er1 172.2(7) . . . . ?
O5 Er1 N1 C1 104.7(9) . . . . ?
O1W Er1 N1 C1 24.7(9) . . . . ?
O2 Er1 N1 C1 176.9(8) . . . . ?
O16 Er1 N1 C1 -115.5(9) 4_576 . . . ?
O15 Er1 N1 C1 -51.4(9) 4_576 . . . ?
O4 Er1 N1 C1 82.9(9) . . . . ?
O1 Er1 N1 C1 179.4(9) . . . . ?
N2 Er1 N1 C1 -28.9(11) . . . . ?
O5 Er1 N1 C9 -68.1(7) . . . . ?
O1W Er1 N1 C9 -148.1(7) . . . . ?
O2 Er1 N1 C9 4.0(8) . . . . ?
O16 Er1 N1 C9 71.7(7) 4_576 . . . ?
O15 Er1 N1 C9 135.8(7) 4_576 . . . ?
O4 Er1 N1 C9 -89.9(7) . . . . ?
O1 Er1 N1 C9 6.5(6) . . . . ?
N2 Er1 N1 C9 158.3(6) . . . . ?
C13 C12 N2 C20 -1.0(17) . . . . ?
C13 C12 N2 Er1 -171.6(9) . . . . ?
C19 C20 N2 C12 177.0(10) . . . . ?
C15 C20 N2 C12 -3.1(14) . . . . ?
C19 C20 N2 Er1 -12.1(12) . . . . ?
C15 C20 N2 Er1 167.8(7) . . . . ?
O5 Er1 N2 C12 -163.2(8) . . . . ?
O1W Er1 N2 C12 -95.3(9) . . . . ?
O2 Er1 N2 C12 118.2(9) . . . . ?
O16 Er1 N2 C12 45.9(9) 4_576 . . . ?
O15 Er1 N2 C12 -18.6(8) 4_576 . . . ?
O4 Er1 N2 C12 -175.3(9) . . . . ?
O1 Er1 N2 C12 92.0(9) . . . . ?
N1 Er1 N2 C12 -40.4(10) . . . . ?
O5 Er1 N2 C20 26.3(8) . . . . ?
O1W Er1 N2 C20 94.2(7) . . . . ?
O2 Er1 N2 C20 -52.3(7) . . . . ?
O16 Er1 N2 C20 -124.5(7) 4_576 . . . ?
O15 Er1 N2 C20 170.9(7) 4_576 . . . ?
O4 Er1 N2 C20 14.2(6) . . . . ?
O1 Er1 N2 C20 -78.5(8) . . . . ?
N1 Er1 N2 C20 149.1(6) . . . . ?
C24 C23 N3 C31 -1.6(16) . . . . ?
C24 C23 N3 Er2 170.5(8) . . . . ?
C30 C31 N3 C23 -178.5(10) . . . . ?
C26 C31 N3 C23 0.6(15) . . . . ?
C30 C31 N3 Er2 9.5(12) . . . . ?
C26 C31 N3 Er2 -171.4(7) . . . . ?
O11 Er2 N3 C23 -101.5(8) . . . . ?
O8 Er2 N3 C23 -178.2(8) . . . . ?
O3 Er2 N3 C23 -24.4(8) . . . . ?
O14 Er2 N3 C23 114.5(8) . . . . ?
O13 Er2 N3 C23 48.9(8) . . . . ?
O10 Er2 N3 C23 -78.1(9) . . . . ?
O7 Er2 N3 C23 -178.2(9) . . . . ?
N4 Er2 N3 C23 50.1(11) . . . . ?
O11 Er2 N3 C31 70.3(7) . . . . ?
O8 Er2 N3 C31 -6.4(8) . . . . ?
O3 Er2 N3 C31 147.5(7) . . . . ?
O14 Er2 N3 C31 -73.6(7) . . . . ?
O13 Er2 N3 C31 -139.3(7) . . . . ?
O10 Er2 N3 C31 93.8(8) . . . . ?
O7 Er2 N3 C31 -6.4(7) . . . . ?
N4 Er2 N3 C31 -138.1(7) . . . . ?
C35 C34 N4 C42 1.0(15) . . . . ?
C35 C34 N4 Er2 176.2(8) . . . . ?
C37 C42 N4 C34 -0.3(13) . . . . ?
C41 C42 N4 C34 -179.2(9) . . . . ?
C37 C42 N4 Er2 -175.6(6) . . . . ?
C41 C42 N4 Er2 5.6(11) . . . . ?
O11 Er2 N4 C34 -177.3(7) . . . . ?
O8 Er2 N4 C34 -102.6(8) . . . . ?
O3 Er2 N4 C34 110.1(8) . . . . ?
O14 Er2 N4 C34 -26.7(8) . . . . ?
O13 Er2 N4 C34 38.0(8) . . . . ?
O10 Er2 N4 C34 179.5(8) . . . . ?
N3 Er2 N4 C34 36.8(11) . . . . ?
O7 Er2 N4 C34 -78.3(8) . . . . ?
O11 Er2 N4 C42 -2.3(7) . . . . ?
O8 Er2 N4 C42 72.4(6) . . . . ?
O3 Er2 N4 C42 -74.9(6) . . . . ?
O14 Er2 N4 C42 148.3(7) . . . . ?
O13 Er2 N4 C42 -147.0(7) . . . . ?
O10 Er2 N4 C42 -5.4(6) . . . . ?
N3 Er2 N4 C42 -148.1(6) . . . . ?
O7 Er2 N4 C42 96.8(7) . . . . ?
C7 C8 O1 C10 0.3(15) . . . . ?
C9 C8 O1 C10 -179.6(9) . . . . ?
C7 C8 O1 Er1 -174.7(9) . . . . ?
C9 C8 O1 Er1 5.3(11) . . . . ?
C11 C10 O1 C8 -174.9(8) . . . . ?
C11 C10 O1 Er1 0.4(11) . . . . ?
O5 Er1 O1 C8 80.9(7) . . . . ?
O1W Er1 O1 C8 31.8(8) . . . . ?
O2 Er1 O1 C8 171.4(7) . . . . ?
O16 Er1 O1 C8 -107.5(7) 4_576 . . . ?
O15 Er1 O1 C8 -58.4(7) 4_576 . . . ?
O4 Er1 O1 C8 126.7(7) . . . . ?
N1 Er1 O1 C8 -6.2(7) . . . . ?
N2 Er1 O1 C8 -158.6(6) . . . . ?
O5 Er1 O1 C10 -93.9(7) . . . . ?
O1W Er1 O1 C10 -143.1(7) . . . . ?
O2 Er1 O1 C10 -3.5(7) . . . . ?
O16 Er1 O1 C10 77.6(7) 4_576 . . . ?
O15 Er1 O1 C10 126.7(7) 4_576 . . . ?
O4 Er1 O1 C10 -48.1(7) . . . . ?
N1 Er1 O1 C10 178.9(8) . . . . ?
N2 Er1 O1 C10 26.5(9) . . . . ?
O3 C11 O2 Er1 171.2(7) . . . . ?
C10 C11 O2 Er1 -11.0(12) . . . . ?
O5 Er1 O2 C11 81.0(8) . . . . ?
O1W Er1 O2 C11 139.3(7) . . . . ?
O16 Er1 O2 C11 -65.7(8) 4_576 . . . ?
O15 Er1 O2 C11 -85.9(8) 4_576 . . . ?
O4 Er1 O2 C11 144.8(8) . . . . ?
O1 Er1 O2 C11 8.0(7) . . . . ?
N1 Er1 O2 C11 10.5(8) . . . . ?
N2 Er1 O2 C11 -155.8(8) . . . . ?
O2 C11 O3 Er2 175.7(7) . . . . ?
C10 C11 O3 Er2 -2.2(16) . . . . ?
O11 Er2 O3 C11 -135.8(11) . . . . ?
O8 Er2 O3 C11 -74.9(12) . . . . ?
O14 Er2 O3 C11 73.7(12) . . . . ?
O13 Er2 O3 C11 67.8(11) . . . . ?
O10 Er2 O3 C11 -69.8(11) . . . . ?
N3 Er2 O3 C11 145.0(11) . . . . ?
O7 Er2 O3 C11 178.1(10) . . . . ?
N4 Er2 O3 C11 -10.4(11) . . . . ?
C18 C19 O4 C21 -2.0(15) . . . . ?
C20 C19 O4 C21 179.7(9) . . . . ?
C18 C19 O4 Er1 -163.9(8) . . . . ?
C20 C19 O4 Er1 17.7(11) . . . . ?
C22 C21 O4 C19 178.7(9) . . . . ?
C22 C21 O4 Er1 -18.5(11) . . . . ?
O5 Er1 O4 C19 174.8(7) . . . . ?
O1W Er1 O4 C19 -100.3(7) . . . . ?
O2 Er1 O4 C19 83.0(7) . . . . ?
O16 Er1 O4 C19 43.5(7) 4_576 . . . ?
O15 Er1 O4 C19 -48.5(8) 4_576 . . . ?
O1 Er1 O4 C19 125.0(6) . . . . ?
N1 Er1 O4 C19 -161.0(6) . . . . ?
N2 Er1 O4 C19 -16.7(6) . . . . ?
O5 Er1 O4 C21 12.9(7) . . . . ?
O1W Er1 O4 C21 97.8(7) . . . . ?
O2 Er1 O4 C21 -78.9(7) . . . . ?
O16 Er1 O4 C21 -118.4(7) 4_576 . . . ?
O15 Er1 O4 C21 149.6(6) 4_576 . . . ?
O1 Er1 O4 C21 -36.9(7) . . . . ?
N1 Er1 O4 C21 37.1(8) . . . . ?
N2 Er1 O4 C21 -178.6(7) . . . . ?
O6 C22 O5 Er1 175.8(9) . . . . ?
C21 C22 O5 Er1 -3.4(16) . . . . ?
O1W Er1 O5 C22 -84.0(10) . . . . ?
O2 Er1 O5 C22 64.9(10) . . . . ?
O16 Er1 O5 C22 116.3(10) 4_576 . . . ?
O15 Er1 O5 C22 -130.3(9) 4_576 . . . ?
O4 Er1 O5 C22 -5.0(9) . . . . ?
O1 Er1 O5 C22 128.1(10) . . . . ?
N1 Er1 O5 C22 -168.8(10) . . . . ?
N2 Er1 O5 C22 -16.9(11) . . . . ?
C29 C30 O7 C32 -7.3(15) . . . . ?
C31 C30 O7 C32 175.5(9) . . . . ?
C29 C30 O7 Er2 177.0(8) . . . . ?
C31 C30 O7 Er2 -0.2(12) . . . . ?
C33 C32 O7 C30 175.4(8) . . . . ?
C33 C32 O7 Er2 -8.6(11) . . . . ?
O11 Er2 O7 C30 -82.7(7) . . . . ?
O8 Er2 O7 C30 -176.7(8) . . . . ?
O3 Er2 O7 C30 -35.6(8) . . . . ?
O14 Er2 O7 C30 97.8(7) . . . . ?
O13 Er2 O7 C30 56.0(8) . . . . ?
O10 Er2 O7 C30 -128.0(7) . . . . ?
N3 Er2 O7 C30 3.3(7) . . . . ?
N4 Er2 O7 C30 156.4(7) . . . . ?
O11 Er2 O7 C32 101.6(7) . . . . ?
O8 Er2 O7 C32 7.6(6) . . . . ?
O3 Er2 O7 C32 148.7(6) . . . . ?
O14 Er2 O7 C32 -77.9(7) . . . . ?
O13 Er2 O7 C32 -119.6(7) . . . . ?
O10 Er2 O7 C32 56.3(7) . . . . ?
N3 Er2 O7 C32 -172.4(7) . . . . ?
N4 Er2 O7 C32 -19.2(8) . . . . ?
O9 C33 O8 Er2 -173.0(7) . . . . ?
C32 C33 O8 Er2 4.4(13) . . . . ?
O11 Er2 O8 C33 -79.4(8) . . . . ?
O3 Er2 O8 C33 -137.8(8) . . . . ?
O14 Er2 O8 C33 63.9(8) . . . . ?
O13 Er2 O8 C33 95.0(8) . . . . ?
O10 Er2 O8 C33 -142.8(8) . . . . ?
N3 Er2 O8 C33 -6.6(9) . . . . ?
O7 Er2 O8 C33 -6.6(8) . . . . ?
N4 Er2 O8 C33 154.0(9) . . . . ?
C40 C41 O10 C43 1.6(14) . . . . ?
C42 C41 O10 C43 -179.9(9) . . . . ?
C40 C41 O10 Er2 176.6(8) . . . . ?
C42 C41 O10 Er2 -4.9(10) . . . . ?
C44 C43 O10 C41 176.5(8) . . . . ?
C44 C43 O10 Er2 1.1(12) . . . . ?
O11 Er2 O10 C41 -171.7(7) . . . . ?
O8 Er2 O10 C41 -78.2(7) . . . . ?
O3 Er2 O10 C41 104.9(7) . . . . ?
O14 Er2 O10 C41 -36.7(8) . . . . ?
O13 Er2 O10 C41 53.3(7) . . . . ?
N3 Er2 O10 C41 162.4(6) . . . . ?
O7 Er2 O10 C41 -122.3(6) . . . . ?
N4 Er2 O10 C41 5.4(6) . . . . ?
O11 Er2 O10 C43 3.3(7) . . . . ?
O8 Er2 O10 C43 96.8(8) . . . . ?
O3 Er2 O10 C43 -80.1(8) . . . . ?
O14 Er2 O10 C43 138.3(7) . . . . ?
O13 Er2 O10 C43 -131.7(7) . . . . ?
N3 Er2 O10 C43 -22.6(9) . . . . ?
O7 Er2 O10 C43 52.7(8) . . . . ?
N4 Er2 O10 C43 -179.7(8) . . . . ?
O12 C44 O11 Er2 -166.2(9) . . . . ?
C43 C44 O11 Er2 14.3(14) . . . . ?
O8 Er2 O11 C44 -83.1(9) . . . . ?
O3 Er2 O11 C44 66.2(9) . . . . ?
O14 Er2 O11 C44 -144.8(8) . . . . ?
O13 Er2 O11 C44 103.3(9) . . . . ?
O10 Er2 O11 C44 -9.9(8) . . . . ?
N3 Er2 O11 C44 152.6(9) . . . . ?
O7 Er2 O11 C44 -145.4(9) . . . . ?
N4 Er2 O11 C44 -13.0(10) . . . . ?
O15 C45 O13 Er2 -168.7(9) . . . . ?
C46 C45 O13 Er2 12.4(11) . . . . ?
O11 Er2 O13 C45 119.7(7) . . . . ?
O8 Er2 O13 C45 -51.4(8) . . . . ?
O3 Er2 O13 C45 157.7(7) . . . . ?
O14 Er2 O13 C45 -17.9(7) . . . . ?
O10 Er2 O13 C45 -151.0(6) . . . . ?
N3 Er2 O13 C45 69.8(7) . . . . ?
O7 Er2 O13 C45 24.6(7) . . . . ?
N4 Er2 O13 C45 -109.6(7) . . . . ?
O16 C46 O14 Er2 152.9(9) . . . . ?
C45 C46 O14 Er2 -25.5(11) . . . . ?
O11 Er2 O14 C46 -116.6(8) . . . . ?
O8 Er2 O14 C46 178.5(8) . . . . ?
O3 Er2 O14 C46 16.7(10) . . . . ?
O13 Er2 O14 C46 22.9(7) . . . . ?
O10 Er2 O14 C46 137.6(7) . . . . ?
N3 Er2 O14 C46 -55.2(8) . . . . ?
O7 Er2 O14 C46 -115.8(8) . . . . ?
N4 Er2 O14 C46 101.8(8) . . . . ?
O13 C45 O15 Er1 -167.8(8) . . . 4_575 ?
C46 C45 O15 Er1 11.1(11) . . . 4_575 ?
O14 C46 O16 Er1 154.8(9) . . . 4_575 ?
C45 C46 O16 Er1 -26.8(12) . . . 4_575 ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         2.724
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.198

#===END
data_2dsm
_database_code_depnum_ccdc_archive 'CCDC 717622'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C52 H38 N4 O17 Sm2, 4(H2 O)'
_chemical_formula_sum            'C52 H46 N4 O21 Sm2'
_chemical_formula_weight         1363.63

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 2/c'
_symmetry_space_group_name_HALL  '-P 2yc'

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

_cell_length_a                   12.3342(3)
_cell_length_b                   11.3752(3)
_cell_length_c                   19.0229(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.810(2)
_cell_angle_gamma                90.00
_cell_volume                     2591.83(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    6111
_cell_measurement_theta_min      1.70
_cell_measurement_theta_max      27.92

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1356
_exptl_absorpt_coefficient_mu    2.329
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5216
_exptl_absorpt_correction_T_max  0.6330
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19266
_diffrn_reflns_av_R_equivalents  0.0513
_diffrn_reflns_av_sigmaI/netI    0.0537
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5081
_reflns_number_gt                3790
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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)+(0.0383P)²+0.6004P] where P=(Fo²+2Fc²)/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         5081
_refine_ls_number_parameters     360
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0332
_refine_ls_wR_factor_ref         0.0815
_refine_ls_wR_factor_gt          0.0738
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.026
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C -0.0206(5) 0.8051(5) 0.4057(4) 0.0570(17) Uani 1 1 d . . .
H1 H -0.0750 0.7673 0.3707 0.068 Uiso 1 1 calc R . .
C2 C -0.0010(5) 0.7647(6) 0.4773(4) 0.0625(18) Uani 1 1 d . . .
H2 H -0.0406 0.7007 0.4888 0.075 Uiso 1 1 calc R . .
C3 C 0.0751(5) 0.8192(5) 0.5290(4) 0.0580(17) Uani 1 1 d . . .
H3 H 0.0883 0.7933 0.5767 0.070 Uiso 1 1 calc R . .
C4 C 0.1348(4) 0.9149(4) 0.5115(3) 0.0411(13) Uani 1 1 d . . .
C5 C 0.2148(6) 0.9762(5) 0.5638(4) 0.0658(18) Uani 1 1 d . . .
H5 H 0.2289 0.9539 0.6122 0.079 Uiso 1 1 calc R . .
C6 C 0.2708(7) 1.0667(6) 0.5440(4) 0.082(2) Uani 1 1 d . . .
H6 H 0.3242 1.1061 0.5788 0.099 Uiso 1 1 calc R . .
C7 C 0.2497(5) 1.1026(5) 0.4709(4) 0.0595(17) Uani 1 1 d . . .
H7 H 0.2894 1.1652 0.4580 0.071 Uiso 1 1 calc R . .
C8 C 0.1717(4) 1.0465(4) 0.4192(3) 0.0349(12) Uani 1 1 d . . .
C9 C 0.1124(4) 0.9496(4) 0.4385(3) 0.0311(11) Uani 1 1 d . . .
C10 C 0.1680(4) 1.1932(4) 0.3285(3) 0.0374(13) Uani 1 1 d . . .
H10A H 0.2480 1.2068 0.3414 0.045 Uiso 1 1 calc R . .
H10B H 0.1332 1.2486 0.3550 0.045 Uiso 1 1 calc R . .
C11 C 0.1233(4) 1.2111(4) 0.2482(3) 0.0327(12) Uani 1 1 d . . .
C12 C 0.7020(4) 0.5818(4) 0.3927(3) 0.0367(12) Uani 1 1 d . . .
H12 H 0.7341 0.5736 0.3534 0.044 Uiso 1 1 calc R . .
C13 C 0.7606(4) 0.5392(4) 0.4597(3) 0.0434(14) Uani 1 1 d . . .
H13 H 0.8292 0.5022 0.4643 0.052 Uiso 1 1 calc R . .
C14 C 0.7169(5) 0.5523(4) 0.5180(3) 0.0456(14) Uani 1 1 d . . .
H14 H 0.7553 0.5239 0.5630 0.055 Uiso 1 1 calc R . .
C15 C 0.6130(4) 0.6088(4) 0.5107(3) 0.0349(12) Uani 1 1 d . . .
C16 C 0.5656(5) 0.6303(5) 0.5696(3) 0.0497(14) Uani 1 1 d . . .
H16 H 0.6016 0.6045 0.6156 0.060 Uiso 1 1 calc R . .
C17 C 0.4671(5) 0.6887(5) 0.5594(3) 0.0527(15) Uani 1 1 d . . .
H17 H 0.4378 0.7063 0.5989 0.063 Uiso 1 1 calc R . .
C18 C 0.4088(5) 0.7229(4) 0.4891(3) 0.0440(14) Uani 1 1 d . . .
H18 H 0.3405 0.7612 0.4826 0.053 Uiso 1 1 calc R . .
C19 C 0.4518(4) 0.7002(3) 0.4308(3) 0.0303(11) Uani 1 1 d . . .
C20 C 0.5578(4) 0.6457(3) 0.4403(3) 0.0270(10) Uani 1 1 d . . .
C21 C 0.3017(4) 0.7963(4) 0.3480(3) 0.0345(12) Uani 1 1 d . . .
H21A H 0.3196 0.8715 0.3720 0.041 Uiso 1 1 calc R . .
H21B H 0.2451 0.7584 0.3678 0.041 Uiso 1 1 calc R . .
C22 C 0.2586(4) 0.8146(3) 0.2683(3) 0.0297(11) Uani 1 1 d . . .
C23 C 0.5000 0.4637(5) 0.2500 0.0243(14) Uani 1 2 d S . .
C24 C 0.5000 0.3348(4) 0.2500 0.0192(13) Uani 1 2 d S . .
C25 C 0.4001(4) 0.2726(3) 0.2428(3) 0.0303(11) Uani 1 1 d . . .
H25 H 0.3333 0.3130 0.2381 0.036 Uiso 1 1 calc R . .
C26 C 0.4007(4) 0.1511(3) 0.2425(3) 0.0326(12) Uani 1 1 d . . .
H26 H 0.3342 0.1098 0.2372 0.039 Uiso 1 1 calc R . .
C27 C 0.5000 0.0910(5) 0.2500 0.0321(17) Uani 1 2 d S . .
C28 C 0.5000 -0.0419(5) 0.2500 0.0295(16) Uani 1 2 d S . .
N1 N 0.0346(3) 0.8948(3) 0.3848(2) 0.0344(10) Uani 1 1 d . . .
N2 N 0.6027(3) 0.6334(3) 0.3820(2) 0.0301(9) Uani 1 1 d . . .
O1 O 0.1444(3) 1.0743(3) 0.34710(19) 0.0324(8) Uani 1 1 d . . .
O2 O 0.0863(3) 1.1231(3) 0.2099(2) 0.0371(8) Uani 1 1 d . . .
O3 O 0.1294(3) 1.3129(3) 0.2256(2) 0.0484(10) Uani 1 1 d . . .
O4 O 0.3997(3) 0.7243(2) 0.36038(19) 0.0305(8) Uani 1 1 d . . .
O5 O 0.3072(2) 0.7678(3) 0.2253(2) 0.0336(8) Uani 1 1 d . . .
O6 O 0.1734(3) 0.8778(3) 0.2506(2) 0.0436(9) Uani 1 1 d . . .
O7 O 0.4174(2) 0.5188(2) 0.26370(19) 0.0279(8) Uani 1 1 d . . .
O8 O 0.5066(3) -0.0940(2) 0.3090(2) 0.0372(8) Uani 1 1 d . . .
O1W O 0.0000 0.7156(4) 0.2500 0.0612(17) Uani 1 2 d S . .
H1W H 0.0606 0.6799 0.2504 0.092 Uiso 1 1 d R . .
O2W O 0.1825(3) 0.5373(3) 0.2877(3) 0.0673(13) Uani 1 1 d . . .
H4W H 0.1723 0.4674 0.2724 0.101 Uiso 1 1 d R . .
H3W H 0.2482 0.5570 0.2857 0.101 Uiso 1 1 d R . .
O3W O -0.0022(5) 0.4539(6) 0.1148(4) 0.125(2) Uani 1 1 d . . .
H5W H 0.0403 0.4138 0.1476 0.187 Uiso 1 1 d R . .
H6W H 0.0279 0.4642 0.0796 0.187 Uiso 1 1 d R . .
Sm1 Sm 0.0000 0.95671(3) 0.2500 0.02453(10) Uani 1 2 d S . .
Sm2 Sm 0.5000 0.71084(2) 0.2500 0.02065(10) Uani 1 2 d S . .


_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
C1 N1 1.339(6) . ?
C1 C2 1.403(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.339(9) . ?
C2 H2 0.9300 . ?
C3 C4 1.399(7) . ?
C3 H3 0.9300 . ?
C4 C9 1.406(7) . ?
C4 C5 1.408(8) . ?
C5 C6 1.343(9) . ?
C5 H5 0.9300 . ?
C6 C7 1.413(9) . ?
C6 H6 0.9300 . ?
C7 C8 1.359(7) . ?
C7 H7 0.9300 . ?
C8 O1 1.369(6) . ?
C8 C9 1.419(6) . ?
C9 N1 1.372(6) . ?
C10 O1 1.445(5) . ?
C10 C11 1.509(8) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 O3 1.243(5) . ?
C11 O2 1.258(6) . ?
C12 N2 1.330(6) . ?
C12 C13 1.393(8) . ?
C12 H12 0.9300 . ?
C13 C14 1.353(8) . ?
C13 H13 0.9300 . ?
C14 C15 1.410(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.403(8) . ?
C15 C20 1.413(7) . ?
C16 C17 1.357(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.412(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.364(7) . ?
C18 H18 0.9300 . ?
C19 O4 1.368(6) . ?
C19 C20 1.419(6) . ?
C20 N2 1.360(6) . ?
C21 O4 1.432(5) . ?
C21 C22 1.497(7) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 O5 1.245(5) . ?
C22 O6 1.250(5) . ?
C23 O7 1.275(4) . ?
C23 C24 1.467(7) . ?
C24 C25 1.399(5) . ?
C25 C26 1.383(6) . ?
C25 H25 0.9300 . ?
C26 C27 1.379(5) . ?
C26 H26 0.9300 . ?
C27 C28 1.512(8) . ?
C28 O8 1.254(4) . ?
N1 Sm1 2.595(4) . ?
N2 Sm2 2.677(4) . ?
O1 Sm1 2.608(3) . ?
O2 Sm1 2.384(3) . ?
O4 Sm2 2.684(3) . ?
O5 Sm2 2.401(3) . ?
O6 Sm1 2.318(3) . ?
O7 Sm2 2.450(3) . ?
O8 Sm2 2.481(3) 1_545 ?
O1W Sm1 2.743(5) . ?
O1W H1W 0.8490 . ?
O2W H4W 0.8456 . ?
O2W H3W 0.8501 . ?
O3W H5W 0.8465 . ?
O3W H6W 0.8468 . ?

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
N1 C1 C2 123.8(6) . . ?
N1 C1 H1 118.1 . . ?
C2 C1 H1 118.1 . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.1(6) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C9 117.6(5) . . ?
C3 C4 C5 122.4(6) . . ?
C9 C4 C5 119.9(5) . . ?
C6 C5 C4 120.1(6) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 120.8(6) . . ?
C5 C6 H6 119.6 . . ?
C7 C6 H6 119.6 . . ?
C8 C7 C6 120.6(6) . . ?
C8 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C7 C8 O1 125.3(5) . . ?
C7 C8 C9 119.8(5) . . ?
O1 C8 C9 114.8(4) . . ?
N1 C9 C4 123.0(4) . . ?
N1 C9 C8 118.2(5) . . ?
C4 C9 C8 118.8(5) . . ?
O1 C10 C11 109.2(4) . . ?
O1 C10 H10A 109.8 . . ?
C11 C10 H10A 109.8 . . ?
O1 C10 H10B 109.8 . . ?
C11 C10 H10B 109.8 . . ?
H10A C10 H10B 108.3 . . ?
O3 C11 O2 125.8(5) . . ?
O3 C11 C10 116.0(4) . . ?
O2 C11 C10 118.2(4) . . ?
N2 C12 C13 123.5(5) . . ?
N2 C12 H12 118.3 . . ?
C13 C12 H12 118.3 . . ?
C14 C13 C12 119.4(5) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 120.0(5) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 122.9(5) . . ?
C16 C15 C20 120.4(5) . . ?
C14 C15 C20 116.7(5) . . ?
C17 C16 C15 120.1(6) . . ?
C17 C16 H16 120.0 . . ?
C15 C16 H16 120.0 . . ?
C16 C17 C18 120.4(6) . . ?
C16 C17 H17 119.8 . . ?
C18 C17 H17 119.8 . . ?
C19 C18 C17 120.6(5) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C18 C19 O4 125.1(4) . . ?
C18 C19 C20 120.3(5) . . ?
O4 C19 C20 114.6(4) . . ?
N2 C20 C15 123.0(4) . . ?
N2 C20 C19 118.8(4) . . ?
C15 C20 C19 118.1(5) . . ?
O4 C21 C22 109.1(4) . . ?
O4 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
O4 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
O5 C22 O6 125.0(5) . . ?
O5 C22 C21 119.8(4) . . ?
O6 C22 C21 115.2(4) . . ?
O7 C23 O7 121.1(5) 2_655 . ?
O7 C23 C24 119.4(2) 2_655 . ?
O7 C23 C24 119.4(2) . . ?
C25 C24 C25 119.2(5) 2_655 . ?
C25 C24 C23 120.4(2) 2_655 . ?
C25 C24 C23 120.4(2) . . ?
C26 C25 C24 120.0(4) . . ?
C26 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C26 C27 C26 120.7(5) 2_655 . ?
C26 C27 C28 119.7(3) 2_655 . ?
C26 C27 C28 119.7(3) . . ?
O8 C28 O8 123.7(5) 2_655 . ?
O8 C28 C27 118.2(3) 2_655 . ?
O8 C28 C27 118.2(3) . . ?
O8 C28 Sm2 61.8(3) 2_655 1_545 ?
O8 C28 Sm2 61.8(3) . 1_545 ?
C27 C28 Sm2 180.0 . 1_545 ?
C1 N1 C9 116.1(5) . . ?
C1 N1 Sm1 121.7(4) . . ?
C9 N1 Sm1 122.2(3) . . ?
C12 N2 C20 117.4(4) . . ?
C12 N2 Sm2 120.1(3) . . ?
C20 N2 Sm2 122.5(3) . . ?
C8 O1 C10 116.5(4) . . ?
C8 O1 Sm1 123.6(3) . . ?
C10 O1 Sm1 116.7(3) . . ?
C11 O2 Sm1 125.1(3) . . ?
C19 O4 C21 117.2(4) . . ?
C19 O4 Sm2 123.9(3) . . ?
C21 O4 Sm2 115.6(3) . . ?
C22 O5 Sm2 126.6(3) . . ?
C22 O6 Sm1 159.8(3) . . ?
C23 O7 Sm2 92.5(3) . . ?
C28 O8 Sm2 91.7(3) . 1_545 ?
Sm1 O1W H1W 118.6 . . ?
H4W O2W H3W 107.3 . . ?
H5W O3W H6W 110.2 . . ?
O6 Sm1 O6 134.42(17) . 2 ?
O6 Sm1 O2 80.03(12) . . ?
O6 Sm1 O2 142.00(12) 2 . ?
O6 Sm1 O2 142.00(12) . 2 ?
O6 Sm1 O2 80.03(11) 2 2 ?
O2 Sm1 O2 74.93(15) . 2 ?
O6 Sm1 N1 80.41(13) . 2 ?
O6 Sm1 N1 87.50(13) 2 2 ?
O2 Sm1 N1 83.08(12) . 2 ?
O2 Sm1 N1 123.44(12) 2 2 ?
O6 Sm1 N1 87.50(13) . . ?
O6 Sm1 N1 80.41(13) 2 . ?
O2 Sm1 N1 123.44(12) . . ?
O2 Sm1 N1 83.08(12) 2 . ?
N1 Sm1 N1 148.53(17) 2 . ?
O6 Sm1 O1 73.85(11) . . ?
O6 Sm1 O1 132.50(12) 2 . ?
O2 Sm1 O1 62.48(11) . . ?
O2 Sm1 O1 69.37(11) 2 . ?
N1 Sm1 O1 139.68(11) 2 . ?
N1 Sm1 O1 61.04(11) . . ?
O6 Sm1 O1 132.50(12) . 2 ?
O6 Sm1 O1 73.85(11) 2 2 ?
O2 Sm1 O1 69.37(11) . 2 ?
O2 Sm1 O1 62.48(11) 2 2 ?
N1 Sm1 O1 61.04(11) 2 2 ?
N1 Sm1 O1 139.68(11) . 2 ?
O1 Sm1 O1 118.28(13) . 2 ?
O6 Sm1 O1W 67.21(9) . . ?
O6 Sm1 O1W 67.21(8) 2 . ?
O2 Sm1 O1W 142.54(8) . . ?
O2 Sm1 O1W 142.54(8) 2 . ?
N1 Sm1 O1W 74.27(8) 2 . ?
N1 Sm1 O1W 74.27(8) . . ?
O1 Sm1 O1W 120.86(7) . . ?
O1 Sm1 O1W 120.86(7) 2 . ?
O5 Sm2 O5 148.70(14) 2_655 . ?
O5 Sm2 O7 129.59(10) 2_655 . ?
O5 Sm2 O7 81.00(10) . . ?
O5 Sm2 O7 81.00(10) 2_655 2_655 ?
O5 Sm2 O7 129.59(10) . 2_655 ?
O7 Sm2 O7 53.90(13) . 2_655 ?
O5 Sm2 O8 76.78(11) 2_655 2_665 ?
O5 Sm2 O8 75.28(11) . 2_665 ?
O7 Sm2 O8 151.22(11) . 2_665 ?
O7 Sm2 O8 136.00(11) 2_655 2_665 ?
O5 Sm2 O8 75.28(11) 2_655 1_565 ?
O5 Sm2 O8 76.78(11) . 1_565 ?
O7 Sm2 O8 136.00(11) . 1_565 ?
O7 Sm2 O8 151.22(11) 2_655 1_565 ?
O8 Sm2 O8 52.95(16) 2_665 1_565 ?
O5 Sm2 N2 119.83(12) 2_655 2_655 ?
O5 Sm2 N2 71.34(11) . 2_655 ?
O7 Sm2 N2 71.99(11) . 2_655 ?
O7 Sm2 N2 73.90(11) 2_655 2_655 ?
O8 Sm2 N2 85.01(11) 2_665 2_655 ?
O8 Sm2 N2 132.53(11) 1_565 2_655 ?
O5 Sm2 N2 71.34(11) 2_655 . ?
O5 Sm2 N2 119.83(12) . . ?
O7 Sm2 N2 73.90(11) . . ?
O7 Sm2 N2 71.99(11) 2_655 . ?
O8 Sm2 N2 132.53(11) 2_665 . ?
O8 Sm2 N2 85.01(11) 1_565 . ?
N2 Sm2 N2 141.59(15) 2_655 . ?
O5 Sm2 O4 61.17(11) 2_655 2_655 ?
O5 Sm2 O4 116.83(11) . 2_655 ?
O7 Sm2 O4 114.53(9) . 2_655 ?
O7 Sm2 O4 71.73(9) 2_655 2_655 ?
O8 Sm2 O4 64.30(10) 2_665 2_655 ?
O8 Sm2 O4 109.36(10) 1_565 2_655 ?
N2 Sm2 O4 59.22(10) 2_655 2_655 ?
N2 Sm2 O4 123.32(11) . 2_655 ?
O5 Sm2 O4 116.83(11) 2_655 . ?
O5 Sm2 O4 61.17(11) . . ?
O7 Sm2 O4 71.73(10) . . ?
O7 Sm2 O4 114.53(9) 2_655 . ?
O8 Sm2 O4 109.36(10) 2_665 . ?
O8 Sm2 O4 64.30(10) 1_565 . ?
N2 Sm2 O4 123.32(11) 2_655 . ?
N2 Sm2 O4 59.22(10) . . ?
O4 Sm2 O4 173.46(12) 2_655 . ?
O5 Sm2 C28 74.35(7) 2_655 1_565 ?
O5 Sm2 C28 74.35(7) . 1_565 ?
O7 Sm2 C28 153.05(6) . 1_565 ?
O7 Sm2 C28 153.05(6) 2_655 1_565 ?
O8 Sm2 C28 26.47(8) 2_665 1_565 ?
O8 Sm2 C28 26.47(8) 1_565 1_565 ?
N2 Sm2 C28 109.20(7) 2_655 1_565 ?
N2 Sm2 C28 109.20(7) . 1_565 ?
O4 Sm2 C28 86.73(6) 2_655 1_565 ?
O4 Sm2 C28 86.73(6) . 1_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.5(11) . . . . ?
C1 C2 C3 C4 -0.4(10) . . . . ?
C2 C3 C4 C9 -0.7(9) . . . . ?
C2 C3 C4 C5 179.3(6) . . . . ?
C3 C4 C5 C6 179.2(7) . . . . ?
C9 C4 C5 C6 -0.9(10) . . . . ?
C4 C5 C6 C7 0.8(12) . . . . ?
C5 C6 C7 C8 0.3(12) . . . . ?
C6 C7 C8 O1 179.8(6) . . . . ?
C6 C7 C8 C9 -1.2(9) . . . . ?
C3 C4 C9 N1 0.8(7) . . . . ?
C5 C4 C9 N1 -179.2(5) . . . . ?
C3 C4 C9 C8 179.9(5) . . . . ?
C5 C4 C9 C8 0.0(7) . . . . ?
C7 C8 C9 N1 -179.8(5) . . . . ?
O1 C8 C9 N1 -0.6(6) . . . . ?
C7 C8 C9 C4 1.0(7) . . . . ?
O1 C8 C9 C4 -179.8(4) . . . . ?
O1 C10 C11 O3 174.0(4) . . . . ?
O1 C10 C11 O2 -7.8(6) . . . . ?
N2 C12 C13 C14 -1.4(8) . . . . ?
C12 C13 C14 C15 -0.2(8) . . . . ?
C13 C14 C15 C16 -176.8(5) . . . . ?
C13 C14 C15 C20 2.2(7) . . . . ?
C14 C15 C16 C17 177.8(5) . . . . ?
C20 C15 C16 C17 -1.2(8) . . . . ?
C15 C16 C17 C18 3.3(8) . . . . ?
C16 C17 C18 C19 -1.5(8) . . . . ?
C17 C18 C19 O4 176.6(5) . . . . ?
C17 C18 C19 C20 -2.3(7) . . . . ?
C16 C15 C20 N2 176.0(4) . . . . ?
C14 C15 C20 N2 -3.0(6) . . . . ?
C16 C15 C20 C19 -2.6(6) . . . . ?
C14 C15 C20 C19 178.4(4) . . . . ?
C18 C19 C20 N2 -174.4(4) . . . . ?
O4 C19 C20 N2 6.6(5) . . . . ?
C18 C19 C20 C15 4.3(6) . . . . ?
O4 C19 C20 C15 -174.7(4) . . . . ?
O4 C21 C22 O5 1.1(6) . . . . ?
O4 C21 C22 O6 -179.1(4) . . . . ?
O7 C23 C24 C25 19.5(3) 2_655 . . 2_655 ?
O7 C23 C24 C25 -160.5(3) . . . 2_655 ?
O7 C23 C24 C25 -160.5(3) 2_655 . . . ?
O7 C23 C24 C25 19.5(3) . . . . ?
C25 C24 C25 C26 -0.3(4) 2_655 . . . ?
C23 C24 C25 C26 179.7(4) . . . . ?
C24 C25 C26 C27 0.6(8) . . . . ?
C25 C26 C27 C26 -0.3(4) . . . 2_655 ?
C25 C26 C27 C28 179.7(4) . . . . ?
C26 C27 C28 O8 -86.9(3) 2_655 . . 2_655 ?
C26 C27 C28 O8 93.1(3) . . . 2_655 ?
C26 C27 C28 O8 93.1(3) 2_655 . . . ?
C26 C27 C28 O8 -86.9(3) . . . . ?
C2 C1 N1 C9 -1.3(9) . . . . ?
C2 C1 N1 Sm1 176.8(5) . . . . ?
C4 C9 N1 C1 0.2(7) . . . . ?
C8 C9 N1 C1 -179.0(5) . . . . ?
C4 C9 N1 Sm1 -177.9(3) . . . . ?
C8 C9 N1 Sm1 2.9(5) . . . . ?
C13 C12 N2 C20 0.7(7) . . . . ?
C13 C12 N2 Sm2 -180.0(4) . . . . ?
C15 C20 N2 C12 1.5(6) . . . . ?
C19 C20 N2 C12 -179.9(4) . . . . ?
C15 C20 N2 Sm2 -177.8(3) . . . . ?
C19 C20 N2 Sm2 0.8(5) . . . . ?
C7 C8 O1 C10 -23.5(7) . . . . ?
C9 C8 O1 C10 157.4(4) . . . . ?
C7 C8 O1 Sm1 177.2(4) . . . . ?
C9 C8 O1 Sm1 -2.0(5) . . . . ?
C11 C10 O1 C8 -174.9(4) . . . . ?
C11 C10 O1 Sm1 -14.1(5) . . . . ?
O3 C11 O2 Sm1 -151.2(4) . . . . ?
C10 C11 O2 Sm1 30.7(5) . . . . ?
C18 C19 O4 C21 11.1(6) . . . . ?
C20 C19 O4 C21 -169.9(4) . . . . ?
C18 C19 O4 Sm2 169.7(3) . . . . ?
C20 C19 O4 Sm2 -11.4(5) . . . . ?
C22 C21 O4 C19 178.8(3) . . . . ?
C22 C21 O4 Sm2 18.5(4) . . . . ?
O6 C22 O5 Sm2 154.7(3) . . . . ?
C21 C22 O5 Sm2 -25.5(6) . . . . ?
O5 C22 O6 Sm1 139.0(8) . . . . ?
C21 C22 O6 Sm1 -40.8(11) . . . . ?
O7 C23 O7 Sm2 0.0 2_655 . . . ?
C24 C23 O7 Sm2 180.0 . . . . ?
O8 C28 O8 Sm2 0.0 2_655 . . 1_545 ?
C27 C28 O8 Sm2 180.0 . . . 1_545 ?
C22 O6 Sm1 O6 -48.4(9) . . . 2 ?
C22 O6 Sm1 O2 150.2(10) . . . . ?
C22 O6 Sm1 O2 101.0(10) . . . 2 ?
C22 O6 Sm1 N1 -125.2(10) . . . 2 ?
C22 O6 Sm1 N1 25.6(10) . . . . ?
C22 O6 Sm1 O1 86.1(10) . . . . ?
C22 O6 Sm1 O1 -160.1(9) . . . 2 ?
C22 O6 Sm1 O1W -48.4(9) . . . . ?
C11 O2 Sm1 O6 -104.2(4) . . . . ?
C11 O2 Sm1 O6 97.5(4) . . . 2 ?
C11 O2 Sm1 O2 47.0(3) . . . 2 ?
C11 O2 Sm1 N1 174.4(4) . . . 2 ?
C11 O2 Sm1 N1 -23.9(4) . . . . ?
C11 O2 Sm1 O1 -27.3(3) . . . . ?
C11 O2 Sm1 O1 112.8(4) . . . 2 ?
C11 O2 Sm1 O1W -133.0(3) . . . . ?
C1 N1 Sm1 O6 -107.8(4) . . . . ?
C9 N1 Sm1 O6 70.2(3) . . . . ?
C1 N1 Sm1 O6 28.1(4) . . . 2 ?
C9 N1 Sm1 O6 -153.9(3) . . . 2 ?
C1 N1 Sm1 O2 175.9(4) . . . . ?
C9 N1 Sm1 O2 -6.1(4) . . . . ?
C1 N1 Sm1 O2 109.1(4) . . . 2 ?
C9 N1 Sm1 O2 -72.9(3) . . . 2 ?
C1 N1 Sm1 N1 -40.8(4) . . . 2 ?
C9 N1 Sm1 N1 137.3(3) . . . 2 ?
C1 N1 Sm1 O1 179.3(4) . . . . ?
C9 N1 Sm1 O1 -2.7(3) . . . . ?
C1 N1 Sm1 O1 78.7(4) . . . 2 ?
C9 N1 Sm1 O1 -103.3(3) . . . 2 ?
C1 N1 Sm1 O1W -40.8(4) . . . . ?
C9 N1 Sm1 O1W 137.3(3) . . . . ?
C8 O1 Sm1 O6 -93.8(3) . . . . ?
C10 O1 Sm1 O6 106.8(3) . . . . ?
C8 O1 Sm1 O6 42.5(4) . . . 2 ?
C10 O1 Sm1 O6 -116.9(3) . . . 2 ?
C8 O1 Sm1 O2 179.2(4) . . . . ?
C10 O1 Sm1 O2 19.8(3) . . . . ?
C8 O1 Sm1 O2 95.9(3) . . . 2 ?
C10 O1 Sm1 O2 -63.4(3) . . . 2 ?
C8 O1 Sm1 N1 -146.3(3) . . . 2 ?
C10 O1 Sm1 N1 54.4(3) . . . 2 ?
C8 O1 Sm1 N1 2.4(3) . . . . ?
C10 O1 Sm1 N1 -156.9(3) . . . . ?
C8 O1 Sm1 O1 136.2(3) . . . 2 ?
C10 O1 Sm1 O1 -23.2(3) . . . 2 ?
C8 O1 Sm1 O1W -43.8(3) . . . . ?
C10 O1 Sm1 O1W 156.8(3) . . . . ?
C22 O5 Sm2 O5 -69.8(3) . . . 2_655 ?
C22 O5 Sm2 O7 99.2(4) . . . . ?
C22 O5 Sm2 O7 124.4(3) . . . 2_655 ?
C22 O5 Sm2 O8 -97.2(3) . . . 2_665 ?
C22 O5 Sm2 O8 -42.5(3) . . . 1_565 ?
C22 O5 Sm2 N2 173.1(4) . . . 2_655 ?
C22 O5 Sm2 N2 33.7(4) . . . . ?
C22 O5 Sm2 O4 -147.8(3) . . . 2_655 ?
C22 O5 Sm2 O4 25.2(3) . . . . ?
C22 O5 Sm2 C28 -69.8(3) . . . 1_565 ?
C23 O7 Sm2 O5 -31.3(2) . . . 2_655 ?
C23 O7 Sm2 O5 156.08(19) . . . . ?
C23 O7 Sm2 O7 0.0 . . . 2_655 ?
C23 O7 Sm2 O8 121.4(2) . . . 2_665 ?
C23 O7 Sm2 O8 -143.75(16) . . . 1_565 ?
C23 O7 Sm2 N2 82.89(18) . . . 2_655 ?
C23 O7 Sm2 N2 -79.18(18) . . . . ?
C23 O7 Sm2 O4 40.6(2) . . . 2_655 ?
C23 O7 Sm2 O4 -141.4(2) . . . . ?
C23 O7 Sm2 C28 180.0 . . . 1_565 ?
C12 N2 Sm2 O5 -44.6(3) . . . 2_655 ?
C20 N2 Sm2 O5 134.7(3) . . . 2_655 ?
C12 N2 Sm2 O5 167.6(3) . . . . ?
C20 N2 Sm2 O5 -13.1(3) . . . . ?
C12 N2 Sm2 O7 98.3(3) . . . . ?
C20 N2 Sm2 O7 -82.4(3) . . . . ?
C12 N2 Sm2 O7 41.8(3) . . . 2_655 ?
C20 N2 Sm2 O7 -139.0(3) . . . 2_655 ?
C12 N2 Sm2 O8 -95.0(3) . . . 2_665 ?
C20 N2 Sm2 O8 84.3(3) . . . 2_665 ?
C12 N2 Sm2 O8 -120.7(3) . . . 1_565 ?
C20 N2 Sm2 O8 58.5(3) . . . 1_565 ?
C12 N2 Sm2 N2 70.2(3) . . . 2_655 ?
C20 N2 Sm2 N2 -110.5(3) . . . 2_655 ?
C12 N2 Sm2 O4 -10.8(4) . . . 2_655 ?
C20 N2 Sm2 O4 168.5(3) . . . 2_655 ?
C12 N2 Sm2 O4 176.3(3) . . . . ?
C20 N2 Sm2 O4 -4.4(3) . . . . ?
C12 N2 Sm2 C28 -109.8(3) . . . 1_565 ?
C20 N2 Sm2 C28 69.5(3) . . . 1_565 ?
C19 O4 Sm2 O5 -35.6(3) . . . 2_655 ?
C21 O4 Sm2 O5 123.2(3) . . . 2_655 ?
C19 O4 Sm2 O5 179.8(3) . . . . ?
C21 O4 Sm2 O5 -21.4(3) . . . . ?
C19 O4 Sm2 O7 90.2(3) . . . . ?
C21 O4 Sm2 O7 -111.0(3) . . . . ?
C19 O4 Sm2 O7 56.5(3) . . . 2_655 ?
C21 O4 Sm2 O7 -144.6(3) . . . 2_655 ?
C19 O4 Sm2 O8 -120.3(3) . . . 2_665 ?
C21 O4 Sm2 O8 38.6(3) . . . 2_665 ?
C19 O4 Sm2 O8 -91.6(3) . . . 1_565 ?
C21 O4 Sm2 O8 67.2(3) . . . 1_565 ?
C19 O4 Sm2 N2 142.8(3) . . . 2_655 ?
C21 O4 Sm2 N2 -58.4(3) . . . 2_655 ?
C19 O4 Sm2 N2 8.4(3) . . . . ?
C21 O4 Sm2 N2 167.2(3) . . . . ?
C19 O4 Sm2 C28 -106.3(3) . . . 1_565 ?
C21 O4 Sm2 C28 52.5(3) . . . 1_565 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C25 H25 O3 0.93 2.47 3.308(5) 150.3 1_545
O3W H5W O3 0.85 1.99 2.832(7) 175.4 1_545
O2W H3W O7 0.85 2.27 3.046(5) 152.5 .
O2W H4W O3 0.85 1.98 2.823(5) 171.5 1_545
O1W H1W O2W 0.85 2.21 2.987(5) 152.1 .

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.115

#===END

data_sm3d
_database_code_depnum_ccdc_archive 'CCDC 717623'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H12 N O7 Sm'
_chemical_formula_sum            'C19 H12 N O7 Sm'
_chemical_formula_weight         516.65

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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   10.8836(2)
_cell_length_b                   10.9362(2)
_cell_length_c                   15.8323(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.4440(10)
_cell_angle_gamma                90.00
_cell_volume                     1672.37(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3943
_cell_measurement_theta_min      2.11
_cell_measurement_theta_max      27.86

_exptl_crystal_description       block
_exptl_crystal_colour            pale-yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1004
_exptl_absorpt_coefficient_mu    3.557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4450
_exptl_absorpt_correction_T_max  0.5344
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15948
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0238
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.25
_reflns_number_total             3028
_reflns_number_gt                2641
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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)+(0.0232P)²+1.1077P] where P=(Fo²+2Fc²)/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         3028
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0198
_refine_ls_wR_factor_ref         0.0482
_refine_ls_wR_factor_gt          0.0455
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.088163(15) 0.510319(12) 0.157605(10) 0.01721(6) Uani 1 1 d . . .
O1 O 0.2416(2) 0.3786(2) 0.30471(16) 0.0309(5) Uani 1 1 d . . .
O2 O -0.0251(2) 0.3733(2) 0.22518(16) 0.0324(5) Uani 1 1 d . . .
O3 O -0.0349(3) 0.1786(2) 0.26615(17) 0.0368(6) Uani 1 1 d . . .
O4 O -0.2720(2) 0.5261(2) -0.11208(16) 0.0281(5) Uani 1 1 d . . .
O5 O -0.1409(2) 0.5271(2) 0.04521(16) 0.0308(5) Uani 1 1 d . . .
O6 O -0.0565(2) 0.68709(19) -0.08841(16) 0.0312(5) Uani 1 1 d . . .
O7 O 0.0877(2) 0.68127(19) 0.06751(16) 0.0302(5) Uani 1 1 d . . .
N1 N 0.3338(3) 0.5908(2) 0.27803(19) 0.0269(6) Uani 1 1 d . . .
C1 C 0.3790(4) 0.6938(3) 0.2610(3) 0.0372(9) Uani 1 1 d . . .
H1 H 0.3150 0.7475 0.2173 0.045 Uiso 1 1 calc R . .
C2 C 0.5190(4) 0.7275(3) 0.3052(3) 0.0406(9) Uani 1 1 d . . .
H2 H 0.5466 0.8007 0.2892 0.049 Uiso 1 1 calc R . .
C3 C 0.6129(4) 0.6535(4) 0.3708(3) 0.0426(10) Uani 1 1 d . . .
H3 H 0.7057 0.6763 0.4018 0.051 Uiso 1 1 calc R . .
C4 C 0.5706(4) 0.5404(3) 0.3927(2) 0.0340(8) Uani 1 1 d . . .
C5 C 0.6618(4) 0.4561(4) 0.4611(3) 0.0460(10) Uani 1 1 d . . .
H5 H 0.7552 0.4750 0.4964 0.055 Uiso 1 1 calc R . .
C6 C 0.6130(4) 0.3485(4) 0.4751(3) 0.0463(10) Uani 1 1 d . . .
H6 H 0.6739 0.2939 0.5198 0.056 Uiso 1 1 calc R . .
C7 C 0.4722(4) 0.3170(3) 0.4234(2) 0.0378(9) Uani 1 1 d . . .
H7 H 0.4410 0.2419 0.4334 0.045 Uiso 1 1 calc R . .
C8 C 0.3820(3) 0.3973(3) 0.3588(2) 0.0277(7) Uani 1 1 d . . .
C9 C 0.4284(3) 0.5123(3) 0.3422(2) 0.0272(8) Uani 1 1 d . . .
C10 C 0.1843(4) 0.2682(3) 0.3212(2) 0.0339(8) Uani 1 1 d . . .
H10A H 0.2119 0.2596 0.3885 0.041 Uiso 1 1 calc R . .
H10B H 0.2185 0.1980 0.3010 0.041 Uiso 1 1 calc R . .
C11 C 0.0281(4) 0.2744(3) 0.2654(2) 0.0289(8) Uani 1 1 d . . .
C12 C -0.2561(3) 0.5206(3) -0.0289(2) 0.0232(7) Uani 1 1 d . . .
C13 C -0.3832(3) 0.5079(3) -0.0142(2) 0.0224(7) Uani 1 1 d . . .
C14 C -0.3687(3) 0.4889(3) 0.0766(2) 0.0256(7) Uani 1 1 d . . .
H14 H -0.2810 0.4806 0.1280 0.031 Uiso 1 1 calc R . .
C15 C -0.5144(3) 0.5177(3) -0.0908(2) 0.0260(7) Uani 1 1 d . . .
H15 H -0.5243 0.5287 -0.1518 0.031 Uiso 1 1 calc R . .
C16 C 0.0133(3) 0.7364(3) -0.0092(2) 0.0236(7) Uani 1 1 d . . .
C17 C 0.0071(3) 0.8733(3) -0.0048(2) 0.0221(7) Uani 1 1 d . . .
C18 C -0.0478(3) 0.9430(3) -0.0877(2) 0.0269(7) Uani 1 1 d . . .
H18 H -0.0801 0.9049 -0.1466 0.032 Uiso 1 1 calc R . .
C19 C 0.0546(3) 0.9317(3) 0.0826(2) 0.0264(7) Uani 1 1 d . . .
H19 H 0.0913 0.8856 0.1383 0.032 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
Sm1 O5 2.308(2) . ?
Sm1 O7 2.350(2) . ?
Sm1 O6 2.373(2) 3_565 ?
Sm1 O3 2.414(2) 2 ?
Sm1 O4 2.451(2) 3_565 ?
Sm1 O2 2.475(2) . ?
Sm1 O1 2.589(2) . ?
Sm1 N1 2.619(3) . ?
O1 C8 1.380(4) . ?
O1 C10 1.436(4) . ?
O2 C11 1.254(4) . ?
O3 C11 1.255(4) . ?
O4 C12 1.249(4) . ?
O5 C12 1.264(4) . ?
O6 C16 1.250(4) . ?
O7 C16 1.261(4) . ?
N1 C1 1.306(4) . ?
N1 C9 1.366(4) . ?
C1 C2 1.402(5) . ?
C1 H1 0.9300 . ?
C2 C3 1.342(5) . ?
C2 H2 0.9300 . ?
C3 C4 1.417(5) . ?
C3 H3 0.9300 . ?
C4 C9 1.410(5) . ?
C4 C5 1.421(5) . ?
C5 C6 1.350(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.407(5) . ?
C6 H6 0.9300 . ?
C7 C8 1.362(5) . ?
C7 H7 0.9300 . ?
C8 C9 1.424(4) . ?
C10 C11 1.514(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.510(4) . ?
C13 C15 1.387(5) . ?
C13 C14 1.388(4) . ?
C14 C15 1.392(5) 3_465 ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.502(4) . ?
C17 C19 1.390(4) . ?
C17 C18 1.391(4) . ?
C18 C19 1.377(5) 3_575 ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?

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
O5 Sm1 O7 76.68(8) . . ?
O5 Sm1 O6 80.84(8) . 3_565 ?
O7 Sm1 O6 118.97(8) . 3_565 ?
O5 Sm1 O3 84.37(8) . 2 ?
O7 Sm1 O3 76.31(8) . 2 ?
O6 Sm1 O3 155.13(8) 3_565 2 ?
O5 Sm1 O4 121.61(8) . 3_565 ?
O7 Sm1 O4 73.99(8) . 3_565 ?
O6 Sm1 O4 71.41(8) 3_565 3_565 ?
O3 Sm1 O4 133.43(8) 2 3_565 ?
O5 Sm1 O2 78.76(8) . . ?
O7 Sm1 O2 151.87(8) . . ?
O6 Sm1 O2 69.73(8) 3_565 . ?
O3 Sm1 O2 87.88(8) 2 . ?
O4 Sm1 O2 131.72(7) 3_565 . ?
O5 Sm1 O1 139.23(7) . . ?
O7 Sm1 O1 143.97(7) . . ?
O6 Sm1 O1 78.77(7) 3_565 . ?
O3 Sm1 O1 100.28(8) 2 . ?
O4 Sm1 O1 84.20(7) 3_565 . ?
O2 Sm1 O1 61.14(7) . . ?
O5 Sm1 N1 155.81(8) . . ?
O7 Sm1 N1 83.71(8) . . ?
O6 Sm1 N1 121.61(8) 3_565 . ?
O3 Sm1 N1 77.27(8) 2 . ?
O4 Sm1 N1 64.60(8) 3_565 . ?
O2 Sm1 N1 115.68(8) . . ?
O1 Sm1 N1 60.89(7) . . ?
C8 O1 C10 117.5(2) . . ?
C8 O1 Sm1 123.07(18) . . ?
C10 O1 Sm1 118.51(18) . . ?
C11 O2 Sm1 122.4(2) . . ?
C11 O3 Sm1 154.1(2) . 2_545 ?
C12 O4 Sm1 124.6(2) . 3_565 ?
C12 O5 Sm1 165.5(2) . . ?
C16 O6 Sm1 138.4(2) . 3_565 ?
C16 O7 Sm1 141.8(2) . . ?
C1 N1 C9 118.0(3) . . ?
C1 N1 Sm1 119.7(2) . . ?
C9 N1 Sm1 119.8(2) . . ?
N1 C1 C2 123.4(3) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C3 C2 C1 119.5(4) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.2 . . ?
C2 C3 C4 119.9(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C9 C4 C3 116.6(3) . . ?
C9 C4 C5 119.3(3) . . ?
C3 C4 C5 124.1(4) . . ?
C6 C5 C4 120.1(4) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 121.5(4) . . ?
C5 C6 H6 119.2 . . ?
C7 C6 H6 119.2 . . ?
C8 C7 C6 119.6(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 O1 125.4(3) . . ?
C7 C8 C9 120.9(3) . . ?
O1 C8 C9 113.7(3) . . ?
N1 C9 C4 122.6(3) . . ?
N1 C9 C8 118.8(3) . . ?
C4 C9 C8 118.6(3) . . ?
O1 C10 C11 108.7(3) . . ?
O1 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
O1 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
H10A C10 H10B 108.3 . . ?
O2 C11 O3 126.8(3) . . ?
O2 C11 C10 117.8(3) . . ?
O3 C11 C10 115.4(3) . . ?
O4 C12 O5 124.9(3) . . ?
O4 C12 C13 118.4(3) . . ?
O5 C12 C13 116.7(3) . . ?
C15 C13 C14 119.8(3) . . ?
C15 C13 C12 120.3(3) . . ?
C14 C13 C12 119.9(3) . . ?
C13 C14 C15 119.9(3) . 3_465 ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 3_465 . ?
C13 C15 C14 120.3(3) . 3_465 ?
C13 C15 H15 119.9 . . ?
C14 C15 H15 119.9 3_465 . ?
O6 C16 O7 125.7(3) . . ?
O6 C16 C17 117.2(3) . . ?
O7 C16 C17 117.1(3) . . ?
C19 C17 C18 119.3(3) . . ?
C19 C17 C16 120.0(3) . . ?
C18 C17 C16 120.7(3) . . ?
C19 C18 C17 120.1(3) 3_575 . ?
C19 C18 H18 119.9 3_575 . ?
C17 C18 H18 119.9 . . ?
C18 C19 C17 120.6(3) 3_575 . ?
C18 C19 H19 119.7 3_575 . ?
C17 C19 H19 119.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O5 Sm1 O1 C8 -178.6(2) . . . . ?
O7 Sm1 O1 C8 -4.5(3) . . . . ?
O6 Sm1 O1 C8 120.0(2) 3_565 . . . ?
O3 Sm1 O1 C8 -85.3(2) 2 . . . ?
O4 Sm1 O1 C8 47.9(2) 3_565 . . . ?
O2 Sm1 O1 C8 -167.1(2) . . . . ?
N1 Sm1 O1 C8 -16.2(2) . . . . ?
O5 Sm1 O1 C10 12.8(3) . . . . ?
O7 Sm1 O1 C10 -173.1(2) . . . . ?
O6 Sm1 O1 C10 -48.6(2) 3_565 . . . ?
O3 Sm1 O1 C10 106.1(2) 2 . . . ?
O4 Sm1 O1 C10 -120.7(2) 3_565 . . . ?
O2 Sm1 O1 C10 24.3(2) . . . . ?
N1 Sm1 O1 C10 175.2(3) . . . . ?
O5 Sm1 O2 C11 141.4(2) . . . . ?
O7 Sm1 O2 C11 170.9(2) . . . . ?
O6 Sm1 O2 C11 57.1(2) 3_565 . . . ?
O3 Sm1 O2 C11 -134.0(2) 2 . . . ?
O4 Sm1 O2 C11 18.8(3) 3_565 . . . ?
O1 Sm1 O2 C11 -31.0(2) . . . . ?
N1 Sm1 O2 C11 -59.2(3) . . . . ?
O7 Sm1 O5 C12 85.5(9) . . . . ?
O6 Sm1 O5 C12 -37.3(8) 3_565 . . . ?
O3 Sm1 O5 C12 162.8(9) 2 . . . ?
O4 Sm1 O5 C12 24.1(9) 3_565 . . . ?
O2 Sm1 O5 C12 -108.3(9) . . . . ?
O1 Sm1 O5 C12 -98.0(8) . . . . ?
N1 Sm1 O5 C12 122.2(8) . . . . ?
O5 Sm1 O7 C16 -12.9(3) . . . . ?
O6 Sm1 O7 C16 58.5(3) 3_565 . . . ?
O3 Sm1 O7 C16 -100.3(3) 2 . . . ?
O4 Sm1 O7 C16 116.0(3) 3_565 . . . ?
O2 Sm1 O7 C16 -42.7(4) . . . . ?
O1 Sm1 O7 C16 171.0(3) . . . . ?
N1 Sm1 O7 C16 -178.7(3) . . . . ?
O5 Sm1 N1 C1 -31.6(4) . . . . ?
O7 Sm1 N1 C1 4.1(3) . . . . ?
O6 Sm1 N1 C1 124.4(2) 3_565 . . . ?
O3 Sm1 N1 C1 -73.2(3) 2 . . . ?
O4 Sm1 N1 C1 79.4(3) 3_565 . . . ?
O2 Sm1 N1 C1 -154.5(2) . . . . ?
O1 Sm1 N1 C1 177.2(3) . . . . ?
O5 Sm1 N1 C9 166.9(2) . . . . ?
O7 Sm1 N1 C9 -157.3(2) . . . . ?
O6 Sm1 N1 C9 -37.0(3) 3_565 . . . ?
O3 Sm1 N1 C9 125.3(2) 2 . . . ?
O4 Sm1 N1 C9 -82.1(2) 3_565 . . . ?
O2 Sm1 N1 C9 44.0(2) . . . . ?
O1 Sm1 N1 C9 15.8(2) . . . . ?
C9 N1 C1 C2 -0.1(5) . . . . ?
Sm1 N1 C1 C2 -161.9(3) . . . . ?
N1 C1 C2 C3 -2.1(6) . . . . ?
C1 C2 C3 C4 1.9(6) . . . . ?
C2 C3 C4 C9 0.3(5) . . . . ?
C2 C3 C4 C5 -179.7(4) . . . . ?
C9 C4 C5 C6 2.3(6) . . . . ?
C3 C4 C5 C6 -177.7(4) . . . . ?
C4 C5 C6 C7 -0.4(6) . . . . ?
C5 C6 C7 C8 -1.0(6) . . . . ?
C6 C7 C8 O1 -179.0(3) . . . . ?
C6 C7 C8 C9 0.5(5) . . . . ?
C10 O1 C8 C7 3.3(5) . . . . ?
Sm1 O1 C8 C7 -165.4(3) . . . . ?
C10 O1 C8 C9 -176.2(3) . . . . ?
Sm1 O1 C8 C9 15.1(4) . . . . ?
C1 N1 C9 C4 2.5(5) . . . . ?
Sm1 N1 C9 C4 164.3(2) . . . . ?
C1 N1 C9 C8 -177.4(3) . . . . ?
Sm1 N1 C9 C8 -15.6(4) . . . . ?
C3 C4 C9 N1 -2.6(5) . . . . ?
C5 C4 C9 N1 177.4(3) . . . . ?
C3 C4 C9 C8 177.3(3) . . . . ?
C5 C4 C9 C8 -2.7(5) . . . . ?
C7 C8 C9 N1 -178.7(3) . . . . ?
O1 C8 C9 N1 0.7(4) . . . . ?
C7 C8 C9 C4 1.4(5) . . . . ?
O1 C8 C9 C4 -179.1(3) . . . . ?
C8 O1 C10 C11 172.1(3) . . . . ?
Sm1 O1 C10 C11 -18.7(3) . . . . ?
Sm1 O2 C11 O3 -147.7(3) . . . . ?
Sm1 O2 C11 C10 33.8(4) . . . . ?
Sm1 O3 C11 O2 -127.3(5) 2_545 . . . ?
Sm1 O3 C11 C10 51.2(7) 2_545 . . . ?
O1 C10 C11 O2 -7.8(4) . . . . ?
O1 C10 C11 O3 173.5(3) . . . . ?
Sm1 O4 C12 O5 19.2(4) 3_565 . . . ?
Sm1 O4 C12 C13 -162.18(19) 3_565 . . . ?
Sm1 O5 C12 O4 -38.0(10) . . . . ?
Sm1 O5 C12 C13 143.3(7) . . . . ?
O4 C12 C13 C15 -8.0(4) . . . . ?
O5 C12 C13 C15 170.8(3) . . . . ?
O4 C12 C13 C14 173.4(3) . . . . ?
O5 C12 C13 C14 -7.9(4) . . . . ?
C15 C13 C14 C15 -1.3(5) . . . 3_465 ?
C12 C13 C14 C15 177.4(3) . . . 3_465 ?
C14 C13 C15 C14 1.3(5) . . . 3_465 ?
C12 C13 C15 C14 -177.3(3) . . . 3_465 ?
Sm1 O6 C16 O7 -7.4(5) 3_565 . . . ?
Sm1 O6 C16 C17 173.1(2) 3_565 . . . ?
Sm1 O7 C16 O6 -43.7(5) . . . . ?
Sm1 O7 C16 C17 135.8(3) . . . . ?
O6 C16 C17 C19 165.0(3) . . . . ?
O7 C16 C17 C19 -14.6(4) . . . . ?
O6 C16 C17 C18 -14.0(4) . . . . ?
O7 C16 C17 C18 166.5(3) . . . . ?
C19 C17 C18 C19 0.1(5) . . . 3_575 ?
C16 C17 C18 C19 179.1(3) . . . 3_575 ?
C18 C17 C19 C18 -0.1(5) . . . 3_575 ?
C16 C17 C19 C18 -179.1(3) . . . 3_575 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.771
_refine_diff_density_min         -0.351
_refine_diff_density_rms         0.082

#===END
data_a2
_database_code_depnum_ccdc_archive 'CCDC 717624'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C19 H12 Eu N O7'
_chemical_formula_sum            'C19 H12 Eu N O7'
_chemical_formula_weight         518.26

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'
Eu Eu -0.1578 3.6682 '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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_HALL  '-P 2ybc'

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

_cell_length_a                   10.8671(3)
_cell_length_b                   10.8974(3)
_cell_length_c                   15.8338(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 117.385(2)
_cell_angle_gamma                90.00
_cell_volume                     1664.96(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    298(2)
_cell_measurement_reflns_used    3926
_cell_measurement_theta_min      2.11
_cell_measurement_theta_max      27.80

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_exptl_absorpt_coefficient_mu    3.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4017
_exptl_absorpt_correction_T_max  0.5129
_exptl_absorpt_process_details   SADABS

_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  'Bruker Smart Apex II CCD area detector'
_diffrn_measurement_method       'φ and ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11917
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.11
_diffrn_reflns_theta_max         25.25
_reflns_number_total             3011
_reflns_number_gt                2595
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2004)'
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_reduction        SAINT
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXTL-XP (Bruker, 2004)'
_computing_publication_material  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)+(0.0510P)²+0.1000P] where P=(Fo²+2Fc²)/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         3011
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0196
_refine_ls_wR_factor_ref         0.0733
_refine_ls_wR_factor_gt          0.0555
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_restrained_S_all      1.010
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Eu1 Eu 0.588145(17) 0.510551(16) 0.157677(13) 0.01464(10) Uani 1 1 d . . .
O1 O 0.7406(3) 0.3793(3) 0.30413(19) 0.0280(7) Uani 1 1 d . . .
O2 O 0.4739(3) 0.3746(3) 0.2248(2) 0.0275(7) Uani 1 1 d . . .
O3 O 0.4637(3) 0.1791(3) 0.2655(2) 0.0304(7) Uani 1 1 d . . .
O4 O 0.4438(3) 0.6865(3) -0.08878(19) 0.0274(6) Uani 1 1 d . . .
O5 O 0.5880(3) 0.6796(3) 0.0675(2) 0.0258(6) Uani 1 1 d . . .
O6 O 0.6404(3) 0.4723(3) -0.0457(2) 0.0260(7) Uani 1 1 d . . .
O7 O 0.7701(3) 0.4742(3) 0.1109(2) 0.0254(6) Uani 1 1 d . . .
N1 N 0.8325(3) 0.5908(3) 0.2768(2) 0.0225(7) Uani 1 1 d . . .
C1 C 0.8781(4) 0.6956(4) 0.2591(3) 0.0319(10) Uani 1 1 d . . .
H1 H 0.8138 0.7492 0.2152 0.038 Uiso 1 1 calc R . .
C2 C 1.0179(4) 0.7300(4) 0.3028(3) 0.0343(10) Uani 1 1 d . . .
H2 H 1.0457 0.8031 0.2865 0.041 Uiso 1 1 calc R . .
C3 C 1.1123(4) 0.6545(5) 0.3697(3) 0.0390(12) Uani 1 1 d . . .
H3 H 1.2052 0.6772 0.4008 0.047 Uiso 1 1 calc R . .
C4 C 1.0698(4) 0.5415(5) 0.3922(3) 0.0296(9) Uani 1 1 d . . .
C5 C 1.1611(5) 0.4583(5) 0.4604(4) 0.0397(12) Uani 1 1 d . . .
H5 H 1.2543 0.4781 0.4956 0.048 Uiso 1 1 calc R . .
C6 C 1.1131(4) 0.3493(5) 0.4751(3) 0.0406(12) Uani 1 1 d . . .
H6 H 1.1744 0.2948 0.5198 0.049 Uiso 1 1 calc R . .
C7 C 0.9718(4) 0.3177(4) 0.4234(3) 0.0350(10) Uani 1 1 d . . .
H7 H 0.9402 0.2425 0.4335 0.042 Uiso 1 1 calc R . .
C8 C 0.8820(4) 0.3987(4) 0.3584(3) 0.0243(9) Uani 1 1 d . . .
C9 C 0.9279(5) 0.5134(4) 0.3414(3) 0.0225(10) Uani 1 1 d . . .
C10 C 0.6826(4) 0.2686(4) 0.3204(3) 0.0286(9) Uani 1 1 d . . .
H10A H 0.7100 0.2597 0.3877 0.034 Uiso 1 1 calc R . .
H10B H 0.7165 0.1980 0.3000 0.034 Uiso 1 1 calc R . .
C11 C 0.5267(4) 0.2758(4) 0.2647(3) 0.0233(9) Uani 1 1 d . . .
C12 C 0.5138(4) 0.7356(4) -0.0090(3) 0.0209(9) Uani 1 1 d . . .
C13 C 0.5077(3) 0.8730(4) -0.0043(2) 0.0188(8) Uani 1 1 d . . .
C14 C 0.5548(4) 0.9312(4) 0.0832(3) 0.0218(8) Uani 1 1 d . . .
H14 H 0.5912 0.8850 0.1388 0.026 Uiso 1 1 calc R . .
C15 C 0.4523(4) 0.9426(4) -0.0878(3) 0.0228(8) Uani 1 1 d . . .
H15 H 0.4202 0.9039 -0.1465 0.027 Uiso 1 1 calc R . .
C16 C 0.7545(4) 0.4793(3) 0.0280(3) 0.0196(9) Uani 1 1 d . . .
C17 C 0.8818(4) 0.4920(3) 0.0139(3) 0.0195(9) Uani 1 1 d . . .
C18 C 1.0140(4) 0.4824(4) 0.0909(3) 0.0237(9) Uani 1 1 d . . .
H18 H 1.0237 0.4718 0.1519 0.028 Uiso 1 1 calc R . .
C19 C 0.8691(4) 0.5116(3) -0.0772(3) 0.0231(9) Uani 1 1 d . . .
H19 H 0.7817 0.5207 -0.1288 0.028 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
Eu1 O6 2.301(3) 3_665 ?
Eu1 O5 2.331(3) . ?
Eu1 O4 2.360(3) 3_665 ?
Eu1 O3 2.408(3) 2_655 ?
Eu1 O7 2.442(3) . ?
Eu1 O2 2.465(3) . ?
Eu1 O1 2.575(3) . ?
Eu1 N1 2.601(3) . ?
O1 C8 1.389(4) . ?
O1 C10 1.438(4) . ?
O2 C11 1.246(5) . ?
O3 C11 1.261(5) . ?
O4 C12 1.256(5) . ?
O5 C12 1.261(4) . ?
O6 C16 1.255(5) . ?
O7 C16 1.246(5) . ?
N1 C1 1.325(5) . ?
N1 C9 1.363(5) . ?
C1 C2 1.400(6) . ?
C1 H1 0.9300 . ?
C2 C3 1.361(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.417(7) . ?
C3 H3 0.9300 . ?
C4 C9 1.406(6) . ?
C4 C5 1.410(7) . ?
C5 C6 1.359(7) . ?
C5 H5 0.9300 . ?
C6 C7 1.410(6) . ?
C6 H6 0.9300 . ?
C7 C8 1.367(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.416(6) . ?
C10 C11 1.510(5) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C12 C13 1.503(6) . ?
C13 C14 1.390(5) . ?
C13 C15 1.398(5) . ?
C14 C15 1.382(6) 3_675 ?
C14 H14 0.9300 . ?
C15 H15 0.9300 . ?
C16 C17 1.505(6) . ?
C17 C18 1.397(6) . ?
C17 C19 1.401(6) . ?
C18 C19 1.384(6) 3_765 ?
C18 H18 0.9300 . ?
C19 H19 0.9300 . ?

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
O6 Eu1 O5 76.55(10) 3_665 . ?
O6 Eu1 O4 80.82(10) 3_665 3_665 ?
O5 Eu1 O4 118.51(10) . 3_665 ?
O6 Eu1 O3 84.67(10) 3_665 2_655 ?
O5 Eu1 O3 76.82(10) . 2_655 ?
O4 Eu1 O3 155.27(10) 3_665 2_655 ?
O6 Eu1 O7 121.14(10) 3_665 . ?
O5 Eu1 O7 73.43(10) . . ?
O4 Eu1 O7 71.34(10) 3_665 . ?
O3 Eu1 O7 133.37(10) 2_655 . ?
O6 Eu1 O2 78.58(10) 3_665 . ?
O5 Eu1 O2 151.71(9) . . ?
O4 Eu1 O2 69.91(9) 3_665 . ?
O3 Eu1 O2 87.69(10) 2_655 . ?
O7 Eu1 O2 132.21(9) . . ?
O6 Eu1 O1 139.29(9) 3_665 . ?
O5 Eu1 O1 144.06(9) . . ?
O4 Eu1 O1 78.94(9) 3_665 . ?
O3 Eu1 O1 99.89(10) 2_655 . ?
O7 Eu1 O1 84.71(9) . . ?
O2 Eu1 O1 61.38(8) . . ?
O6 Eu1 N1 155.69(10) 3_665 . ?
O5 Eu1 N1 83.75(10) . . ?
O4 Eu1 N1 121.67(10) 3_665 . ?
O3 Eu1 N1 77.01(10) 2_655 . ?
O7 Eu1 N1 64.86(10) . . ?
O2 Eu1 N1 115.98(10) . . ?
O1 Eu1 N1 60.97(9) . . ?
O6 Eu1 Eu1 52.07(7) 3_665 3_665 ?
O5 Eu1 Eu1 58.35(7) . 3_665 ?
O4 Eu1 Eu1 62.56(7) 3_665 3_665 ?
O3 Eu1 Eu1 121.69(7) 2_655 3_665 ?
O7 Eu1 Eu1 69.07(7) . 3_665 ?
O2 Eu1 Eu1 114.19(7) . 3_665 ?
O1 Eu1 Eu1 138.36(7) . 3_665 ?
N1 Eu1 Eu1 126.80(7) . 3_665 ?
C8 O1 C10 117.9(3) . . ?
C8 O1 Eu1 122.9(2) . . ?
C10 O1 Eu1 118.3(2) . . ?
C11 O2 Eu1 122.1(2) . . ?
C11 O3 Eu1 153.9(3) . 2_645 ?
C12 O4 Eu1 138.2(3) . 3_665 ?
C12 O5 Eu1 142.2(2) . . ?
C16 O6 Eu1 165.1(3) . 3_665 ?
C16 O7 Eu1 125.2(3) . . ?
C1 N1 C9 117.6(3) . . ?
C1 N1 Eu1 119.5(3) . . ?
C9 N1 Eu1 120.4(3) . . ?
N1 C1 C2 123.5(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.8(4) . . ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C2 C3 C4 120.3(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C9 C4 C5 119.9(4) . . ?
C9 C4 C3 116.4(4) . . ?
C5 C4 C3 123.7(4) . . ?
C6 C5 C4 120.2(4) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 121.0(4) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C8 C7 C6 119.2(4) . . ?
C8 C7 H7 120.4 . . ?
C6 C7 H7 120.4 . . ?
C7 C8 O1 124.8(4) . . ?
C7 C8 C9 121.4(4) . . ?
O1 C8 C9 113.7(4) . . ?
N1 C9 C4 123.3(4) . . ?
N1 C9 C8 118.5(4) . . ?
C4 C9 C8 118.2(4) . . ?
O1 C10 C11 108.5(3) . . ?
O1 C10 H10A 110.0 . . ?
C11 C10 H10A 110.0 . . ?
O1 C10 H10B 110.0 . . ?
C11 C10 H10B 110.0 . . ?
H10A C10 H10B 108.4 . . ?
O2 C11 O3 127.0(4) . . ?
O2 C11 C10 118.2(4) . . ?
O3 C11 C10 114.8(4) . . ?
O4 C12 O5 125.7(4) . . ?
O4 C12 C13 117.0(3) . . ?
O5 C12 C13 117.2(3) . . ?
C14 C13 C15 119.8(4) . . ?
C14 C13 C12 120.0(3) . . ?
C15 C13 C12 120.2(3) . . ?
C15 C14 C13 120.2(3) 3_675 . ?
C15 C14 H14 119.9 3_675 . ?
C13 C14 H14 119.9 . . ?
C14 C15 C13 120.0(3) 3_675 . ?
C14 C15 H15 120.0 3_675 . ?
C13 C15 H15 120.0 . . ?
O7 C16 O6 125.1(4) . . ?
O7 C16 C17 118.1(4) . . ?
O6 C16 C17 116.8(4) . . ?
C18 C17 C19 118.9(4) . . ?
C18 C17 C16 120.7(4) . . ?
C19 C17 C16 120.3(4) . . ?
C19 C18 C17 120.6(4) 3_765 . ?
C19 C18 H18 119.7 3_765 . ?
C17 C18 H18 119.7 . . ?
C18 C19 C17 120.4(4) 3_765 . ?
C18 C19 H19 119.8 3_765 . ?
C17 C19 H19 119.8 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O6 Eu1 O1 C8 -178.3(3) 3_665 . . . ?
O5 Eu1 O1 C8 -3.8(4) . . . . ?
O4 Eu1 O1 C8 120.2(3) 3_665 . . . ?
O3 Eu1 O1 C8 -85.0(3) 2_655 . . . ?
O7 Eu1 O1 C8 48.2(3) . . . . ?
O2 Eu1 O1 C8 -166.8(3) . . . . ?
N1 Eu1 O1 C8 -15.9(3) . . . . ?
Eu1 Eu1 O1 C8 98.1(3) 3_665 . . . ?
O6 Eu1 O1 C10 13.1(3) 3_665 . . . ?
O5 Eu1 O1 C10 -172.4(3) . . . . ?
O4 Eu1 O1 C10 -48.5(3) 3_665 . . . ?
O3 Eu1 O1 C10 106.4(3) 2_655 . . . ?
O7 Eu1 O1 C10 -120.4(3) . . . . ?
O2 Eu1 O1 C10 24.6(3) . . . . ?
N1 Eu1 O1 C10 175.5(3) . . . . ?
Eu1 Eu1 O1 C10 -70.5(3) 3_665 . . . ?
O6 Eu1 O2 C11 141.3(3) 3_665 . . . ?
O5 Eu1 O2 C11 170.1(3) . . . . ?
O4 Eu1 O2 C11 57.0(3) 3_665 . . . ?
O3 Eu1 O2 C11 -133.7(3) 2_655 . . . ?
O7 Eu1 O2 C11 19.3(3) . . . . ?
O1 Eu1 O2 C11 -31.1(3) . . . . ?
N1 Eu1 O2 C11 -59.4(3) . . . . ?
Eu1 Eu1 O2 C11 102.4(3) 3_665 . . . ?
O6 Eu1 O5 C12 -12.2(4) 3_665 . . . ?
O4 Eu1 O5 C12 59.3(4) 3_665 . . . ?
O3 Eu1 O5 C12 -99.8(4) 2_655 . . . ?
O7 Eu1 O5 C12 116.5(4) . . . . ?
O2 Eu1 O5 C12 -41.3(5) . . . . ?
O1 Eu1 O5 C12 171.5(4) . . . . ?
N1 Eu1 O5 C12 -177.9(4) . . . . ?
Eu1 Eu1 O5 C12 41.3(4) 3_665 . . . ?
O6 Eu1 O7 C16 10.0(3) 3_665 . . . ?
O5 Eu1 O7 C16 -52.4(3) . . . . ?
O4 Eu1 O7 C16 76.4(3) 3_665 . . . ?
O3 Eu1 O7 C16 -104.9(3) 2_655 . . . ?
O2 Eu1 O7 C16 113.6(3) . . . . ?
O1 Eu1 O7 C16 156.5(3) . . . . ?
N1 Eu1 O7 C16 -143.2(3) . . . . ?
Eu1 Eu1 O7 C16 9.4(3) 3_665 . . . ?
O6 Eu1 N1 C1 -31.3(4) 3_665 . . . ?
O5 Eu1 N1 C1 4.5(3) . . . . ?
O4 Eu1 N1 C1 124.3(3) 3_665 . . . ?
O3 Eu1 N1 C1 -73.4(3) 2_655 . . . ?
O7 Eu1 N1 C1 79.1(3) . . . . ?
O2 Eu1 N1 C1 -154.3(3) . . . . ?
O1 Eu1 N1 C1 177.4(3) . . . . ?
Eu1 Eu1 N1 C1 46.7(3) 3_665 . . . ?
O6 Eu1 N1 C9 166.9(3) 3_665 . . . ?
O5 Eu1 N1 C9 -157.3(3) . . . . ?
O4 Eu1 N1 C9 -37.5(3) 3_665 . . . ?
O3 Eu1 N1 C9 124.9(3) 2_655 . . . ?
O7 Eu1 N1 C9 -82.7(3) . . . . ?
O2 Eu1 N1 C9 44.0(3) . . . . ?
O1 Eu1 N1 C9 15.6(3) . . . . ?
Eu1 Eu1 N1 C9 -115.1(3) 3_665 . . . ?
C9 N1 C1 C2 0.2(6) . . . . ?
Eu1 N1 C1 C2 -162.1(3) . . . . ?
N1 C1 C2 C3 -2.4(7) . . . . ?
C1 C2 C3 C4 1.9(7) . . . . ?
C2 C3 C4 C9 0.5(7) . . . . ?
C2 C3 C4 C5 180.0(4) . . . . ?
C9 C4 C5 C6 2.2(7) . . . . ?
C3 C4 C5 C6 -177.2(5) . . . . ?
C4 C5 C6 C7 -0.6(8) . . . . ?
C5 C6 C7 C8 -0.6(7) . . . . ?
C6 C7 C8 O1 -179.0(4) . . . . ?
C6 C7 C8 C9 0.4(6) . . . . ?
C10 O1 C8 C7 3.1(6) . . . . ?
Eu1 O1 C8 C7 -165.6(3) . . . . ?
C10 O1 C8 C9 -176.4(4) . . . . ?
Eu1 O1 C8 C9 15.0(5) . . . . ?
C1 N1 C9 C4 2.5(6) . . . . ?
Eu1 N1 C9 C4 164.6(3) . . . . ?
C1 N1 C9 C8 -177.4(4) . . . . ?
Eu1 N1 C9 C8 -15.3(5) . . . . ?
C5 C4 C9 N1 177.7(4) . . . . ?
C3 C4 C9 N1 -2.9(6) . . . . ?
C5 C4 C9 C8 -2.4(6) . . . . ?
C3 C4 C9 C8 177.0(4) . . . . ?
C7 C8 C9 N1 -178.9(4) . . . . ?
O1 C8 C9 N1 0.5(5) . . . . ?
C7 C8 C9 C4 1.1(6) . . . . ?
O1 C8 C9 C4 -179.4(3) . . . . ?
C8 O1 C10 C11 171.9(3) . . . . ?
Eu1 O1 C10 C11 -19.0(4) . . . . ?
Eu1 O2 C11 O3 -147.6(3) . . . . ?
Eu1 O2 C11 C10 33.9(5) . . . . ?
Eu1 O3 C11 O2 -127.5(5) 2_645 . . . ?
Eu1 O3 C11 C10 51.1(8) 2_645 . . . ?
O1 C10 C11 O2 -7.8(5) . . . . ?
O1 C10 C11 O3 173.5(3) . . . . ?
Eu1 O4 C12 O5 -6.9(6) 3_665 . . . ?
Eu1 O4 C12 C13 173.5(2) 3_665 . . . ?
Eu1 O5 C12 O4 -44.8(6) . . . . ?
Eu1 O5 C12 C13 134.8(3) . . . . ?
O4 C12 C13 C14 164.9(3) . . . . ?
O5 C12 C13 C14 -14.7(5) . . . . ?
O4 C12 C13 C15 -13.8(5) . . . . ?
O5 C12 C13 C15 166.6(3) . . . . ?
C15 C13 C14 C15 -0.4(5) . . . 3_675 ?
C12 C13 C14 C15 -179.1(3) . . . 3_675 ?
C14 C13 C15 C14 0.4(5) . . . 3_675 ?
C12 C13 C15 C14 179.1(3) . . . 3_675 ?
Eu1 O7 C16 O6 -19.3(6) . . . . ?
Eu1 O7 C16 C17 162.1(2) . . . . ?
Eu1 O6 C16 O7 38.6(13) 3_665 . . . ?
Eu1 O6 C16 C17 -142.8(9) 3_665 . . . ?
O7 C16 C17 C18 8.1(5) . . . . ?
O6 C16 C17 C18 -170.6(4) . . . . ?
O7 C16 C17 C19 -173.0(3) . . . . ?
O6 C16 C17 C19 8.3(5) . . . . ?
C19 C17 C18 C19 -1.9(6) . . . 3_765 ?
C16 C17 C18 C19 177.0(3) . . . 3_765 ?
C18 C17 C19 C18 1.9(6) . . . 3_765 ?
C16 C17 C19 C18 -177.0(3) . . . 3_765 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.25
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.743
_refine_diff_density_rms         0.262

#===END


