
# Electronic Supplementary Material (ESI) 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        'Wuping Liao'
_publ_contact_author_email       WPLIAO@CIAC.JL.CN

_publ_section_title              
;
3D metal-organic frameworks incorporating
water-soluble tetra-p-sulfonatocalix[4]arene
;
loop_
_publ_author_name
'Wuping Liao'
'Ce Liu'
'Xiao-Fei Wang'
'Hong-Jie Zhang'
'Xiao-Jun Zhao'
;
Guang-Shan Zhu
;

####END

# Attachment 'compd-amine-squeeze-revised.cif'

data_Nd-N(CH3)4-squeeze
_database_code_depnum_ccdc_archive 'CCDC 714471'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '((CH3)4N) Nd (C12H8N2)2 (C28H20S4O16) 3.5H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         '[(CH3)4N] Nd [C12H8N2]2 [C28H20S4O16] 3.5H2O'
_chemical_formula_sum            'C56 H55 N5 Nd O19.50 S4'
_chemical_formula_weight         1382.53

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/m c m'

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

_cell_length_a                   18.9307(13)
_cell_length_b                   18.9307(13)
_cell_length_c                   20.989(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7521.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    145(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2684
_exptl_absorpt_coefficient_mu    0.857
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8246
_exptl_absorpt_correction_T_max  0.8829
_exptl_absorpt_process_details   
; SADABS, Sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      145(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56661
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3580
_reflns_number_gt                2678
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was used.
All non-hydrogen atoms except the ammonium atoms
were refined anisotropically. The phenolic oxygen atoms and ammonium
cations were refined without hydrogen.
The partially occupied site of the ammonium cation with N2 atom was
refined with a charge constraint and the site occupation factor of N2
was set to 0.125.
The short contact C16...C17 might be due to
the disorder of the carbon atoms on the tetra-alkylammonium cations.
;

_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)+(0.1294P)²+16.9206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00066(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3580
_refine_ls_number_parameters     190
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.0860
_refine_ls_R_factor_gt           0.0691
_refine_ls_wR_factor_ref         0.2238
_refine_ls_wR_factor_gt          0.2120
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.092
_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
Nd1A Nd 0.0000 0.5000 0.2500 0.0365(10) Uani 0.901(17) 4 d SP . .
Nd1B Nd 0.0000 0.5000 0.220(2) 0.0365(10) Uani 0.049(8) 2 d SP . .
S1 S 0.07257(10) 0.34335(10) 0.16461(8) 0.0675(6) Uani 1 1 d . . .
N1 N 0.1198(2) 0.4539(2) 0.3002(2) 0.0485(12) Uani 1 1 d . . .
C1 C 0.3487(4) 0.3487(4) 0.1700(3) 0.054(2) Uani 1 2 d S . .
H1A H 0.3410 0.3410 0.2161 0.065 Uiso 1 2 calc SR . .
H1B H 0.3855 0.3855 0.1652 0.065 Uiso 1 2 calc SR . .
C2 C 0.2812(3) 0.3747(3) 0.1405(2) 0.0499(15) Uani 1 1 d . . .
C3 C 0.2157(3) 0.3523(3) 0.1639(3) 0.0551(16) Uani 1 1 d . . .
H3 H 0.2141 0.3224 0.2002 0.066 Uiso 1 1 calc R . .
C4 C 0.1534(3) 0.3727(4) 0.1353(3) 0.0542(16) Uani 1 1 d . . .
C5 C 0.1547(3) 0.4188(3) 0.0837(2) 0.0555(17) Uani 1 1 d . . .
H5 H 0.1117 0.4344 0.0651 0.067 Uiso 1 1 calc R . .
C6 C 0.2181(3) 0.4417(3) 0.0596(2) 0.0496(15) Uani 1 1 d . . .
C7 C 0.2817(3) 0.4200(3) 0.0869(2) 0.0530(17) Uani 1 1 d . . .
C8 C 0.2169(5) 0.4877(5) 0.0000 0.054(2) Uani 1 2 d S . .
H8A H 0.1737 0.5173 0.0000 0.065 Uiso 1 2 calc SR . .
H8B H 0.2584 0.5195 0.0000 0.065 Uiso 1 2 calc SR . .
C9 C 0.1227(4) 0.4095(4) 0.3486(4) 0.0673(19) Uani 1 1 d . . .
H9 H 0.0788 0.3937 0.3653 0.081 Uiso 1 1 calc R . .
C10 C 0.1832(4) 0.3836(4) 0.3775(4) 0.074(2) Uani 1 1 d . . .
H10 H 0.1805 0.3517 0.4124 0.089 Uiso 1 1 calc R . .
C11 C 0.2464(4) 0.4054(3) 0.3540(4) 0.0674(19) Uani 1 1 d . . .
H11 H 0.2892 0.3889 0.3723 0.081 Uiso 1 1 calc R . .
C12 C 0.2477(3) 0.4527(4) 0.3025(3) 0.0573(17) Uani 1 1 d . . .
C13 C 0.3131(3) 0.4790(4) 0.2739(3) 0.065(2) Uani 1 1 d . . .
H13 H 0.3571 0.4645 0.2914 0.078 Uiso 1 1 calc R . .
C14 C 0.1823(3) 0.4759(3) 0.2771(3) 0.0440(13) Uani 1 1 d . . .
O1 O 0.3445(2) 0.4436(2) 0.0633(2) 0.0652(12) Uani 1 1 d . . .
O2 O 0.0380(3) 0.3071(3) 0.1129(2) 0.0839(15) Uani 1 1 d . . .
O3 O 0.0344(2) 0.4085(2) 0.18107(17) 0.0594(12) Uani 1 1 d . . .
O4 O 0.0869(3) 0.3007(3) 0.2197(3) 0.0965(19) Uani 1 1 d . . .
N2 N 0.1877(18) 0.1877(18) 0.0000 0.176(6) Uiso 0.50 4 d SPD . .
C15 C 0.2401(18) 0.2401(18) 0.0000 0.176(6) Uiso 0.50 4 d SPD . .
C16 C 0.1196(15) 0.221(2) 0.0000 0.176(6) Uiso 0.50 2 d SPD . .
C17 C 0.184(3) 0.184(3) 0.0695(8) 0.176(6) Uiso 0.25 2 d SPD . .
N3 N 0.0000 0.0000 0.2500 0.176(6) Uiso 1 8 d SD . .
C18 C -0.0394(7) 0.0394(7) 0.3009(9) 0.176(6) Uiso 1 2 d SD . .


_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
Nd1A Nd1B 0.62(4) . ?
Nd1A Nd1B 0.62(4) 5 ?
Nd1A O3 2.349(4) . ?
Nd1A O3 2.349(4) 6_565 ?
Nd1A O3 2.349(4) 5 ?
Nd1A O3 2.349(4) 2_565 ?
Nd1A N1 2.649(5) 6_565 ?
Nd1A N1 2.649(5) 5 ?
Nd1A N1 2.649(5) 2_565 ?
Nd1A N1 2.649(5) . ?
Nd1B Nd1B 1.24(9) 5 ?
Nd1B O3 2.027(18) 2_565 ?
Nd1B O3 2.027(18) . ?
Nd1B N1 2.469(9) 6_565 ?
Nd1B N1 2.469(9) 5 ?
Nd1B O3 2.77(3) 6_565 ?
Nd1B O3 2.77(3) 5 ?
Nd1B N1 2.95(3) 2_565 ?
Nd1B N1 2.95(3) . ?
S1 O4 1.437(5) . ?
S1 O2 1.441(5) . ?
S1 O3 1.470(4) . ?
S1 C4 1.741(7) . ?
N1 C9 1.321(8) . ?
N1 C14 1.344(7) . ?
N1 Nd1B 2.469(9) 5 ?
C1 C2 1.502(7) . ?
C1 C2 1.502(7) 16 ?
C2 C3 1.400(9) . ?
C2 C7 1.415(8) . ?
C3 C4 1.378(8) . ?
C4 C5 1.390(8) . ?
C5 C6 1.373(8) . ?
C6 C7 1.394(7) . ?
C6 C8 1.525(7) . ?
C7 O1 1.364(8) . ?
C8 C6 1.525(7) 10 ?
C9 C10 1.385(9) . ?
C10 C11 1.359(10) . ?
C11 C12 1.405(10) . ?
C12 C14 1.418(7) . ?
C12 C13 1.463(9) . ?
C13 C13 1.279(15) 6_565 ?
C14 C14 1.457(12) 6_565 ?
O3 Nd1B 2.77(3) 5 ?
N2 C15 1.40(2) . ?
N2 C16 1.433(18) 7 ?
N2 C16 1.433(18) . ?
N2 C17 1.464(19) . ?
N2 C17 1.464(19) 10 ?
C16 C17 2.023(18) . ?
C16 C17 2.023(18) 10 ?
C17 C16 2.023(18) 7 ?
N3 C18 1.501(15) 2 ?
N3 C18 1.501(15) 11_556 ?
N3 C18 1.501(15) 12_556 ?
N3 C18 1.501(15) . ?

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
Nd1B Nd1A Nd1B 179.998(3) . 5 ?
Nd1B Nd1A O3 51.98(10) . . ?
Nd1B Nd1A O3 128.02(10) 5 . ?
Nd1B Nd1A O3 128.02(10) . 6_565 ?
Nd1B Nd1A O3 51.98(10) 5 6_565 ?
O3 Nd1A O3 147.8(2) . 6_565 ?
Nd1B Nd1A O3 128.02(10) . 5 ?
Nd1B Nd1A O3 51.98(10) 5 5 ?
O3 Nd1A O3 85.0(2) . 5 ?
O3 Nd1A O3 104.0(2) 6_565 5 ?
Nd1B Nd1A O3 51.98(10) . 2_565 ?
Nd1B Nd1A O3 128.02(10) 5 2_565 ?
O3 Nd1A O3 104.0(2) . 2_565 ?
O3 Nd1A O3 85.0(2) 6_565 2_565 ?
O3 Nd1A O3 147.8(2) 5 2_565 ?
Nd1B Nd1A N1 66.56(11) . 6_565 ?
Nd1B Nd1A N1 113.44(11) 5 6_565 ?
O3 Nd1A N1 76.12(15) . 6_565 ?
O3 Nd1A N1 76.39(15) 6_565 6_565 ?
O3 Nd1A N1 136.49(15) 5 6_565 ?
O3 Nd1A N1 75.52(14) 2_565 6_565 ?
Nd1B Nd1A N1 66.56(11) . 5 ?
Nd1B Nd1A N1 113.44(11) 5 5 ?
O3 Nd1A N1 75.52(14) . 5 ?
O3 Nd1A N1 136.49(15) 6_565 5 ?
O3 Nd1A N1 76.39(15) 5 5 ?
O3 Nd1A N1 76.12(15) 2_565 5 ?
N1 Nd1A N1 133.1(2) 6_565 5 ?
Nd1B Nd1A N1 113.44(11) . 2_565 ?
Nd1B Nd1A N1 66.56(11) 5 2_565 ?
O3 Nd1A N1 136.50(15) . 2_565 ?
O3 Nd1A N1 75.52(14) 6_565 2_565 ?
O3 Nd1A N1 76.12(15) 5 2_565 ?
O3 Nd1A N1 76.39(15) 2_565 2_565 ?
N1 Nd1A N1 141.6(2) 6_565 2_565 ?
N1 Nd1A N1 62.2(2) 5 2_565 ?
Nd1B Nd1A N1 113.44(11) . . ?
Nd1B Nd1A N1 66.56(11) 5 . ?
O3 Nd1A N1 76.39(15) . . ?
O3 Nd1A N1 76.12(15) 6_565 . ?
O3 Nd1A N1 75.52(14) 5 . ?
O3 Nd1A N1 136.49(15) 2_565 . ?
N1 Nd1A N1 62.2(2) 6_565 . ?
N1 Nd1A N1 141.6(2) 5 . ?
N1 Nd1A N1 133.1(2) 2_565 . ?
Nd1A Nd1B Nd1B 0.001(5) . 5 ?
Nd1A Nd1B O3 114.1(11) . 2_565 ?
Nd1B Nd1B O3 114.1(11) 5 2_565 ?
Nd1A Nd1B O3 114.1(11) . . ?
Nd1B Nd1B O3 114.1(11) 5 . ?
O3 Nd1B O3 132(2) 2_565 . ?
Nd1A Nd1B N1 100.1(10) . 6_565 ?
Nd1B Nd1B N1 100.1(10) 5 6_565 ?
O3 Nd1B N1 85.5(6) 2_565 6_565 ?
O3 Nd1B N1 86.2(6) . 6_565 ?
Nd1A Nd1B N1 100.1(10) . 5 ?
Nd1B Nd1B N1 100.1(10) 5 5 ?
O3 Nd1B N1 86.3(6) 2_565 5 ?
O3 Nd1B N1 85.5(6) . 5 ?
N1 Nd1B N1 160(2) 6_565 5 ?
Nd1A Nd1B O3 41.8(6) . 6_565 ?
Nd1B Nd1B O3 41.8(6) 5 6_565 ?
O3 Nd1B O3 81.1(6) 2_565 6_565 ?
O3 Nd1B O3 139.6(11) . 6_565 ?
N1 Nd1B O3 72.2(5) 6_565 6_565 ?
N1 Nd1B O3 124.6(11) 5 6_565 ?
Nd1A Nd1B O3 41.8(6) . 5 ?
Nd1B Nd1B O3 41.8(6) 5 5 ?
O3 Nd1B O3 139.6(11) 2_565 5 ?
O3 Nd1B O3 81.1(6) . 5 ?
N1 Nd1B O3 124.6(11) 6_565 5 ?
N1 Nd1B O3 72.2(5) 5 5 ?
O3 Nd1B O3 83.7(12) 6_565 5 ?
Nd1A Nd1B N1 55.4(7) . 2_565 ?
Nd1B Nd1B N1 55.4(7) 5 2_565 ?
O3 Nd1B N1 74.4(4) 2_565 2_565 ?
O3 Nd1B N1 137.0(5) . 2_565 ?
N1 Nd1B N1 134.6(9) 6_565 2_565 ?
N1 Nd1B N1 59.8(4) 5 2_565 ?
O3 Nd1B N1 64.8(7) 6_565 2_565 ?
O3 Nd1B N1 65.3(7) 5 2_565 ?
Nd1A Nd1B N1 55.4(7) . . ?
Nd1B Nd1B N1 55.4(7) 5 . ?
O3 Nd1B N1 137.0(5) 2_565 . ?
O3 Nd1B N1 74.4(4) . . ?
N1 Nd1B N1 59.8(4) 6_565 . ?
N1 Nd1B N1 134.6(9) 5 . ?
O3 Nd1B N1 65.3(7) 6_565 . ?
O3 Nd1B N1 64.8(7) 5 . ?
N1 Nd1B N1 110.9(14) 2_565 . ?
O4 S1 O2 115.2(4) . . ?
O4 S1 O3 112.0(3) . . ?
O2 S1 O3 110.7(3) . . ?
O4 S1 C4 107.3(3) . . ?
O2 S1 C4 106.5(3) . . ?
O3 S1 C4 104.3(3) . . ?
C9 N1 C14 116.1(5) . . ?
C9 N1 Nd1B 113.4(9) . 5 ?
C14 N1 Nd1B 129.5(7) . 5 ?
C9 N1 Nd1A 123.4(4) . . ?
C14 N1 Nd1A 120.5(4) . . ?
Nd1B N1 Nd1A 13.3(10) 5 . ?
C9 N1 Nd1B 131.0(6) . . ?
C14 N1 Nd1B 112.3(6) . . ?
Nd1B N1 Nd1B 24.4(17) 5 . ?
Nd1A N1 Nd1B 11.1(7) . . ?
C2 C1 C2 112.9(7) . 16 ?
C3 C2 C7 117.9(5) . . ?
C3 C2 C1 120.7(6) . . ?
C7 C2 C1 121.4(6) . . ?
C4 C3 C2 121.3(5) . . ?
C3 C4 C5 120.0(6) . . ?
C3 C4 S1 120.5(5) . . ?
C5 C4 S1 119.4(5) . . ?
C6 C5 C4 120.0(5) . . ?
C5 C6 C7 120.7(5) . . ?
C5 C6 C8 118.0(6) . . ?
C7 C6 C8 121.2(6) . . ?
O1 C7 C6 120.5(5) . . ?
O1 C7 C2 119.5(5) . . ?
C6 C7 C2 120.0(6) . . ?
C6 C8 C6 110.3(7) 10 . ?
N1 C9 C10 126.6(7) . . ?
C11 C10 C9 117.5(7) . . ?
C10 C11 C12 119.3(6) . . ?
C11 C12 C14 118.1(6) . . ?
C11 C12 C13 123.2(6) . . ?
C14 C12 C13 118.7(6) . . ?
C13 C13 C12 122.2(4) 6_565 . ?
N1 C14 C12 122.4(6) . . ?
N1 C14 C14 118.4(3) . 6_565 ?
C12 C14 C14 119.2(4) . 6_565 ?
S1 O3 Nd1B 166.1(9) . . ?
S1 O3 Nd1A 154.1(2) . . ?
Nd1B O3 Nd1A 13.9(11) . . ?
S1 O3 Nd1B 144.5(6) . 5 ?
Nd1B O3 Nd1B 24.1(17) . 5 ?
Nd1A O3 Nd1B 10.1(6) . 5 ?
C15 N2 C16 109(3) . 7 ?
C15 N2 C16 109(3) . . ?
C16 N2 C16 141(5) 7 . ?
C15 N2 C17 94(3) . . ?
C16 N2 C17 88.6(11) 7 . ?
C16 N2 C17 88.6(11) . . ?
C15 N2 C17 94(3) . 10 ?
C16 N2 C17 88.6(11) 7 10 ?
C16 N2 C17 88.6(11) . 10 ?
C17 N2 C17 171(7) . 10 ?
N2 C16 C17 46.3(8) . . ?
N2 C16 C17 46.3(8) . 10 ?
C17 C16 C17 92.4(13) . 10 ?
N2 C17 C16 45.1(8) . 7 ?
N2 C17 C16 45.1(8) . . ?
C16 C17 C16 83.9(18) 7 . ?
C18 N3 C18 120.4(10) 2 11_556 ?
C18 N3 C18 120.4(10) 2 12_556 ?
C18 N3 C18 89.3(17) 11_556 12_556 ?
C18 N3 C18 89.3(17) 2 . ?
C18 N3 C18 120.4(10) 11_556 . ?
C18 N3 C18 120.4(10) 12_556 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.736
_refine_diff_density_min         -1.322
_refine_diff_density_rms         0.125

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.023 0.018 -0.028 2557 1124 ' '
_platon_squeeze_details          
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.
;

###END

data_Eu-N(C2H5)4-squeeze
_database_code_depnum_ccdc_archive 'CCDC 714472'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '((C2H5)4N) Eu (C12H8N2)2 (C28H20S4O16) 5H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         '[(C2H5)4N] Eu [C12H8N2]2 [C28H20S4O16] 5H2O'
_chemical_formula_sum            'C60 H66 Eu N5 O21 S4'
_chemical_formula_weight         1473.38

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/m c m'

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

_cell_length_a                   19.1147(4)
_cell_length_b                   19.1147(4)
_cell_length_c                   21.1495(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7727.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    185(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2824
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7972
_exptl_absorpt_correction_T_max  0.8681
_exptl_absorpt_process_details   
; SADABS, Sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      185(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 AXS Apex CCD diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49026
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3660
_reflns_number_gt                2775
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was used.
All non-hydrogen atoms except the ammonium atoms
were refined anisotropically. The phenolic oxygen atoms and ammonium
cations were refined without hydrogen.
The partially occupied site of the ammonium cation with N2 atom was
refined with a charge constraint and the site occupation factor of N2
was set to 0.125.
The short contact C15...C17, C16-C22, C21-C21 and C21-C22 might be due to
the disorder of the carbon atoms on the tetra-alkylammonium cations.
;

_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)+(0.1233P)²+13.9369P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00006(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3660
_refine_ls_number_parameters     198
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_gt           0.0629
_refine_ls_wR_factor_ref         0.2178
_refine_ls_wR_factor_gt          0.2064
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.171
_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
Eu1 Eu 0.0000 0.5000 0.2500 0.0366(3) Uani 1 4 d S . .
S1 S 0.07317(8) 0.34597(9) 0.16741(7) 0.0548(5) Uani 1 1 d . . .
N1 N 0.1158(2) 0.4568(3) 0.3017(2) 0.0495(13) Uani 1 1 d . . .
C1 C 0.3475(3) 0.3475(3) 0.1694(3) 0.0392(17) Uani 1 2 d S . .
H1A H 0.3839 0.3839 0.1644 0.047 Uiso 1 2 calc SR . .
H1B H 0.3401 0.3401 0.2153 0.047 Uiso 1 2 calc SR . .
C2 C 0.2802(3) 0.3733(3) 0.1402(2) 0.0371(12) Uani 1 1 d . . .
C3 C 0.2164(3) 0.3516(3) 0.1646(2) 0.0414(13) Uani 1 1 d . . .
H3 H 0.2151 0.3218 0.2006 0.050 Uiso 1 1 calc R . .
C4 C 0.1540(3) 0.3737(3) 0.1364(3) 0.0450(13) Uani 1 1 d . . .
C5 C 0.1553(3) 0.4180(3) 0.0845(2) 0.0493(15) Uani 1 1 d . . .
H5 H 0.1127 0.4337 0.0664 0.059 Uiso 1 1 calc R . .
C6 C 0.2177(3) 0.4390(3) 0.0594(2) 0.0438(13) Uani 1 1 d . . .
C7 C 0.2800(3) 0.4169(3) 0.0869(2) 0.0394(12) Uani 1 1 d . . .
C8 C 0.2173(5) 0.4848(4) 0.0000 0.047(2) Uani 1 2 d S . .
H8A H 0.2590 0.5155 0.0000 0.056 Uiso 1 2 calc SR . .
H8B H 0.1751 0.5148 0.0000 0.056 Uiso 1 2 calc SR . .
C9 C 0.1171(4) 0.4140(4) 0.3519(3) 0.0636(19) Uani 1 1 d . . .
H9 H 0.0738 0.3997 0.3698 0.076 Uiso 1 1 calc R . .
C10 C 0.1788(4) 0.3895(3) 0.3791(4) 0.069(2) Uani 1 1 d . . .
H10 H 0.1772 0.3589 0.4144 0.083 Uiso 1 1 calc R . .
C11 C 0.2403(3) 0.4098(3) 0.3550(3) 0.0610(18) Uani 1 1 d . . .
H11 H 0.2828 0.3936 0.3732 0.073 Uiso 1 1 calc R . .
C12 C 0.2418(3) 0.4547(3) 0.3029(3) 0.0459(14) Uani 1 1 d . . .
C13 C 0.3073(3) 0.4790(3) 0.2754(3) 0.0586(18) Uani 1 1 d . . .
H13 H 0.3505 0.4650 0.2937 0.070 Uiso 1 1 calc R . .
C14 C 0.1781(3) 0.4766(3) 0.2765(3) 0.0435(13) Uani 1 1 d . . .
O1 O 0.3428(2) 0.4389(2) 0.06306(19) 0.0591(11) Uani 1 1 d . . .
O2 O 0.0372(2) 0.3090(3) 0.1163(2) 0.0701(13) Uani 1 1 d . . .
O3 O 0.0350(2) 0.4106(3) 0.18248(19) 0.0574(12) Uani 1 1 d . . .
O4 O 0.0875(2) 0.3043(3) 0.2225(2) 0.0797(16) Uani 1 1 d . . .
N2 N 0.1593(12) 0.1593(12) 0.0000 0.097(2) Uiso 0.50 4 d SP . .
C15 C 0.1288(18) 0.1763(18) 0.0586(14) 0.097(2) Uiso 0.25 1 d PD . .
C16 C 0.1606(10) 0.1606(10) 0.1205(13) 0.097(2) Uiso 0.50 2 d SPD . .
C17 C 0.1789(18) 0.238(3) 0.0000 0.097(2) Uiso 0.25 2 d SPD . .
C18 C 0.2524(13) 0.2524(13) 0.0000 0.097(2) Uiso 0.50 4 d SPD . .
C19 C 0.075(2) 0.176(3) 0.0000 0.097(2) Uiso 0.25 2 d SPD . .
C20 C 0.000(2) 0.161(3) 0.0000 0.097(2) Uiso 0.25 2 d SPD . .
N3 N 0.0000 0.0000 0.2500 0.097(2) Uiso 1 8 d S . .
C21 C -0.0010(8) 0.0646(10) 0.2205(9) 0.097(2) Uiso 0.50 1 d PD . .
C22 C 0.0718(5) 0.0718(5) 0.2121(7) 0.097(2) Uiso 1 2 d SD . .


_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 O3 2.326(4) 6_565 ?
Eu1 O3 2.326(4) 5 ?
Eu1 O3 2.326(4) 2_565 ?
Eu1 O3 2.326(4) . ?
Eu1 N1 2.603(5) 6_565 ?
Eu1 N1 2.603(5) . ?
Eu1 N1 2.603(5) 5 ?
Eu1 N1 2.603(5) 2_565 ?
S1 O4 1.437(5) . ?
S1 O2 1.463(5) . ?
S1 O3 1.469(4) . ?
S1 C4 1.760(6) . ?
N1 C9 1.340(8) . ?
N1 C14 1.360(7) . ?
C1 C2 1.510(6) 16 ?
C1 C2 1.510(6) . ?
C2 C3 1.387(7) . ?
C2 C7 1.402(7) . ?
C3 C4 1.398(7) . ?
C4 C5 1.387(8) . ?
C5 C6 1.366(8) . ?
C6 C7 1.393(7) . ?
C6 C8 1.530(7) . ?
C7 O1 1.368(6) . ?
C8 C6 1.530(7) 10 ?
C9 C10 1.394(9) . ?
C10 C11 1.339(10) . ?
C11 C12 1.397(9) . ?
C12 C14 1.402(7) . ?
C12 C13 1.458(8) . ?
C13 C13 1.341(15) 6_565 ?
C14 C14 1.435(12) 6_565 ?
N2 C15 1.41(3) 7 ?
N2 C15 1.41(3) 16 ?
N2 C15 1.41(3) 10 ?
N2 C15 1.41(3) . ?
N2 C17 1.56(6) 7 ?
N2 C17 1.56(6) . ?
N2 C19 1.64(5) . ?
N2 C19 1.64(5) 7 ?
C15 C15 1.29(7) 16 ?
C15 C16 1.475(19) . ?
C15 C19 1.61(4) . ?
C15 C17 1.97(5) . ?
C16 C15 1.475(19) 16 ?
C17 C18 1.430(19) . ?
C17 C17 1.61(10) 7 ?
C17 C15 1.97(5) 10 ?
C18 C17 1.430(19) 7 ?
C19 C20 1.46(2) . ?
C19 C15 1.61(4) 10 ?
N3 C21 1.383(19) . ?
N3 C21 1.383(19) 11_556 ?
N3 C21 1.383(19) 16 ?
N3 C21 1.383(19) 2 ?
N3 C21 1.383(19) 5 ?
N3 C21 1.383(19) 6 ?
N3 C21 1.383(19) 15 ?
N3 C21 1.383(19) 12_556 ?
C21 C21 1.25(4) 5 ?
C21 C22 1.411(14) . ?
C21 C21 1.72(3) 15 ?
C21 C21 1.77(4) 16 ?
C21 C22 1.97(2) 12_556 ?
C22 C21 1.411(14) 16 ?
C22 C21 1.97(2) 11_556 ?
C22 C21 1.97(2) 5 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Eu1 O3 104.2(2) 6_565 5 ?
O3 Eu1 O3 85.4(2) 6_565 2_565 ?
O3 Eu1 O3 146.6(2) 5 2_565 ?
O3 Eu1 O3 146.6(2) 6_565 . ?
O3 Eu1 O3 85.4(2) 5 . ?
O3 Eu1 O3 104.2(2) 2_565 . ?
O3 Eu1 N1 77.29(16) 6_565 6_565 ?
O3 Eu1 N1 137.37(15) 5 6_565 ?
O3 Eu1 N1 75.71(14) 2_565 6_565 ?
O3 Eu1 N1 74.40(16) . 6_565 ?
O3 Eu1 N1 74.40(15) 6_565 . ?
O3 Eu1 N1 75.71(14) 5 . ?
O3 Eu1 N1 137.36(15) 2_565 . ?
O3 Eu1 N1 77.29(16) . . ?
N1 Eu1 N1 63.5(2) 6_565 . ?
O3 Eu1 N1 137.36(15) 6_565 5 ?
O3 Eu1 N1 77.29(16) 5 5 ?
O3 Eu1 N1 74.40(16) 2_565 5 ?
O3 Eu1 N1 75.71(14) . 5 ?
N1 Eu1 N1 130.3(2) 6_565 5 ?
N1 Eu1 N1 143.0(2) . 5 ?
O3 Eu1 N1 75.71(14) 6_565 2_565 ?
O3 Eu1 N1 74.40(15) 5 2_565 ?
O3 Eu1 N1 77.29(16) 2_565 2_565 ?
O3 Eu1 N1 137.37(15) . 2_565 ?
N1 Eu1 N1 143.0(2) 6_565 2_565 ?
N1 Eu1 N1 130.3(2) . 2_565 ?
N1 Eu1 N1 63.5(2) 5 2_565 ?
O4 S1 O2 114.9(3) . . ?
O4 S1 O3 112.6(3) . . ?
O2 S1 O3 109.4(3) . . ?
O4 S1 C4 107.5(3) . . ?
O2 S1 C4 106.4(3) . . ?
O3 S1 C4 105.3(3) . . ?
C9 N1 C14 117.6(5) . . ?
C9 N1 Eu1 122.8(4) . . ?
C14 N1 Eu1 119.5(4) . . ?
C2 C1 C2 112.9(6) 16 . ?
C3 C2 C7 118.4(5) . . ?
C3 C2 C1 119.9(5) . . ?
C7 C2 C1 121.7(5) . . ?
C2 C3 C4 120.0(5) . . ?
C5 C4 C3 120.5(6) . . ?
C5 C4 S1 119.6(4) . . ?
C3 C4 S1 120.0(5) . . ?
C6 C5 C4 120.2(5) . . ?
C5 C6 C7 119.6(5) . . ?
C5 C6 C8 119.0(6) . . ?
C7 C6 C8 121.4(6) . . ?
O1 C7 C6 120.2(5) . . ?
O1 C7 C2 118.5(5) . . ?
C6 C7 C2 121.3(5) . . ?
C6 C8 C6 110.3(6) . 10 ?
N1 C9 C10 123.3(7) . . ?
C11 C10 C9 119.3(6) . . ?
C10 C11 C12 119.7(5) . . ?
C11 C12 C14 118.8(6) . . ?
C11 C12 C13 121.9(5) . . ?
C14 C12 C13 119.4(6) . . ?
C13 C13 C12 120.7(4) 6_565 . ?
N1 C14 C12 121.4(6) . . ?
N1 C14 C14 118.7(3) . 6_565 ?
C12 C14 C14 119.9(4) . 6_565 ?
S1 O3 Eu1 153.3(3) . . ?
C15 N2 C15 123(2) 7 16 ?
C15 N2 C15 54(2) 7 10 ?
C15 N2 C15 165(4) 16 10 ?
C15 N2 C15 165(4) 7 . ?
C15 N2 C15 54(2) 16 . ?
C15 N2 C15 123(2) 10 . ?
C15 N2 C17 82.8(19) 7 7 ?
C15 N2 C17 82.8(19) 16 7 ?
C15 N2 C17 110(2) 10 7 ?
C15 N2 C17 110(2) . 7 ?
C15 N2 C17 110(2) 7 . ?
C15 N2 C17 110(2) 16 . ?
C15 N2 C17 82.8(19) 10 . ?
C15 N2 C17 82.8(19) . . ?
C17 N2 C17 62(3) 7 . ?
C15 N2 C19 108(2) 7 . ?
C15 N2 C19 108(2) 16 . ?
C15 N2 C19 63.2(14) 10 . ?
C15 N2 C19 63.2(14) . . ?
C17 N2 C19 155(3) 7 . ?
C17 N2 C19 93(2) . . ?
C15 N2 C19 63.2(14) 7 7 ?
C15 N2 C19 63.2(14) 16 7 ?
C15 N2 C19 108(2) 10 7 ?
C15 N2 C19 108(2) . 7 ?
C17 N2 C19 93(2) 7 7 ?
C17 N2 C19 155(3) . 7 ?
C19 N2 C19 112(4) . 7 ?
C15 C15 N2 62.8(12) 16 . ?
C15 C15 C16 64.2(14) 16 . ?
N2 C15 C16 124(3) . . ?
C15 C15 C19 117(2) 16 . ?
N2 C15 C19 65(2) . . ?
C16 C15 C19 161(3) . . ?
C15 C15 C17 94.7(17) 16 . ?
N2 C15 C17 52(2) . . ?
C16 C15 C17 119(3) . . ?
C19 C15 C17 80(2) . . ?
C15 C16 C15 52(3) . 16 ?
C18 C17 N2 115(4) . . ?
C18 C17 C17 56(2) . 7 ?
N2 C17 C17 58.9(16) . 7 ?
C18 C17 C15 126(2) . 10 ?
N2 C17 C15 45.3(14) . 10 ?
C17 C17 C15 85.3(17) 7 10 ?
C18 C17 C15 126(2) . . ?
N2 C17 C15 45.3(14) . . ?
C17 C17 C15 85.3(17) 7 . ?
C15 C17 C15 78(2) 10 . ?
C17 C18 C17 69(5) 7 . ?
C20 C19 C15 128.8(19) . . ?
C20 C19 C15 128.8(19) . 10 ?
C15 C19 C15 101(4) . 10 ?
C20 C19 N2 157(5) . . ?
C15 C19 N2 51.3(18) . . ?
C15 C19 N2 51.3(18) 10 . ?
C21 N3 C21 101.8(6) . 11_556 ?
C21 N3 C21 79.7(13) . 16 ?
C21 N3 C21 53.7(16) 11_556 16 ?
C21 N3 C21 126.3(16) . 2 ?
C21 N3 C21 101.8(6) 11_556 2 ?
C21 N3 C21 76.7(13) 16 2 ?
C21 N3 C21 53.7(16) . 5 ?
C21 N3 C21 76.7(13) 11_556 5 ?
C21 N3 C21 101.8(6) 16 5 ?
C21 N3 C21 178.4(12) 2 5 ?
C21 N3 C21 178.4(12) . 6 ?
C21 N3 C21 79.7(13) 11_556 6 ?
C21 N3 C21 101.8(6) 16 6 ?
C21 N3 C21 53.7(16) 2 6 ?
C21 N3 C21 126.3(16) 5 6 ?
C21 N3 C21 76.7(13) . 15 ?
C21 N3 C21 178.4(12) 11_556 15 ?
C21 N3 C21 126.3(16) 16 15 ?
C21 N3 C21 79.7(13) 2 15 ?
C21 N3 C21 101.8(6) 5 15 ?
C21 N3 C21 101.8(6) 6 15 ?
C21 N3 C21 101.8(6) . 12_556 ?
C21 N3 C21 126.3(16) 11_556 12_556 ?
C21 N3 C21 178.4(12) 16 12_556 ?
C21 N3 C21 101.8(6) 2 12_556 ?
C21 N3 C21 79.7(13) 5 12_556 ?
C21 N3 C21 76.7(13) 6 12_556 ?
C21 N3 C21 53.7(16) 15 12_556 ?
C21 C21 N3 63.1(8) 5 . ?
C21 C21 C22 95.4(18) 5 . ?
N3 C21 C22 97.5(12) . . ?
C21 C21 C21 91.3(10) 5 15 ?
N3 C21 C21 51.6(7) . 15 ?
C22 C21 C21 140.2(9) . 15 ?
C21 C21 C21 88.7(10) 5 16 ?
N3 C21 C21 50.1(6) . 16 ?
C22 C21 C21 51.1(9) . 16 ?
C21 C21 C21 90.001(2) 15 16 ?
C21 C21 C22 45.4(11) 5 12_556 ?
N3 C21 C22 75.3(8) . 12_556 ?
C22 C21 C22 139.6(13) . 12_556 ?
C21 C21 C22 64.2(5) 15 12_556 ?
C21 C21 C22 122.4(7) 16 12_556 ?
C21 C22 C21 77.8(17) 16 . ?
C21 C22 C21 39.1(13) 16 11_556 ?
C21 C22 C21 76.8(14) . 11_556 ?
C21 C22 C21 76.8(14) 16 5 ?
C21 C22 C21 39.1(13) . 5 ?
C21 C22 C21 51.6(11) 11_556 5 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         1.685
_refine_diff_density_min         -2.726
_refine_diff_density_rms         0.131

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.246 0.241 -0.088 2221 640 ' '
_platon_squeeze_details          
;
P. van der Sluis and A. L. Spek, Acta Crystallogr., 1990, A46, 194.
;
###END


# Attachment 'compd-amine-revised.cif'

data_Nd-N(CH3)4
_database_code_depnum_ccdc_archive 'CCDC 739383'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '[(CH3)4N] Nd [C12H8N2]2 [C28H20S4O16] 3.5H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         '[(CH3)4N] Nd [C12H8N2]2 [C28H20S4O16] 3.5H2O'
_chemical_formula_sum            'C56 H55 N5 Nd O19.50 S4'
_chemical_formula_weight         1382.53

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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/m c m'

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

_cell_length_a                   18.9307(13)
_cell_length_b                   18.9307(13)
_cell_length_c                   20.989(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7521.9(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    145(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2824
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8235
_exptl_absorpt_correction_T_max  0.8821
_exptl_absorpt_process_details   
; SADABS, Sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      145(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 AXS Apex CCD diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            56661
_diffrn_reflns_av_R_equivalents  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0234
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.08
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3580
_reflns_number_gt                2699
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
All non-hydrogen atoms except the water oxygen atoms and the ammonium atoms
were refined anisotropically. The phenolic oxygen, water and ammonium
atoms were refined without hydrogen.
The partially occupied site of the ammonium cation with N2 atom was
refined with a charge constraint and the site occupation factor of N2
was set to 0.125.
The short contact C15...C17 might be due to
the disorder of the carbon atoms on the tetra-alkylammonium cations.
;

_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)+(0.1804P)²+83.9760P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.018(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3580
_refine_ls_number_parameters     196
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1514
_refine_ls_R_factor_gt           0.1259
_refine_ls_wR_factor_ref         0.3685
_refine_ls_wR_factor_gt          0.3533
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.136
_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
Nd1A Nd 0.0000 0.5000 0.2500 0.039(2) Uani 0.88(3) 4 d SP . .
Nd1B Nd 0.0000 0.5000 0.221(3) 0.039(2) Uani 0.059(16) 2 d SP . .
S1 S 0.07249(18) 0.3433(2) 0.16456(14) 0.0716(11) Uani 1 1 d . . .
N1 N 0.1199(5) 0.4540(5) 0.2999(5) 0.055(2) Uani 1 1 d . . .
C1 C 0.3494(8) 0.3494(8) 0.1697(7) 0.061(5) Uani 1 2 d S . .
H1A H 0.3414 0.3414 0.2158 0.073 Uiso 1 2 calc SR . .
H1B H 0.3862 0.3862 0.1653 0.073 Uiso 1 2 calc SR . .
C2 C 0.2817(6) 0.3753(6) 0.1397(4) 0.053(3) Uani 1 1 d . . .
C3 C 0.2160(6) 0.3519(6) 0.1635(5) 0.060(3) Uani 1 1 d . . .
H3 H 0.2145 0.3210 0.1992 0.072 Uiso 1 1 calc R . .
C4 C 0.1541(7) 0.3737(7) 0.1350(5) 0.065(3) Uani 1 1 d . . .
C5 C 0.1563(6) 0.4201(6) 0.0838(5) 0.061(3) Uani 1 1 d . . .
H5 H 0.1134 0.4369 0.0658 0.073 Uiso 1 1 calc R . .
C6 C 0.2185(6) 0.4416(6) 0.0593(4) 0.053(3) Uani 1 1 d . . .
C7 C 0.2818(6) 0.4195(6) 0.0875(4) 0.053(3) Uani 1 1 d . . .
C8 C 0.2178(9) 0.4884(9) 0.0000 0.058(4) Uani 1 2 d S . .
H8A H 0.1750 0.5185 0.0000 0.069 Uiso 1 2 calc SR . .
H8B H 0.2598 0.5196 0.0000 0.069 Uiso 1 2 calc SR . .
C9 C 0.1217(7) 0.4101(7) 0.3485(7) 0.073(4) Uani 1 1 d . . .
H9 H 0.0777 0.3948 0.3653 0.088 Uiso 1 1 calc R . .
C10 C 0.1828(8) 0.3840(7) 0.3776(7) 0.081(4) Uani 1 1 d . . .
H10 H 0.1801 0.3522 0.4125 0.097 Uiso 1 1 calc R . .
C11 C 0.2473(7) 0.4058(7) 0.3540(7) 0.070(4) Uani 1 1 d . . .
H11 H 0.2903 0.3898 0.3723 0.084 Uiso 1 1 calc R . .
C12 C 0.2470(5) 0.4528(6) 0.3017(6) 0.058(3) Uani 1 1 d . . .
C13 C 0.3127(6) 0.4781(7) 0.2740(6) 0.072(4) Uani 1 1 d . . .
H13 H 0.3564 0.4626 0.2913 0.086 Uiso 1 1 calc R . .
C14 C 0.1824(5) 0.4755(5) 0.2766(5) 0.049(2) Uani 1 1 d . . .
O1 O 0.3436(4) 0.4426(5) 0.0635(4) 0.069(2) Uani 1 1 d . . .
O2 O 0.0388(6) 0.3073(6) 0.1128(4) 0.090(3) Uani 1 1 d . . .
O3 O 0.0346(4) 0.4081(5) 0.1813(3) 0.066(2) Uani 1 1 d . . .
O4 O 0.0869(6) 0.2999(6) 0.2192(5) 0.100(4) Uani 1 1 d . . .
N2 N 0.186(3) 0.186(3) 0.0000 0.167(11) Uiso 0.50 4 d SPD . .
C15 C 0.238(3) 0.238(3) 0.0000 0.167(11) Uiso 0.50 4 d SPD . .
C16 C 0.114(2) 0.209(4) 0.0000 0.167(11) Uiso 0.50 2 d SPD . .
C17 C 0.191(3) 0.191(3) 0.0681(12) 0.167(11) Uiso 0.25 2 d SPD . .
N3 N 0.0000 0.0000 0.2500 0.167(11) Uiso 1 8 d SD . .
C18 C -0.0409(11) 0.0409(11) 0.2936(16) 0.167(11) Uiso 1 2 d SD . .
O1W O 0.5000 0.5000 0.2500 0.133(14) Uiso 1 8 d S . .
O2W O -0.0302(19) 0.3589(18) 0.0000 0.209(12) Uiso 1 2 d S . .
O3W O 0.309(2) 0.309(2) 0.5000 0.28(3) Uiso 1 4 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
Nd1A Nd1B 0.60(7) 5 ?
Nd1A Nd1B 0.60(7) . ?
Nd1A O3 2.353(8) . ?
Nd1A O3 2.353(8) 5 ?
Nd1A O3 2.353(8) 2_565 ?
Nd1A O3 2.353(8) 6_565 ?
Nd1A N1 2.647(9) 5 ?
Nd1A N1 2.647(9) 2_565 ?
Nd1A N1 2.647(9) 6_565 ?
Nd1A N1 2.647(9) . ?
Nd1B Nd1B 1.20(13) 5 ?
Nd1B O3 2.04(3) . ?
Nd1B O3 2.04(3) 2_565 ?
Nd1B N1 2.472(15) 5 ?
Nd1B N1 2.472(15) 6_565 ?
Nd1B O3 2.76(5) 5 ?
Nd1B O3 2.76(5) 6_565 ?
Nd1B N1 2.94(4) 2_565 ?
Nd1B N1 2.94(4) . ?
S1 O2 1.432(10) . ?
S1 O4 1.436(10) . ?
S1 O3 1.463(9) . ?
S1 C4 1.761(15) . ?
N1 C9 1.317(15) . ?
N1 C14 1.343(13) . ?
N1 Nd1B 2.472(15) 5 ?
C1 C2 1.511(13) . ?
C1 C2 1.511(13) 16 ?
C2 C7 1.378(15) . ?
C2 C3 1.412(17) . ?
C3 C4 1.379(16) . ?
C4 C5 1.390(16) . ?
C5 C6 1.347(16) . ?
C6 C7 1.402(14) . ?
C6 C8 1.527(14) . ?
C7 O1 1.345(14) . ?
C8 C6 1.527(14) 10 ?
C9 C10 1.399(18) . ?
C10 C11 1.38(2) . ?
C11 C12 1.414(19) . ?
C12 C14 1.398(14) . ?
C12 C13 1.454(17) . ?
C13 C13 1.31(3) 6_565 ?
C14 C14 1.45(2) 6_565 ?
O3 Nd1B 2.76(5) 5 ?
N2 C15 1.40(2) . ?
N2 C16 1.42(2) 7 ?
N2 C16 1.42(2) . ?
N2 C17 1.44(2) 10 ?
N2 C17 1.44(2) . ?
C15 C17 1.91(7) 10 ?
C15 C17 1.91(7) . ?
N3 C18 1.428(18) . ?
N3 C18 1.428(18) 12_556 ?
N3 C18 1.428(18) 2 ?
N3 C18 1.428(18) 11_556 ?

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
Nd1B Nd1A Nd1B 179.99(5) 5 . ?
Nd1B Nd1A O3 127.79(19) 5 . ?
Nd1B Nd1A O3 52.21(19) . . ?
Nd1B Nd1A O3 52.21(19) 5 5 ?
Nd1B Nd1A O3 127.79(19) . 5 ?
O3 Nd1A O3 84.6(4) . 5 ?
Nd1B Nd1A O3 127.79(19) 5 2_565 ?
Nd1B Nd1A O3 52.21(19) . 2_565 ?
O3 Nd1A O3 104.4(4) . 2_565 ?
O3 Nd1A O3 147.6(4) 5 2_565 ?
Nd1B Nd1A O3 52.21(19) 5 6_565 ?
Nd1B Nd1A O3 127.79(19) . 6_565 ?
O3 Nd1A O3 147.6(4) . 6_565 ?
O3 Nd1A O3 104.4(4) 5 6_565 ?
O3 Nd1A O3 84.6(4) 2_565 6_565 ?
Nd1B Nd1A N1 113.3(2) 5 5 ?
Nd1B Nd1A N1 66.7(2) . 5 ?
O3 Nd1A N1 75.7(3) . 5 ?
O3 Nd1A N1 76.1(3) 5 5 ?
O3 Nd1A N1 76.2(3) 2_565 5 ?
O3 Nd1A N1 136.4(3) 6_565 5 ?
Nd1B Nd1A N1 66.7(2) 5 2_565 ?
Nd1B Nd1A N1 113.3(2) . 2_565 ?
O3 Nd1A N1 136.4(3) . 2_565 ?
O3 Nd1A N1 76.2(3) 5 2_565 ?
O3 Nd1A N1 76.1(3) 2_565 2_565 ?
O3 Nd1A N1 75.7(3) 6_565 2_565 ?
N1 Nd1A N1 61.9(4) 5 2_565 ?
Nd1B Nd1A N1 113.3(2) 5 6_565 ?
Nd1B Nd1A N1 66.7(2) . 6_565 ?
O3 Nd1A N1 76.2(3) . 6_565 ?
O3 Nd1A N1 136.4(3) 5 6_565 ?
O3 Nd1A N1 75.7(3) 2_565 6_565 ?
O3 Nd1A N1 76.1(3) 6_565 6_565 ?
N1 Nd1A N1 133.4(4) 5 6_565 ?
N1 Nd1A N1 141.6(4) 2_565 6_565 ?
Nd1B Nd1A N1 66.7(2) 5 . ?
Nd1B Nd1A N1 113.3(2) . . ?
O3 Nd1A N1 76.1(3) . . ?
O3 Nd1A N1 75.7(3) 5 . ?
O3 Nd1A N1 136.4(3) 2_565 . ?
O3 Nd1A N1 76.2(3) 6_565 . ?
N1 Nd1A N1 141.6(4) 5 . ?
N1 Nd1A N1 133.4(4) 2_565 . ?
N1 Nd1A N1 61.9(4) 6_565 . ?
Nd1A Nd1B Nd1B 0.003(8) . 5 ?
Nd1A Nd1B O3 114.4(17) . . ?
Nd1B Nd1B O3 114.4(17) 5 . ?
Nd1A Nd1B O3 114.4(17) . 2_565 ?
Nd1B Nd1B O3 114.4(17) 5 2_565 ?
O3 Nd1B O3 131(3) . 2_565 ?
Nd1A Nd1B N1 100.4(15) . 5 ?
Nd1B Nd1B N1 100.4(15) 5 5 ?
O3 Nd1B N1 85.4(9) . 5 ?
O3 Nd1B N1 86.0(10) 2_565 5 ?
Nd1A Nd1B N1 100.4(15) . 6_565 ?
Nd1B Nd1B N1 100.4(15) 5 6_565 ?
O3 Nd1B N1 86.0(10) . 6_565 ?
O3 Nd1B N1 85.4(9) 2_565 6_565 ?
N1 Nd1B N1 159(3) 5 6_565 ?
Nd1A Nd1B O3 42.3(9) . 5 ?
Nd1B Nd1B O3 42.3(9) 5 5 ?
O3 Nd1B O3 81.0(9) . 5 ?
O3 Nd1B O3 140.0(16) 2_565 5 ?
N1 Nd1B O3 72.2(7) 5 5 ?
N1 Nd1B O3 125.0(16) 6_565 5 ?
Nd1A Nd1B O3 42.3(9) . 6_565 ?
Nd1B Nd1B O3 42.3(9) 5 6_565 ?
O3 Nd1B O3 140.0(16) . 6_565 ?
O3 Nd1B O3 81.0(9) 2_565 6_565 ?
N1 Nd1B O3 125.0(16) 5 6_565 ?
N1 Nd1B O3 72.2(7) 6_565 6_565 ?
O3 Nd1B O3 84.7(19) 5 6_565 ?
Nd1A Nd1B N1 55.9(11) . 2_565 ?
Nd1B Nd1B N1 55.9(11) 5 2_565 ?
O3 Nd1B N1 137.1(8) . 2_565 ?
O3 Nd1B N1 74.4(6) 2_565 2_565 ?
N1 Nd1B N1 59.7(6) 5 2_565 ?
N1 Nd1B N1 135.0(14) 6_565 2_565 ?
O3 Nd1B N1 65.7(11) 5 2_565 ?
O3 Nd1B N1 65.3(11) 6_565 2_565 ?
Nd1A Nd1B N1 55.9(11) . . ?
Nd1B Nd1B N1 55.9(11) 5 . ?
O3 Nd1B N1 74.4(6) . . ?
O3 Nd1B N1 137.1(8) 2_565 . ?
N1 Nd1B N1 135.0(14) 5 . ?
N1 Nd1B N1 59.7(6) 6_565 . ?
O3 Nd1B N1 65.3(11) 5 . ?
O3 Nd1B N1 65.7(11) 6_565 . ?
N1 Nd1B N1 112(2) 2_565 . ?
O2 S1 O4 114.7(8) . . ?
O2 S1 O3 111.3(6) . . ?
O4 S1 O3 112.4(6) . . ?
O2 S1 C4 106.2(6) . . ?
O4 S1 C4 107.5(6) . . ?
O3 S1 C4 103.9(6) . . ?
C9 N1 C14 116.8(10) . . ?
C9 N1 Nd1B 112.7(14) . 5 ?
C14 N1 Nd1B 129.5(12) . 5 ?
C9 N1 Nd1A 122.4(8) . . ?
C14 N1 Nd1A 120.8(7) . . ?
Nd1B N1 Nd1A 12.9(15) 5 . ?
C9 N1 Nd1B 129.9(10) . . ?
C14 N1 Nd1B 112.8(10) . . ?
Nd1B N1 Nd1B 24(3) 5 . ?
Nd1A N1 Nd1B 10.8(11) . . ?
C2 C1 C2 112.2(13) . 16 ?
C7 C2 C3 118.3(10) . . ?
C7 C2 C1 121.9(12) . . ?
C3 C2 C1 119.8(11) . . ?
C4 C3 C2 120.0(10) . . ?
C3 C4 C5 119.9(13) . . ?
C3 C4 S1 119.7(10) . . ?
C5 C4 S1 120.4(9) . . ?
C6 C5 C4 120.9(10) . . ?
C5 C6 C7 119.7(10) . . ?
C5 C6 C8 118.6(11) . . ?
C7 C6 C8 121.6(12) . . ?
O1 C7 C2 119.7(9) . . ?
O1 C7 C6 119.3(9) . . ?
C2 C7 C6 121.0(11) . . ?
C6 C8 C6 109.1(13) 10 . ?
N1 C9 C10 125.6(13) . . ?
C11 C10 C9 117.9(12) . . ?
C10 C11 C12 117.7(11) . . ?
C14 C12 C11 119.3(11) . . ?
C14 C12 C13 119.8(12) . . ?
C11 C12 C13 120.9(10) . . ?
C13 C13 C12 121.1(7) 6_565 . ?
N1 C14 C12 122.7(10) . . ?
N1 C14 C14 118.3(6) . 6_565 ?
C12 C14 C14 119.0(7) . 6_565 ?
S1 O3 Nd1B 166.1(14) . . ?
S1 O3 Nd1A 154.6(5) . . ?
Nd1B O3 Nd1A 13.4(17) . . ?
S1 O3 Nd1B 145.3(10) . 5 ?
Nd1B O3 Nd1B 23(3) . 5 ?
Nd1A O3 Nd1B 9.9(9) . 5 ?
C15 N2 C16 117(5) . 7 ?
C15 N2 C16 117(5) . . ?
C16 N2 C16 126(10) 7 . ?
C15 N2 C17 85(4) . 10 ?
C16 N2 C17 92.5(15) 7 10 ?
C16 N2 C17 92.5(15) . 10 ?
C15 N2 C17 85(4) . . ?
C16 N2 C17 92.5(15) 7 . ?
C16 N2 C17 92.5(15) . . ?
C17 N2 C17 169(7) 10 . ?
N2 C15 C17 48.4(17) . 10 ?
N2 C15 C17 48.4(17) . . ?
C17 C15 C17 97(3) 10 . ?
N2 C17 C15 47(2) . . ?
C18 N3 C18 114.3(18) . 12_556 ?
C18 N3 C18 100(3) . 2 ?
C18 N3 C18 114.3(18) 12_556 2 ?
C18 N3 C18 114.3(18) . 11_556 ?
C18 N3 C18 100(3) 12_556 11_556 ?
C18 N3 C18 114.3(18) 2 11_556 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         2.684
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.386

###END

data_Eu-N(C2H5)4
_database_code_depnum_ccdc_archive 'CCDC 739384'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            '[(C2H5)4N] Eu [C12H8N2]2 [C28H20S4O16] 5H2O'
_chemical_melting_point          ?
_chemical_formula_moiety         '[(C2H5)4N] Eu [C12H8N2]2 [C28H20S4O16] 5H2O'
_chemical_formula_sum            'C60 H66 Eu N5 O21 S4'
_chemical_formula_weight         1473.38

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'P 42/m c m'

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

_cell_length_a                   19.1147(4)
_cell_length_b                   19.1147(4)
_cell_length_c                   21.1495(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     7727.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    184(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3056
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7957
_exptl_absorpt_correction_T_max  0.8670
_exptl_absorpt_process_details   
; SADABS, Sheldrick, 1996
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      185(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 AXS Apex CCD diffractometer'
_diffrn_measurement_method       'ω scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            49026
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0180
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3660
_reflns_number_gt                2648
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'SMART (Bruker, 2001)'
_computing_cell_refinement       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT+ (Bruker, 1999)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXTL (1998)'

_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.
All non-hydrogen atoms except the water oxygen atoms and the ammonium
atoms were refined anisotropically. The phenolic oxygen atoms, water
and ammonium cations were refined without hydrogen.
The partially occupied site of the ammonium cation with N2 atom was
refined with a charge constraint and the site occupation factor of N2
was set to 0.125.
The short contact C15...C17, C16-C22 and C21-C22 might be due to
the disorder of the carbon atoms on the tetra-alkylammonium cations.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    none
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0006(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3660
_refine_ls_number_parameters     206
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0926
_refine_ls_wR_factor_ref         0.3644
_refine_ls_wR_factor_gt          0.3401
_refine_ls_goodness_of_fit_ref   1.551
_refine_ls_restrained_S_all      1.553
_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
Eu1 Eu 0.0000 0.5000 0.2500 0.0359(5) Uani 1 4 d S . .
S1 S 0.07324(11) 0.34609(12) 0.16747(10) 0.0549(7) Uani 1 1 d . . .
N1 N 0.1155(3) 0.4575(4) 0.3020(3) 0.0488(17) Uani 1 1 d . . .
C1 C 0.3473(4) 0.3473(4) 0.1685(4) 0.039(2) Uani 1 2 d S . .
H1A H 0.3836 0.3836 0.1624 0.047 Uiso 1 2 calc SR . .
H1B H 0.3408 0.3408 0.2146 0.047 Uiso 1 2 calc SR . .
C2 C 0.2796(4) 0.3727(4) 0.1401(3) 0.0391(17) Uani 1 1 d . . .
C3 C 0.2172(4) 0.3521(4) 0.1640(3) 0.0388(16) Uani 1 1 d . . .
H3 H 0.2165 0.3226 0.2001 0.047 Uiso 1 1 calc R . .
C4 C 0.1538(4) 0.3728(4) 0.1369(3) 0.0452(18) Uani 1 1 d . . .
C5 C 0.1555(4) 0.4194(4) 0.0840(3) 0.051(2) Uani 1 1 d . . .
H5 H 0.1130 0.4362 0.0663 0.061 Uiso 1 1 calc R . .
C6 C 0.2176(4) 0.4396(4) 0.0590(3) 0.0416(17) Uani 1 1 d . . .
C7 C 0.2804(4) 0.4165(4) 0.0873(3) 0.0411(17) Uani 1 1 d . . .
C8 C 0.2163(6) 0.4837(6) 0.0000 0.049(3) Uani 1 2 d S . .
H8A H 0.2573 0.5153 0.0000 0.059 Uiso 1 2 calc SR . .
H8B H 0.1736 0.5130 0.0000 0.059 Uiso 1 2 calc SR . .
C9 C 0.1159(5) 0.4138(5) 0.3513(5) 0.062(2) Uani 1 1 d . . .
H9 H 0.0725 0.3984 0.3681 0.075 Uiso 1 1 calc R . .
C10 C 0.1791(6) 0.3897(5) 0.3795(5) 0.072(3) Uani 1 1 d . . .
H10 H 0.1778 0.3598 0.4153 0.086 Uiso 1 1 calc R . .
C11 C 0.2395(5) 0.4096(5) 0.3550(5) 0.066(3) Uani 1 1 d . . .
H11 H 0.2818 0.3935 0.3736 0.079 Uiso 1 1 calc R . .
C12 C 0.2424(4) 0.4541(4) 0.3022(4) 0.0432(18) Uani 1 1 d . . .
C13 C 0.3076(4) 0.4777(5) 0.2763(4) 0.062(3) Uani 1 1 d . . .
H13 H 0.3505 0.4631 0.2947 0.075 Uiso 1 1 calc R . .
C14 C 0.1784(4) 0.4765(4) 0.2770(4) 0.0434(18) Uani 1 1 d . . .
O1 O 0.3421(3) 0.4390(3) 0.0636(3) 0.0620(16) Uani 1 1 d . . .
O2 O 0.0376(3) 0.3085(4) 0.1170(3) 0.0700(18) Uani 1 1 d . . .
O3 O 0.0352(3) 0.4103(4) 0.1830(3) 0.0596(17) Uani 1 1 d . . .
O4 O 0.0862(3) 0.3042(4) 0.2220(3) 0.078(2) Uani 1 1 d . . .
N2 N 0.1565(16) 0.1565(16) 0.0000 0.103(4) Uiso 0.50 4 d SP . .
C15 C 0.126(3) 0.180(3) 0.0626(19) 0.103(4) Uiso 0.25 1 d PD . .
C16 C 0.1600(14) 0.1600(14) 0.1230(18) 0.103(4) Uiso 0.50 2 d SPD . .
C17 C 0.179(2) 0.239(4) 0.0000 0.103(4) Uiso 0.25 2 d SPD . .
C18 C 0.2526(18) 0.2526(18) 0.0000 0.103(4) Uiso 0.50 4 d SPD . .
C19 C 0.074(3) 0.180(4) 0.0000 0.103(4) Uiso 0.25 2 d SPD . .
C20 C -0.002(3) 0.168(5) 0.0000 0.103(4) Uiso 0.25 2 d SPD . .
N3 N 0.0000 0.0000 0.2500 0.103(4) Uiso 1 8 d S . .
C21 C 0.0007(10) 0.0610(15) 0.2200(13) 0.103(4) Uiso 0.50 1 d PD . .
C22 C 0.0745(7) 0.0745(7) 0.2156(9) 0.103(4) Uiso 1 2 d SD . .
O1W O -0.0197(9) 0.3554(9) 0.0000 0.140(5) Uiso 1 2 d S . .
O2W O 0.4240(8) 0.4240(8) 0.4072(9) 0.198(7) Uiso 1 2 d S . .
O3W O 0.3001(15) 0.3001(15) 0.5000 0.253(16) Uiso 1 4 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
Eu1 O3 2.324(6) 6_565 ?
Eu1 O3 2.324(6) 5 ?
Eu1 O3 2.324(6) 2_565 ?
Eu1 O3 2.324(6) . ?
Eu1 N1 2.598(6) . ?
Eu1 N1 2.598(6) 5 ?
Eu1 N1 2.598(6) 6_565 ?
Eu1 N1 2.598(6) 2_565 ?
S1 O4 1.425(6) . ?
S1 O2 1.456(7) . ?
S1 O3 1.464(6) . ?
S1 C4 1.746(9) . ?
N1 C9 1.334(11) . ?
N1 C14 1.364(10) . ?
C1 C2 1.507(8) 16 ?
C1 C2 1.507(8) . ?
C2 C3 1.354(10) . ?
C2 C7 1.396(10) . ?
C3 C4 1.398(10) . ?
C4 C5 1.431(11) . ?
C5 C6 1.355(10) . ?
C6 C7 1.413(9) . ?
C6 C8 1.506(9) . ?
C7 O1 1.350(8) . ?
C8 C6 1.506(9) 10 ?
C9 C10 1.423(12) . ?
C10 C11 1.321(14) . ?
C11 C12 1.406(13) . ?
C12 C14 1.400(10) . ?
C12 C13 1.434(11) . ?
C13 C13 1.40(2) 6_565 ?
C14 C14 1.452(16) 6_565 ?
N2 C15 1.51(5) . ?
N2 C15 1.51(5) 7 ?
N2 C15 1.51(5) 10 ?
N2 C15 1.51(5) 16 ?
N2 C17 1.64(8) . ?
N2 C17 1.64(8) 7 ?
N2 C19 1.65(6) . ?
N2 C19 1.65(6) 7 ?
C15 C15 1.46(9) 16 ?
C15 C16 1.482(19) . ?
C15 C19 1.67(5) . ?
C15 C17 2.00(7) . ?
C16 C15 1.482(19) 16 ?
C17 C18 1.44(2) . ?
C17 C17 1.64(13) 7 ?
C17 C15 2.00(7) 10 ?
C18 C17 1.44(2) 7 ?
C19 C20 1.46(2) . ?
C19 C15 1.67(5) 10 ?
N3 C21 1.33(3) 15 ?
N3 C21 1.33(3) 11_556 ?
N3 C21 1.33(3) 5 ?
N3 C21 1.33(3) 2 ?
N3 C21 1.33(3) 16 ?
N3 C21 1.33(3) 12_556 ?
N3 C21 1.33(3) 6 ?
N3 C21 1.33(3) . ?
C21 C21 1.27(5) 5 ?
C21 C22 1.436(16) . ?
C21 C21 1.63(5) 16 ?
C21 C21 1.67(5) 15 ?
C21 C22 2.00(3) 12_556 ?
C22 C21 1.436(16) 16 ?
C22 C21 2.00(3) 11_556 ?
C22 C21 2.00(3) 5 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Eu1 O3 104.9(3) 6_565 5 ?
O3 Eu1 O3 84.9(3) 6_565 2_565 ?
O3 Eu1 O3 146.4(3) 5 2_565 ?
O3 Eu1 O3 146.4(3) 6_565 . ?
O3 Eu1 O3 84.9(3) 5 . ?
O3 Eu1 O3 104.9(3) 2_565 . ?
O3 Eu1 N1 74.1(2) 6_565 . ?
O3 Eu1 N1 75.9(2) 5 . ?
O3 Eu1 N1 137.3(2) 2_565 . ?
O3 Eu1 N1 77.4(2) . . ?
O3 Eu1 N1 137.3(2) 6_565 5 ?
O3 Eu1 N1 77.4(2) 5 5 ?
O3 Eu1 N1 74.1(2) 2_565 5 ?
O3 Eu1 N1 75.9(2) . 5 ?
N1 Eu1 N1 143.5(3) . 5 ?
O3 Eu1 N1 77.4(2) 6_565 6_565 ?
O3 Eu1 N1 137.3(2) 5 6_565 ?
O3 Eu1 N1 75.9(2) 2_565 6_565 ?
O3 Eu1 N1 74.1(2) . 6_565 ?
N1 Eu1 N1 63.6(3) . 6_565 ?
N1 Eu1 N1 129.9(3) 5 6_565 ?
O3 Eu1 N1 75.9(2) 6_565 2_565 ?
O3 Eu1 N1 74.1(2) 5 2_565 ?
O3 Eu1 N1 77.4(2) 2_565 2_565 ?
O3 Eu1 N1 137.3(2) . 2_565 ?
N1 Eu1 N1 129.9(3) . 2_565 ?
N1 Eu1 N1 63.6(3) 5 2_565 ?
N1 Eu1 N1 143.5(3) 6_565 2_565 ?
O4 S1 O2 113.4(5) . . ?
O4 S1 O3 112.1(4) . . ?
O2 S1 O3 110.2(4) . . ?
O4 S1 C4 108.1(4) . . ?
O2 S1 C4 106.6(4) . . ?
O3 S1 C4 106.0(4) . . ?
C9 N1 C14 117.7(7) . . ?
C9 N1 Eu1 122.1(5) . . ?
C14 N1 Eu1 120.1(5) . . ?
C2 C1 C2 113.3(8) 16 . ?
C3 C2 C7 118.9(6) . . ?
C3 C2 C1 121.0(7) . . ?
C7 C2 C1 120.2(7) . . ?
C2 C3 C4 121.9(7) . . ?
C3 C4 C5 118.6(7) . . ?
C3 C4 S1 122.0(6) . . ?
C5 C4 S1 119.4(6) . . ?
C6 C5 C4 120.1(7) . . ?
C5 C6 C7 119.4(7) . . ?
C5 C6 C8 117.9(7) . . ?
C7 C6 C8 122.6(8) . . ?
O1 C7 C2 119.8(6) . . ?
O1 C7 C6 119.1(6) . . ?
C2 C7 C6 121.1(7) . . ?
C6 C8 C6 111.9(9) . 10 ?
N1 C9 C10 122.3(9) . . ?
C11 C10 C9 119.0(9) . . ?
C10 C11 C12 121.3(8) . . ?
C14 C12 C11 117.0(7) . . ?
C14 C12 C13 121.2(8) . . ?
C11 C12 C13 121.8(7) . . ?
C13 C13 C12 119.6(5) 6_565 . ?
N1 C14 C12 122.7(7) . . ?
N1 C14 C14 118.1(4) . 6_565 ?
C12 C14 C14 119.2(5) . 6_565 ?
S1 O3 Eu1 154.0(4) . . ?
C15 N2 C15 174(5) . 7 ?
C15 N2 C15 122(3) . 10 ?
C15 N2 C15 58(3) 7 10 ?
C15 N2 C15 58(3) . 16 ?
C15 N2 C15 122(3) 7 16 ?
C15 N2 C15 174(5) 10 16 ?
C15 N2 C17 79(2) . . ?
C15 N2 C17 107(3) 7 . ?
C15 N2 C17 79(2) 10 . ?
C15 N2 C17 107(3) 16 . ?
C15 N2 C17 107(3) . 7 ?
C15 N2 C17 79(2) 7 7 ?
C15 N2 C17 107(3) 10 7 ?
C15 N2 C17 79(2) 16 7 ?
C17 N2 C17 60(4) . 7 ?
C15 N2 C19 63.5(17) . . ?
C15 N2 C19 113(2) 7 . ?
C15 N2 C19 63.5(17) 10 . ?
C15 N2 C19 113(2) 16 . ?
C17 N2 C19 89(3) . . ?
C17 N2 C19 149(4) 7 . ?
C15 N2 C19 113(2) . 7 ?
C15 N2 C19 63.5(17) 7 7 ?
C15 N2 C19 113(2) 10 7 ?
C15 N2 C19 63.5(17) 16 7 ?
C17 N2 C19 149(4) . 7 ?
C17 N2 C19 89(3) 7 7 ?
C19 N2 C19 122(6) . 7 ?
C15 C15 C16 61(2) 16 . ?
C15 C15 N2 61.2(15) 16 . ?
C16 C15 N2 121(3) . . ?
C15 C15 C19 115(3) 16 . ?
C16 C15 C19 161(5) . . ?
N2 C15 C19 62(3) . . ?
C15 C15 C17 93(2) 16 . ?
C16 C15 C17 120(3) . . ?
N2 C15 C17 53(3) . . ?
C19 C15 C17 77(3) . . ?
C15 C16 C15 59(4) 16 . ?
C18 C17 C17 55(3) . 7 ?
C18 C17 N2 115(5) . . ?
C17 C17 N2 60(2) 7 . ?
C18 C17 C15 126(3) . . ?
C17 C17 C15 87(2) 7 . ?
N2 C17 C15 48(2) . . ?
C18 C17 C15 126(3) . 10 ?
C17 C17 C15 87(2) 7 10 ?
N2 C17 C15 48(2) . 10 ?
C15 C17 C15 83(3) . 10 ?
C17 C18 C17 70(6) . 7 ?
C20 C19 N2 155(7) . . ?
C20 C19 C15 127(2) . . ?
N2 C19 C15 54(2) . . ?
C20 C19 C15 127(2) . 10 ?
N2 C19 C15 54(2) . 10 ?
C15 C19 C15 105(5) . 10 ?
C21 N3 C21 178.8(17) 15 11_556 ?
C21 N3 C21 103.2(10) 15 5 ?
C21 N3 C21 77.9(18) 11_556 5 ?
C21 N3 C21 75.7(18) 15 2 ?
C21 N3 C21 103.2(10) 11_556 2 ?
C21 N3 C21 178.8(17) 5 2 ?
C21 N3 C21 123(2) 15 16 ?
C21 N3 C21 57(2) 11_556 16 ?
C21 N3 C21 103.2(10) 5 16 ?
C21 N3 C21 77.9(18) 2 16 ?
C21 N3 C21 57(2) 15 12_556 ?
C21 N3 C21 123(2) 11_556 12_556 ?
C21 N3 C21 75.7(18) 5 12_556 ?
C21 N3 C21 103.2(10) 2 12_556 ?
C21 N3 C21 178.8(17) 16 12_556 ?
C21 N3 C21 103.2(10) 15 6 ?
C21 N3 C21 75.7(18) 11_556 6 ?
C21 N3 C21 123(2) 5 6 ?
C21 N3 C21 57(2) 2 6 ?
C21 N3 C21 103.2(10) 16 6 ?
C21 N3 C21 77.9(18) 12_556 6 ?
C21 N3 C21 77.9(18) 15 . ?
C21 N3 C21 103.2(10) 11_556 . ?
C21 N3 C21 57(2) 5 . ?
C21 N3 C21 123(2) 2 . ?
C21 N3 C21 75.7(18) 16 . ?
C21 N3 C21 103.2(10) 12_556 . ?
C21 N3 C21 178.8(17) 6 . ?
C21 C21 N3 61.4(12) 5 . ?
C21 C21 C22 95(2) 5 . ?
N3 C21 C22 101.5(18) . . ?
C21 C21 C21 90.9(12) 5 16 ?
N3 C21 C21 52.2(9) . 16 ?
C22 C21 C21 55.5(13) . 16 ?
C21 C21 C21 89.1(12) 5 15 ?
N3 C21 C21 51.1(9) . 15 ?
C22 C21 C21 145.2(13) . 15 ?
C21 C21 C21 90.000(3) 16 15 ?
C21 C21 C22 45.7(13) 5 12_556 ?
N3 C21 C22 77.3(11) . 12_556 ?
C22 C21 C22 136.7(17) . 12_556 ?
C21 C21 C22 126.9(10) 16 12_556 ?
C21 C21 C22 65.3(8) 15 12_556 ?
C21 C22 C21 69(3) . 16 ?
C21 C22 C21 73(2) . 11_556 ?
C21 C22 C21 39.3(18) 16 11_556 ?
C21 C22 C21 39.3(18) . 5 ?
C21 C22 C21 73(2) 16 5 ?
C21 C22 C21 49.4(15) 11_556 5 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.807
_refine_diff_density_min         -2.852
_refine_diff_density_rms         0.223

