Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Stuart Batten'
_publ_contact_author_address     
;
School of Chemistry
Monash University
Clayton
Vic
3800
AUSTRALIA
;

_publ_contact_author_email       STUART.BATTEN@SCI.MONASH.EDU.AU

_publ_section_title              
;
Homoleptic 12-Coordinate Lanthanoids With ?2-Nitroso
Ligands
;
loop_
_publ_author_name
'S. Batten'
'Anthony S. R. Chesman'
'G. Deacon'
'Ekaterina I. Izgorodina'
'David Turner'

data_c:\docume~1\owner\mydocu~1\xray\anthony\ac1591\swap
_database_code_depnum_ccdc_archive 'CCDC 633462'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraethylammonium hexa(dicyanonitrosomethanido)cerate
;
_chemical_name_common            
'tetraethylammonium hexa(dicyanonitrosomethanido)cerate'
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 Ce1 N18 O6,3(N1 C8 H20)'
_chemical_formula_sum            'C42 H60 Ce1 N21 O6'
_chemical_formula_weight         1095.23

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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   Ia-3

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

_cell_length_a                   22.535(3)
_cell_length_b                   22.535(3)
_cell_length_c                   22.535(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11444(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    12456
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       plate
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4520
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_type   Empirical
_exptl_absorpt_correction_T_min  0.8754
_exptl_absorpt_correction_T_max  0.9666
_exptl_absorpt_process_details   SORTAV

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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  'Nonius KappaCCD'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10633
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         27.48
_reflns_number_total             2199
_reflns_number_gt                1164
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Hooft, 1999)'
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0433P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2199
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0303
_refine_ls_wR_factor_ref         0.0863
_refine_ls_wR_factor_gt          0.0681
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_restrained_S_all      0.920
_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
Ce1 Ce 0.5000 0.5000 0.5000 0.02302(12) Uani 1 6 d S . .
O1 O 0.41879(8) 0.55642(8) 0.44615(8) 0.0335(5) Uani 1 1 d . . .
N1 N 0.43403(9) 0.51606(10) 0.40797(10) 0.0304(5) Uani 1 1 d . . .
C1 C 0.40539(12) 0.51323(11) 0.35750(12) 0.0292(7) Uani 1 1 d . . .
N2 N 0.43569(12) 0.43012(12) 0.28552(11) 0.0547(7) Uani 1 1 d . . .
C3 C 0.35851(12) 0.55393(13) 0.34402(11) 0.0335(7) Uani 1 1 d . . .
C2 C 0.42173(13) 0.46734(14) 0.31765(13) 0.0392(8) Uani 1 1 d . . .
N4 N 0.65523(14) 0.5000 0.2500 0.0319(8) Uani 1 2 d S . .
C4 C 0.61695(13) 0.49023(12) 0.19548(12) 0.0364(7) Uani 1 1 d . . .
H4A H 0.5941 0.5269 0.1877 0.044 Uiso 1 1 calc R . .
H4B H 0.6433 0.4835 0.1610 0.044 Uiso 1 1 calc R . .
N3 N 0.32116(11) 0.58736(12) 0.33573(10) 0.0485(7) Uani 1 1 d . . .
C5 C 0.57402(14) 0.43891(14) 0.19978(13) 0.0540(9) Uani 1 1 d . . .
H5A H 0.5961 0.4021 0.2070 0.081 Uiso 1 1 calc R . .
H5B H 0.5518 0.4355 0.1626 0.081 Uiso 1 1 calc R . .
H5C H 0.5463 0.4459 0.2326 0.081 Uiso 1 1 calc R . .
C6 C 0.69313(13) 0.44598(14) 0.26312(12) 0.0441(8) Uani 1 1 d . . .
H6A H 0.7178 0.4546 0.2984 0.053 Uiso 1 1 calc R . .
H6B H 0.6666 0.4125 0.2735 0.053 Uiso 1 1 calc R . .
C7 C 0.73369(14) 0.42629(16) 0.21299(15) 0.0645(10) Uani 1 1 d . . .
H7A H 0.7097 0.4140 0.1789 0.097 Uiso 1 1 calc R . .
H7B H 0.7581 0.3928 0.2263 0.097 Uiso 1 1 calc R . .
H7C H 0.7595 0.4593 0.2014 0.097 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ce1 0.02302(12) 0.02302(12) 0.02302(12) -0.00170(10) -0.00170(10) -0.00170(10)
O1 0.0351(11) 0.0340(11) 0.0315(11) -0.0063(9) -0.0047(9) 0.0024(9)
N1 0.0314(14) 0.0291(13) 0.0307(14) -0.0011(10) -0.0007(11) -0.0027(10)
C1 0.0299(16) 0.0319(17) 0.0260(16) 0.0011(12) -0.0054(13) -0.0018(12)
N2 0.074(2) 0.0497(18) 0.0401(17) -0.0047(14) -0.0078(14) 0.0040(15)
C3 0.0328(17) 0.0441(18) 0.0235(15) -0.0008(13) -0.0039(13) -0.0040(14)
C2 0.0434(19) 0.041(2) 0.0328(19) 0.0016(15) -0.0061(14) -0.0003(15)
N4 0.0372(19) 0.039(2) 0.0198(16) 0.0001(15) 0.000 0.000
C4 0.0413(18) 0.046(2) 0.0220(16) 0.0024(13) -0.0036(13) -0.0026(14)
N3 0.0386(16) 0.0623(19) 0.0447(16) 0.0042(14) -0.0051(13) 0.0107(14)
C5 0.058(2) 0.064(2) 0.0396(19) -0.0011(17) -0.0123(16) -0.0162(18)
C6 0.0448(19) 0.050(2) 0.037(2) -0.0005(14) -0.0056(14) 0.0108(16)
C7 0.070(2) 0.078(3) 0.045(2) -0.011(2) 0.0055(18) 0.026(2)

_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
Ce1 O1 2.5374(18) 3 ?
Ce1 O1 2.5374(18) . ?
Ce1 O1 2.5374(18) 26_666 ?
Ce1 O1 2.5374(18) 2 ?
Ce1 O1 2.5374(18) 27_666 ?
Ce1 O1 2.5374(18) 25_666 ?
Ce1 N1 2.577(2) 3 ?
Ce1 N1 2.577(2) 2 ?
Ce1 N1 2.577(2) . ?
Ce1 N1 2.577(2) 27_666 ?
Ce1 N1 2.577(2) 26_666 ?
Ce1 N1 2.577(2) 25_666 ?
O1 N1 1.298(2) . ?
N1 C1 1.309(3) . ?
C1 C2 1.418(4) . ?
C1 C3 1.432(4) . ?
N2 C2 1.152(3) . ?
C3 N3 1.145(3) . ?
N4 C4 1.517(3) . ?
N4 C4 1.517(3) 11_565 ?
N4 C6 1.516(3) 11_565 ?
N4 C6 1.516(3) . ?
C4 C5 1.511(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.519(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ce1 O1 104.84(4) 3 . ?
O1 Ce1 O1 75.16(4) 3 26_666 ?
O1 Ce1 O1 75.16(4) . 26_666 ?
O1 Ce1 O1 104.84(4) 3 2 ?
O1 Ce1 O1 104.84(4) . 2 ?
O1 Ce1 O1 180.0 26_666 2 ?
O1 Ce1 O1 180.0 3 27_666 ?
O1 Ce1 O1 75.16(4) . 27_666 ?
O1 Ce1 O1 104.84(4) 26_666 27_666 ?
O1 Ce1 O1 75.16(4) 2 27_666 ?
O1 Ce1 O1 75.16(4) 3 25_666 ?
O1 Ce1 O1 180.0 . 25_666 ?
O1 Ce1 O1 104.84(4) 26_666 25_666 ?
O1 Ce1 O1 75.16(4) 2 25_666 ?
O1 Ce1 O1 104.84(4) 27_666 25_666 ?
O1 Ce1 N1 29.39(5) 3 3 ?
O1 Ce1 N1 103.22(6) . 3 ?
O1 Ce1 N1 102.96(7) 26_666 3 ?
O1 Ce1 N1 77.04(7) 2 3 ?
O1 Ce1 N1 150.61(5) 27_666 3 ?
O1 Ce1 N1 76.78(6) 25_666 3 ?
O1 Ce1 N1 103.22(6) 3 2 ?
O1 Ce1 N1 77.04(7) . 2 ?
O1 Ce1 N1 150.61(5) 26_666 2 ?
O1 Ce1 N1 29.39(5) 2 2 ?
O1 Ce1 N1 76.78(6) 27_666 2 ?
O1 Ce1 N1 102.96(7) 25_666 2 ?
N1 Ce1 N1 74.33(8) 3 2 ?
O1 Ce1 N1 77.04(7) 3 . ?
O1 Ce1 N1 29.39(5) . . ?
O1 Ce1 N1 76.78(6) 26_666 . ?
O1 Ce1 N1 103.22(6) 2 . ?
O1 Ce1 N1 102.96(7) 27_666 . ?
O1 Ce1 N1 150.61(5) 25_666 . ?
N1 Ce1 N1 74.33(8) 3 . ?
N1 Ce1 N1 74.33(8) 2 . ?
O1 Ce1 N1 150.61(5) 3 27_666 ?
O1 Ce1 N1 76.78(6) . 27_666 ?
O1 Ce1 N1 77.04(7) 26_666 27_666 ?
O1 Ce1 N1 102.96(7) 2 27_666 ?
O1 Ce1 N1 29.39(5) 27_666 27_666 ?
O1 Ce1 N1 103.22(6) 25_666 27_666 ?
N1 Ce1 N1 180.00(7) 3 27_666 ?
N1 Ce1 N1 105.67(8) 2 27_666 ?
N1 Ce1 N1 105.67(8) . 27_666 ?
O1 Ce1 N1 76.78(6) 3 26_666 ?
O1 Ce1 N1 102.96(7) . 26_666 ?
O1 Ce1 N1 29.39(5) 26_666 26_666 ?
O1 Ce1 N1 150.61(5) 2 26_666 ?
O1 Ce1 N1 103.22(6) 27_666 26_666 ?
O1 Ce1 N1 77.04(7) 25_666 26_666 ?
N1 Ce1 N1 105.67(8) 3 26_666 ?
N1 Ce1 N1 180.00(7) 2 26_666 ?
N1 Ce1 N1 105.67(8) . 26_666 ?
N1 Ce1 N1 74.33(8) 27_666 26_666 ?
O1 Ce1 N1 102.96(7) 3 25_666 ?
O1 Ce1 N1 150.61(5) . 25_666 ?
O1 Ce1 N1 103.22(6) 26_666 25_666 ?
O1 Ce1 N1 76.78(6) 2 25_666 ?
O1 Ce1 N1 77.04(7) 27_666 25_666 ?
O1 Ce1 N1 29.39(5) 25_666 25_666 ?
N1 Ce1 N1 105.67(8) 3 25_666 ?
N1 Ce1 N1 105.67(8) 2 25_666 ?
N1 Ce1 N1 180.0 . 25_666 ?
N1 Ce1 N1 74.33(8) 27_666 25_666 ?
N1 Ce1 N1 74.33(8) 26_666 25_666 ?
N1 O1 Ce1 77.01(13) . . ?
O1 N1 C1 118.7(2) . . ?
O1 N1 Ce1 73.60(13) . . ?
C1 N1 Ce1 167.57(19) . . ?
N1 C1 C2 117.2(2) . . ?
N1 C1 C3 121.1(2) . . ?
C2 C1 C3 121.6(2) . . ?
N3 C3 C1 177.0(3) . . ?
N2 C2 C1 179.2(3) . . ?
C4 N4 C4 110.7(3) . 11_565 ?
C4 N4 C6 106.19(14) . 11_565 ?
C4 N4 C6 111.20(15) 11_565 11_565 ?
C4 N4 C6 111.20(15) . . ?
C4 N4 C6 106.19(14) 11_565 . ?
C6 N4 C6 111.4(3) 11_565 . ?
C5 C4 N4 115.0(2) . . ?
C5 C4 H4A 108.5 . . ?
N4 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
N4 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N4 115.4(2) . . ?
C7 C6 H6A 108.4 . . ?
N4 C6 H6A 108.4 . . ?
C7 C6 H6B 108.4 . . ?
N4 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.076

# Attachment 'Gd_Et.CIF'

data_C:\AC1922\AC1922.CIF
_database_code_depnum_ccdc_archive 'CCDC 633463'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraethylammonium hexa(dicyanonitrosomethanido)gadolinium(III)
;
_chemical_name_common            
;tetraethylammonium
hexa(dicyanonitrosomethanido)gadolinium(iii)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 Gd1 N18 O6, 3(C8 H20 N1)'
_chemical_formula_sum            'C42 H60 Gd1 N21 O6'
_chemical_formula_weight         1112.36

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           cubic
_symmetry_space_group_name_H-M   Ia-3

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

_cell_length_a                   22.3927(4)
_cell_length_b                   22.3927(4)
_cell_length_c                   22.3927(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11228.4(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(1)
_cell_measurement_reflns_used    11568
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4568
_exptl_absorpt_coefficient_mu    1.242
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6921
_exptl_absorpt_correction_T_max  0.8552
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(1)
_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 X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11568
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2162
_reflns_number_gt                1468
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker)'
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2162
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0261
_refine_ls_wR_factor_ref         0.0685
_refine_ls_wR_factor_gt          0.0580
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_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
Gd1 Gd 0.5000 0.5000 0.5000 0.01901(9) Uani 1 6 d S . .
O1 O 0.42024(7) 0.55604(7) 0.44921(7) 0.0275(4) Uani 1 1 d . . .
N4 N 0.65884(13) 0.5000 0.2500 0.0279(6) Uani 1 2 d S . .
N1 N 0.43596(8) 0.51610(8) 0.41054(9) 0.0256(4) Uani 1 1 d . . .
N3 N 0.32418(10) 0.58966(11) 0.33708(10) 0.0421(6) Uani 1 1 d . . .
N2 N 0.43849(12) 0.43114(11) 0.28649(11) 0.0497(6) Uani 1 1 d . . .
C3 C 0.36103(11) 0.55589(12) 0.34567(10) 0.0306(5) Uani 1 1 d . . .
C1 C 0.40786(10) 0.51433(10) 0.35932(10) 0.0255(5) Uani 1 1 d . . .
C2 C 0.42473(12) 0.46840(12) 0.31882(11) 0.0339(6) Uani 1 1 d . . .
C4 C 0.62065(11) 0.48973(12) 0.19534(11) 0.0333(6) Uani 1 1 d . . .
H4A H 0.5977 0.5266 0.1871 0.040 Uiso 1 1 calc R . .
H4B H 0.6473 0.4826 0.1608 0.040 Uiso 1 1 calc R . .
C5 C 0.57750(13) 0.43830(13) 0.19996(12) 0.0466(7) Uani 1 1 d . . .
H5A H 0.5498 0.4455 0.2330 0.070 Uiso 1 1 calc R . .
H5B H 0.5997 0.4013 0.2073 0.070 Uiso 1 1 calc R . .
H5C H 0.5550 0.4347 0.1626 0.070 Uiso 1 1 calc R . .
C6 C 0.69725(12) 0.44606(13) 0.26347(11) 0.0384(7) Uani 1 1 d . . .
H6A H 0.7219 0.4551 0.2990 0.046 Uiso 1 1 calc R . .
H6B H 0.6707 0.4123 0.2740 0.046 Uiso 1 1 calc R . .
C7 C 0.73835(14) 0.42610(16) 0.21355(14) 0.0563(9) Uani 1 1 d . . .
H7A H 0.7643 0.4593 0.2019 0.084 Uiso 1 1 calc R . .
H7B H 0.7144 0.4135 0.1791 0.084 Uiso 1 1 calc R . .
H7C H 0.7629 0.3926 0.2274 0.084 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Gd1 0.01901(9) 0.01901(9) 0.01901(9) -0.00133(6) -0.00133(6) -0.00133(6)
O1 0.0287(9) 0.0278(9) 0.0260(9) -0.0043(7) -0.0014(7) 0.0017(7)
N4 0.0289(15) 0.0364(16) 0.0183(13) 0.0050(12) 0.000 0.000
N1 0.0268(10) 0.0237(10) 0.0264(10) 0.0008(8) -0.0005(8) -0.0020(8)
N3 0.0365(13) 0.0540(15) 0.0357(12) 0.0024(11) -0.0066(10) 0.0084(11)
N2 0.0671(17) 0.0453(15) 0.0368(14) -0.0060(12) -0.0033(12) 0.0037(13)
C3 0.0274(13) 0.0393(14) 0.0250(12) 0.0013(11) -0.0031(10) -0.0042(11)
C1 0.0258(12) 0.0269(12) 0.0237(11) 0.0014(9) -0.0011(10) -0.0028(10)
C2 0.0391(15) 0.0345(15) 0.0282(13) 0.0035(12) -0.0051(11) 0.0014(12)
C4 0.0340(14) 0.0458(16) 0.0201(12) 0.0023(11) -0.0036(10) -0.0021(12)
C5 0.0477(17) 0.0554(18) 0.0367(15) 0.0000(14) -0.0082(13) -0.0117(15)
C6 0.0400(15) 0.0458(17) 0.0294(14) 0.0014(12) -0.0024(11) 0.0098(13)
C7 0.0553(19) 0.072(2) 0.0412(18) -0.0063(17) 0.0028(14) 0.0226(17)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Gd1 O1 2.4612(16) 26_666 ?
Gd1 O1 2.4612(16) . ?
Gd1 O1 2.4612(16) 27_666 ?
Gd1 O1 2.4612(16) 25_666 ?
Gd1 O1 2.4612(16) 3 ?
Gd1 O1 2.4612(16) 2 ?
Gd1 N1 2.4899(19) 27_666 ?
Gd1 N1 2.4899(19) 26_666 ?
Gd1 N1 2.4899(19) . ?
Gd1 N1 2.4899(19) 2 ?
Gd1 N1 2.4899(19) 25_666 ?
Gd1 N1 2.4899(19) 3 ?
O1 N1 1.294(2) . ?
N4 C4 1.511(3) . ?
N4 C4 1.511(3) 11_565 ?
N4 C6 1.513(3) 11_565 ?
N4 C6 1.513(3) . ?
N1 C1 1.309(3) . ?
N3 C3 1.136(3) . ?
N2 C2 1.147(3) . ?
C3 C1 1.435(3) . ?
C1 C2 1.422(4) . ?
C4 C5 1.507(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.515(4) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Gd1 O1 74.32(4) 26_666 . ?
O1 Gd1 O1 105.68(4) 26_666 27_666 ?
O1 Gd1 O1 74.32(4) . 27_666 ?
O1 Gd1 O1 105.68(4) 26_666 25_666 ?
O1 Gd1 O1 180.00(6) . 25_666 ?
O1 Gd1 O1 105.68(4) 27_666 25_666 ?
O1 Gd1 O1 74.32(4) 26_666 3 ?
O1 Gd1 O1 105.68(4) . 3 ?
O1 Gd1 O1 180.0 27_666 3 ?
O1 Gd1 O1 74.32(4) 25_666 3 ?
O1 Gd1 O1 180.0 26_666 2 ?
O1 Gd1 O1 105.68(4) . 2 ?
O1 Gd1 O1 74.32(4) 27_666 2 ?
O1 Gd1 O1 74.32(4) 25_666 2 ?
O1 Gd1 O1 105.68(4) 3 2 ?
O1 Gd1 N1 77.10(6) 26_666 27_666 ?
O1 Gd1 N1 75.57(6) . 27_666 ?
O1 Gd1 N1 30.29(5) 27_666 27_666 ?
O1 Gd1 N1 104.43(6) 25_666 27_666 ?
O1 Gd1 N1 149.71(5) 3 27_666 ?
O1 Gd1 N1 102.90(6) 2 27_666 ?
O1 Gd1 N1 30.29(5) 26_666 26_666 ?
O1 Gd1 N1 102.90(6) . 26_666 ?
O1 Gd1 N1 104.43(6) 27_666 26_666 ?
O1 Gd1 N1 77.10(6) 25_666 26_666 ?
O1 Gd1 N1 75.57(6) 3 26_666 ?
O1 Gd1 N1 149.71(5) 2 26_666 ?
N1 Gd1 N1 74.72(7) 27_666 26_666 ?
O1 Gd1 N1 75.57(6) 26_666 . ?
O1 Gd1 N1 30.29(5) . . ?
O1 Gd1 N1 102.90(6) 27_666 . ?
O1 Gd1 N1 149.71(5) 25_666 . ?
O1 Gd1 N1 77.10(6) 3 . ?
O1 Gd1 N1 104.43(6) 2 . ?
N1 Gd1 N1 105.28(7) 27_666 . ?
N1 Gd1 N1 105.28(7) 26_666 . ?
O1 Gd1 N1 149.71(5) 26_666 2 ?
O1 Gd1 N1 77.10(6) . 2 ?
O1 Gd1 N1 75.57(6) 27_666 2 ?
O1 Gd1 N1 102.90(6) 25_666 2 ?
O1 Gd1 N1 104.43(6) 3 2 ?
O1 Gd1 N1 30.29(5) 2 2 ?
N1 Gd1 N1 105.28(7) 27_666 2 ?
N1 Gd1 N1 180.000(1) 26_666 2 ?
N1 Gd1 N1 74.72(7) . 2 ?
O1 Gd1 N1 104.43(6) 26_666 25_666 ?
O1 Gd1 N1 149.71(5) . 25_666 ?
O1 Gd1 N1 77.10(6) 27_666 25_666 ?
O1 Gd1 N1 30.29(5) 25_666 25_666 ?
O1 Gd1 N1 102.90(6) 3 25_666 ?
O1 Gd1 N1 75.57(6) 2 25_666 ?
N1 Gd1 N1 74.72(7) 27_666 25_666 ?
N1 Gd1 N1 74.72(7) 26_666 25_666 ?
N1 Gd1 N1 180.0 . 25_666 ?
N1 Gd1 N1 105.28(7) 2 25_666 ?
O1 Gd1 N1 102.90(6) 26_666 3 ?
O1 Gd1 N1 104.43(6) . 3 ?
O1 Gd1 N1 149.71(5) 27_666 3 ?
O1 Gd1 N1 75.57(6) 25_666 3 ?
O1 Gd1 N1 30.29(5) 3 3 ?
O1 Gd1 N1 77.10(6) 2 3 ?
N1 Gd1 N1 180.00(9) 27_666 3 ?
N1 Gd1 N1 105.28(7) 26_666 3 ?
N1 Gd1 N1 74.72(7) . 3 ?
N1 Gd1 N1 74.72(7) 2 3 ?
N1 Gd1 N1 105.28(7) 25_666 3 ?
N1 O1 Gd1 76.08(11) . . ?
C4 N4 C4 111.0(3) . 11_565 ?
C4 N4 C6 106.37(13) . 11_565 ?
C4 N4 C6 111.20(14) 11_565 11_565 ?
C4 N4 C6 111.20(14) . . ?
C4 N4 C6 106.37(13) 11_565 . ?
C6 N4 C6 110.7(3) 11_565 . ?
O1 N1 C1 118.47(19) . . ?
O1 N1 Gd1 73.63(11) . . ?
C1 N1 Gd1 167.85(17) . . ?
N3 C3 C1 177.3(3) . . ?
N1 C1 C2 116.9(2) . . ?
N1 C1 C3 121.2(2) . . ?
C2 C1 C3 121.8(2) . . ?
N2 C2 C1 179.5(3) . . ?
C5 C4 N4 115.1(2) . . ?
C5 C4 H4A 108.5 . . ?
N4 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
N4 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7 C6 N4 115.7(2) . . ?
C7 C6 H6A 108.4 . . ?
N4 C6 H6A 108.4 . . ?
C7 C6 H6B 108.4 . . ?
N4 C6 H6B 108.4 . . ?
H6A C6 H6B 107.4 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.057

# Attachment 'La_Et.CIF'

data_c:\docume~1\owner\mydocu~1\xray\anthony\ac1667\isom_la
_database_code_depnum_ccdc_archive 'CCDC 633464'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraethylammonium [hexa(dicyanonitrosomethanido)lanthanate(III)]
;
_chemical_name_common            
;tetraethylammonium
(hexa(dicyanonitrosomethanido)lanthanate(iii))
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 La1 N18 O6, 3 (N1 C8 H20)'
_chemical_formula_sum            'C42 H60 La1 N21 O6'
_chemical_formula_weight         1094.02

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'
La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   Ia-3
_symmetry_space_group_name_Hall  -I2b2c3

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

_cell_length_a                   22.5835(1)
_cell_length_b                   22.5835(1)
_cell_length_c                   22.5835(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11517.91(9)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    14018
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4512
_exptl_absorpt_coefficient_mu    0.801
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7837
_exptl_absorpt_correction_T_max  0.9031
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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 X8 Apex II CCD'
_diffrn_measurement_method       'phi scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14014
_diffrn_reflns_av_R_equivalents  0.0444
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         27.45
_reflns_number_total             2204
_reflns_number_gt                1562
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker)'
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0414P)^2^+14.5461P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2204
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0374
_refine_ls_wR_factor_ref         0.0980
_refine_ls_wR_factor_gt          0.0857
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
La1 La 0.5000 0.5000 0.5000 0.02356(13) Uani 1 6 d S . .
O1 O 0.41805(9) 0.55650(8) 0.44541(8) 0.0342(4) Uani 1 1 d . . .
N4 N 0.65488(15) 0.5000 0.2500 0.0357(8) Uani 1 2 d S . .
N1 N 0.43357(9) 0.51612(9) 0.40771(9) 0.0296(5) Uani 1 1 d . . .
N3 N 0.32065(12) 0.58648(13) 0.33482(12) 0.0535(7) Uani 1 1 d . . .
N2 N 0.43551(14) 0.43033(13) 0.28578(12) 0.0577(8) Uani 1 1 d . . .
C3 C 0.35771(12) 0.55350(13) 0.34376(12) 0.0365(6) Uani 1 1 d . . .
C1 C 0.40483(12) 0.51326(11) 0.35735(12) 0.0301(6) Uani 1 1 d . . .
C2 C 0.42163(13) 0.46743(13) 0.31751(13) 0.0395(7) Uani 1 1 d . . .
C4 C 0.61683(14) 0.49146(14) 0.19547(12) 0.0426(7) Uani 1 1 d . . .
H4A H 0.5944 0.5284 0.1882 0.051 Uiso 1 1 calc R . .
H4B H 0.6431 0.4850 0.1610 0.051 Uiso 1 1 calc R . .
C5 C 0.57346(17) 0.44043(17) 0.19897(15) 0.0623(10) Uani 1 1 d . . .
H5A H 0.5459 0.4471 0.2319 0.093 Uiso 1 1 calc R . .
H5B H 0.5952 0.4034 0.2055 0.093 Uiso 1 1 calc R . .
H5C H 0.5512 0.4378 0.1618 0.093 Uiso 1 1 calc R . .
C6 C 0.69259(15) 0.44585(16) 0.26188(13) 0.0497(8) Uani 1 1 d . . .
H6A H 0.6661 0.4119 0.2702 0.060 Uiso 1 1 calc R . .
H6B H 0.7165 0.4531 0.2979 0.060 Uiso 1 1 calc R . .
C7 C 0.73403(19) 0.4288(2) 0.21178(18) 0.0746(12) Uani 1 1 d . . .
H7A H 0.7597 0.4625 0.2021 0.112 Uiso 1 1 calc R . .
H7B H 0.7107 0.4179 0.1768 0.112 Uiso 1 1 calc R . .
H7C H 0.7584 0.3951 0.2240 0.112 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
La1 0.02356(13) 0.02356(13) 0.02356(13) -0.00148(8) -0.00148(8) -0.00148(8)
O1 0.0352(10) 0.0331(10) 0.0342(10) -0.0050(8) -0.0027(8) 0.0050(8)
N4 0.0416(19) 0.044(2) 0.0213(15) 0.0030(14) 0.000 0.000
N1 0.0307(12) 0.0291(11) 0.0291(11) 0.0009(9) -0.0017(9) -0.0011(9)
N3 0.0412(15) 0.0686(19) 0.0507(16) 0.0092(14) -0.0056(13) 0.0134(14)
N2 0.081(2) 0.0524(18) 0.0396(16) -0.0069(13) -0.0073(15) 0.0075(15)
C3 0.0306(15) 0.0454(17) 0.0333(15) 0.0045(13) -0.0039(12) -0.0019(13)
C1 0.0309(14) 0.0299(14) 0.0295(14) 0.0022(10) -0.0030(11) -0.0024(11)
C2 0.0465(18) 0.0411(17) 0.0309(15) 0.0017(13) -0.0056(13) -0.0011(14)
C4 0.0497(18) 0.0557(19) 0.0224(14) 0.0031(12) -0.0058(13) -0.0075(15)
C5 0.067(2) 0.078(3) 0.0417(19) -0.0007(17) -0.0100(17) -0.020(2)
C6 0.055(2) 0.060(2) 0.0346(17) -0.0004(14) -0.0034(14) 0.0127(17)
C7 0.079(3) 0.092(3) 0.053(2) -0.013(2) 0.012(2) 0.028(2)

_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
La1 O1 2.5639(19) 26_666 ?
La1 O1 2.5639(19) 27_666 ?
La1 O1 2.5639(19) . ?
La1 O1 2.5639(19) 3 ?
La1 O1 2.5639(19) 2 ?
La1 O1 2.5639(19) 25_666 ?
La1 N1 2.594(2) 26_666 ?
La1 N1 2.594(2) 27_666 ?
La1 N1 2.594(2) 2 ?
La1 N1 2.594(2) . ?
La1 N1 2.594(2) 25_666 ?
La1 N1 2.594(2) 3 ?
O1 N1 1.296(3) . ?
N4 C6 1.514(4) 11_565 ?
N4 C6 1.514(4) . ?
N4 C4 1.514(3) . ?
N4 C4 1.514(3) 11_565 ?
N1 C1 1.311(3) . ?
N3 C3 1.138(4) . ?
N2 C2 1.146(4) . ?
C3 C1 1.433(4) . ?
C1 C2 1.423(4) . ?
C4 C5 1.514(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.518(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 La1 O1 104.57(4) 26_666 27_666 ?
O1 La1 O1 75.43(4) 26_666 . ?
O1 La1 O1 75.43(4) 27_666 . ?
O1 La1 O1 75.43(4) 26_666 3 ?
O1 La1 O1 180.0 27_666 3 ?
O1 La1 O1 104.57(4) . 3 ?
O1 La1 O1 180.00(6) 26_666 2 ?
O1 La1 O1 75.43(4) 27_666 2 ?
O1 La1 O1 104.57(4) . 2 ?
O1 La1 O1 104.57(4) 3 2 ?
O1 La1 O1 104.57(4) 26_666 25_666 ?
O1 La1 O1 104.57(4) 27_666 25_666 ?
O1 La1 O1 180.00(7) . 25_666 ?
O1 La1 O1 75.43(4) 3 25_666 ?
O1 La1 O1 75.43(4) 2 25_666 ?
O1 La1 N1 29.10(6) 26_666 26_666 ?
O1 La1 N1 102.89(6) 27_666 26_666 ?
O1 La1 N1 102.98(7) . 26_666 ?
O1 La1 N1 77.11(6) 3 26_666 ?
O1 La1 N1 150.90(6) 2 26_666 ?
O1 La1 N1 77.02(7) 25_666 26_666 ?
O1 La1 N1 77.02(7) 26_666 27_666 ?
O1 La1 N1 29.10(6) 27_666 27_666 ?
O1 La1 N1 77.11(6) . 27_666 ?
O1 La1 N1 150.90(6) 3 27_666 ?
O1 La1 N1 102.98(7) 2 27_666 ?
O1 La1 N1 102.89(6) 25_666 27_666 ?
N1 La1 N1 74.28(7) 26_666 27_666 ?
O1 La1 N1 150.90(6) 26_666 2 ?
O1 La1 N1 77.11(6) 27_666 2 ?
O1 La1 N1 77.02(7) . 2 ?
O1 La1 N1 102.89(6) 3 2 ?
O1 La1 N1 29.10(6) 2 2 ?
O1 La1 N1 102.98(7) 25_666 2 ?
N1 La1 N1 180.0 26_666 2 ?
N1 La1 N1 105.72(7) 27_666 2 ?
O1 La1 N1 77.11(6) 26_666 . ?
O1 La1 N1 102.98(7) 27_666 . ?
O1 La1 N1 29.10(6) . . ?
O1 La1 N1 77.02(7) 3 . ?
O1 La1 N1 102.89(6) 2 . ?
O1 La1 N1 150.90(6) 25_666 . ?
N1 La1 N1 105.72(7) 26_666 . ?
N1 La1 N1 105.72(7) 27_666 . ?
N1 La1 N1 74.28(7) 2 . ?
O1 La1 N1 102.89(6) 26_666 25_666 ?
O1 La1 N1 77.02(7) 27_666 25_666 ?
O1 La1 N1 150.90(6) . 25_666 ?
O1 La1 N1 102.98(7) 3 25_666 ?
O1 La1 N1 77.11(6) 2 25_666 ?
O1 La1 N1 29.10(6) 25_666 25_666 ?
N1 La1 N1 74.28(7) 26_666 25_666 ?
N1 La1 N1 74.28(7) 27_666 25_666 ?
N1 La1 N1 105.72(7) 2 25_666 ?
N1 La1 N1 180.0 . 25_666 ?
O1 La1 N1 102.98(7) 26_666 3 ?
O1 La1 N1 150.90(6) 27_666 3 ?
O1 La1 N1 102.89(6) . 3 ?
O1 La1 N1 29.10(6) 3 3 ?
O1 La1 N1 77.02(7) 2 3 ?
O1 La1 N1 77.11(6) 25_666 3 ?
N1 La1 N1 105.72(7) 26_666 3 ?
N1 La1 N1 180.00(9) 27_666 3 ?
N1 La1 N1 74.28(7) 2 3 ?
N1 La1 N1 74.28(7) . 3 ?
N1 La1 N1 105.72(7) 25_666 3 ?
N1 O1 La1 76.73(12) . . ?
C6 N4 C6 111.5(4) 11_565 . ?
C6 N4 C4 106.14(16) 11_565 . ?
C6 N4 C4 111.12(17) . . ?
C6 N4 C4 111.12(17) 11_565 11_565 ?
C6 N4 C4 106.14(16) . 11_565 ?
C4 N4 C4 110.9(3) . 11_565 ?
O1 N1 C1 118.1(2) . . ?
O1 N1 La1 74.17(12) . . ?
C1 N1 La1 167.56(19) . . ?
N3 C3 C1 177.6(3) . . ?
N1 C1 C2 116.9(2) . . ?
N1 C1 C3 121.5(2) . . ?
C2 C1 C3 121.6(3) . . ?
N2 C2 C1 179.4(4) . . ?
C5 C4 N4 114.9(2) . . ?
C5 C4 H4A 108.5 . . ?
N4 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
N4 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 C7 114.8(3) . . ?
N4 C6 H6A 108.6 . . ?
C7 C6 H6A 108.6 . . ?
N4 C6 H6B 108.6 . . ?
C7 C6 H6B 108.6 . . ?
H6A C6 H6B 107.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.45
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.074

# Attachment 'Nd_Et.CIF'

data_c:\docume~1\owner\mydocu~1\xray\anthony\ac1669\isom_nd
_database_code_depnum_ccdc_archive 'CCDC 633465'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
tetraethylammonium hexa(dicyanonitrosomethanido)neodymiate(III)
;
_chemical_name_common            
;tetraethylammonium
hexa(dicyanonitrosomethanido)neodymiate(iii)
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C18 N18 Nd1 O6, 3(C8 H20 N1)'
_chemical_formula_sum            'C42 H60 N21 Nd1 O6'
_chemical_formula_weight         1099.35

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

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   Ia-3
_symmetry_space_group_name_Hall  -I2b2c3

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

_cell_length_a                   22.4898(3)
_cell_length_b                   22.4898(3)
_cell_length_c                   22.4898(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11375.1(3)
_cell_formula_units_Z            8
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    14413
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4536
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7461
_exptl_absorpt_correction_T_max  0.8840
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(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 X8 Apex II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14411
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         27.47
_reflns_number_total             2179
_reflns_number_gt                1624
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART (Bruker)'
_computing_cell_refinement       'Bruker SMART (Bruker)'
_computing_data_reduction        'Bruker SAINT (Bruker)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+14.7401P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2179
_refine_ls_number_parameters     109
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0588
_refine_ls_wR_factor_gt          0.0525
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_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
Nd1 Nd 0.5000 0.5000 0.5000 0.01940(8) Uani 1 6 d S . .
O1 O 0.41926(6) 0.55647(6) 0.44762(6) 0.0267(3) Uani 1 1 d . . .
N4 N 0.65688(11) 0.5000 0.2500 0.0280(5) Uani 1 2 d S . .
N1 N 0.43462(7) 0.51624(7) 0.40924(7) 0.0240(4) Uani 1 1 d . . .
N3 N 0.32253(9) 0.58856(10) 0.33604(9) 0.0419(5) Uani 1 1 d . . .
N2 N 0.43695(10) 0.43065(9) 0.28619(9) 0.0483(6) Uani 1 1 d . . .
C3 C 0.35948(10) 0.55495(10) 0.34468(9) 0.0297(5) Uani 1 1 d . . .
C1 C 0.40642(9) 0.51406(9) 0.35820(9) 0.0247(4) Uani 1 1 d . . .
C2 C 0.42333(10) 0.46772(10) 0.31797(10) 0.0327(5) Uani 1 1 d . . .
C4 C 0.61855(10) 0.48999(10) 0.19543(9) 0.0329(5) Uani 1 1 d . . .
H4A H 0.5955 0.5267 0.1876 0.039 Uiso 1 1 calc R . .
H4B H 0.6449 0.4832 0.1609 0.039 Uiso 1 1 calc R . .
C5 C 0.57567(12) 0.43848(12) 0.19996(11) 0.0463(6) Uani 1 1 d . . .
H5A H 0.5477 0.4457 0.2326 0.069 Uiso 1 1 calc R . .
H5B H 0.5978 0.4018 0.2077 0.069 Uiso 1 1 calc R . .
H5C H 0.5537 0.4345 0.1625 0.069 Uiso 1 1 calc R . .
C6 C 0.69497(11) 0.44600(11) 0.26340(10) 0.0366(6) Uani 1 1 d . . .
H6A H 0.6684 0.4125 0.2738 0.044 Uiso 1 1 calc R . .
H6B H 0.7197 0.4548 0.2988 0.044 Uiso 1 1 calc R . .
C7 C 0.73567(13) 0.42620(14) 0.21336(12) 0.0570(8) Uani 1 1 d . . .
H7A H 0.7618 0.4591 0.2020 0.085 Uiso 1 1 calc R . .
H7B H 0.7117 0.4142 0.1790 0.085 Uiso 1 1 calc R . .
H7C H 0.7598 0.3924 0.2267 0.085 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nd1 0.01940(8) 0.01940(8) 0.01940(8) -0.00164(6) -0.00164(6) -0.00164(6)
O1 0.0274(7) 0.0270(8) 0.0257(8) -0.0044(6) -0.0025(6) 0.0032(6)
N4 0.0310(13) 0.0359(14) 0.0172(11) 0.0017(11) 0.000 0.000
N1 0.0240(9) 0.0237(9) 0.0244(9) -0.0002(7) -0.0005(7) -0.0020(7)
N3 0.0340(11) 0.0541(13) 0.0377(11) 0.0027(10) -0.0057(9) 0.0092(10)
N2 0.0652(15) 0.0423(13) 0.0375(12) -0.0073(10) -0.0044(11) 0.0068(11)
C3 0.0277(11) 0.0374(12) 0.0240(11) 0.0015(9) -0.0033(9) -0.0027(10)
C1 0.0247(10) 0.0262(11) 0.0233(10) 0.0006(8) -0.0018(8) -0.0017(8)
C2 0.0391(13) 0.0341(13) 0.0249(11) 0.0009(10) -0.0055(10) -0.0002(10)
C4 0.0368(12) 0.0432(14) 0.0186(10) 0.0033(9) -0.0042(9) -0.0028(10)
C5 0.0491(15) 0.0570(16) 0.0329(13) 0.0010(12) -0.0081(12) -0.0144(13)
C6 0.0398(13) 0.0434(14) 0.0266(12) 0.0014(10) -0.0033(9) 0.0092(11)
C7 0.0600(19) 0.069(2) 0.0416(16) -0.0082(14) 0.0034(13) 0.0231(15)

_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
Nd1 O1 2.5096(14) 26_666 ?
Nd1 O1 2.5096(14) 27_666 ?
Nd1 O1 2.5096(14) 3 ?
Nd1 O1 2.5096(14) . ?
Nd1 O1 2.5096(14) 2 ?
Nd1 O1 2.5096(14) 25_666 ?
Nd1 N1 2.5421(17) 27_666 ?
Nd1 N1 2.5421(17) 26_666 ?
Nd1 N1 2.5421(17) . ?
Nd1 N1 2.5421(17) 3 ?
Nd1 N1 2.5421(17) 25_666 ?
Nd1 N1 2.5421(17) 2 ?
O1 N1 1.297(2) . ?
N4 C6 1.516(3) 11_565 ?
N4 C6 1.516(3) . ?
N4 C4 1.517(2) . ?
N4 C4 1.517(2) 11_565 ?
N1 C1 1.312(3) . ?
N3 C3 1.140(3) . ?
N2 C2 1.140(3) . ?
C3 C1 1.433(3) . ?
C1 C2 1.432(3) . ?
C4 C5 1.511(3) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 C7 1.517(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Nd1 O1 105.31(4) 26_666 27_666 ?
O1 Nd1 O1 74.69(4) 26_666 3 ?
O1 Nd1 O1 180.0 27_666 3 ?
O1 Nd1 O1 74.69(4) 26_666 . ?
O1 Nd1 O1 74.69(4) 27_666 . ?
O1 Nd1 O1 105.31(3) 3 . ?
O1 Nd1 O1 180.0 26_666 2 ?
O1 Nd1 O1 74.69(4) 27_666 2 ?
O1 Nd1 O1 105.31(4) 3 2 ?
O1 Nd1 O1 105.31(4) . 2 ?
O1 Nd1 O1 105.31(4) 26_666 25_666 ?
O1 Nd1 O1 105.31(3) 27_666 25_666 ?
O1 Nd1 O1 74.69(4) 3 25_666 ?
O1 Nd1 O1 180.00(6) . 25_666 ?
O1 Nd1 O1 74.69(4) 2 25_666 ?
O1 Nd1 N1 77.24(5) 26_666 27_666 ?
O1 Nd1 N1 29.75(5) 27_666 27_666 ?
O1 Nd1 N1 150.25(5) 3 27_666 ?
O1 Nd1 N1 76.19(5) . 27_666 ?
O1 Nd1 N1 102.76(5) 2 27_666 ?
O1 Nd1 N1 103.81(5) 25_666 27_666 ?
O1 Nd1 N1 29.75(5) 26_666 26_666 ?
O1 Nd1 N1 103.81(5) 27_666 26_666 ?
O1 Nd1 N1 76.19(5) 3 26_666 ?
O1 Nd1 N1 102.76(5) . 26_666 ?
O1 Nd1 N1 150.25(5) 2 26_666 ?
O1 Nd1 N1 77.24(5) 25_666 26_666 ?
N1 Nd1 N1 74.57(6) 27_666 26_666 ?
O1 Nd1 N1 76.19(5) 26_666 . ?
O1 Nd1 N1 102.76(5) 27_666 . ?
O1 Nd1 N1 77.24(5) 3 . ?
O1 Nd1 N1 29.75(5) . . ?
O1 Nd1 N1 103.81(5) 2 . ?
O1 Nd1 N1 150.25(5) 25_666 . ?
N1 Nd1 N1 105.43(6) 27_666 . ?
N1 Nd1 N1 105.43(6) 26_666 . ?
O1 Nd1 N1 102.76(5) 26_666 3 ?
O1 Nd1 N1 150.25(5) 27_666 3 ?
O1 Nd1 N1 29.75(5) 3 3 ?
O1 Nd1 N1 103.81(5) . 3 ?
O1 Nd1 N1 77.24(5) 2 3 ?
O1 Nd1 N1 76.19(5) 25_666 3 ?
N1 Nd1 N1 180.00(6) 27_666 3 ?
N1 Nd1 N1 105.43(6) 26_666 3 ?
N1 Nd1 N1 74.57(6) . 3 ?
O1 Nd1 N1 103.81(5) 26_666 25_666 ?
O1 Nd1 N1 77.24(5) 27_666 25_666 ?
O1 Nd1 N1 102.76(5) 3 25_666 ?
O1 Nd1 N1 150.25(5) . 25_666 ?
O1 Nd1 N1 76.19(5) 2 25_666 ?
O1 Nd1 N1 29.75(5) 25_666 25_666 ?
N1 Nd1 N1 74.57(6) 27_666 25_666 ?
N1 Nd1 N1 74.57(6) 26_666 25_666 ?
N1 Nd1 N1 180.0 . 25_666 ?
N1 Nd1 N1 105.43(6) 3 25_666 ?
O1 Nd1 N1 150.25(5) 26_666 2 ?
O1 Nd1 N1 76.19(5) 27_666 2 ?
O1 Nd1 N1 103.81(5) 3 2 ?
O1 Nd1 N1 77.24(5) . 2 ?
O1 Nd1 N1 29.75(5) 2 2 ?
O1 Nd1 N1 102.76(5) 25_666 2 ?
N1 Nd1 N1 105.43(6) 27_666 2 ?
N1 Nd1 N1 180.0 26_666 2 ?
N1 Nd1 N1 74.57(6) . 2 ?
N1 Nd1 N1 74.57(6) 3 2 ?
N1 Nd1 N1 105.43(6) 25_666 2 ?
N1 O1 Nd1 76.51(10) . . ?
C6 N4 C6 111.2(2) 11_565 . ?
C6 N4 C4 106.21(12) 11_565 . ?
C6 N4 C4 111.29(12) . . ?
C6 N4 C4 111.29(12) 11_565 11_565 ?
C6 N4 C4 106.21(12) . 11_565 ?
C4 N4 C4 110.7(2) . 11_565 ?
O1 N1 C1 118.64(17) . . ?
O1 N1 Nd1 73.74(9) . . ?
C1 N1 Nd1 167.56(14) . . ?
N3 C3 C1 177.3(2) . . ?
N1 C1 C2 116.85(19) . . ?
N1 C1 C3 121.18(19) . . ?
C2 C1 C3 121.93(19) . . ?
N2 C2 C1 179.6(3) . . ?
C5 C4 N4 114.97(17) . . ?
C5 C4 H4A 108.5 . . ?
N4 C4 H4A 108.5 . . ?
C5 C4 H4B 108.5 . . ?
N4 C4 H4B 108.5 . . ?
H4A C4 H4B 107.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 C7 115.36(19) . . ?
N4 C6 H6A 108.4 . . ?
C7 C6 H6A 108.4 . . ?
N4 C6 H6B 108.4 . . ?
C7 C6 H6B 108.4 . . ?
H6A C6 H6B 107.5 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.050