# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

_publ_contact_author_name        'Dr Shunichi Fukuzumi'
_publ_contact_author_email       fukuzumi@chem.eng.osaka-u.ac.jp

_publ_section_title              
;
X-ray crystal structure of
[HSm{VIVO(TPPS)}]n and encapsulation of nitrogen
molecules in 1-D channels

;
loop_
_publ_author_name
'Wentong Chen'
Y.Yamada
'Guang-Ning Liu'
A.Kubota
T.Ichikawa
Y.Kojima
'Guo-Cong Guo'
S.Fukuzumi

# Attachment '- H[SmV(TPPS)O]n-2.CIF'

data_1
_database_code_depnum_ccdc_archive 'CCDC 799402'
#TrackingRef '- H[SmV(TPPS)O]n-2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'H[SmV(TPPS)O]n'
;
_chemical_name_common            H(SmV(TPPS)O)n
_chemical_melting_point          'not measured'
_chemical_formula_moiety         H[SmV(TPPS)O]n
_chemical_formula_sum            'C44 H26 N4 O13 S4 Sm V'
_chemical_formula_weight         1146.25

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TETRAGONAL
_symmetry_space_group_name_H-M   P4/mcc

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

_cell_length_a                   15.368(3)
_cell_length_b                   15.368(3)
_cell_length_c                   9.914(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2341.5(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    123.1500
_cell_measurement_reflns_used    5485
_cell_measurement_theta_min      3.3561
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.1800
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0900
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1142
_exptl_absorpt_coefficient_mu    1.687
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.817
_exptl_absorpt_correction_T_max  0.859
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123.1500
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12683
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         25.02
_reflns_number_total             990
_reflns_number_gt                955
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_structure_solution    'Siemens SHELXTL^TM^ 5'
_computing_structure_refinement  'Siemens SHELXTL^TM^ 5'
_computing_molecular_graphics    ?
_computing_publication_material  'Siemens SHELXTL^TM^ 5'

_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^)+(0.1081P)^2^+17.7769P] 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         990
_refine_ls_number_parameters     95
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0648
_refine_ls_wR_factor_ref         0.1703
_refine_ls_wR_factor_gt          0.1677
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_restrained_S_all      1.086
_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
Sm1 Sm -0.5000 -0.5000 -1.7500 0.02312(8) Uani 1 8 d S . .
V1 V 0.0000 0.0000 -1.89758(18) 0.0757(11) Uani 0.50 4 d SPDU . .
S1 S -0.31842(6) -0.52680(5) -2.0000 0.0270(2) Uani 1 2 d S . .
N1 N -0.1304(3) -0.0324(3) -2.0000 0.0840(18) Uani 1 2 d SU . .
O1 O -0.37246(14) -0.53096(13) -1.8806(3) 0.0527(6) Uani 1 1 d . . .
O2 O -0.25117(16) -0.59034(16) -2.0000 0.0312(7) Uani 1 2 d S . .
O3 O 0.0000 0.0000 -1.7500 0.121(6) Uani 1 8 d SD . .
C1 C -0.2656(2) -0.4254(2) -2.0000 0.0298(10) Uani 1 2 d S . .
C2 C -0.2425(2) -0.3869(2) -2.1186(4) 0.0623(11) Uani 1 1 d . . .
H2A H -0.2608 -0.4117 -2.1994 0.075 Uiso 1 1 calc R . .
C3 C -0.1923(3) -0.3117(3) -2.1221(5) 0.0812(13) Uani 1 1 d U . .
H3A H -0.1743 -0.2874 -2.2034 0.097 Uiso 1 1 calc R . .
C4 C -0.1702(3) -0.2745(3) -2.0000 0.0560(14) Uani 1 2 d SU . .
C5 C -0.1180(4) -0.1929(3) -2.0000 0.0690(17) Uani 1 2 d SU . .
C6 C -0.1651(3) -0.1120(3) -2.0000 0.0711(17) Uani 1 2 d SU . .
C7 C -0.2557(3) -0.1057(4) -2.0000 0.0675(17) Uani 1 2 d SU . .
H7A H -0.2942 -0.1524 -2.0000 0.081 Uiso 1 2 calc SR . .
C8 C -0.2783(4) -0.0207(4) -2.0000 0.0705(18) Uani 1 2 d SU . .
H8A H -0.3345 0.0018 -2.0000 0.085 Uiso 1 2 calc SR . .
C9 C -0.1972(4) 0.0287(4) -2.0000 0.080(2) Uani 1 2 d SU . .

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
Sm1 0.01947(9) 0.01947(9) 0.03042(18) 0.000 0.000 0.000
V1 0.0376(7) 0.0376(7) 0.152(3) 0.000 0.000 0.000
S1 0.0187(4) 0.0184(3) 0.0440(5) 0.000 0.000 -0.0007(3)
N1 0.042(2) 0.051(2) 0.159(4) 0.000 0.000 0.0058(19)
O1 0.0469(11) 0.0303(9) 0.0810(14) -0.0131(10) 0.0373(10) -0.0076(8)
O2 0.0241(11) 0.0203(11) 0.0493(14) 0.000 0.000 0.0048(10)
O3 0.034(2) 0.034(2) 0.296(19) 0.000 0.000 0.000
C1 0.0164(15) 0.0206(16) 0.052(2) 0.000 0.000 -0.0019(13)
C2 0.0532(17) 0.0557(17) 0.078(2) 0.0267(16) -0.0069(18) -0.0324(14)
C3 0.061(2) 0.0658(19) 0.117(3) 0.0501(19) -0.010(2) -0.0207(17)
C4 0.034(2) 0.0305(19) 0.103(3) 0.000 0.000 -0.0044(17)
C5 0.047(2) 0.044(2) 0.117(4) 0.000 0.000 -0.001(2)
C6 0.040(2) 0.039(2) 0.134(4) 0.000 0.000 0.002(2)
C7 0.036(2) 0.051(3) 0.116(4) 0.000 0.000 -0.009(2)
C8 0.039(2) 0.052(3) 0.121(4) 0.000 0.000 0.005(2)
C9 0.061(3) 0.061(3) 0.118(4) 0.000 0.000 -0.004(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.397(2) 4_545 ?
Sm1 O1 2.397(2) 2_445 ?
Sm1 O1 2.397(2) 6_541 ?
Sm1 O1 2.397(2) . ?
Sm1 O1 2.397(2) 3_455 ?
Sm1 O1 2.397(2) 5_451 ?
Sm1 O1 2.397(2) 8_441 ?
Sm1 O1 2.397(2) 7_551 ?
V1 O3 1.4632(19) . ?
V1 V1 2.031(4) 9_551 ?
V1 N1 2.301(5) 3 ?
V1 N1 2.301(5) . ?
V1 N1 2.301(5) 9_551 ?
V1 N1 2.301(5) 11_551 ?
V1 V1 2.926(4) 5_551 ?
S1 O2 1.422(3) . ?
S1 O1 1.447(2) 10_551 ?
S1 O1 1.447(2) . ?
S1 C1 1.757(3) . ?
N1 C6 1.335(7) . ?
N1 C9 1.391(8) . ?
N1 V1 2.301(5) 9_551 ?
O3 V1 1.4632(19) 5_551 ?
C1 C2 1.364(4) . ?
C1 C2 1.364(4) 10_551 ?
C2 C3 1.390(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.381(5) . ?
C3 H3A 0.9300 . ?
C4 C3 1.381(5) 10_551 ?
C4 C5 1.489(7) . ?
C5 C9 1.374(9) 3 ?
C5 C6 1.439(7) . ?
C6 C7 1.396(7) . ?
C7 C8 1.352(8) . ?
C7 H7A 0.9300 . ?
C8 C9 1.459(9) . ?
C8 H8A 0.9300 . ?
C9 C5 1.374(9) 11_551 ?

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 Sm1 O1 73.03(6) 4_545 2_445 ?
O1 Sm1 O1 128.06(10) 4_545 6_541 ?
O1 Sm1 O1 157.10(10) 2_445 6_541 ?
O1 Sm1 O1 73.03(6) 4_545 . ?
O1 Sm1 O1 114.59(12) 2_445 . ?
O1 Sm1 O1 70.29(12) 6_541 . ?
O1 Sm1 O1 114.59(12) 4_545 3_455 ?
O1 Sm1 O1 73.03(6) 2_445 3_455 ?
O1 Sm1 O1 88.13(11) 6_541 3_455 ?
O1 Sm1 O1 73.03(6) . 3_455 ?
O1 Sm1 O1 88.13(11) 4_545 5_451 ?
O1 Sm1 O1 70.29(12) 2_445 5_451 ?
O1 Sm1 O1 114.59(12) 6_541 5_451 ?
O1 Sm1 O1 157.10(10) . 5_451 ?
O1 Sm1 O1 128.06(10) 3_455 5_451 ?
O1 Sm1 O1 70.29(12) 4_545 8_441 ?
O1 Sm1 O1 128.06(10) 2_445 8_441 ?
O1 Sm1 O1 73.03(6) 6_541 8_441 ?
O1 Sm1 O1 88.13(11) . 8_441 ?
O1 Sm1 O1 157.10(10) 3_455 8_441 ?
O1 Sm1 O1 73.03(6) 5_451 8_441 ?
O1 Sm1 O1 157.10(10) 4_545 7_551 ?
O1 Sm1 O1 88.13(11) 2_445 7_551 ?
O1 Sm1 O1 73.03(6) 6_541 7_551 ?
O1 Sm1 O1 128.06(10) . 7_551 ?
O1 Sm1 O1 70.29(12) 3_455 7_551 ?
O1 Sm1 O1 73.03(6) 5_451 7_551 ?
O1 Sm1 O1 114.59(12) 8_441 7_551 ?
O3 V1 V1 180.000(1) . 9_551 ?
O3 V1 N1 116.19(7) . 3 ?
V1 V1 N1 63.81(7) 9_551 3 ?
O3 V1 N1 116.19(7) . . ?
V1 V1 N1 63.81(7) 9_551 . ?
N1 V1 N1 78.77(6) 3 . ?
O3 V1 N1 116.19(7) . 9_551 ?
V1 V1 N1 63.81(7) 9_551 9_551 ?
N1 V1 N1 78.77(6) 3 9_551 ?
N1 V1 N1 127.62(14) . 9_551 ?
O3 V1 N1 116.19(7) . 11_551 ?
V1 V1 N1 63.81(7) 9_551 11_551 ?
N1 V1 N1 127.62(14) 3 11_551 ?
N1 V1 N1 78.77(6) . 11_551 ?
N1 V1 N1 78.77(5) 9_551 11_551 ?
O3 V1 V1 0.0 . 5_551 ?
V1 V1 V1 180.000(1) 9_551 5_551 ?
N1 V1 V1 116.19(7) 3 5_551 ?
N1 V1 V1 116.19(7) . 5_551 ?
N1 V1 V1 116.19(7) 9_551 5_551 ?
N1 V1 V1 116.19(7) 11_551 5_551 ?
O2 S1 O1 112.75(10) . 10_551 ?
O2 S1 O1 112.75(10) . . ?
O1 S1 O1 109.7(2) 10_551 . ?
O2 S1 C1 105.88(16) . . ?
O1 S1 C1 107.71(11) 10_551 . ?
O1 S1 C1 107.71(11) . . ?
C6 N1 C9 108.9(5) . . ?
C6 N1 V1 123.1(3) . 9_551 ?
C9 N1 V1 119.8(3) . 9_551 ?
C6 N1 V1 123.1(3) . . ?
C9 N1 V1 119.8(3) . . ?
V1 N1 V1 52.38(14) 9_551 . ?
S1 O1 Sm1 154.46(15) . . ?
V1 O3 V1 180.000(1) . 5_551 ?
C2 C1 C2 119.2(4) . 10_551 ?
C2 C1 S1 120.3(2) . . ?
C2 C1 S1 120.3(2) 10_551 . ?
C1 C2 C3 121.8(4) . . ?
C1 C2 H2A 119.1 . . ?
C3 C2 H2A 119.1 . . ?
C4 C3 C2 117.3(4) . . ?
C4 C3 H3A 121.4 . . ?
C2 C3 H3A 121.4 . . ?
C3 C4 C3 122.5(5) . 10_551 ?
C3 C4 C5 118.8(2) . . ?
C3 C4 C5 118.8(2) 10_551 . ?
C9 C5 C6 123.0(5) 3 . ?
C9 C5 C4 119.9(5) 3 . ?
C6 C5 C4 117.2(5) . . ?
N1 C6 C7 109.6(5) . . ?
N1 C6 C5 126.2(5) . . ?
C7 C6 C5 124.2(5) . . ?
C8 C7 C6 108.9(5) . . ?
C8 C7 H7A 125.6 . . ?
C6 C7 H7A 125.6 . . ?
C7 C8 C9 106.4(5) . . ?
C7 C8 H8A 126.8 . . ?
C9 C8 H8A 126.8 . . ?
C5 C9 N1 129.7(6) 11_551 . ?
C5 C9 C8 124.1(6) 11_551 . ?
N1 C9 C8 106.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.892
_diffrn_reflns_theta_full        25.02
_diffrn_measured_fraction_theta_full 0.892
_refine_diff_density_max         0.946
_refine_diff_density_min         -1.218
_refine_diff_density_rms         0.130

#===END --------------------------------------------------


# Attachment '- H[SmV(TPPS)O]n with N2-2.CIF'

data_n2
_database_code_depnum_ccdc_archive 'CCDC 826943'
#TrackingRef '- H[SmV(TPPS)O]n with N2-2.CIF'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
'[HSm{VIVO(TPPS)}.2N2]n'
;
_chemical_name_common            (HSm(VIVO(TPPS)).2N2)n
_chemical_melting_point          'not measured'
_chemical_formula_moiety         '[HSm{VIVO(TPPS)}.2N2]n'
_chemical_formula_sum            'C44 H26 N8 O13 S4 Sm V'
_chemical_formula_weight         1204.24

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'
V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           TETRAGONAL
_symmetry_space_group_name_H-M   P4/mcc

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

_cell_length_a                   15.3904(8)
_cell_length_b                   15.3904(8)
_cell_length_c                   9.8586(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2335.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.710
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1194
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7276
_exptl_absorpt_correction_T_max  0.7276
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71070
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Mercury CCD'
_diffrn_measurement_method       w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            16832
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_sigmaI/netI    0.0221
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.61
_diffrn_reflns_theta_max         27.48
_reflns_number_total             1415
_reflns_number_gt                1366
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_structure_solution    'Siemens SHELXTL^TM^ 5'
_computing_structure_refinement  'Siemens SHELXTL^TM^ 5'
_computing_molecular_graphics    ?
_computing_publication_material  'Siemens SHELXTL^TM^ 5'

_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^)+(0.1000P)^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         1415
_refine_ls_number_parameters     102
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0764
_refine_ls_wR_factor_ref         0.2338
_refine_ls_wR_factor_gt          0.2328
_refine_ls_goodness_of_fit_ref   1.998
_refine_ls_restrained_S_all      1.998
_refine_ls_shift/su_max          0.062
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.5000 0.5000 0.2500 0.0213(4) Uani 1 8 d S . .
S1 S 0.32117(13) 0.47399(15) 0.0000 0.0293(6) Uani 1 2 d S . .
O2 O 0.2530(4) 0.4104(4) 0.0000 0.0359(15) Uani 1 2 d S . .
C1 C 0.2684(5) 0.5755(6) 0.0000 0.0285(19) Uani 1 2 d S . .
C4 C 0.1697(6) 0.7271(5) 0.0000 0.037(2) Uani 1 2 d S . .
C7 C 0.2591(6) 0.8945(7) 0.0000 0.048(3) Uani 1 2 d S . .
H3 H 0.2999 0.8481 0.0000 0.058 Uiso 1 2 calc SR . .
N1 N 0.1304(6) 0.9700(6) 0.0000 0.062(3) Uani 1 2 d S . .
C3 C 0.1948(4) 0.6879(5) 0.1208(9) 0.0453(19) Uani 1 1 d . . .
H5 H 0.1777 0.7127 0.2049 0.054 Uiso 1 1 calc R . .
C2 C 0.2444(4) 0.6132(5) 0.1197(8) 0.0414(17) Uani 1 1 d . . .
H6 H 0.2620 0.5877 0.2031 0.050 Uiso 1 1 calc R . .
C5 C 0.1171(6) 0.8090(6) 0.0000 0.044(3) Uani 1 2 d S . .
C6 C 0.1635(6) 0.8867(7) 0.0000 0.046(3) Uani 1 2 d S . .
C9 C 0.1963(6) 1.0274(7) 0.0000 0.051(3) Uani 1 2 d S . .
O1 O 0.3736(4) 0.4694(3) 0.1223(7) 0.0579(17) Uani 1 1 d . . .
C8 C 0.2774(6) 0.9799(7) 0.0000 0.048(3) Uani 1 2 d S . .
H4 H 0.3339 1.0047 0.0000 0.058 Uiso 1 2 calc SR . .
O3 O 0.0000 0.0000 0.2500 0.100(12) Uani 1 8 d S . .
N11 N 0.0693(15) 0.479(3) 0.0000 0.057(11) Uiso 0.25 2 d SPD . .
N22 N 0.0000 0.5000 0.2500 0.17(4) Uiso 0.50 4 d SPD . .
N21 N 0.0000 0.5000 0.138(2) 0.21(8) Uiso 0.25 2 d SPD . .
V1 V 0.0000 0.0000 0.088(4) 0.31(2) Uani 0.50 4 d SP . .
N12 N 0.0000 0.5000 0.0000 0.23(6) Uiso 0.50 4 d SPD . .

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
Sm1 0.0160(4) 0.0160(4) 0.0320(6) 0.000 0.000 0.000
S1 0.0198(10) 0.0193(10) 0.0489(13) 0.000 0.000 0.0008(8)
O2 0.025(3) 0.026(3) 0.057(4) 0.000 0.000 -0.004(2)
C1 0.015(4) 0.019(4) 0.052(5) 0.000 0.000 0.004(3)
C4 0.022(4) 0.015(4) 0.075(7) 0.000 0.000 0.000(3)
C7 0.020(4) 0.032(5) 0.092(9) 0.000 0.000 0.003(4)
N1 0.031(5) 0.024(4) 0.131(10) 0.000 0.000 0.004(4)
C3 0.029(3) 0.037(4) 0.070(5) -0.015(3) -0.002(3) 0.009(3)
C2 0.032(3) 0.040(4) 0.052(5) -0.004(3) -0.008(3) 0.014(3)
C5 0.024(4) 0.011(4) 0.097(9) 0.000 0.000 0.005(3)
C6 0.012(4) 0.032(5) 0.095(9) 0.000 0.000 0.001(4)
C9 0.018(4) 0.023(5) 0.111(10) 0.000 0.000 -0.004(4)
O1 0.056(3) 0.027(3) 0.090(4) -0.009(3) -0.040(3) 0.008(2)
C8 0.015(4) 0.029(4) 0.101(10) 0.000 0.000 0.002(4)
O3 0.102(18) 0.102(18) 0.10(3) 0.000 0.000 0.000
V1 0.30(3) 0.30(3) 0.33(5) 0.000 0.000 0.000

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sm1 O1 2.365(5) . ?
Sm1 O1 2.365(5) 5_665 ?
Sm1 O1 2.365(5) 8_655 ?
Sm1 O1 2.365(5) 4_655 ?
Sm1 O1 2.365(5) 6 ?
Sm1 O1 2.365(5) 2_665 ?
Sm1 O1 2.365(5) 3_565 ?
Sm1 O1 2.365(5) 7_565 ?
S1 O2 1.435(7) . ?
S1 O1 1.452(5) . ?
S1 O1 1.452(5) 10 ?
S1 C1 1.761(9) . ?
C1 C2 1.366(8) 10 ?
C1 C2 1.366(8) . ?
C4 C3 1.390(9) 10 ?
C4 C3 1.390(9) . ?
C4 C5 1.499(11) . ?
C7 C8 1.344(14) . ?
C7 C6 1.476(12) . ?
C7 H3 0.9500 . ?
N1 C9 1.345(14) . ?
N1 C6 1.379(13) . ?
N1 V1 2.236(18) 9_565 ?
N1 V1 2.236(18) 1_565 ?
C3 C2 1.379(9) . ?
C3 H5 0.9500 . ?
C2 H6 0.9500 . ?
C5 C9 1.383(13) 7_465 ?
C5 C6 1.393(14) . ?
C9 C5 1.383(13) 15_665 ?
C9 C8 1.446(13) . ?
C8 H4 0.9500 . ?
O3 V1 1.59(4) . ?
O3 V1 1.59(4) 3 ?
N11 N12 1.114(19) . ?
N11 N21 1.76(2) 9_565 ?
N22 N21 1.10(2) . ?
N22 N21 1.10(2) 3_565 ?
N21 N11 1.76(2) 9_565 ?
V1 V1 1.74(8) 9 ?
V1 N1 2.236(18) 15_655 ?
V1 N1 2.236(18) 1_545 ?
V1 N1 2.236(18) 7_455 ?
V1 N1 2.236(18) 9_565 ?
N12 N11 1.114(19) 9_565 ?
N12 N21 1.36(2) 9_565 ?

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 Sm1 O1 127.7(3) . 5_665 ?
O1 Sm1 O1 73.52(17) . 8_655 ?
O1 Sm1 O1 157.0(3) 5_665 8_655 ?
O1 Sm1 O1 157.0(3) . 4_655 ?
O1 Sm1 O1 73.52(17) 5_665 4_655 ?
O1 Sm1 O1 87.5(3) 8_655 4_655 ?
O1 Sm1 O1 87.5(3) . 6 ?
O1 Sm1 O1 115.6(4) 5_665 6 ?
O1 Sm1 O1 69.3(3) 8_655 6 ?
O1 Sm1 O1 73.52(17) 4_655 6 ?
O1 Sm1 O1 115.6(4) . 2_665 ?
O1 Sm1 O1 87.5(3) 5_665 2_665 ?
O1 Sm1 O1 73.52(17) 8_655 2_665 ?
O1 Sm1 O1 69.3(3) 4_655 2_665 ?
O1 Sm1 O1 127.7(3) 6 2_665 ?
O1 Sm1 O1 69.3(3) . 3_565 ?
O1 Sm1 O1 73.52(17) 5_665 3_565 ?
O1 Sm1 O1 127.7(3) 8_655 3_565 ?
O1 Sm1 O1 115.6(4) 4_655 3_565 ?
O1 Sm1 O1 73.52(17) 6 3_565 ?
O1 Sm1 O1 157.0(3) 2_665 3_565 ?
O1 Sm1 O1 73.52(17) . 7_565 ?
O1 Sm1 O1 69.3(3) 5_665 7_565 ?
O1 Sm1 O1 115.6(4) 8_655 7_565 ?
O1 Sm1 O1 127.7(3) 4_655 7_565 ?
O1 Sm1 O1 157.0(3) 6 7_565 ?
O1 Sm1 O1 73.52(17) 2_665 7_565 ?
O1 Sm1 O1 87.5(3) 3_565 7_565 ?
O2 S1 O1 111.9(3) . . ?
O2 S1 O1 111.9(3) . 10 ?
O1 S1 O1 112.2(6) . 10 ?
O2 S1 C1 105.5(5) . . ?
O1 S1 C1 107.4(3) . . ?
O1 S1 C1 107.4(3) 10 . ?
C2 C1 C2 119.5(8) 10 . ?
C2 C1 S1 120.1(4) 10 . ?
C2 C1 S1 120.1(4) . . ?
C3 C4 C3 117.9(8) 10 . ?
C3 C4 C5 121.0(4) 10 . ?
C3 C4 C5 121.0(4) . . ?
C8 C7 C6 106.7(8) . . ?
C8 C7 H3 126.7 . . ?
C6 C7 H3 126.6 . . ?
C9 N1 C6 109.4(9) . . ?
C9 N1 V1 122.8(7) . 9_565 ?
C6 N1 V1 121.6(7) . 9_565 ?
C9 N1 V1 122.8(7) . 1_565 ?
C6 N1 V1 121.6(7) . 1_565 ?
V1 N1 V1 46(2) 9_565 1_565 ?
C2 C3 C4 120.6(7) . . ?
C2 C3 H5 119.7 . . ?
C4 C3 H5 119.7 . . ?
C1 C2 C3 120.7(7) . . ?
C1 C2 H6 119.6 . . ?
C3 C2 H6 119.7 . . ?
C9 C5 C6 124.3(9) 7_465 . ?
C9 C5 C4 119.3(8) 7_465 . ?
C6 C5 C4 116.4(8) . . ?
N1 C6 C5 127.4(9) . . ?
N1 C6 C7 107.1(8) . . ?
C5 C6 C7 125.5(9) . . ?
N1 C9 C5 127.6(10) . 15_665 ?
N1 C9 C8 108.6(9) . . ?
C5 C9 C8 123.8(9) 15_665 . ?
S1 O1 Sm1 152.8(4) . . ?
C7 C8 C9 108.3(9) . . ?
C7 C8 H4 125.8 . . ?
C9 C8 H4 125.9 . . ?
V1 O3 V1 180.000(3) . 3 ?
N12 N11 N21 50.7(6) . 9_565 ?
N21 N22 N21 180.000(4) . 3_565 ?
N22 N21 N11 140.7(6) . 9_565 ?
O3 V1 V1 180.000(1) . 9 ?
O3 V1 N1 112.9(10) . 15_655 ?
V1 V1 N1 67.1(10) 9 15_655 ?
O3 V1 N1 112.9(10) . 1_545 ?
V1 V1 N1 67.1(10) 9 1_545 ?
N1 V1 N1 81.3(7) 15_655 1_545 ?
O3 V1 N1 112.9(10) . 7_455 ?
V1 V1 N1 67.1(10) 9 7_455 ?
N1 V1 N1 134(2) 15_655 7_455 ?
N1 V1 N1 81.3(7) 1_545 7_455 ?
O3 V1 N1 112.9(10) . 9_565 ?
V1 V1 N1 67.1(10) 9 9_565 ?
N1 V1 N1 81.3(7) 15_655 9_565 ?
N1 V1 N1 134(2) 1_545 9_565 ?
N1 V1 N1 81.3(7) 7_455 9_565 ?
N11 N12 N11 180.000(3) . 9_565 ?
N11 N12 N21 90.000(2) . 9_565 ?
N11 N12 N21 90.000(2) 9_565 9_565 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 S1 C1 C2 -87.1(7) . . . 10 ?
O1 S1 C1 C2 153.3(7) . . . 10 ?
O1 S1 C1 C2 32.4(8) 10 . . 10 ?
O2 S1 C1 C2 87.1(7) . . . . ?
O1 S1 C1 C2 -32.4(8) . . . . ?
O1 S1 C1 C2 -153.3(7) 10 . . . ?
C3 C4 C3 C2 1.1(13) 10 . . . ?
C5 C4 C3 C2 -179.1(8) . . . . ?
C2 C1 C2 C3 1.3(14) 10 . . . ?
S1 C1 C2 C3 -173.0(6) . . . . ?
C4 C3 C2 C1 -1.2(11) . . . . ?
C3 C4 C5 C9 89.9(7) 10 . . 7_465 ?
C3 C4 C5 C9 -89.9(7) . . . 7_465 ?
C3 C4 C5 C6 -90.1(7) 10 . . . ?
C3 C4 C5 C6 90.1(7) . . . . ?
C9 N1 C6 C5 180.0 . . . . ?
V1 N1 C6 C5 -27.2(11) 9_565 . . . ?
V1 N1 C6 C5 27.2(11) 1_565 . . . ?
C9 N1 C6 C7 0.0 . . . . ?
V1 N1 C6 C7 152.8(11) 9_565 . . . ?
V1 N1 C6 C7 -152.8(11) 1_565 . . . ?
C9 C5 C6 N1 0.0 7_465 . . . ?
C4 C5 C6 N1 180.0 . . . . ?
C9 C5 C6 C7 180.0 7_465 . . . ?
C4 C5 C6 C7 0.0 . . . . ?
C8 C7 C6 N1 0.0 . . . . ?
C8 C7 C6 C5 180.0 . . . . ?
C6 N1 C9 C5 180.0 . . . 15_665 ?
V1 N1 C9 C5 27.6(12) 9_565 . . 15_665 ?
V1 N1 C9 C5 -27.6(12) 1_565 . . 15_665 ?
C6 N1 C9 C8 0.0 . . . . ?
V1 N1 C9 C8 -152.4(12) 9_565 . . . ?
V1 N1 C9 C8 152.4(12) 1_565 . . . ?
O2 S1 O1 Sm1 163.0(7) . . . . ?
O1 S1 O1 Sm1 36.2(10) 10 . . . ?
C1 S1 O1 Sm1 -81.6(8) . . . . ?
O1 Sm1 O1 S1 85.1(8) 5_665 . . . ?
O1 Sm1 O1 S1 -84.9(7) 8_655 . . . ?
O1 Sm1 O1 S1 -120.3(8) 4_655 . . . ?
O1 Sm1 O1 S1 -154.0(9) 6 . . . ?
O1 Sm1 O1 S1 -22.9(7) 2_665 . . . ?
O1 Sm1 O1 S1 132.7(9) 3_565 . . . ?
O1 Sm1 O1 S1 39.1(8) 7_565 . . . ?
C6 C7 C8 C9 0.0 . . . . ?
N1 C9 C8 C7 0.0 . . . . ?
C5 C9 C8 C7 180.0 15_665 . . . ?
N21 N22 N21 N11 0(100) 3_565 . . 9_565 ?
V1 O3 V1 V1 0.0 3 . . 9 ?
V1 O3 V1 N1 0(100) 3 . . 15_655 ?
V1 O3 V1 N1 0(100) 3 . . 1_545 ?
V1 O3 V1 N1 0(100) 3 . . 7_455 ?
V1 O3 V1 N1 0(100) 3 . . 9_565 ?
N21 N11 N12 N11 -90.000(1) 9_565 . . 9_565 ?

_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         4.208
_refine_diff_density_min         -1.471
_refine_diff_density_rms         0.198