# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2004

data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182
_journal_volume                  ?
_journal_year                    ?
_journal_page_first              ?

_publ_section_title              
;
Octahedral Metal Clusters as Building Units in a
Neutral Layered Honeycomb Network, [Zn(en)]2[Nb6Cl12(CN)6]
;
_publ_contact_author_name        'Abdessadek Lachgar'
_publ_contact_author_address     
;Department of Chemistry
Wake Forest University
Winston Salem
NC 27109
;
_publ_contact_author_email       lachgar@wfu.edu
_publ_contact_author_fax         13367584656
loop_
_publ_author_name
'Abdou Lachgar'
'Cynthia S. Day'
'Bangbo Yan'

data_1
_database_code_depnum_ccdc_archive 'CCDC 240364'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H26 Cl12 N6 Na4 Nb6 O13'
_chemical_formula_weight         1465.15

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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/amd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z+1/2'
'x, -y, -z'
'y+1/4, x+3/4, -z+1/4'
'-y+1/4, -x+1/4, -z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1'
'x+1/2, -y+1/2, -z+1/2'
'y+3/4, x+5/4, -z+3/4'
'-y+3/4, -x+3/4, -z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z-1/2'
'-x, y, z'
'-y-1/4, -x-3/4, z-1/4'
'y-1/4, x-1/4, z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'
'-y+1/4, -x-1/4, z+1/4'
'y+1/4, x+1/4, z-1/4'

_cell_length_a                   14.2313(11)
_cell_length_b                   14.2313(11)
_cell_length_c                   19.413(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3931.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       partial
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    2.475
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2808
_exptl_absorpt_coefficient_mu    2.605
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.831
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(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  'CCD area detector'
_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            20074
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.05
_diffrn_reflns_theta_max         30.53
_reflns_number_total             1605
_reflns_number_gt                1244
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0353P)^2^+31.5218P] 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         1605
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0702
_refine_ls_R_factor_gt           0.0489
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0936
_refine_ls_goodness_of_fit_ref   1.169
_refine_ls_restrained_S_all      1.169
_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
Nb1 Nb 0.5000 0.2500 0.01864(4) 0.01259(16) Uani 1 4 d S . .
Nb2 Nb 0.39710(2) 0.35290(2) 0.1250 0.01273(14) Uani 1 2 d S . .
Cl1 Cl 0.5000 0.49219(9) 0.12605(8) 0.0181(3) Uani 1 2 d S . .
Cl2 Cl 0.37832(7) 0.37058(8) -0.00051(5) 0.0183(2) Uani 1 1 d . . .
C1 C 0.5000 0.2500 -0.0987(5) 0.0235(19) Uani 1 4 d S . .
N1 N 0.5000 0.2500 -0.1583(4) 0.035(2) Uani 1 4 d S . .
C2 C 0.2845(3) 0.4655(3) 0.1250 0.0220(12) Uani 1 2 d S . .
N2 N 0.2263(3) 0.5237(3) 0.1250 0.0376(15) Uani 1 2 d S . .
Na1 Na 0.2500 0.2500 -0.2500 0.0420(11) Uani 1 4 d S . .
Na2 Na 0.1111(3) 0.6389(3) 0.1250 0.0423(16) Uani 0.50 2 d SP . .
O1 O 0.2624(5) 0.2500 -0.3741(4) 0.059(2) Uani 1 2 d S . .
O2 O 0.1288(4) 0.3654(3) -0.2499(3) 0.0519(12) Uani 1 1 d . . .
O3 O 0.0000 0.7500 0.1583(17) 0.115(12) Uani 0.50 4 d SP . .

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
Nb1 0.0133(4) 0.0135(4) 0.0110(3) 0.000 0.000 0.000
Nb2 0.01225(17) 0.01225(17) 0.0137(2) 0.00015(18) 0.00015(18) 0.00119(17)
Cl1 0.0184(6) 0.0126(6) 0.0232(7) -0.0011(8) 0.000 0.000
Cl2 0.0204(7) 0.0180(7) 0.0163(4) 0.0026(5) -0.0020(5) 0.0028(4)
C1 0.005(5) 0.043(8) 0.022(4) 0.000 0.000 0.000
N1 0.067(9) 0.018(5) 0.019(4) 0.000 0.000 0.000
C2 0.0207(17) 0.0207(17) 0.025(3) 0.010(2) 0.010(2) -0.004(2)
N2 0.034(2) 0.034(2) 0.045(4) -0.005(3) -0.005(3) 0.011(3)
Na1 0.036(3) 0.041(3) 0.049(3) 0.000 0.001(2) 0.000
Na2 0.039(2) 0.039(2) 0.049(4) -0.002(3) -0.002(3) 0.017(3)
O1 0.061(5) 0.057(4) 0.059(4) 0.000 -0.034(5) 0.000
O2 0.049(4) 0.048(3) 0.059(3) 0.004(3) -0.008(3) 0.010(2)
O3 0.059(19) 0.14(3) 0.15(3) 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.

Hydrogen atoms were not located.
;

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
Nb1 C1 2.278(9) . ?
Nb1 Cl2 2.4660(10) 22_655 ?
Nb1 Cl2 2.4660(10) 29 ?
Nb1 Cl2 2.4660(10) 10_554 ?
Nb1 Cl2 2.4660(10) . ?
Nb1 Nb2 2.9243(6) 27_565 ?
Nb1 Nb2 2.9243(6) . ?
Nb1 Nb2 2.9243(6) 10_554 ?
Nb1 Nb2 2.9243(6) 20_656 ?
Nb2 C2 2.266(6) . ?
Nb2 Cl2 2.4640(10) . ?
Nb2 Cl2 2.4640(10) 16_554 ?
Nb2 Cl1 2.4647(11) 20_656 ?
Nb2 Cl1 2.4647(11) . ?
Nb2 Nb1 2.9243(6) 27_565 ?
Nb2 Nb2 2.9287(7) 27_565 ?
Nb2 Nb2 2.9287(7) 20_656 ?
Cl1 Nb2 2.4647(11) 27_565 ?
C1 N1 1.157(12) . ?
C2 N2 1.172(9) . ?
N2 Na2 2.319(9) . ?
Na1 O2 2.382(4) 29 ?
Na1 O2 2.382(4) 5_554 ?
Na1 O2 2.382(4) 25_554 ?
Na1 O2 2.382(4) . ?
Na1 O1 2.415(7) . ?
Na1 O1 2.415(7) 25_554 ?
Na1 Na2 3.5065(5) 11_544 ?
Na1 Na2 3.5065(5) 19_565 ?
Na1 Na2 3.5065(5) 2_564 ?
Na1 Na2 3.5065(5) 26_545 ?
Na2 O3 2.327(11) 27_465 ?
Na2 O3 2.327(11) . ?
Na2 O1 2.396(6) 2_565 ?
Na2 O1 2.396(6) 28 ?
Na2 O2 2.438(6) 12_454 ?
Na2 O2 2.438(6) 6_565 ?
Na2 Na2 3.162(9) 20_666 ?
Na2 Na2 3.162(9) 27_465 ?
Na2 Na1 3.5065(5) 12_454 ?
Na2 Na1 3.5065(5) 2_565 ?
O1 Na2 2.396(6) 2_564 ?
O1 Na2 2.396(6) 19_565 ?
O2 Na2 2.438(6) 11_544 ?
O3 O3 1.29(6) 27_465 ?
O3 Na2 2.327(11) 27_465 ?
O3 Na2 2.327(11) 20_666 ?
O3 Na2 2.327(11) 10_464 ?

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
C1 Nb1 Cl2 81.33(3) . 22_655 ?
C1 Nb1 Cl2 81.33(3) . 29 ?
Cl2 Nb1 Cl2 162.66(6) 22_655 29 ?
C1 Nb1 Cl2 81.33(3) . 10_554 ?
Cl2 Nb1 Cl2 88.19(5) 22_655 10_554 ?
Cl2 Nb1 Cl2 89.20(5) 29 10_554 ?
C1 Nb1 Cl2 81.33(3) . . ?
Cl2 Nb1 Cl2 89.20(5) 22_655 . ?
Cl2 Nb1 Cl2 88.19(5) 29 . ?
Cl2 Nb1 Cl2 162.66(6) 10_554 . ?
C1 Nb1 Nb2 134.914(12) . 27_565 ?
Cl2 Nb1 Nb2 53.59(3) 22_655 27_565 ?
Cl2 Nb1 Nb2 143.76(3) 29 27_565 ?
Cl2 Nb1 Nb2 95.93(3) 10_554 27_565 ?
Cl2 Nb1 Nb2 96.29(3) . 27_565 ?
C1 Nb1 Nb2 134.914(12) . . ?
Cl2 Nb1 Nb2 96.29(3) 22_655 . ?
Cl2 Nb1 Nb2 95.93(3) 29 . ?
Cl2 Nb1 Nb2 143.76(3) 10_554 . ?
Cl2 Nb1 Nb2 53.59(3) . . ?
Nb2 Nb1 Nb2 60.099(14) 27_565 . ?
C1 Nb1 Nb2 134.914(12) . 10_554 ?
Cl2 Nb1 Nb2 95.93(3) 22_655 10_554 ?
Cl2 Nb1 Nb2 96.29(3) 29 10_554 ?
Cl2 Nb1 Nb2 53.59(3) 10_554 10_554 ?
Cl2 Nb1 Nb2 143.76(3) . 10_554 ?
Nb2 Nb1 Nb2 60.099(14) 27_565 10_554 ?
Nb2 Nb1 Nb2 90.17(2) . 10_554 ?
C1 Nb1 Nb2 134.914(12) . 20_656 ?
Cl2 Nb1 Nb2 143.76(3) 22_655 20_656 ?
Cl2 Nb1 Nb2 53.59(3) 29 20_656 ?
Cl2 Nb1 Nb2 96.29(3) 10_554 20_656 ?
Cl2 Nb1 Nb2 95.93(3) . 20_656 ?
Nb2 Nb1 Nb2 90.17(2) 27_565 20_656 ?
Nb2 Nb1 Nb2 60.099(14) . 20_656 ?
Nb2 Nb1 Nb2 60.099(14) 10_554 20_656 ?
C2 Nb2 Cl2 81.44(3) . . ?
C2 Nb2 Cl2 81.44(3) . 16_554 ?
Cl2 Nb2 Cl2 162.87(5) . 16_554 ?
C2 Nb2 Cl1 81.46(11) . 20_656 ?
Cl2 Nb2 Cl1 88.01(5) . 20_656 ?
Cl2 Nb2 Cl1 89.45(5) 16_554 20_656 ?
C2 Nb2 Cl1 81.46(11) . . ?
Cl2 Nb2 Cl1 89.45(5) . . ?
Cl2 Nb2 Cl1 88.01(5) 16_554 . ?
Cl1 Nb2 Cl1 162.90(4) 20_656 . ?
C2 Nb2 Nb1 135.086(12) . . ?
Cl2 Nb2 Nb1 53.65(3) . . ?
Cl2 Nb2 Nb1 143.48(3) 16_554 . ?
Cl1 Nb2 Nb1 95.71(3) 20_656 . ?
Cl1 Nb2 Nb1 96.38(3) . . ?
C2 Nb2 Nb1 135.086(12) . 27_565 ?
Cl2 Nb2 Nb1 143.48(3) . 27_565 ?
Cl2 Nb2 Nb1 53.65(3) 16_554 27_565 ?
Cl1 Nb2 Nb1 96.38(3) 20_656 27_565 ?
Cl1 Nb2 Nb1 95.71(3) . 27_565 ?
Nb1 Nb2 Nb1 89.83(2) . 27_565 ?
C2 Nb2 Nb2 135.0 . 27_565 ?
Cl2 Nb2 Nb2 96.23(3) . 27_565 ?
Cl2 Nb2 Nb2 95.86(3) 16_554 27_565 ?
Cl1 Nb2 Nb2 143.55(2) 20_656 27_565 ?
Cl1 Nb2 Nb2 53.55(2) . 27_565 ?
Nb1 Nb2 Nb2 59.950(7) . 27_565 ?
Nb1 Nb2 Nb2 59.950(7) 27_565 27_565 ?
C2 Nb2 Nb2 135.0 . 20_656 ?
Cl2 Nb2 Nb2 95.86(3) . 20_656 ?
Cl2 Nb2 Nb2 96.23(3) 16_554 20_656 ?
Cl1 Nb2 Nb2 53.55(2) 20_656 20_656 ?
Cl1 Nb2 Nb2 143.55(2) . 20_656 ?
Nb1 Nb2 Nb2 59.950(7) . 20_656 ?
Nb1 Nb2 Nb2 59.950(7) 27_565 20_656 ?
Nb2 Nb2 Nb2 90.0 27_565 20_656 ?
Nb2 Cl1 Nb2 72.90(4) . 27_565 ?
Nb2 Cl2 Nb1 72.76(3) . . ?
N1 C1 Nb1 180.0 . . ?
N2 C2 Nb2 180.0(5) . . ?
C2 N2 Na2 180.0(5) . . ?
O2 Na1 O2 180.0(3) 29 5_554 ?
O2 Na1 O2 92.8(3) 29 25_554 ?
O2 Na1 O2 87.2(3) 5_554 25_554 ?
O2 Na1 O2 87.2(3) 29 . ?
O2 Na1 O2 92.8(3) 5_554 . ?
O2 Na1 O2 180.0 25_554 . ?
O2 Na1 O1 93.08(19) 29 . ?
O2 Na1 O1 86.92(19) 5_554 . ?
O2 Na1 O1 86.92(19) 25_554 . ?
O2 Na1 O1 93.08(19) . . ?
O2 Na1 O1 86.92(19) 29 25_554 ?
O2 Na1 O1 93.08(19) 5_554 25_554 ?
O2 Na1 O1 93.08(19) 25_554 25_554 ?
O2 Na1 O1 86.92(19) . 25_554 ?
O1 Na1 O1 180.0 . 25_554 ?
O2 Na1 Na2 84.36(17) 29 11_544 ?
O2 Na1 Na2 95.64(17) 5_554 11_544 ?
O2 Na1 Na2 136.04(13) 25_554 11_544 ?
O2 Na1 Na2 43.96(13) . 11_544 ?
O1 Na1 Na2 137.00(13) . 11_544 ?
O1 Na1 Na2 43.00(13) 25_554 11_544 ?
O2 Na1 Na2 95.64(17) 29 19_565 ?
O2 Na1 Na2 84.36(17) 5_554 19_565 ?
O2 Na1 Na2 43.96(13) 25_554 19_565 ?
O2 Na1 Na2 136.04(13) . 19_565 ?
O1 Na1 Na2 43.00(13) . 19_565 ?
O1 Na1 Na2 137.00(13) 25_554 19_565 ?
Na2 Na1 Na2 180.00(12) 11_544 19_565 ?
O2 Na1 Na2 136.04(13) 29 2_564 ?
O2 Na1 Na2 43.96(13) 5_554 2_564 ?
O2 Na1 Na2 84.36(17) 25_554 2_564 ?
O2 Na1 Na2 95.64(17) . 2_564 ?
O1 Na1 Na2 43.00(13) . 2_564 ?
O1 Na1 Na2 137.00(13) 25_554 2_564 ?
Na2 Na1 Na2 126.40(17) 11_544 2_564 ?
Na2 Na1 Na2 53.60(17) 19_565 2_564 ?
O2 Na1 Na2 43.96(13) 29 26_545 ?
O2 Na1 Na2 136.04(13) 5_554 26_545 ?
O2 Na1 Na2 95.64(17) 25_554 26_545 ?
O2 Na1 Na2 84.36(17) . 26_545 ?
O1 Na1 Na2 137.00(13) . 26_545 ?
O1 Na1 Na2 43.00(13) 25_554 26_545 ?
Na2 Na1 Na2 53.60(17) 11_544 26_545 ?
Na2 Na1 Na2 126.40(17) 19_565 26_545 ?
Na2 Na1 Na2 180.00(12) 2_564 26_545 ?
N2 Na2 O3 163.9(8) . 27_465 ?
N2 Na2 O3 163.9(8) . . ?
O3 Na2 O3 32.3(15) 27_465 . ?
N2 Na2 O1 86.28(19) . 2_565 ?
O3 Na2 O1 93.69(19) 27_465 2_565 ?
O3 Na2 O1 93.45(18) . 2_565 ?
N2 Na2 O1 86.28(19) . 28 ?
O3 Na2 O1 93.45(18) 27_465 28 ?
O3 Na2 O1 93.69(19) . 28 ?
O1 Na2 O1 172.6(4) 2_565 28 ?
N2 Na2 O2 84.8(2) . 12_454 ?
O3 Na2 O2 79.1(8) 27_465 12_454 ?
O3 Na2 O2 111.3(8) . 12_454 ?
O1 Na2 O2 93.2(2) 2_565 12_454 ?
O1 Na2 O2 86.1(2) 28 12_454 ?
N2 Na2 O2 84.8(2) . 6_565 ?
O3 Na2 O2 111.3(8) 27_465 6_565 ?
O3 Na2 O2 79.1(8) . 6_565 ?
O1 Na2 O2 86.1(2) 2_565 6_565 ?
O1 Na2 O2 93.2(2) 28 6_565 ?
O2 Na2 O2 169.6(4) 12_454 6_565 ?
N2 Na2 Na2 135.000(1) . 20_666 ?
O3 Na2 Na2 47.2(2) 27_465 20_666 ?
O3 Na2 Na2 47.2(2) . 20_666 ?
O1 Na2 Na2 48.72(19) 2_565 20_666 ?
O1 Na2 Na2 138.71(19) 28 20_666 ?
O2 Na2 Na2 95.92(16) 12_454 20_666 ?
O2 Na2 Na2 91.43(15) 6_565 20_666 ?
N2 Na2 Na2 135.000(1) . 27_465 ?
O3 Na2 Na2 47.2(2) 27_465 27_465 ?
O3 Na2 Na2 47.2(2) . 27_465 ?
O1 Na2 Na2 138.71(19) 2_565 27_465 ?
O1 Na2 Na2 48.72(19) 28 27_465 ?
O2 Na2 Na2 91.43(15) 12_454 27_465 ?
O2 Na2 Na2 95.92(16) 6_565 27_465 ?
Na2 Na2 Na2 90.0 20_666 27_465 ?
N2 Na2 Na1 85.42(10) . 12_454 ?
O3 Na2 Na1 83.4(5) 27_465 12_454 ?
O3 Na2 Na1 105.6(5) . 12_454 ?
O1 Na2 Na1 135.71(17) 2_565 12_454 ?
O1 Na2 Na1 43.43(17) 28 12_454 ?
O2 Na2 Na1 42.69(10) 12_454 12_454 ?
O2 Na2 Na1 136.10(11) 6_565 12_454 ?
Na2 Na2 Na1 124.32(8) 20_666 12_454 ?
Na2 Na2 Na1 63.20(8) 27_465 12_454 ?
N2 Na2 Na1 85.42(10) . 2_565 ?
O3 Na2 Na1 105.6(5) 27_465 2_565 ?
O3 Na2 Na1 83.4(5) . 2_565 ?
O1 Na2 Na1 43.43(17) 2_565 2_565 ?
O1 Na2 Na1 135.71(17) 28 2_565 ?
O2 Na2 Na1 136.10(11) 12_454 2_565 ?
O2 Na2 Na1 42.69(10) 6_565 2_565 ?
Na2 Na2 Na1 63.20(8) 20_666 2_565 ?
Na2 Na2 Na1 124.32(8) 27_465 2_565 ?
Na1 Na2 Na1 170.8(2) 12_454 2_565 ?
Na2 O1 Na2 82.6(4) 2_564 19_565 ?
Na2 O1 Na1 93.57(19) 2_564 . ?
Na2 O1 Na1 93.57(19) 19_565 . ?
Na1 O2 Na2 93.35(17) . 11_544 ?
O3 O3 Na2 73.9(8) 27_465 27_465 ?
O3 O3 Na2 73.9(8) 27_465 20_666 ?
Na2 O3 Na2 147.7(15) 27_465 20_666 ?
O3 O3 Na2 73.9(8) 27_465 10_464 ?
Na2 O3 Na2 85.6(4) 27_465 10_464 ?
Na2 O3 Na2 85.6(4) 20_666 10_464 ?
O3 O3 Na2 73.9(8) 27_465 . ?
Na2 O3 Na2 85.6(4) 27_465 . ?
Na2 O3 Na2 85.6(4) 20_666 . ?
Na2 O3 Na2 147.7(15) 10_464 . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        30.53
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         1.386
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.181

data_a24c2f
_database_code_depnum_ccdc_archive 'CCDC 240365'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H16 Cl12 N10 Nb6 Zn2'
_chemical_formula_weight         1389.93

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   P-3
_symmetry_Int_Tables_number      147

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'

_cell_length_a                   10.8914(10)
_cell_length_b                   10.8914(10)
_cell_length_c                   8.6850(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     892.2(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       retangular
_exptl_crystal_colour            'dark green'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    4.097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.791
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_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            9092
_diffrn_reflns_av_R_equivalents  0.0699
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.32
_diffrn_reflns_theta_max         30.46
_reflns_number_total             1770
_reflns_number_gt                1278
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

The structure was initially solved in the P-3m1. Nb1, Cl1, Cl2, Zn1, C1
and N1  were fist located and were refined anisotropically
and this gave R1/wR2 == 0.0695/0.2076. The highest two residual electron
density peaks Q1 == 2.77 A^3^ (located at 2.39 A to Zn1, sof == 0.5) and
Q2 == 2.60 e/A^3^ (located at 1.53 A to Q1, sof == 0.5) were found. They
were assigned as N2 and C2 respectively and refined isotropically. Their
big thermal parameters (U == 0.167 for N2 and U == 0.145 for C2) indicated
they were partially occupied. In the meantime, a peak of  1.47 e/A^3^
located at 2.08 A to Zn1,  1.37 A to N2  and 1.52 A to C2 was found.
This peak was assigned as N2'. These atoms were anisotropically refined
with fixed occupancies(sof(N2)==0.1667, sof(C2)==0.3333, sof(N2')==0.1667).
This gave one en molecule per Zn and was confirmed by elemental analysis.
The final refinement led to R1/wR2 == 0.0598/0.1338. However, the Fo^2^
values were consistently larger than the Fc^2^ values. The model was
in a centrosymmetric space group and en was highly disordered. The
R(int)(0.069) for a higher symmetry Laue group(p-3m1) is only slightly
higher than the R(int)(0.063) for a lower symmetry Laue group(p-3).
This indicates the possible merohedral twin
in a lower symmetry laue group. The structure was
subsequently solved in P-3 using merohedral twin. Similar to the model
of p-3m1, the en was disordered (sof(N2)==0.3333, sof(C2)==0.6667,
sof(N2')==0.3333). At the final stage of refinement, all atoms except
for N2' were refined anisotropically. This led to R1/wR2 == 0.0568/0.1154
and basf == 0.492(8). Attempts to fix the carbon-carbon distances and
carbon-nitrogen distances for en, and to locate the hydrogen atoms
were not made due to the disorder of en.

;

_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^)+(0.0550P)^2^+3.7808P] 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         1770
_refine_ls_number_parameters     72
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0917
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1307
_refine_ls_wR_factor_gt          0.1154
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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
Nb1 Nb 0.0885(2) 0.17857(6) 0.13735(6) 0.0223(2) Uani 1 1 d . . .
Zn1 Zn 0.3333 0.6667 0.47109(17) 0.0372(4) Uani 1 3 d S . .
Cl1 Cl -0.0043(10) 0.3141(5) -0.0075(6) 0.0329(5) Uani 1 1 d . . .
Cl2 Cl 0.2100(2) 0.1076(7) 0.32313(19) 0.0338(5) Uani 1 1 d . . .
C1 C 0.195(3) 0.3733(9) 0.2886(9) 0.029(3) Uani 1 1 d . . .
N1 N 0.237(2) 0.4741(8) 0.3614(9) 0.051(2) Uani 1 1 d . . .
N2 N 0.289(11) 0.551(4) 0.674(3) 0.10(2) Uani 0.33 1 d P . .
C2 C 0.386(6) 0.639(5) 0.803(2) 0.096(16) Uani 0.67 1 d P . .
N2' N 0.409(5) 0.567(5) 0.666(3) 0.044(7) Uiso 0.33 1 d P . .

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
Nb1 0.0260(10) 0.0233(3) 0.0171(3) -0.0038(2) -0.0067(8) 0.0119(10)
Zn1 0.0440(6) 0.0440(6) 0.0237(7) 0.000 0.000 0.0220(3)
Cl1 0.0409(13) 0.028(2) 0.0342(11) -0.0024(19) -0.0074(10) 0.020(2)
Cl2 0.0396(10) 0.050(3) 0.0218(7) -0.001(2) -0.0119(7) 0.030(3)
C1 0.029(9) 0.031(4) 0.029(3) -0.007(3) 0.004(7) 0.016(7)
N1 0.049(11) 0.047(5) 0.035(4) -0.007(3) 0.010(10) 0.008(11)
N2 0.11(4) 0.11(3) 0.022(12) 0.030(14) 0.00(3) -0.01(4)
C2 0.19(5) 0.043(11) 0.051(9) 0.001(14) -0.02(2) 0.053(18)

_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
Nb1 C1 2.260(8) . ?
Nb1 Cl1 2.426(5) 5 ?
Nb1 Cl2 2.445(5) . ?
Nb1 Cl2 2.466(6) 2 ?
Nb1 Cl1 2.505(5) . ?
Nb1 Nb1 2.9173(11) 2 ?
Nb1 Nb1 2.9173(11) 3 ?
Nb1 Nb1 2.9203(10) 6 ?
Nb1 Nb1 2.9203(10) 5 ?
Zn1 N1 2.051(8) 3_565 ?
Zn1 N1 2.051(8) . ?
Zn1 N1 2.051(8) 2_665 ?
Zn1 N2 2.08(3) 3_565 ?
Zn1 N2 2.08(3) 2_665 ?
Zn1 N2 2.08(3) . ?
Zn1 N2' 2.37(2) 2_665 ?
Zn1 N2' 2.37(2) 3_565 ?
Zn1 N2' 2.37(2) . ?
Cl1 Nb1 2.426(5) 6 ?
Cl2 Nb1 2.466(6) 3 ?
C1 N1 1.145(11) . ?
N2 N2' 1.23(12) . ?
N2 C2 1.46(8) 3_565 ?
N2 C2 1.51(6) . ?
N2 N2' 1.69(12) 3_565 ?
C2 C2 1.33(5) 3_565 ?
C2 C2 1.33(5) 2_665 ?
C2 N2 1.46(8) 2_665 ?
C2 N2' 1.51(3) . ?
N2' N2 1.69(12) 2_665 ?

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
C1 Nb1 Cl1 78.3(6) . 5 ?
C1 Nb1 Cl2 78.9(6) . . ?
Cl1 Nb1 Cl2 88.1(2) 5 . ?
C1 Nb1 Cl2 83.5(5) . 2 ?
Cl1 Nb1 Cl2 161.8(2) 5 2 ?
Cl2 Nb1 Cl2 88.67(9) . 2 ?
C1 Nb1 Cl1 84.8(6) . . ?
Cl1 Nb1 Cl1 88.68(2) 5 . ?
Cl2 Nb1 Cl1 163.6(2) . . ?
Cl2 Nb1 Cl1 89.4(2) 2 . ?
C1 Nb1 Nb1 136.7(6) . 2 ?
Cl1 Nb1 Nb1 144.94(15) 5 2 ?
Cl2 Nb1 Nb1 96.25(13) . 2 ?
Cl2 Nb1 Nb1 53.22(15) 2 2 ?
Cl1 Nb1 Nb1 95.6(2) . 2 ?
C1 Nb1 Nb1 132.8(6) . 3 ?
Cl1 Nb1 Nb1 96.7(2) 5 3 ?
Cl2 Nb1 Nb1 53.90(16) . 3 ?
Cl2 Nb1 Nb1 95.77(11) 2 3 ?
Cl1 Nb1 Nb1 142.45(13) . 3 ?
Nb1 Nb1 Nb1 60.0 2 3 ?
C1 Nb1 Nb1 137.2(6) . 6 ?
Cl1 Nb1 Nb1 97.27(14) 5 6 ?
Cl2 Nb1 Nb1 143.90(17) . 6 ?
Cl2 Nb1 Nb1 95.87(12) 2 6 ?
Cl1 Nb1 Nb1 52.45(14) . 6 ?
Nb1 Nb1 Nb1 60.035(14) 2 6 ?
Nb1 Nb1 Nb1 90.0 3 6 ?
C1 Nb1 Nb1 133.2(6) . 5 ?
Cl1 Nb1 Nb1 54.94(15) 5 5 ?
Cl2 Nb1 Nb1 96.34(11) . 5 ?
Cl2 Nb1 Nb1 143.22(15) 2 5 ?
Cl1 Nb1 Nb1 94.89(13) . 5 ?
Nb1 Nb1 Nb1 90.0 2 5 ?
Nb1 Nb1 Nb1 60.035(14) 3 5 ?
Nb1 Nb1 Nb1 59.93(3) 6 5 ?
N1 Zn1 N1 100.2(3) 3_565 . ?
N1 Zn1 N1 100.2(3) 3_565 2_665 ?
N1 Zn1 N1 100.2(3) . 2_665 ?
N1 Zn1 N2 86.0(11) 3_565 3_565 ?
N1 Zn1 N2 125(4) . 3_565 ?
N1 Zn1 N2 133(4) 2_665 3_565 ?
N1 Zn1 N2 125(3) 3_565 2_665 ?
N1 Zn1 N2 133(4) . 2_665 ?
N1 Zn1 N2 86.0(11) 2_665 2_665 ?
N2 Zn1 N2 55(2) 3_565 2_665 ?
N1 Zn1 N2 133(4) 3_565 . ?
N1 Zn1 N2 86.0(11) . . ?
N1 Zn1 N2 125(3) 2_665 . ?
N2 Zn1 N2 55(2) 3_565 . ?
N2 Zn1 N2 55(2) 2_665 . ?
N1 Zn1 N2' 93.8(12) 3_565 2_665 ?
N1 Zn1 N2' 161.7(7) . 2_665 ?
N1 Zn1 N2' 88.7(12) 2_665 2_665 ?
N2 Zn1 N2' 44(3) 3_565 2_665 ?
N2 Zn1 N2' 31(3) 2_665 2_665 ?
N2 Zn1 N2' 75.9(11) . 2_665 ?
N1 Zn1 N2' 88.7(12) 3_565 3_565 ?
N1 Zn1 N2' 93.8(12) . 3_565 ?
N1 Zn1 N2' 161.7(7) 2_665 3_565 ?
N2 Zn1 N2' 31(3) 3_565 3_565 ?
N2 Zn1 N2' 75.9(11) 2_665 3_565 ?
N2 Zn1 N2' 44(3) . 3_565 ?
N2' Zn1 N2' 74.7(9) 2_665 3_565 ?
N1 Zn1 N2' 161.7(7) 3_565 . ?
N1 Zn1 N2' 88.7(12) . . ?
N1 Zn1 N2' 93.8(12) 2_665 . ?
N2 Zn1 N2' 75.9(11) 3_565 . ?
N2 Zn1 N2' 44(3) 2_665 . ?
N2 Zn1 N2' 31(3) . . ?
N2' Zn1 N2' 74.7(9) 2_665 . ?
N2' Zn1 N2' 74.7(9) 3_565 . ?
Nb1 Cl1 Nb1 72.61(6) 6 . ?
Nb1 Cl2 Nb1 72.89(5) . 3 ?
N1 C1 Nb1 173(3) . . ?
C1 N1 Zn1 172.6(16) . . ?
N2' N2 C2 120(4) . 3_565 ?
N2' N2 C2 66(4) . . ?
C2 N2 C2 53(2) 3_565 . ?
N2' N2 N2' 159(3) . 3_565 ?
C2 N2 N2' 57(4) 3_565 3_565 ?
C2 N2 N2' 106(5) . 3_565 ?
N2' N2 Zn1 87(3) . . ?
C2 N2 Zn1 114(5) 3_565 . ?
C2 N2 Zn1 111(2) . . ?
N2' N2 Zn1 77(3) 3_565 . ?
C2 C2 C2 60.000(3) 3_565 2_665 ?
C2 C2 N2 102(2) 3_565 2_665 ?
C2 C2 N2 65(4) 2_665 2_665 ?
C2 C2 N2 61(5) 3_565 . ?
C2 C2 N2 100(5) 2_665 . ?
N2 C2 N2 80(3) 2_665 . ?
C2 C2 N2' 109(4) 3_565 . ?
C2 C2 N2' 128.2(13) 2_665 . ?
N2 C2 N2' 69(4) 2_665 . ?
N2 C2 N2' 48(5) . . ?
N2 N2' C2 66(3) . . ?
N2 N2' N2 80(4) . 2_665 ?
C2 N2' N2 54(2) . 2_665 ?
N2 N2' Zn1 61.3(19) . . ?
C2 N2' Zn1 97.9(14) . . ?
N2 N2' Zn1 58.9(12) 2_665 . ?

_diffrn_measured_fraction_theta_max 0.975
_diffrn_reflns_theta_full        30.46
_diffrn_measured_fraction_theta_full 0.975
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.674
_refine_diff_density_rms         0.246