# Electronic Supplementary Material (ESI) for CrystEngComm
# This journal is © The Royal Society of Chemistry 2012


data_publication_text
_journal_name_full               CrystEngComm
_journal_coden_cambridge         1350
#TrackingRef '- compound_4.cif'

_publ_contact_author_name        'Professor Frances Lloret'
_publ_contact_author_address     
;Instituto de Ciencia Molecular (ICMol),
Universitat de Valencia, 46980 Paterna, Valencia, Spain.
;
_publ_contact_author_email       francisco.lloret@uv.es
_publ_contact_author_phone       +34963544440
_publ_contact_author_fax         +34963543273
loop_
_publ_author_name
_publ_author_address
F.Lloret
;Instituto de Ciencia Molecular (ICMol),
Universitat de Valencia, 46980 Paterna, Valencia, Spain.
;
M.-C.Dul ''
R.Lescouezec ''
L.-M.Chamoreau ''
Y.Journaux ''
R.Carrasco ''
M.Castellano ''
R.Ruiz-Garcia ''
J.Cano ''
M.Julve ''
C.Ruiz-Perez ''
O.Fabelo ''
E.Pardo ''

data_compound_1
_database_code_depnum_ccdc_archive 'CCDC 844822'
#TrackingRef '- compound_4.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H42 N6 Na8 Ni2 O33'
_chemical_melting_point          ?

_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1316.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni 0.3393 1.1124 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_int_tables_number      176
_chemical_absolute_configuration ?

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

_cell_length_a                   12.606(3)
_cell_length_b                   12.606(3)
_cell_length_c                   19.668(4)
_cell_angle_alpha                90.000(15)
_cell_angle_beta                 90.000(18)
_cell_angle_gamma                120.000(19)
_cell_volume                     2706.8(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Green
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.615
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1344
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12800
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_sigmaI/netI    0.0387
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.55
_diffrn_reflns_theta_max         22.99
_reflns_number_total             1284
_reflns_number_gt                966
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_cell_refinement       ?
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_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^)+(0.0938P)^2^+12.4670P] 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         1284
_refine_ls_number_parameters     139
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0767
_refine_ls_wR_factor_ref         0.2140
_refine_ls_wR_factor_gt          0.1925
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.126
_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
Ni1 Ni 0.3333 0.6667 0.57657(7) 0.0407(6) Uani 1 3 d S . .
O1 O 0.4711(5) 0.6743(5) 0.5129(2) 0.0489(13) Uani 1 1 d . . .
O2 O 0.6275(5) 0.6406(6) 0.5196(3) 0.0645(16) Uani 1 1 d . . .
O3 O 0.5227(5) 0.4900(5) 0.6275(2) 0.0594(15) Uani 1 1 d . . .
N1 N 0.3751(5) 0.5486(5) 0.6266(3) 0.0397(14) Uani 1 1 d . . .
C1 C 0.5289(7) 0.6272(7) 0.5397(4) 0.0475(18) Uani 1 1 d . . .
C2 C 0.4700(7) 0.5472(6) 0.6045(4) 0.0446(18) Uani 1 1 d . . .
C3 C 0.3218(6) 0.4865(6) 0.6888(3) 0.0384(16) Uani 1 1 d . . .
C4 C 0.2107(7) 0.3803(6) 0.6889(4) 0.0464(18) Uani 1 1 d . . .
H4 H 0.1728 0.3435 0.6481 0.056 Uiso 1 1 calc R . .
C6 C 0.3773(9) 0.5368(10) 0.7500 0.041(2) Uani 1 2 d S . .
H6 H 0.4545 0.6066 0.7500 0.050 Uiso 1 2 calc SR . .
C5 C 0.1557(11) 0.3287(10) 0.7500 0.057(3) Uani 1 2 d S . .
H5 H 0.0797 0.2574 0.7500 0.068 Uiso 1 2 calc SR . .
Na1 Na 0.3117(4) 0.4897(4) 0.43253(17) 0.0771(12) Uani 1 1 d . . .
Na2 Na 0.8006(15) 0.8268(14) 0.4652(9) 0.124(5) Uani 0.33 1 d P . .
O1W O 0.3333 0.6667 0.3545(6) 0.089(4) Uani 1 3 d S . .
O2W O 0.1342(9) 0.3665(11) 0.3675(7) 0.182(6) Uani 1 1 d . . .
O3W O -0.127(8) -0.064(5) 0.341(5) 0.22(4) Uani 0.17 1 d P . .
O4W O 0.600(2) 0.476(2) 0.7500 0.237(13) Uani 1 2 d S . .
O5W O 0.1541(18) 0.351(2) 0.2500 0.212(9) Uani 1 2 d S . .

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
Ni1 0.0457(7) 0.0457(7) 0.0308(9) 0.000 0.000 0.0228(4)
O1 0.060(3) 0.063(3) 0.036(3) 0.008(2) 0.009(2) 0.039(3)
O2 0.055(3) 0.086(4) 0.057(3) 0.004(3) 0.014(3) 0.039(3)
O3 0.079(4) 0.079(4) 0.047(3) 0.003(3) 0.004(3) 0.059(3)
N1 0.043(3) 0.049(3) 0.033(3) -0.004(3) 0.000(3) 0.027(3)
C1 0.053(5) 0.049(4) 0.038(4) -0.008(3) 0.002(4) 0.024(4)
C2 0.052(5) 0.045(4) 0.037(4) -0.008(3) -0.006(3) 0.024(4)
C3 0.049(4) 0.044(4) 0.028(3) 0.001(3) 0.001(3) 0.028(4)
C4 0.056(5) 0.034(4) 0.043(4) -0.005(3) -0.006(4) 0.019(4)
C6 0.045(6) 0.048(6) 0.039(6) 0.000 0.000 0.030(5)
C5 0.053(7) 0.048(7) 0.054(7) 0.000 0.000 0.014(6)
Na1 0.080(2) 0.115(3) 0.061(2) -0.007(2) 0.0019(18) 0.067(2)
Na2 0.106(10) 0.097(10) 0.141(13) 0.014(9) 0.025(10) 0.031(8)
O1W 0.104(6) 0.104(6) 0.057(7) 0.000 0.000 0.052(3)
O2W 0.118(8) 0.209(11) 0.251(14) -0.122(11) -0.097(9) 0.107(8)
O3W 0.30(8) 0.10(4) 0.32(10) 0.10(6) 0.10(8) 0.15(6)
O4W 0.43(3) 0.48(3) 0.067(7) 0.000 0.000 0.43(3)
O5W 0.173(17) 0.29(3) 0.170(16) 0.000 0.000 0.118(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
Ni1 N1 2.060(6) 3_665 ?
Ni1 N1 2.060(6) 4_565 ?
Ni1 N1 2.060(6) . ?
Ni1 O1 2.104(5) 3_665 ?
Ni1 O1 2.104(5) 4_565 ?
Ni1 O1 2.104(5) . ?
Ni1 Na1 3.531(4) 4_565 ?
Ni1 Na1 3.531(4) 3_665 ?
Ni1 Na1 3.531(4) . ?
O1 C1 1.263(9) . ?
O1 Na1 2.300(6) 3_665 ?
O1 Na1 2.697(6) . ?
O2 C1 1.233(9) . ?
O2 Na1 2.330(7) 7_666 ?
O2 Na2 2.508(16) . ?
O3 C2 1.283(9) . ?
O3 Na1 2.299(6) 7_666 ?
N1 C2 1.281(9) . ?
N1 C3 1.427(8) . ?
C1 C2 1.563(11) . ?
C1 Na1 3.077(9) 7_666 ?
C2 Na1 3.098(9) 7_666 ?
C3 C4 1.370(10) . ?
C3 C6 1.377(9) . ?
C4 C5 1.377(9) . ?
C6 C3 1.377(8) 8_557 ?
C5 C4 1.377(9) 8_557 ?
Na1 O3 2.299(6) 7_666 ?
Na1 O1 2.300(6) 4_565 ?
Na1 O2 2.330(7) 7_666 ?
Na1 O2W 2.362(9) . ?
Na1 O1W 2.608(8) . ?
Na1 C1 3.077(9) 7_666 ?
Na1 C2 3.098(9) 7_666 ?
Na1 Na1 3.651(7) 3_665 ?
Na1 Na1 3.651(7) 4_565 ?
Na1 Na2 3.686(19) 4_565 ?
Na2 O2W 2.67(2) 3_665 ?
Na2 O3W 2.73(8) 1_665 ?
Na2 Na2 2.73(2) 10_656 ?
Na2 Na2 2.73(2) 9_566 ?
Na2 Na1 3.686(19) 3_665 ?
Na2 Na1 4.039(16) 7_666 ?
Na2 Na2 4.10(3) 4_675 ?
Na2 Na2 4.10(3) 3_765 ?
O1W Na1 2.608(8) 4_565 ?
O1W Na1 2.608(8) 3_665 ?
O2W Na2 2.67(2) 4_565 ?
O3W Na2 2.73(8) 1_445 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 99.09(19) 3_665 4_565 ?
N1 Ni1 N1 99.09(19) 3_665 . ?
N1 Ni1 N1 99.09(19) 4_565 . ?
N1 Ni1 O1 79.3(2) 3_665 3_665 ?
N1 Ni1 O1 93.7(2) 4_565 3_665 ?
N1 Ni1 O1 167.2(2) . 3_665 ?
N1 Ni1 O1 167.2(2) 3_665 4_565 ?
N1 Ni1 O1 79.3(2) 4_565 4_565 ?
N1 Ni1 O1 93.7(2) . 4_565 ?
O1 Ni1 O1 88.16(19) 3_665 4_565 ?
N1 Ni1 O1 93.7(2) 3_665 . ?
N1 Ni1 O1 167.2(2) 4_565 . ?
N1 Ni1 O1 79.3(2) . . ?
O1 Ni1 O1 88.16(19) 3_665 . ?
O1 Ni1 O1 88.16(19) 4_565 . ?
N1 Ni1 Na1 117.70(17) 3_665 4_565 ?
N1 Ni1 Na1 83.89(16) 4_565 4_565 ?
N1 Ni1 Na1 142.27(17) . 4_565 ?
O1 Ni1 Na1 38.63(15) 3_665 4_565 ?
O1 Ni1 Na1 49.63(15) 4_565 4_565 ?
O1 Ni1 Na1 89.74(15) . 4_565 ?
N1 Ni1 Na1 83.89(16) 3_665 3_665 ?
N1 Ni1 Na1 142.27(17) 4_565 3_665 ?
N1 Ni1 Na1 117.70(17) . 3_665 ?
O1 Ni1 Na1 49.63(15) 3_665 3_665 ?
O1 Ni1 Na1 89.74(15) 4_565 3_665 ?
O1 Ni1 Na1 38.63(15) . 3_665 ?
Na1 Ni1 Na1 62.26(11) 4_565 3_665 ?
N1 Ni1 Na1 142.27(17) 3_665 . ?
N1 Ni1 Na1 117.70(17) 4_565 . ?
N1 Ni1 Na1 83.89(16) . . ?
O1 Ni1 Na1 89.74(15) 3_665 . ?
O1 Ni1 Na1 38.63(15) 4_565 . ?
O1 Ni1 Na1 49.63(15) . . ?
Na1 Ni1 Na1 62.26(11) 4_565 . ?
Na1 Ni1 Na1 62.26(11) 3_665 . ?
C1 O1 Ni1 112.7(4) . . ?
C1 O1 Na1 136.6(5) . 3_665 ?
Ni1 O1 Na1 106.5(2) . 3_665 ?
C1 O1 Na1 101.3(4) . . ?
Ni1 O1 Na1 93.90(19) . . ?
Na1 O1 Na1 93.6(2) 3_665 . ?
C1 O2 Na1 116.0(5) . 7_666 ?
C1 O2 Na2 127.6(7) . . ?
Na1 O2 Na2 113.1(5) 7_666 . ?
C2 O3 Na1 116.9(5) . 7_666 ?
C2 N1 C3 118.1(6) . . ?
C2 N1 Ni1 115.2(5) . . ?
C3 N1 Ni1 125.8(4) . . ?
O2 C1 O1 125.5(7) . . ?
O2 C1 C2 118.1(7) . . ?
O1 C1 C2 116.4(6) . . ?
O2 C1 Na1 42.9(4) . 7_666 ?
O1 C1 Na1 165.4(5) . 7_666 ?
C2 C1 Na1 76.1(4) . 7_666 ?
N1 C2 O3 129.5(7) . . ?
N1 C2 C1 114.5(6) . . ?
O3 C2 C1 116.0(7) . . ?
N1 C2 Na1 170.8(5) . 7_666 ?
O3 C2 Na1 41.4(4) . 7_666 ?
C1 C2 Na1 74.6(4) . 7_666 ?
C4 C3 C6 119.0(7) . . ?
C4 C3 N1 120.5(6) . . ?
C6 C3 N1 120.3(7) . . ?
C3 C4 C5 119.3(7) . . ?
C3 C6 C3 121.8(10) . 8_557 ?
C4 C5 C4 121.5(10) 8_557 . ?
O3 Na1 O1 159.0(3) 7_666 4_565 ?
O3 Na1 O2 71.7(2) 7_666 7_666 ?
O1 Na1 O2 108.3(2) 4_565 7_666 ?
O3 Na1 O2W 107.7(4) 7_666 . ?
O1 Na1 O2W 92.5(3) 4_565 . ?
O2 Na1 O2W 107.0(4) 7_666 . ?
O3 Na1 O1W 84.3(2) 7_666 . ?
O1 Na1 O1W 92.2(2) 4_565 . ?
O2 Na1 O1W 155.6(2) 7_666 . ?
O2W Na1 O1W 84.4(4) . . ?
O3 Na1 O1 87.8(2) 7_666 . ?
O1 Na1 O1 71.2(2) 4_565 . ?
O2 Na1 O1 90.3(2) 7_666 . ?
O2W Na1 O1 159.5(3) . . ?
O1W Na1 O1 83.8(2) . . ?
O3 Na1 C1 51.0(2) 7_666 7_666 ?
O1 Na1 C1 125.6(2) 4_565 7_666 ?
O2 Na1 C1 21.12(18) 7_666 7_666 ?
O2W Na1 C1 114.3(3) . 7_666 ?
O1W Na1 C1 134.4(2) . 7_666 ?
O1 Na1 C1 85.77(19) . 7_666 ?
O3 Na1 C2 21.68(19) 7_666 7_666 ?
O1 Na1 C2 149.6(2) 4_565 7_666 ?
O2 Na1 C2 50.2(2) 7_666 7_666 ?
O2W Na1 C2 113.3(3) . 7_666 ?
O1W Na1 C2 105.6(2) . 7_666 ?
O1 Na1 C2 86.14(19) . 7_666 ?
C1 Na1 C2 29.3(2) 7_666 7_666 ?
O3 Na1 Ni1 124.2(2) 7_666 . ?
O1 Na1 Ni1 34.83(13) 4_565 . ?
O2 Na1 Ni1 99.91(17) 7_666 . ?
O2W Na1 Ni1 126.8(3) . . ?
O1W Na1 Ni1 89.4(2) . . ?
O1 Na1 Ni1 36.47(11) . . ?
C1 Na1 Ni1 107.32(16) 7_666 . ?
C2 Na1 Ni1 119.30(17) 7_666 . ?
O3 Na1 Na1 79.0(2) 7_666 3_665 ?
O1 Na1 Na1 83.88(15) 4_565 3_665 ?
O2 Na1 Na1 122.0(2) 7_666 3_665 ?
O2W Na1 Na1 129.4(4) . 3_665 ?
O1W Na1 Na1 45.56(16) . 3_665 ?
O1 Na1 Na1 38.95(14) . 3_665 ?
C1 Na1 Na1 108.2(2) 7_666 3_665 ?
C2 Na1 Na1 91.2(2) 7_666 3_665 ?
Ni1 Na1 Na1 58.87(5) . 3_665 ?
O3 Na1 Na1 128.93(19) 7_666 4_565 ?
O1 Na1 Na1 47.49(16) 4_565 4_565 ?
O2 Na1 Na1 155.57(15) 7_666 4_565 ?
O2W Na1 Na1 80.8(3) . 4_565 ?
O1W Na1 Na1 45.56(15) . 4_565 ?
O1 Na1 Na1 78.95(13) . 4_565 ?
C1 Na1 Na1 164.66(19) 7_666 4_565 ?
C2 Na1 Na1 148.4(2) 7_666 4_565 ?
Ni1 Na1 Na1 58.87(5) . 4_565 ?
Na1 Na1 Na1 60.000(2) 3_665 4_565 ?
O3 Na1 Na2 125.6(3) 7_666 4_565 ?
O1 Na1 Na2 72.7(3) 4_565 4_565 ?
O2 Na1 Na2 74.4(3) 7_666 4_565 ?
O2W Na1 Na2 46.2(5) . 4_565 ?
O1W Na1 Na2 125.8(3) . 4_565 ?
O1 Na1 Na2 133.7(3) . 4_565 ?
C1 Na1 Na2 92.3(3) 7_666 4_565 ?
C2 Na1 Na2 113.1(3) 7_666 4_565 ?
Ni1 Na1 Na2 102.5(3) . 4_565 ?
Na1 Na1 Na2 155.2(3) 3_665 4_565 ?
Na1 Na1 Na2 97.1(3) 4_565 4_565 ?
O2 Na2 O2W 81.4(5) . 3_665 ?
O2 Na2 O3W 140(2) . 1_665 ?
O2W Na2 O3W 61(2) 3_665 1_665 ?
O2 Na2 Na2 92.7(9) . 10_656 ?
O2W Na2 Na2 153.3(8) 3_665 10_656 ?
O3W Na2 Na2 114.9(18) 1_665 10_656 ?
O2 Na2 Na2 107.2(9) . 9_566 ?
O2W Na2 Na2 109.4(7) 3_665 9_566 ?
O3W Na2 Na2 97.4(14) 1_665 9_566 ?
Na2 Na2 Na2 97.2(8) 10_656 9_566 ?
O2 Na2 Na1 70.6(4) . 3_665 ?
O2W Na2 Na1 39.7(3) 3_665 3_665 ?
O3W Na2 Na1 86.1(17) 1_665 3_665 ?
Na2 Na2 Na1 158.8(9) 10_656 3_665 ?
Na2 Na2 Na1 76.4(5) 9_566 3_665 ?
O2 Na2 Na1 32.0(3) . 7_666 ?
O2W Na2 Na1 104.2(5) 3_665 7_666 ?
O3W Na2 Na1 143.9(14) 1_665 7_666 ?
Na2 Na2 Na1 62.5(6) 10_656 7_666 ?
Na2 Na2 Na1 118.8(8) 9_566 7_666 ?
Na1 Na2 Na1 102.5(3) 3_665 7_666 ?
O2 Na2 Na2 148.6(6) . 4_675 ?
O2W Na2 Na2 108.6(6) 3_665 4_675 ?
O3W Na2 Na2 63.6(17) 1_665 4_675 ?
Na2 Na2 Na2 90.000(7) 10_656 4_675 ?
Na2 Na2 Na2 41.4(4) 9_566 4_675 ?
Na1 Na2 Na2 97.6(6) 3_665 4_675 ?
Na1 Na2 Na2 146.3(3) 7_666 4_675 ?
O2 Na2 Na2 133.4(7) . 3_765 ?
O2W Na2 Na2 133.8(4) 3_665 3_765 ?
O3W Na2 Na2 75.6(18) 1_665 3_765 ?
Na2 Na2 Na2 41.4(4) 10_656 3_765 ?
Na2 Na2 Na2 90.000(6) 9_566 3_765 ?
Na1 Na2 Na2 155.7(5) 3_665 3_765 ?
Na1 Na2 Na2 101.7(6) 7_666 3_765 ?
Na2 Na2 Na2 60.000(4) 4_675 3_765 ?
Na1 O1W Na1 88.9(3) 4_565 3_665 ?
Na1 O1W Na1 88.9(3) 4_565 . ?
Na1 O1W Na1 88.9(3) 3_665 . ?
Na1 O2W Na2 94.0(6) . 4_565 ?

_diffrn_measured_fraction_theta_max 0.986
_diffrn_reflns_theta_full        22.99
_diffrn_measured_fraction_theta_full 0.986
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.595
_refine_diff_density_rms         0.112

data_compound_2
_database_code_depnum_ccdc_archive 'CCDC 844823'
#TrackingRef '- compound_5.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H12 Co2 N6 O18, 2 Na, 17(H2 O)'
_chemical_formula_sum            'C30 H46 Co2 N6 Na8 O35'
_chemical_formula_weight         1352.51

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'
Co Co 0.3494 0.9721 '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'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_Int_Tables_number      176

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

_cell_length_a                   12.625(2)
_cell_length_b                   12.625(2)
_cell_length_c                   19.867(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2742.4(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    29
_cell_measurement_theta_min      3.8
_cell_measurement_theta_max      14.8

_exptl_crystal_description       needle
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1380
_exptl_absorpt_coefficient_mu    0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.261
_exptl_absorpt_correction_T_max  0.819
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;

_diffrn_ambient_temperature      250(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  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_detector_area_resol_mean 9
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            41039
_diffrn_reflns_av_R_equivalents  0.1311
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         27.49
_reflns_number_total             2175
_reflns_number_gt                1522
_reflns_threshold_expression     >2\s(I)

_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_cell_refinement       'Dirax/lsq (Duisenberg & Schreurs,1989-2000)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs 1990-2000)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

_refine_special_details          
;
We are totally conscious of the poor quality of the data with hight values of
Rint and resulting hight values of wR2.
The disorder in the region of atom Na2 is complicated and the model proposed
do not lead to a clear coordination environement of Na2 atom.
There is a little residual density in that region but its refinement
did not improve the model and did not gave a sensible environnement for atoms.
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^ > 2\s(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^)+(0.1406P)^2^+3.8814P] 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         2175
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0809
_refine_ls_wR_factor_ref         0.2621
_refine_ls_wR_factor_gt          0.2390
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.134
_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
Co1 Co 0.3333 0.6667 0.57715(5) 0.0394(4) Uani 1 3 d S . .
O1 O 0.4685(3) 0.6710(4) 0.51353(16) 0.0529(10) Uani 1 1 d . . .
O2 O 0.6257(4) 0.6395(4) 0.5190(2) 0.0626(11) Uani 1 1 d . . .
O3 O 0.5205(4) 0.4880(4) 0.62766(17) 0.0574(10) Uani 1 1 d . . .
N1 N 0.3772(4) 0.5504(4) 0.62728(19) 0.0413(9) Uani 1 1 d . . .
C1 C 0.5273(5) 0.6253(5) 0.5401(2) 0.0460(11) Uani 1 1 d . . .
C2 C 0.4723(5) 0.5474(5) 0.6044(2) 0.0455(11) Uani 1 1 d . . .
C3 C 0.3239(4) 0.4885(4) 0.6891(2) 0.0390(10) Uani 1 1 d . . .
C4 C 0.2098(5) 0.3800(5) 0.6890(2) 0.0457(12) Uani 1 1 d . . .
H4 H 0.1704 0.3444 0.6482 0.055 Uiso 1 1 calc R . .
C6 C 0.3790(6) 0.5398(6) 0.7500 0.0385(14) Uani 1 2 d S . .
H6 H 0.4560 0.6114 0.7500 0.046 Uiso 1 2 calc SR . .
C5 C 0.1560(7) 0.3260(7) 0.7500 0.0522(18) Uani 1 2 d S . .
H5 H 0.0817 0.2513 0.7500 0.063 Uiso 1 2 calc SR . .
Na1 Na 0.3108(2) 0.4905(3) 0.43275(12) 0.0689(7) Uani 1 1 d . . .
Na2 Na 0.8042(9) 0.8218(9) 0.4708(5) 0.155(4) Uani 0.33 1 d P . .
O5W O 0.8042(9) 0.8218(9) 0.4708(5) 0.155(4) Uani 0.33 1 d P . .
O1W O 0.3333 0.6667 0.3531(4) 0.090(3) Uani 1 3 d S . .
O2WA O 0.1196(9) 0.3449(11) 0.3846(7) 0.106(3) Uani 0.67 1 d P . .
O2WB O 0.164(2) 0.402(4) 0.3475(11) 0.140(12) Uani 0.33 1 d P . .
O4WA O 0.6212(13) 0.4917(13) 0.7500 0.099(4) Uiso 0.67 2 d SP . .
O4WB O 0.1508(14) 0.3452(14) 0.2500 0.119(5) Uiso 0.67 2 d SP . .
O4WC O 0.5336(17) 0.4058(17) 0.7500 0.129(5) Uiso 0.67 2 d SP . .
O3W O -0.097(4) 0.018(4) 0.400(2) 0.122(13) Uiso 0.17 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
Co1 0.0460(5) 0.0460(5) 0.0261(6) 0.000 0.000 0.0230(2)
O1 0.060(2) 0.070(2) 0.0317(17) 0.0068(16) 0.0082(15) 0.0353(19)
O2 0.056(2) 0.075(3) 0.055(2) -0.002(2) 0.0152(18) 0.032(2)
O3 0.072(3) 0.078(3) 0.043(2) -0.0001(18) 0.0033(18) 0.053(2)
N1 0.047(2) 0.048(2) 0.0298(19) -0.0053(16) 0.0017(16) 0.0247(19)
C1 0.049(3) 0.051(3) 0.039(2) -0.011(2) 0.000(2) 0.025(2)
C2 0.048(3) 0.056(3) 0.033(2) -0.010(2) -0.001(2) 0.026(2)
C3 0.048(3) 0.040(2) 0.034(2) -0.0007(18) 0.0018(19) 0.025(2)
C4 0.049(3) 0.046(3) 0.041(3) -0.010(2) -0.005(2) 0.023(2)
C6 0.040(3) 0.043(3) 0.033(3) 0.000 0.000 0.021(3)
C5 0.051(4) 0.043(4) 0.056(4) 0.000 0.000 0.018(3)
Na1 0.0673(15) 0.0881(18) 0.0609(15) -0.0105(12) 0.0040(11) 0.0461(14)
Na2 0.124(6) 0.146(7) 0.142(8) 0.005(6) 0.033(6) 0.028(5)
O5W 0.124(6) 0.146(7) 0.142(8) 0.005(6) 0.033(6) 0.028(5)
O1W 0.109(4) 0.109(4) 0.052(5) 0.000 0.000 0.054(2)
O2WA 0.074(6) 0.115(7) 0.130(9) -0.061(7) -0.029(6) 0.046(5)
O2WB 0.106(17) 0.28(4) 0.074(12) -0.020(17) 0.002(11) 0.13(2)

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s 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
Co1 N1 2.065(4) 5_565 ?
Co1 N1 2.065(4) 3_665 ?
Co1 N1 2.065(4) . ?
Co1 O1 2.102(4) 3_665 ?
Co1 O1 2.102(4) 5_565 ?
Co1 O1 2.102(4) . ?
Co1 Na1 3.553(2) 5_565 ?
Co1 Na1 3.553(3) 3_665 ?
Co1 Na1 3.553(2) . ?
O1 C1 1.261(6) . ?
O1 Na1 2.328(4) 3_665 ?
O1 Na1 2.683(5) . ?
O2 C1 1.236(6) . ?
O2 Na1 2.361(5) 7_666 ?
O2 Na2 2.471(10) . ?
O3 C2 1.267(6) . ?
O3 Na1 2.340(4) 7_666 ?
N1 C2 1.301(7) . ?
N1 C3 1.430(6) . ?
C1 C2 1.550(7) . ?
C1 Na1 3.098(6) 7_666 ?
C2 Na1 3.097(6) 7_666 ?
C3 C6 1.385(6) . ?
C3 C4 1.406(7) . ?
C4 C5 1.390(6) . ?
C4 H4 0.9400 . ?
C6 C3 1.385(5) 8_557 ?
C6 H6 0.9400 . ?
C5 C4 1.390(6) 8_557 ?
C5 H5 0.9400 . ?
Na1 O1 2.328(4) 5_565 ?
Na1 O3 2.340(4) 7_666 ?
Na1 O2WB 2.34(2) . ?
Na1 O2 2.361(5) 7_666 ?
Na1 O2WA 2.384(9) . ?
Na1 O1W 2.626(6) . ?
Na1 C2 3.097(6) 7_666 ?
Na1 C1 3.098(6) 7_666 ?
Na1 Na1 3.630(5) 3_665 ?
Na1 Na1 3.630(5) 5_565 ?
Na2 O2WA 2.388(18) 3_665 ?
Na2 O3W 2.42(5) 3_665 ?
Na2 O3W 2.57(5) 1_665 ?
Na2 O5W 2.639(12) 9_566 ?
Na2 Na2 2.639(12) 9_566 ?
Na2 O5W 2.639(13) 11_656 ?
Na2 Na2 2.639(13) 11_656 ?
Na2 O3W 2.76(5) 11_666 ?
Na2 Na1 3.787(12) 3_665 ?
Na2 Na1 3.950(10) 7_666 ?
Na2 Na2 4.103(16) 5_675 ?
O1W Na1 2.626(6) 5_565 ?
O1W Na1 2.626(6) 3_665 ?
O2WA O2WB 0.99(3) . ?
O2WA Na2 2.388(18) 5_565 ?
O4WA O4WC 1.096(19) . ?
O3W Na2 2.42(5) 5_565 ?
O3W Na2 2.57(5) 1_445 ?
O3W Na2 2.76(5) 9_456 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Co1 N1 98.70(14) 5_565 3_665 ?
N1 Co1 N1 98.70(14) 5_565 . ?
N1 Co1 N1 98.70(14) 3_665 . ?
N1 Co1 O1 95.39(15) 5_565 3_665 ?
N1 Co1 O1 78.80(15) 3_665 3_665 ?
N1 Co1 O1 165.91(16) . 3_665 ?
N1 Co1 O1 78.80(15) 5_565 5_565 ?
N1 Co1 O1 165.91(15) 3_665 5_565 ?
N1 Co1 O1 95.39(15) . 5_565 ?
O1 Co1 O1 87.59(14) 3_665 5_565 ?
N1 Co1 O1 165.91(16) 5_565 . ?
N1 Co1 O1 95.39(15) 3_665 . ?
N1 Co1 O1 78.80(15) . . ?
O1 Co1 O1 87.59(14) 3_665 . ?
O1 Co1 O1 87.59(14) 5_565 . ?
N1 Co1 Na1 84.88(11) 5_565 5_565 ?
N1 Co1 Na1 117.40(12) 3_665 5_565 ?
N1 Co1 Na1 142.88(12) . 5_565 ?
O1 Co1 Na1 38.91(11) 3_665 5_565 ?
O1 Co1 Na1 48.78(11) 5_565 5_565 ?
O1 Co1 Na1 88.91(11) . 5_565 ?
N1 Co1 Na1 142.88(11) 5_565 3_665 ?
N1 Co1 Na1 84.88(11) 3_665 3_665 ?
N1 Co1 Na1 117.40(12) . 3_665 ?
O1 Co1 Na1 48.78(11) 3_665 3_665 ?
O1 Co1 Na1 88.91(11) 5_565 3_665 ?
O1 Co1 Na1 38.91(11) . 3_665 ?
Na1 Co1 Na1 61.44(8) 5_565 3_665 ?
N1 Co1 Na1 117.40(12) 5_565 . ?
N1 Co1 Na1 142.88(12) 3_665 . ?
N1 Co1 Na1 84.88(11) . . ?
O1 Co1 Na1 88.91(11) 3_665 . ?
O1 Co1 Na1 38.91(11) 5_565 . ?
O1 Co1 Na1 48.78(12) . . ?
Na1 Co1 Na1 61.44(8) 5_565 . ?
Na1 Co1 Na1 61.44(8) 3_665 . ?
C1 O1 Co1 113.1(3) . . ?
C1 O1 Na1 135.7(3) . 3_665 ?
Co1 O1 Na1 106.52(18) . 3_665 ?
C1 O1 Na1 102.6(3) . . ?
Co1 O1 Na1 95.11(15) . . ?
Na1 O1 Na1 92.57(17) 3_665 . ?
C1 O2 Na1 115.3(4) . 7_666 ?
C1 O2 Na2 130.4(5) . . ?
Na1 O2 Na2 109.7(3) 7_666 . ?
C2 O3 Na1 115.1(3) . 7_666 ?
C2 N1 C3 118.2(4) . . ?
C2 N1 Co1 115.5(3) . . ?
C3 N1 Co1 125.6(3) . . ?
O2 C1 O1 124.8(5) . . ?
O2 C1 C2 118.1(5) . . ?
O1 C1 C2 117.1(4) . . ?
O2 C1 Na1 43.5(3) . 7_666 ?
O1 C1 Na1 165.3(3) . 7_666 ?
C2 C1 Na1 75.5(3) . 7_666 ?
O3 C2 N1 127.9(5) . . ?
O3 C2 C1 118.7(4) . . ?
N1 C2 C1 113.4(4) . . ?
O3 C2 Na1 43.2(2) . 7_666 ?
N1 C2 Na1 171.0(4) . 7_666 ?
C1 C2 Na1 75.5(3) . 7_666 ?
C6 C3 C4 119.1(5) . . ?
C6 C3 N1 120.4(4) . . ?
C4 C3 N1 120.3(4) . . ?
C5 C4 C3 119.2(5) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C3 C6 C3 121.8(6) . 8_557 ?
C3 C6 H6 119.1 . . ?
C3 C6 H6 119.1 8_557 . ?
C4 C5 C4 121.4(7) 8_557 . ?
C4 C5 H5 119.3 8_557 . ?
C4 C5 H5 119.3 . . ?
O1 Na1 O3 158.39(19) 5_565 7_666 ?
O1 Na1 O2WB 101.1(5) 5_565 . ?
O3 Na1 O2WB 98.1(5) 7_666 . ?
O1 Na1 O2 108.41(17) 5_565 7_666 ?
O3 Na1 O2 71.49(15) 7_666 7_666 ?
O2WB Na1 O2 115.3(9) . 7_666 ?
O1 Na1 O2WA 88.1(3) 5_565 . ?
O3 Na1 O2WA 113.3(3) 7_666 . ?
O2WB Na1 O2WA 24.2(7) . . ?
O2 Na1 O2WA 101.0(4) 7_666 . ?
O1 Na1 O1W 93.13(18) 5_565 . ?
O3 Na1 O1W 83.45(15) 7_666 . ?
O2WB Na1 O1W 72.0(9) . . ?
O2 Na1 O1W 154.51(16) 7_666 . ?
O2WA Na1 O1W 92.9(4) . . ?
O1 Na1 O1 70.61(18) 5_565 . ?
O3 Na1 O1 87.83(15) 7_666 . ?
O2WB Na1 O1 155.8(9) . . ?
O2 Na1 O1 88.94(16) 7_666 . ?
O2WA Na1 O1 158.5(3) . . ?
O1W Na1 O1 85.47(17) . . ?
O1 Na1 C2 149.52(17) 5_565 7_666 ?
O3 Na1 C2 21.73(14) 7_666 7_666 ?
O2WB Na1 C2 107.7(6) . 7_666 ?
O2 Na1 C2 49.83(14) 7_666 7_666 ?
O2WA Na1 C2 114.7(3) . 7_666 ?
O1W Na1 C2 104.92(16) . 7_666 ?
O1 Na1 C2 86.30(14) . 7_666 ?
O1 Na1 C1 125.72(16) 5_565 7_666 ?
O3 Na1 C1 50.71(14) 7_666 7_666 ?
O2WB Na1 C1 117.0(8) . 7_666 ?
O2 Na1 C1 21.13(13) 7_666 7_666 ?
O2WA Na1 C1 111.0(3) . 7_666 ?
O1W Na1 C1 133.39(15) . 7_666 ?
O1 Na1 C1 84.93(14) . 7_666 ?
C2 Na1 C1 28.97(14) 7_666 7_666 ?
O1 Na1 Co1 34.57(10) 5_565 . ?
O3 Na1 Co1 123.94(14) 7_666 . ?
O2WB Na1 Co1 132.8(6) . . ?
O2 Na1 Co1 99.12(12) 7_666 . ?
O2WA Na1 Co1 122.7(3) . . ?
O1W Na1 Co1 90.90(17) . . ?
O1 Na1 Co1 36.12(8) . . ?
C2 Na1 Co1 119.27(12) 7_666 . ?
C1 Na1 Co1 106.82(11) 7_666 . ?
O1 Na1 Na1 83.76(11) 5_565 3_665 ?
O3 Na1 Na1 78.46(15) 7_666 3_665 ?
O2WB Na1 Na1 118.3(9) . 3_665 ?
O2 Na1 Na1 121.13(16) 7_666 3_665 ?
O2WA Na1 Na1 137.5(3) . 3_665 ?
O1W Na1 Na1 46.27(12) . 3_665 ?
O1 Na1 Na1 39.84(10) . 3_665 ?
C2 Na1 Na1 91.13(14) 7_666 3_665 ?
C1 Na1 Na1 107.49(15) 7_666 3_665 ?
Co1 Na1 Na1 59.28(4) . 3_665 ?
O1 Na1 Na1 47.59(12) 5_565 5_565 ?
O3 Na1 Na1 128.53(13) 7_666 5_565 ?
O2WB Na1 Na1 78.6(8) . 5_565 ?
O2 Na1 Na1 155.66(11) 7_666 5_565 ?
O2WA Na1 Na1 84.1(3) . 5_565 ?
O1W Na1 Na1 46.27(12) . 5_565 ?
O1 Na1 Na1 79.30(10) . 5_565 ?
C2 Na1 Na1 148.29(14) 7_666 5_565 ?
C1 Na1 Na1 164.22(13) 7_666 5_565 ?
Co1 Na1 Na1 59.28(4) . 5_565 ?
Na1 Na1 Na1 60.0 3_665 5_565 ?
O2WA Na2 O3W 98.7(11) 3_665 3_665 ?
O2WA Na2 O2 78.9(4) 3_665 . ?
O3W Na2 O2 142.6(12) 3_665 . ?
O2WA Na2 O3W 77.8(10) 3_665 1_665 ?
O3W Na2 O3W 56(2) 3_665 1_665 ?
O2 Na2 O3W 152.6(11) . 1_665 ?
O2WA Na2 O5W 103.6(6) 3_665 9_566 ?
O3W Na2 O5W 108.6(11) 3_665 9_566 ?
O2 Na2 O5W 108.2(5) . 9_566 ?
O3W Na2 O5W 64.1(11) 1_665 9_566 ?
O2WA Na2 Na2 103.6(6) 3_665 9_566 ?
O3W Na2 Na2 108.6(11) 3_665 9_566 ?
O2 Na2 Na2 108.2(5) . 9_566 ?
O3W Na2 Na2 64.1(11) 1_665 9_566 ?
O5W Na2 Na2 0.0(6) 9_566 9_566 ?
O2WA Na2 O5W 153.3(6) 3_665 11_656 ?
O3W Na2 O5W 66.1(11) 3_665 11_656 ?
O2 Na2 O5W 99.8(6) . 11_656 ?
O3W Na2 O5W 107.5(10) 1_665 11_656 ?
O5W Na2 O5W 102.1(4) 9_566 11_656 ?
Na2 Na2 O5W 102.1(4) 9_566 11_656 ?
O2WA Na2 Na2 153.3(6) 3_665 11_656 ?
O3W Na2 Na2 66.1(11) 3_665 11_656 ?
O2 Na2 Na2 99.8(6) . 11_656 ?
O3W Na2 Na2 107.5(10) 1_665 11_656 ?
O5W Na2 Na2 102.1(4) 9_566 11_656 ?
Na2 Na2 Na2 102.1(4) 9_566 11_656 ?
O5W Na2 Na2 0.0(6) 11_656 11_656 ?
O2WA Na2 O3W 148.9(11) 3_665 11_666 ?
O3W Na2 O3W 108.1(19) 3_665 11_666 ?
O2 Na2 O3W 88.8(10) . 11_666 ?
O3W Na2 O3W 103.9(18) 1_665 11_666 ?
O5W Na2 O3W 53.2(10) 9_566 11_666 ?
Na2 Na2 O3W 53.2(10) 9_566 11_666 ?
O5W Na2 O3W 56.7(10) 11_656 11_666 ?
Na2 Na2 O3W 56.7(10) 11_656 11_666 ?
O2WA Na2 Na1 37.4(3) 3_665 3_665 ?
O3W Na2 Na1 129.3(11) 3_665 3_665 ?
O2 Na2 Na1 68.7(3) . 3_665 ?
O3W Na2 Na1 84.1(11) 1_665 3_665 ?
O5W Na2 Na1 73.4(4) 9_566 3_665 ?
Na2 Na2 Na1 73.4(4) 9_566 3_665 ?
O5W Na2 Na1 164.6(5) 11_656 3_665 ?
Na2 Na2 Na1 164.6(5) 11_656 3_665 ?
O3W Na2 Na1 111.4(10) 11_666 3_665 ?
O2WA Na2 Na1 104.4(4) 3_665 7_666 ?
O3W Na2 Na1 115.3(11) 3_665 7_666 ?
O2 Na2 Na1 34.25(19) . 7_666 ?
O3W Na2 Na1 171.4(11) 1_665 7_666 ?
O5W Na2 Na1 122.6(5) 9_566 7_666 ?
Na2 Na2 Na1 122.6(5) 9_566 7_666 ?
O5W Na2 Na1 66.8(4) 11_656 7_666 ?
Na2 Na2 Na1 66.8(4) 11_656 7_666 ?
O3W Na2 Na1 78.6(9) 11_666 7_666 ?
Na1 Na2 Na1 102.8(2) 3_665 7_666 ?
O2WA Na2 Na2 105.6(5) 3_665 5_675 ?
O3W Na2 Na2 69.8(11) 3_665 5_675 ?
O2 Na2 Na2 147.1(4) . 5_675 ?
O3W Na2 Na2 33.5(10) 1_665 5_675 ?
O5W Na2 Na2 39.0(2) 9_566 5_675 ?
Na2 Na2 Na2 39.0(2) 9_566 5_675 ?
O5W Na2 Na2 90.000(3) 11_656 5_675 ?
Na2 Na2 Na2 90.000(3) 11_656 5_675 ?
O3W Na2 Na2 70.5(9) 11_666 5_675 ?
Na1 Na2 Na2 94.8(4) 3_665 5_675 ?
Na1 Na2 Na2 148.3(2) 7_666 5_675 ?
Na1 O1W Na1 87.5(2) 5_565 3_665 ?
Na1 O1W Na1 87.5(2) 5_565 . ?
Na1 O1W Na1 87.5(2) 3_665 . ?
O2WB O2WA Na1 75.4(17) . . ?
O2WB O2WA Na2 176(2) . 5_565 ?
Na1 O2WA Na2 105.1(5) . 5_565 ?
O2WA O2WB Na1 80.4(15) . . ?
Na2 O3W Na2 110.7(18) 5_565 1_445 ?
Na2 O3W Na2 60.8(11) 5_565 9_456 ?
Na2 O3W Na2 59.2(10) 1_445 9_456 ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.120