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


data_global
_journal_name_full               'Dalton Trans.'
_journal_coden_cambridge         0222
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Abrahams, Brendan F.'
_publ_contact_author_email       bfa@unimelb.edu.au
loop_
_publ_author_name
B.F.Abrahams
C.Abrahams
M.Haywood
T.Hudson
B.Moubaraki
;
K.S.Murray
;
R.Robson

data_CTA3AMO2final
_database_code_depnum_ccdc_archive 'CCDC 857015'
#TrackingRef '- CTA3AMO2final.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'H14 Cu2 Na5 O19 S4'
_chemical_formula_weight         688.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   15.3366(6)
_cell_length_b                   9.4848(3)
_cell_length_c                   13.7078(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 106.926(4)
_cell_angle_gamma                90.00
_cell_volume                     1907.62(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(1)
_cell_measurement_reflns_used    2720
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      28.54

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.061
_exptl_crystal_size_mid          0.031
_exptl_crystal_size_min          0.007
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.397
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1372
_exptl_absorpt_coefficient_mu    2.871
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8535
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0803
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.99
_reflns_number_total             4085
_reflns_number_gt                3042
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
H atoms on water molecules were refined with a restrained O-H separation
and an isotropic displacement parameter equal to 1.5 times the Ueq value
of the O atom to which it is bound.
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^)+(0.0416P)^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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4085
_refine_ls_number_parameters     313
_refine_ls_number_restraints     19
_refine_ls_R_factor_all          0.0740
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1025
_refine_ls_wR_factor_gt          0.0941
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      0.999
_refine_ls_shift/su_max          0.001
_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
Cu1 Cu 0.33219(4) 0.05807(6) 0.19391(4) 0.00747(16) Uani 1 1 d . . .
Cu2 Cu 0.47103(4) 0.75045(6) 0.49166(4) 0.00747(15) Uani 1 1 d . . .
S1 S 0.41823(8) 0.03979(13) 0.08331(9) 0.0058(3) Uani 1 1 d . . .
O1 O 0.3676(2) 0.0794(3) -0.0226(2) 0.0103(7) Uani 1 1 d . . .
O2 O 0.4503(2) -0.1110(3) 0.0856(2) 0.0076(7) Uani 1 1 d . . .
O3 O 0.5067(2) 0.1272(3) 0.1129(2) 0.0080(7) Uani 1 1 d . . .
S2 S 0.41630(8) 0.04075(12) 0.36196(9) 0.0059(3) Uani 1 1 d . . .
O4 O 0.5058(2) 0.1257(3) 0.3897(2) 0.0078(7) Uani 1 1 d . . .
O5 O 0.4465(2) -0.1104(3) 0.3827(2) 0.0063(7) Uani 1 1 d U . .
O6 O 0.3661(2) 0.0856(4) 0.4340(2) 0.0102(8) Uani 1 1 d . . .
S3 S 0.25408(8) -0.15165(13) 0.17344(9) 0.0073(3) Uani 1 1 d . . .
O7 O 0.2004(2) -0.1593(4) 0.2501(2) 0.0117(8) Uani 1 1 d . . .
O8 O 0.1862(2) -0.1703(4) 0.0692(2) 0.0119(8) Uani 1 1 d . . .
O9 O 0.3149(2) -0.2791(4) 0.1911(2) 0.0095(7) Uani 1 1 d . . .
S4 S 0.28806(8) 0.28857(13) 0.17948(9) 0.0066(3) Uani 1 1 d . . .
O10 O 0.2336(2) 0.3389(4) 0.2485(2) 0.0089(7) Uani 1 1 d . . .
O11 O 0.2370(2) 0.3358(4) 0.0729(2) 0.0094(7) Uani 1 1 d . . .
O12 O 0.3748(2) 0.3728(4) 0.2096(2) 0.0098(7) Uani 1 1 d . . .
Na1 Na 0.47848(12) -0.2236(2) 0.24390(13) 0.0079(4) Uani 1 1 d . . .
Na2 Na 0.33827(13) 0.5387(2) 0.32367(14) 0.0115(4) Uani 1 1 d . . .
Na3 Na 0.24648(13) 0.2553(2) 0.41730(14) 0.0103(4) Uani 1 1 d . . .
Na4 Na 0.34446(13) -0.4636(2) 0.07191(14) 0.0118(4) Uani 1 1 d . . .
Na5 Na 0.00847(13) 0.0457(2) 0.38438(14) 0.0136(4) Uani 1 1 d . . .
O13 O 0.3005(3) 0.7613(4) 0.4456(3) 0.0190(9) Uani 1 1 d D . .
H1 H 0.264(3) 0.735(6) 0.476(4) 0.028 Uiso 1 1 d D . .
H2 H 0.268(3) 0.796(6) 0.393(2) 0.028 Uiso 1 1 d D . .
O14 O 0.1102(2) -0.0460(4) 0.5343(3) 0.0146(8) Uani 1 1 d D . .
H3 H 0.151(3) 0.014(4) 0.548(4) 0.022 Uiso 1 1 d D . .
H4 H 0.128(4) -0.127(2) 0.535(4) 0.022 Uiso 1 1 d D . .
O15 O -0.0768(3) 0.1475(4) 0.2279(3) 0.0153(8) Uani 1 1 d D . .
H5 H -0.042(3) 0.194(5) 0.204(4) 0.023 Uiso 1 1 d D . .
H6 H -0.107(3) 0.213(4) 0.240(4) 0.023 Uiso 1 1 d D . .
O16 O 0.1334(2) 0.0833(4) 0.3188(3) 0.0135(8) Uani 1 1 d D . .
H7 H 0.161(3) 0.015(4) 0.308(4) 0.020 Uiso 1 1 d D . .
H8 H 0.115(4) 0.130(5) 0.266(2) 0.020 Uiso 1 1 d D . .
O17 O 0.0101(3) 0.2809(4) 0.4592(3) 0.0177(8) Uani 1 1 d D . .
H9 H 0.043(3) 0.340(5) 0.445(4) 0.027 Uiso 1 1 d D . .
H10 H -0.0426(16) 0.308(6) 0.434(4) 0.027 Uiso 1 1 d D . .
O18 O -0.0499(3) -0.1960(4) 0.3396(3) 0.0169(8) Uani 1 1 d D . .
H11 H -0.041(4) -0.219(6) 0.3994(16) 0.025 Uiso 1 1 d D . .
H12 H -0.1052(9) -0.184(6) 0.323(4) 0.025 Uiso 1 1 d D . .
O19 O 0.1427(3) 0.4496(4) 0.4243(3) 0.0156(8) Uani 1 1 d D . .
H13 H 0.158(4) 0.489(5) 0.480(2) 0.023 Uiso 1 1 d D . .
H14 H 0.122(4) 0.493(6) 0.370(4) 0.023 Uiso 1 1 d . . .

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
Cu1 0.0107(3) 0.0050(3) 0.0074(3) 0.0003(3) 0.0035(2) -0.0002(2)
Cu2 0.0138(3) 0.0038(3) 0.0056(3) 0.0003(3) 0.0041(2) 0.0000(2)
S1 0.0093(6) 0.0030(6) 0.0058(5) -0.0001(5) 0.0033(5) 0.0005(5)
O1 0.0143(18) 0.0089(19) 0.0082(17) 0.0014(15) 0.0041(15) 0.0026(15)
O2 0.0163(19) 0.0014(17) 0.0069(17) 0.0017(14) 0.0061(15) 0.0031(14)
O3 0.0105(17) 0.0069(18) 0.0077(17) -0.0016(15) 0.0046(14) -0.0032(14)
S2 0.0093(6) 0.0021(6) 0.0064(6) 0.0005(5) 0.0027(5) 0.0005(5)
O4 0.0107(17) 0.0070(18) 0.0059(16) -0.0006(15) 0.0028(14) -0.0024(14)
O5 0.0083(10) 0.0040(10) 0.0064(10) 0.0008(8) 0.0017(8) 0.0004(8)
O6 0.0120(18) 0.0109(19) 0.0080(17) -0.0003(15) 0.0032(14) 0.0047(15)
S3 0.0096(6) 0.0050(6) 0.0071(6) -0.0005(5) 0.0023(5) -0.0001(5)
O7 0.0126(18) 0.0121(19) 0.0138(18) 0.0005(16) 0.0091(15) -0.0004(15)
O8 0.0133(18) 0.0092(19) 0.0111(17) 0.0008(16) 0.0001(15) 0.0007(15)
O9 0.0113(18) 0.0070(18) 0.0095(17) 0.0021(15) 0.0017(14) -0.0008(14)
S4 0.0083(6) 0.0057(6) 0.0064(6) 0.0008(5) 0.0029(5) 0.0006(5)
O10 0.0087(17) 0.0127(19) 0.0066(16) -0.0037(15) 0.0045(14) -0.0014(15)
O11 0.0105(17) 0.0109(19) 0.0049(16) -0.0025(15) -0.0007(14) 0.0005(15)
O12 0.0114(18) 0.0091(19) 0.0091(17) -0.0023(15) 0.0034(14) -0.0008(15)
Na1 0.0110(10) 0.0067(10) 0.0068(9) 0.0001(8) 0.0038(8) 0.0005(8)
Na2 0.0151(10) 0.0096(11) 0.0088(9) -0.0002(8) 0.0018(8) -0.0034(9)
Na3 0.0134(10) 0.0092(11) 0.0092(9) 0.0019(8) 0.0046(8) 0.0005(8)
Na4 0.0167(10) 0.0100(11) 0.0102(10) 0.0002(8) 0.0060(8) -0.0026(9)
Na5 0.0135(10) 0.0120(11) 0.0153(10) 0.0001(9) 0.0042(8) 0.0003(9)
O13 0.017(2) 0.024(2) 0.015(2) 0.0131(18) 0.0035(16) -0.0004(18)
O14 0.0125(19) 0.010(2) 0.0197(19) -0.0019(19) 0.0017(16) -0.0032(16)
O15 0.017(2) 0.013(2) 0.017(2) 0.0015(17) 0.0083(16) 0.0051(17)
O16 0.016(2) 0.010(2) 0.0156(19) 0.0005(17) 0.0068(16) 0.0031(16)
O17 0.015(2) 0.015(2) 0.023(2) 0.0022(18) 0.0042(17) -0.0036(17)
O18 0.017(2) 0.019(2) 0.0142(19) 0.0002(18) 0.0043(17) 0.0023(18)
O19 0.021(2) 0.016(2) 0.0099(19) -0.0010(17) 0.0041(17) 0.0014(17)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 S4 2.2801(14) . ?
Cu1 S1 2.2880(12) . ?
Cu1 S2 2.2951(13) . ?
Cu1 S3 2.2967(14) . ?
Cu1 Na1 3.4275(19) . ?
Cu1 Na1 3.4646(19) 2_655 ?
Cu2 O2 1.935(3) 4_566 ?
Cu2 O5 1.946(3) 1_565 ?
Cu2 O4 1.953(3) 3_666 ?
Cu2 O3 1.955(3) 2_655 ?
Cu2 Na4 3.211(2) 4_566 ?
Cu2 Na2 3.279(2) . ?
Cu2 Na1 3.4355(18) 4_566 ?
Cu2 Na1 3.4401(18) 1_565 ?
S1 O1 1.482(3) . ?
S1 O2 1.510(3) . ?
S1 O3 1.540(3) . ?
S1 Na1 3.280(2) . ?
S1 Na1 3.312(2) 2_655 ?
O1 Na2 2.312(4) 4_565 ?
O1 Na3 2.387(4) 4_565 ?
O2 Cu2 1.935(3) 4_565 ?
O2 Na1 2.343(3) . ?
O3 Cu2 1.955(3) 2_645 ?
O3 Na1 2.377(4) 2_655 ?
O3 Na2 2.431(4) 2_645 ?
S2 O6 1.480(3) . ?
S2 O5 1.509(3) . ?
S2 O4 1.541(3) . ?
S2 Na1 3.274(2) . ?
S2 Na1 3.327(2) 2_655 ?
O4 Cu2 1.953(3) 3_666 ?
O4 Na4 2.359(4) 2_655 ?
O4 Na1 2.390(4) 2_655 ?
O5 Cu2 1.946(3) 1_545 ?
O5 Na1 2.357(3) . ?
O6 Na4 2.321(4) 4_556 ?
O6 Na3 2.401(4) . ?
S3 O9 1.503(3) . ?
S3 O8 1.513(3) . ?
S3 O7 1.513(3) . ?
S3 Na1 3.363(2) . ?
O9 Na1 2.456(4) . ?
O9 Na2 2.457(4) 1_545 ?
O9 Na4 2.523(4) . ?
S4 O12 1.503(4) . ?
S4 O11 1.510(3) . ?
S4 O10 1.510(3) . ?
S4 Na4 3.032(2) 1_565 ?
S4 Na2 3.040(2) . ?
O10 Na3 2.399(4) . ?
O10 Na2 2.503(4) . ?
O11 Na3 2.345(4) 4_565 ?
O11 Na4 2.520(4) 1_565 ?
O12 Na1 2.338(4) 2_655 ?
O12 Na4 2.383(4) 1_565 ?
O12 Na2 2.397(4) . ?
Na1 O12 2.338(4) 2_645 ?
Na1 O3 2.377(4) 2_645 ?
Na1 O4 2.390(4) 2_645 ?
Na1 S1 3.312(2) 2_645 ?
Na1 S2 3.327(2) 2_645 ?
Na2 O1 2.312(4) 4_566 ?
Na2 O3 2.431(4) 2_655 ?
Na2 O9 2.457(4) 1_565 ?
Na2 O13 2.855(5) . ?
Na2 Na3 3.451(3) . ?
Na2 Na4 3.480(3) 1_565 ?
Na2 Na1 3.503(3) 1_565 ?
Na2 Na1 4.058(3) 2_655 ?
Na3 O11 2.345(4) 4_566 ?
Na3 O1 2.387(4) 4_566 ?
Na3 O19 2.455(4) . ?
Na3 O16 2.476(4) . ?
Na3 Na4 3.543(3) 4_556 ?
Na3 Na5 4.064(3) . ?
Na4 O6 2.321(4) 4 ?
Na4 O4 2.359(4) 2_645 ?
Na4 O12 2.383(4) 1_545 ?
Na4 O11 2.520(4) 1_545 ?
Na4 O13 2.541(5) 4_565 ?
Na4 S4 3.032(2) 1_545 ?
Na4 Cu2 3.211(2) 4_565 ?
Na4 Na2 3.480(3) 1_545 ?
Na4 Na3 3.543(3) 4 ?
Na4 Na1 3.980(3) 2_645 ?
Na5 O14 2.356(4) . ?
Na5 O15 2.368(4) . ?
Na5 O16 2.369(4) . ?
Na5 O14 2.394(4) 3_556 ?
Na5 O17 2.452(4) . ?
Na5 O18 2.473(5) . ?
Na5 Na5 3.368(4) 3_556 ?
O13 Na4 2.541(5) 4_566 ?
O14 Na5 2.394(4) 3_556 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S4 Cu1 S1 103.24(5) . . ?
S4 Cu1 S2 102.81(5) . . ?
S1 Cu1 S2 113.31(5) . . ?
S4 Cu1 S3 133.53(5) . . ?
S1 Cu1 S3 103.55(5) . . ?
S2 Cu1 S3 100.45(5) . . ?
S4 Cu1 Na1 157.72(5) . . ?
S1 Cu1 Na1 66.62(4) . . ?
S2 Cu1 Na1 66.40(4) . . ?
S3 Cu1 Na1 68.72(5) . . ?
S4 Cu1 Na1 69.80(5) . 2_655 ?
S1 Cu1 Na1 66.71(4) . 2_655 ?
S2 Cu1 Na1 67.04(4) . 2_655 ?
S3 Cu1 Na1 156.58(5) . 2_655 ?
Na1 Cu1 Na1 87.921(16) . 2_655 ?
O2 Cu2 O5 160.33(14) 4_566 1_565 ?
O2 Cu2 O4 83.26(13) 4_566 3_666 ?
O5 Cu2 O4 100.30(13) 1_565 3_666 ?
O2 Cu2 O3 100.15(13) 4_566 2_655 ?
O5 Cu2 O3 83.04(13) 1_565 2_655 ?
O4 Cu2 O3 160.35(14) 3_666 2_655 ?
O2 Cu2 Na4 88.26(10) 4_566 4_566 ?
O5 Cu2 Na4 80.52(10) 1_565 4_566 ?
O4 Cu2 Na4 46.97(10) 3_666 4_566 ?
O3 Cu2 Na4 151.61(10) 2_655 4_566 ?
O2 Cu2 Na2 81.95(10) 4_566 . ?
O5 Cu2 Na2 86.25(10) 1_565 . ?
O4 Cu2 Na2 151.46(10) 3_666 . ?
O3 Cu2 Na2 47.48(10) 2_655 . ?
Na4 Cu2 Na2 108.21(5) 4_566 . ?
O2 Cu2 Na1 40.87(10) 4_566 4_566 ?
O5 Cu2 Na1 139.92(10) 1_565 4_566 ?
O4 Cu2 Na1 42.44(10) 3_666 4_566 ?
O3 Cu2 Na1 137.03(10) 2_655 4_566 ?
Na4 Cu2 Na1 63.13(5) 4_566 4_566 ?
Na2 Cu2 Na1 119.56(5) . 4_566 ?
O2 Cu2 Na1 139.87(10) 4_566 1_565 ?
O5 Cu2 Na1 41.25(9) 1_565 1_565 ?
O4 Cu2 Na1 136.77(10) 3_666 1_565 ?
O3 Cu2 Na1 41.93(10) 2_655 1_565 ?
Na4 Cu2 Na1 119.37(5) 4_566 1_565 ?
Na2 Cu2 Na1 62.79(5) . 1_565 ?
Na1 Cu2 Na1 176.35(6) 4_566 1_565 ?
O1 S1 O2 109.59(19) . . ?
O1 S1 O3 106.92(19) . . ?
O2 S1 O3 104.32(19) . . ?
O1 S1 Cu1 113.05(14) . . ?
O2 S1 Cu1 107.80(13) . . ?
O3 S1 Cu1 114.76(13) . . ?
O1 S1 Na1 144.67(15) . . ?
O2 S1 Na1 40.37(12) . . ?
O3 S1 Na1 100.31(14) . . ?
Cu1 S1 Na1 73.57(4) . . ?
O1 S1 Na1 122.26(15) . 2_655 ?
O2 S1 Na1 122.80(14) . 2_655 ?
O3 S1 Na1 41.07(12) . 2_655 ?
Cu1 S1 Na1 73.91(4) . 2_655 ?
Na1 S1 Na1 93.07(3) . 2_655 ?
S1 O1 Na2 132.6(2) . 4_565 ?
S1 O1 Na3 129.64(19) . 4_565 ?
Na2 O1 Na3 94.48(13) 4_565 4_565 ?
S1 O2 Cu2 138.53(19) . 4_565 ?
S1 O2 Na1 114.96(17) . . ?
Cu2 O2 Na1 106.43(15) 4_565 . ?
S1 O3 Cu2 117.23(19) . 2_645 ?
S1 O3 Na1 113.74(17) . 2_655 ?
Cu2 O3 Na1 104.74(14) 2_645 2_655 ?
S1 O3 Na2 127.11(19) . 2_645 ?
Cu2 O3 Na2 96.18(13) 2_645 2_645 ?
Na1 O3 Na2 93.53(13) 2_655 2_645 ?
O6 S2 O5 109.77(19) . . ?
O6 S2 O4 106.48(18) . . ?
O5 S2 O4 104.34(18) . . ?
O6 S2 Cu1 113.57(14) . . ?
O5 S2 Cu1 108.02(13) . . ?
O4 S2 Cu1 114.24(13) . . ?
O6 S2 Na1 146.38(15) . . ?
O5 S2 Na1 41.16(12) . . ?
O4 S2 Na1 98.98(13) . . ?
Cu1 S2 Na1 73.63(5) . . ?
O6 S2 Na1 120.71(15) . 2_655 ?
O5 S2 Na1 124.00(13) . 2_655 ?
O4 S2 Na1 41.08(12) . 2_655 ?
Cu1 S2 Na1 73.52(4) . 2_655 ?
Na1 S2 Na1 92.91(3) . 2_655 ?
S2 O4 Cu2 116.98(18) . 3_666 ?
S2 O4 Na4 127.36(19) . 2_655 ?
Cu2 O4 Na4 95.79(14) 3_666 2_655 ?
S2 O4 Na1 113.87(17) . 2_655 ?
Cu2 O4 Na1 104.11(14) 3_666 2_655 ?
Na4 O4 Na1 94.38(13) 2_655 2_655 ?
S2 O5 Cu2 140.29(19) . 1_545 ?
S2 O5 Na1 113.93(17) . . ?
Cu2 O5 Na1 105.77(14) 1_545 . ?
S2 O6 Na4 128.7(2) . 4_556 ?
S2 O6 Na3 131.29(19) . . ?
Na4 O6 Na3 97.21(13) 4_556 . ?
O9 S3 O8 106.40(19) . . ?
O9 S3 O7 106.74(19) . . ?
O8 S3 O7 106.61(19) . . ?
O9 S3 Cu1 113.54(14) . . ?
O8 S3 Cu1 114.04(14) . . ?
O7 S3 Cu1 109.05(14) . . ?
O9 S3 Na1 41.83(13) . . ?
O8 S3 Na1 127.79(14) . . ?
O7 S3 Na1 120.61(14) . . ?
Cu1 S3 Na1 71.76(5) . . ?
S3 O9 Na1 114.09(18) . . ?
S3 O9 Na2 129.36(18) . 1_545 ?
Na1 O9 Na2 90.93(12) . 1_545 ?
S3 O9 Na4 132.36(18) . . ?
Na1 O9 Na4 88.80(12) . . ?
Na2 O9 Na4 88.64(12) 1_545 . ?
O12 S4 O11 106.06(19) . . ?
O12 S4 O10 105.46(18) . . ?
O11 S4 O10 106.68(19) . . ?
O12 S4 Cu1 105.59(14) . . ?
O11 S4 Cu1 115.17(14) . . ?
O10 S4 Cu1 116.94(14) . . ?
O12 S4 Na4 50.71(14) . 1_565 ?
O11 S4 Na4 55.99(14) . 1_565 ?
O10 S4 Na4 110.34(14) . 1_565 ?
Cu1 S4 Na4 131.77(6) . 1_565 ?
O12 S4 Na2 50.97(13) . . ?
O11 S4 Na2 111.06(14) . . ?
O10 S4 Na2 55.07(13) . . ?
Cu1 S4 Na2 132.79(6) . . ?
Na4 S4 Na2 69.93(6) 1_565 . ?
S4 O10 Na3 126.5(2) . . ?
S4 O10 Na2 95.28(16) . . ?
Na3 O10 Na2 89.46(12) . . ?
S4 O11 Na3 128.2(2) . 4_565 ?
S4 O11 Na4 94.23(16) . 1_565 ?
Na3 O11 Na4 93.42(13) 4_565 1_565 ?
S4 O12 Na1 124.9(2) . 2_655 ?
S4 O12 Na4 100.07(17) . 1_565 ?
Na1 O12 Na4 114.91(14) 2_655 1_565 ?
S4 O12 Na2 99.88(16) . . ?
Na1 O12 Na2 117.93(15) 2_655 . ?
Na4 O12 Na2 93.43(13) 1_565 . ?
O12 Na1 O2 88.70(13) 2_645 . ?
O12 Na1 O5 90.66(13) 2_645 . ?
O2 Na1 O5 120.95(13) . . ?
O12 Na1 O3 98.90(13) 2_645 2_645 ?
O2 Na1 O3 169.72(14) . 2_645 ?
O5 Na1 O3 66.21(12) . 2_645 ?
O12 Na1 O4 97.98(13) 2_645 2_645 ?
O2 Na1 O4 66.13(12) . 2_645 ?
O5 Na1 O4 169.13(14) . 2_645 ?
O3 Na1 O4 105.70(13) 2_645 2_645 ?
O12 Na1 O9 169.34(14) 2_645 . ?
O2 Na1 O9 85.85(12) . . ?
O5 Na1 O9 84.33(12) . . ?
O3 Na1 O9 87.70(12) 2_645 . ?
O4 Na1 O9 88.18(12) 2_645 . ?
O12 Na1 S2 87.79(10) 2_645 . ?
O2 Na1 S2 96.14(10) . . ?
O5 Na1 S2 24.91(8) . . ?
O3 Na1 S2 91.09(9) 2_645 . ?
O4 Na1 S2 161.05(11) 2_645 . ?
O9 Na1 S2 83.71(9) . . ?
O12 Na1 S1 86.89(10) 2_645 . ?
O2 Na1 S1 24.67(8) . . ?
O5 Na1 S1 96.35(10) . . ?
O3 Na1 S1 161.51(10) 2_645 . ?
O4 Na1 S1 90.73(9) 2_645 . ?
O9 Na1 S1 84.34(9) . . ?
S2 Na1 S1 71.49(5) . . ?
O12 Na1 S1 81.27(10) 2_645 2_645 ?
O2 Na1 S1 153.12(11) . 2_645 ?
O5 Na1 S1 84.25(9) . 2_645 ?
O3 Na1 S1 25.20(8) 2_645 2_645 ?
O4 Na1 S1 90.52(9) 2_645 2_645 ?
O9 Na1 S1 107.48(10) . 2_645 ?
S2 Na1 S1 108.23(6) . 2_645 ?
S1 Na1 S1 168.15(7) . 2_645 ?
O12 Na1 S2 80.28(10) 2_645 2_645 ?
O2 Na1 S2 83.35(9) . 2_645 ?
O5 Na1 S2 154.06(11) . 2_645 ?
O3 Na1 S2 91.07(9) 2_645 2_645 ?
O4 Na1 S2 25.05(8) 2_645 2_645 ?
O9 Na1 S2 108.11(10) . 2_645 ?
S2 Na1 S2 168.06(7) . 2_645 ?
S1 Na1 S2 107.26(5) . 2_645 ?
S1 Na1 S2 70.43(5) 2_645 2_645 ?
O12 Na1 S3 145.27(11) 2_645 . ?
O2 Na1 S3 75.18(9) . . ?
O5 Na1 S3 72.75(9) . . ?
O3 Na1 S3 101.64(10) 2_645 . ?
O4 Na1 S3 102.98(10) 2_645 . ?
O9 Na1 S3 24.09(8) . . ?
S2 Na1 S3 64.24(4) . . ?
S1 Na1 S3 65.66(4) . . ?
S1 Na1 S3 125.41(6) 2_645 . ?
S2 Na1 S3 126.65(6) 2_645 . ?
O12 Na1 Cu1 105.75(10) 2_645 . ?
O2 Na1 Cu1 61.71(9) . . ?
O5 Na1 Cu1 61.87(9) . . ?
O3 Na1 Cu1 121.92(10) 2_645 . ?
O4 Na1 Cu1 121.27(10) 2_645 . ?
O9 Na1 Cu1 63.59(9) . . ?
S2 Na1 Cu1 39.98(3) . . ?
S1 Na1 Cu1 39.81(3) . . ?
S1 Na1 Cu1 145.09(6) 2_645 . ?
S2 Na1 Cu1 143.99(6) 2_645 . ?
S3 Na1 Cu1 39.52(3) . . ?
O1 Na2 O12 104.80(13) 4_566 . ?
O1 Na2 O3 86.01(13) 4_566 2_655 ?
O12 Na2 O3 94.01(13) . 2_655 ?
O1 Na2 O9 164.29(14) 4_566 1_565 ?
O12 Na2 O9 89.47(13) . 1_565 ?
O3 Na2 O9 86.48(12) 2_655 1_565 ?
O1 Na2 O10 86.53(13) 4_566 . ?
O12 Na2 O10 58.55(11) . . ?
O3 Na2 O10 148.41(14) 2_655 . ?
O9 Na2 O10 106.87(13) 1_565 . ?
O1 Na2 O13 81.01(12) 4_566 . ?
O12 Na2 O13 173.35(13) . . ?
O3 Na2 O13 83.07(12) 2_655 . ?
O9 Na2 O13 84.40(12) 1_565 . ?
O10 Na2 O13 125.85(13) . . ?
O1 Na2 S4 99.18(10) 4_566 . ?
O12 Na2 S4 29.15(8) . . ?
O3 Na2 S4 122.57(11) 2_655 . ?
O9 Na2 S4 96.49(10) 1_565 . ?
O10 Na2 S4 29.65(7) . . ?
O13 Na2 S4 154.36(11) . . ?
O1 Na2 Cu2 74.96(10) 4_566 . ?
O12 Na2 Cu2 130.15(11) . . ?
O3 Na2 Cu2 36.35(8) 2_655 . ?
O9 Na2 Cu2 90.90(9) 1_565 . ?
O10 Na2 Cu2 160.97(10) . . ?
O13 Na2 Cu2 47.65(8) . . ?
S4 Na2 Cu2 157.30(7) . . ?
O1 Na2 Na3 43.60(9) 4_566 . ?
O12 Na2 Na3 85.94(10) . . ?
O3 Na2 Na3 126.74(11) 2_655 . ?
O9 Na2 Na3 146.67(11) 1_565 . ?
O10 Na2 Na3 44.04(8) . . ?
O13 Na2 Na3 100.60(9) . . ?
S4 Na2 Na3 65.18(5) . . ?
Cu2 Na2 Na3 116.94(6) . . ?
O1 Na2 Na4 147.83(11) 4_566 1_565 ?
O12 Na2 Na4 43.13(9) . 1_565 ?
O3 Na2 Na4 92.92(9) 2_655 1_565 ?
O9 Na2 Na4 46.45(9) 1_565 1_565 ?
O10 Na2 Na4 77.68(9) . 1_565 ?
O13 Na2 Na4 130.84(10) . 1_565 ?
S4 Na2 Na4 54.92(5) . 1_565 ?
Cu2 Na2 Na4 120.64(6) . 1_565 ?
Na3 Na2 Na4 119.73(7) . 1_565 ?
O1 Na2 Na1 128.46(11) 4_566 1_565 ?
O12 Na2 Na1 86.42(10) . 1_565 ?
O3 Na2 Na1 42.63(8) 2_655 1_565 ?
O9 Na2 Na1 44.52(9) 1_565 1_565 ?
O10 Na2 Na1 137.48(10) . 1_565 ?
O13 Na2 Na1 87.40(9) . 1_565 ?
S4 Na2 Na1 111.20(6) . 1_565 ?
Cu2 Na2 Na1 60.86(4) . 1_565 ?
Na3 Na2 Na1 166.27(8) . 1_565 ?
Na4 Na2 Na1 59.86(5) 1_565 1_565 ?
O1 Na2 Na1 86.94(10) 4_566 2_655 ?
O12 Na2 Na1 30.61(9) . 2_655 ?
O3 Na2 Na1 67.86(9) 2_655 2_655 ?
O9 Na2 Na1 102.93(10) 1_565 2_655 ?
O10 Na2 Na1 81.11(9) . 2_655 ?
O13 Na2 Na1 149.24(10) . 2_655 ?
S4 Na2 Na1 55.54(4) . 2_655 ?
Cu2 Na2 Na1 101.90(6) . 2_655 ?
Na3 Na2 Na1 89.53(6) . 2_655 ?
Na4 Na2 Na1 63.20(5) 1_565 2_655 ?
Na1 Na2 Na1 78.14(4) 1_565 2_655 ?
O11 Na3 O1 100.13(13) 4_566 4_566 ?
O11 Na3 O10 171.78(14) 4_566 . ?
O1 Na3 O10 87.31(12) 4_566 . ?
O11 Na3 O6 85.06(13) 4_566 . ?
O1 Na3 O6 84.89(13) 4_566 . ?
O10 Na3 O6 99.20(12) . . ?
O11 Na3 O19 91.65(13) 4_566 . ?
O1 Na3 O19 86.67(14) 4_566 . ?
O10 Na3 O19 85.24(13) . . ?
O6 Na3 O19 170.25(15) . . ?
O11 Na3 O16 91.98(13) 4_566 . ?
O1 Na3 O16 166.49(13) 4_566 . ?
O10 Na3 O16 81.02(13) . . ?
O6 Na3 O16 90.27(13) . . ?
O19 Na3 O16 99.03(14) . . ?
O11 Na3 Na2 139.93(11) 4_566 . ?
O1 Na3 Na2 41.92(9) 4_566 . ?
O10 Na3 Na2 46.50(9) . . ?
O6 Na3 Na2 100.06(10) . . ?
O19 Na3 Na2 76.64(10) . . ?
O16 Na3 Na2 127.39(11) . . ?
O11 Na3 Na4 45.24(9) 4_566 4_556 ?
O1 Na3 Na4 98.88(10) 4_566 4_556 ?
O10 Na3 Na4 137.44(11) . 4_556 ?
O6 Na3 Na4 40.53(9) . 4_556 ?
O19 Na3 Na4 136.88(11) . 4_556 ?
O16 Na3 Na4 85.38(10) . 4_556 ?
Na2 Na3 Na4 133.08(7) . 4_556 ?
O11 Na3 Na5 68.25(9) 4_566 . ?
O1 Na3 Na5 160.60(10) 4_566 . ?
O10 Na3 Na5 103.63(10) . . ?
O6 Na3 Na5 108.62(10) . . ?
O19 Na3 Na5 78.47(10) . . ?
O16 Na3 Na5 32.16(9) . . ?
Na2 Na3 Na5 142.20(7) . . ?
Na4 Na3 Na5 83.99(6) 4_556 . ?
O6 Na4 O4 89.97(13) 4 2_645 ?
O6 Na4 O12 106.20(14) 4 1_545 ?
O4 Na4 O12 95.98(13) 2_645 1_545 ?
O6 Na4 O11 82.92(12) 4 1_545 ?
O4 Na4 O11 149.94(14) 2_645 1_545 ?
O12 Na4 O11 58.73(12) 1_545 1_545 ?
O6 Na4 O9 165.51(14) 4 . ?
O4 Na4 O9 87.33(12) 2_645 . ?
O12 Na4 O9 88.25(12) 1_545 . ?
O11 Na4 O9 106.22(12) 1_545 . ?
O6 Na4 O13 83.91(13) 4 4_565 ?
O4 Na4 O13 85.92(13) 2_645 4_565 ?
O12 Na4 O13 169.68(14) 1_545 4_565 ?
O11 Na4 O13 122.00(14) 1_545 4_565 ?
O9 Na4 O13 81.70(12) . 4_565 ?
O6 Na4 S4 97.94(11) 4 1_545 ?
O4 Na4 S4 124.54(11) 2_645 1_545 ?
O12 Na4 S4 29.22(9) 1_545 1_545 ?
O11 Na4 S4 29.78(8) 1_545 1_545 ?
O9 Na4 S4 95.31(9) . 1_545 ?
O13 Na4 S4 149.36(12) 4_565 1_545 ?
O6 Na4 Cu2 77.92(9) 4 4_565 ?
O4 Na4 Cu2 37.24(8) 2_645 4_565 ?
O12 Na4 Cu2 133.10(11) 1_545 4_565 ?
O11 Na4 Cu2 159.86(10) 1_545 4_565 ?
O9 Na4 Cu2 91.47(9) . 4_565 ?
O13 Na4 Cu2 50.06(9) 4_565 4_565 ?
S4 Na4 Cu2 160.29(8) 1_545 4_565 ?
O6 Na4 Na2 149.58(12) 4 1_545 ?
O4 Na4 Na2 94.74(10) 2_645 1_545 ?
O12 Na4 Na2 43.44(9) 1_545 1_545 ?
O11 Na4 Na2 78.03(9) 1_545 1_545 ?
O9 Na4 Na2 44.91(8) . 1_545 ?
O13 Na4 Na2 126.36(11) 4_565 1_545 ?
S4 Na4 Na2 55.15(5) 1_545 1_545 ?
Cu2 Na4 Na2 121.98(7) 4_565 1_545 ?
O6 Na4 Na1 132.88(11) 4 . ?
O4 Na4 Na1 43.16(9) 2_645 . ?
O12 Na4 Na1 87.06(10) 1_545 . ?
O11 Na4 Na1 138.37(10) 1_545 . ?
O9 Na4 Na1 44.82(8) . . ?
O13 Na4 Na1 87.44(10) 4_565 . ?
S4 Na4 Na1 111.90(6) 1_545 . ?
Cu2 Na4 Na1 61.59(5) 4_565 . ?
Na2 Na4 Na1 60.39(5) 1_545 . ?
O6 Na4 Na3 42.26(9) 4 4 ?
O4 Na4 Na3 129.01(11) 2_645 4 ?
O12 Na4 Na3 85.19(10) 1_545 4 ?
O11 Na4 Na3 41.35(8) 1_545 4 ?
O9 Na4 Na3 143.53(10) . 4 ?
O13 Na4 Na3 101.53(10) 4_565 4 ?
S4 Na4 Na3 63.51(5) 1_545 4 ?
Cu2 Na4 Na3 118.70(6) 4_565 4 ?
Na2 Na4 Na3 117.96(7) 1_545 4 ?
Na1 Na4 Na3 168.18(8) . 4 ?
O6 Na4 Na1 88.55(10) 4 2_645 ?
O4 Na4 Na1 68.96(9) 2_645 2_645 ?
O12 Na4 Na1 32.20(9) 1_545 2_645 ?
O11 Na4 Na1 81.65(9) 1_545 2_645 ?
O9 Na4 Na1 103.71(9) . 2_645 ?
O13 Na4 Na1 153.78(11) 4_565 2_645 ?
S4 Na4 Na1 56.60(5) 1_545 2_645 ?
Cu2 Na4 Na1 103.81(6) 4_565 2_645 ?
Na2 Na4 Na1 65.50(5) 1_545 2_645 ?
Na1 Na4 Na1 79.42(4) . 2_645 ?
Na3 Na4 Na1 89.29(6) 4 2_645 ?
O14 Na5 O15 172.57(15) . . ?
O14 Na5 O16 89.06(14) . . ?
O15 Na5 O16 83.64(14) . . ?
O14 Na5 O14 89.67(14) . 3_556 ?
O15 Na5 O14 97.30(14) . 3_556 ?
O16 Na5 O14 170.03(16) . 3_556 ?
O14 Na5 O17 92.74(14) . . ?
O15 Na5 O17 86.77(14) . . ?
O16 Na5 O17 96.38(14) . . ?
O14 Na5 O17 73.80(13) 3_556 . ?
O14 Na5 O18 88.50(14) . . ?
O15 Na5 O18 95.09(14) . . ?
O16 Na5 O18 108.63(14) . . ?
O14 Na5 O18 81.22(13) 3_556 . ?
O17 Na5 O18 154.98(15) . . ?
O14 Na5 Na5 45.30(10) . 3_556 ?
O15 Na5 Na5 141.60(13) . 3_556 ?
O16 Na5 Na5 133.52(14) . 3_556 ?
O14 Na5 Na5 44.37(10) 3_556 3_556 ?
O17 Na5 Na5 80.51(11) . 3_556 ?
O18 Na5 Na5 82.72(11) . 3_556 ?
O14 Na5 Na3 74.85(10) . . ?
O15 Na5 Na3 98.19(11) . . ?
O16 Na5 Na3 33.80(10) . . ?
O14 Na5 Na3 136.67(11) 3_556 . ?
O17 Na5 Na3 67.00(10) . . ?
O18 Na5 Na3 136.83(11) . . ?
Na5 Na5 Na3 109.53(8) 3_556 . ?
Na4 O13 Na2 153.98(17) 4_566 . ?
Na5 O14 Na5 90.33(14) . 3_556 ?
Na5 O16 Na3 114.04(15) . . ?

_diffrn_measured_fraction_theta_max 0.984
_diffrn_reflns_theta_full        26.99
_diffrn_measured_fraction_theta_full 0.984
_refine_diff_density_max         1.672
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.166

# Attachment '- cta343e2final.cif'

data_cta343e2final
_database_code_depnum_ccdc_archive 'CCDC 857016'
#TrackingRef '- cta343e2final.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H42 Cu5 N9 O20 S4'
_chemical_formula_weight         1414.77

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I41/a

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

_cell_length_a                   25.2401(10)
_cell_length_b                   25.2401(10)
_cell_length_c                   7.4556(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4749.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1781
_cell_measurement_theta_min      3.49
_cell_measurement_theta_max      73.37

_exptl_crystal_description       rod
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.043
_exptl_crystal_size_mid          0.041
_exptl_crystal_size_min          0.036
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2856
_exptl_absorpt_coefficient_mu    4.926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.806
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Oxford Diffraction Excalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 16.0711
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5564
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0416
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         3.50
_diffrn_reflns_theta_max         69.94
_reflns_number_total             2207
_reflns_number_gt                1673
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_cell_refinement       
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_data_reduction        
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May 8 2007,13:10:02)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
The asymmetric unit of the compound consists of one quarter of the
formula unit: {[CuII(H2O)(bipy)]4[CuI(SO3)4](NO3).H2O. As a result the
asymmetric unit contains only one quarter of a nitrate anion. The
nitrate atoms, which lie within the channels formed between the
interleaving bipy ligands, were assigned to general positions and as
such are only able to have maximum site occupancies of 0.25.
The atoms of the disordered nitrate were restrained to chemically
sensible positions and were each refined with isotropic displacement
parameters and a fixed site occupancy of 0.25. Similarly the oxygen of
a disordered water molecule within the channel was also included in the
model with a site occupancy of 0.25. The coordinates of the water
molecule were close to those of the nitrate nitrogen atom and this
necessitated the application of a common isotropic displacement
parameter to the nitrate nitrogen atom and the water oxygen atom.
Hydrogen atoms were not assigned to the disordered water molecule.
Analysis of the anisotropic displacement parameters of the C and N
atoms belonging to the bipy ligands were suggestive of disorder within
the coordinated ligand. Attempts to model the bipy over two closely
separated sites were successful with one position being more dominant
than the other. Both locations of the bipy ligand lie in the same plane.
Given that the nitrate ion occupancy was only 0.25 and the fact that the
bipy hydrogen atoms border the channels occupied by the nitrate and
water molecule, it was considered likely that the bipy disorder is
linked to the disorder apparent with the nitrate ion and for this reason
the major and minor locations of the bipy ligand were assigned site
occupancies of 0.75 and 0.25 respectively.
H atoms on the coordinated water molecule were refined with a restrained
O-H separation and an isotropic displacement parameter equal to 1.5
times the Ueq value of the O atom to which it is bound.
Water hydrogen atoms bound to the coordinated water molecule were refined
with restrained O-H distances and isotropic displacement parameters.
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^)+(0.0752P)^2^+16.4145P] 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         2207
_refine_ls_number_parameters     238
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0570
_refine_ls_wR_factor_ref         0.1571
_refine_ls_wR_factor_gt          0.1462
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.154
_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
Cu1 Cu 0.5000 0.7500 0.1250 0.0310(4) Uani 1 4 d S . .
Cu2 Cu 0.63668(3) 0.75256(4) -0.07268(10) 0.0433(3) Uani 1 1 d . . .
O1 O 0.59905(17) 0.80025(18) -0.2424(5) 0.0426(10) Uani 1 1 d D A .
H1O H 0.5684(12) 0.809(3) -0.211(10) 0.064 Uiso 1 1 d D . .
H2O H 0.597(3) 0.783(3) -0.339(6) 0.064 Uiso 1 1 d D . .
S1 S 0.53476(5) 0.68280(5) -0.03502(17) 0.0338(3) Uani 1 1 d . . .
O2 O 0.54540(18) 0.63707(15) 0.0869(5) 0.0431(10) Uani 1 1 d . A .
O3 O 0.50028(16) 0.66314(16) -0.1856(5) 0.0408(9) Uani 1 1 d . A .
O4 O 0.58787(15) 0.69521(16) -0.1236(5) 0.0379(9) Uani 1 1 d . A .
N1A N 0.7035(3) 0.7993(5) -0.0988(10) 0.0375(17) Uani 0.75 1 d P A 1
N2A N 0.6893(3) 0.7077(4) 0.0399(10) 0.040(2) Uani 0.75 1 d P A 1
C1A C 0.7076(4) 0.8477(5) -0.1732(11) 0.040(2) Uani 0.75 1 d P A 1
H1A H 0.6762 0.8647 -0.2134 0.048 Uiso 0.75 1 calc PR A 1
C2A C 0.7548(4) 0.8739(5) -0.1939(12) 0.047(2) Uani 0.75 1 d P A 1
H2A H 0.7560 0.9083 -0.2454 0.056 Uiso 0.75 1 calc PR A 1
C3A C 0.8003(5) 0.8490(5) -0.1383(14) 0.053(2) Uani 0.75 1 d P A 1
H3A H 0.8336 0.8657 -0.1550 0.064 Uiso 0.75 1 calc PR A 1
C4A C 0.7977(4) 0.7993(6) -0.0577(14) 0.044(2) Uani 0.75 1 d P A 1
H4A H 0.8288 0.7821 -0.0157 0.053 Uiso 0.75 1 calc PR A 1
C5A C 0.7481(3) 0.7757(5) -0.0406(11) 0.038(2) Uani 0.75 1 d P A 1
C6A C 0.7393(3) 0.7234(6) 0.0383(11) 0.0348(18) Uani 0.75 1 d P A 1
C7A C 0.7799(4) 0.6917(5) 0.1063(12) 0.050(2) Uani 0.75 1 d P A 1
H7A H 0.8155 0.7039 0.1054 0.060 Uiso 0.75 1 calc PR A 1
C8A C 0.7677(4) 0.6428(6) 0.1744(13) 0.046(2) Uani 0.75 1 d P A 1
H8A H 0.7951 0.6208 0.2197 0.055 Uiso 0.75 1 calc PR A 1
C9A C 0.7158(5) 0.6253(4) 0.1775(12) 0.049(2) Uani 0.75 1 d P A 1
H9A H 0.7069 0.5914 0.2243 0.059 Uiso 0.75 1 calc PR A 1
C10A C 0.6772(5) 0.6591(6) 0.1096(14) 0.043(2) Uani 0.75 1 d P A 1
H10A H 0.6412 0.6481 0.1118 0.051 Uiso 0.75 1 calc PR A 1
N1B N 0.7071(10) 0.7783(9) -0.081(3) 0.027(6) Uiso 0.25 1 d P A 2
N2B N 0.6835(9) 0.6884(11) 0.057(3) 0.012(5) Uiso 0.25 1 d P A 2
C1B C 0.7119(11) 0.8247(16) -0.147(4) 0.028(7) Uiso 0.25 1 d P A 2
H1B H 0.6816 0.8428 -0.1919 0.033 Uiso 0.25 1 calc PR A 2
C2B C 0.7663(14) 0.8511(11) -0.156(4) 0.035(6) Uiso 0.25 1 d P A 2
H2B H 0.7716 0.8853 -0.2059 0.042 Uiso 0.25 1 calc PR A 2
C3B C 0.8040(15) 0.8234(17) -0.090(5) 0.040(9) Uiso 0.25 1 d P A 2
H3B H 0.8384 0.8386 -0.0936 0.048 Uiso 0.25 1 calc PR A 2
C4B C 0.7998(10) 0.7748(11) -0.016(3) 0.033(6) Uiso 0.25 1 d P A 2
H4B H 0.8299 0.7566 0.0283 0.039 Uiso 0.25 1 calc PR A 2
C5B C 0.7474(11) 0.7516(15) -0.008(4) 0.025(6) Uiso 0.25 1 d P A 2
C6B C 0.7364(10) 0.7006(10) 0.063(3) 0.023(6) Uiso 0.25 1 d P A 2
C7B C 0.7724(11) 0.6684(13) 0.142(4) 0.021(6) Uiso 0.25 1 d P A 2
H7B H 0.8082 0.6793 0.1532 0.025 Uiso 0.25 1 calc PR A 2
C8B C 0.7562(12) 0.6195(11) 0.204(4) 0.034(6) Uiso 0.25 1 d P A 2
H8B H 0.7816 0.5957 0.2531 0.040 Uiso 0.25 1 calc PR A 2
C9B C 0.7025(11) 0.6047(11) 0.197(4) 0.035(7) Uiso 0.25 1 d P A 2
H9B H 0.6906 0.5714 0.2406 0.042 Uiso 0.25 1 calc PR A 2
C10B C 0.6671(12) 0.6415(12) 0.121(4) 0.029(7) Uiso 0.25 1 d P A 2
H10B H 0.6305 0.6330 0.1152 0.035 Uiso 0.25 1 calc PR A 2
N3 N 0.7580(15) 0.9941(13) -0.078(8) 0.176(12) Uiso 0.25 1 d PD B 3
O5 O 0.7515(14) 1.0050(15) 0.088(10) 0.096(9) Uiso 0.25 1 d PD B 3
O6 O 0.7168(11) 0.9944(11) -0.178(4) 0.083(7) Uiso 0.25 1 d PD B 3
O7 O 0.804(2) 0.9835(18) -0.142(6) 0.161(16) Uiso 0.25 1 d PD B 3
O8 O 0.749(3) 0.994(2) -0.293(18) 0.176(12) Uiso 0.25 1 d P C 4

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
Cu1 0.0337(5) 0.0337(5) 0.0256(7) 0.000 0.000 0.000
Cu2 0.0315(5) 0.0702(7) 0.0283(4) -0.0028(4) -0.0002(3) 0.0003(4)
O1 0.042(2) 0.056(3) 0.0297(19) 0.0022(18) 0.0019(17) -0.006(2)
S1 0.0405(7) 0.0349(7) 0.0260(6) -0.0023(5) 0.0007(5) 0.0013(5)
O2 0.065(3) 0.035(2) 0.0298(19) 0.0035(16) 0.0062(18) 0.0051(19)
O3 0.041(2) 0.047(2) 0.0352(19) -0.0103(18) 0.0000(17) -0.0016(18)
O4 0.037(2) 0.051(2) 0.0260(17) 0.0001(16) 0.0015(15) 0.0039(18)
N1A 0.043(4) 0.044(6) 0.025(4) 0.002(4) -0.003(3) 0.004(4)
N2A 0.048(5) 0.039(5) 0.034(4) -0.001(4) 0.005(3) -0.003(4)
C1A 0.046(5) 0.043(5) 0.031(4) 0.000(4) 0.001(3) -0.003(4)
C2A 0.045(5) 0.058(6) 0.038(4) -0.003(4) -0.002(4) -0.003(5)
C3A 0.046(6) 0.069(8) 0.044(5) -0.012(5) 0.009(4) -0.020(5)
C4A 0.042(5) 0.042(6) 0.048(5) -0.009(5) -0.001(4) 0.003(5)
C5A 0.037(5) 0.049(6) 0.027(4) -0.009(4) 0.005(3) 0.002(4)
C6A 0.030(4) 0.046(6) 0.028(4) -0.001(5) -0.003(3) 0.005(4)
C7A 0.052(6) 0.060(7) 0.037(5) -0.004(5) 0.001(4) 0.001(5)
C8A 0.052(6) 0.049(7) 0.037(5) 0.003(5) -0.008(4) 0.011(5)
C9A 0.063(7) 0.047(6) 0.038(4) -0.002(4) -0.007(4) 0.004(5)
C10A 0.044(6) 0.047(7) 0.038(5) -0.004(6) -0.004(4) -0.002(5)

_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
Cu1 S1 2.2517(13) 15_565 ?
Cu1 S1 2.2517(13) . ?
Cu1 S1 2.2517(13) 12_766 ?
Cu1 S1 2.2517(13) 6_564 ?
Cu2 N1B 1.89(3) . ?
Cu2 N2A 1.937(9) . ?
Cu2 O4 1.938(4) . ?
Cu2 O1 1.988(4) . ?
Cu2 N1A 2.067(11) . ?
Cu2 O2 2.149(4) 12_766 ?
Cu2 N2B 2.22(3) . ?
S1 O2 1.493(4) . ?
S1 O3 1.504(4) . ?
S1 O4 1.527(4) . ?
O2 Cu2 2.149(4) 15_565 ?
N1A C5A 1.346(13) . ?
N1A C1A 1.347(13) . ?
N2A C6A 1.323(13) . ?
N2A C10A 1.366(14) . ?
C1A C2A 1.370(12) . ?
C2A C3A 1.372(16) . ?
C3A C4A 1.391(16) . ?
C4A C5A 1.394(14) . ?
C5A C6A 1.461(14) . ?
C6A C7A 1.395(14) . ?
C7A C8A 1.369(15) . ?
C8A C9A 1.382(16) . ?
C9A C10A 1.392(14) . ?
N1B C1B 1.28(4) . ?
N1B C5B 1.33(4) . ?
N2B C10B 1.34(3) . ?
N2B C6B 1.37(4) . ?
C1B C2B 1.53(4) . ?
C2B C3B 1.28(5) . ?
C3B C4B 1.35(4) . ?
C4B C5B 1.45(4) . ?
C5B C6B 1.42(4) . ?
C6B C7B 1.35(4) . ?
C7B C8B 1.38(4) . ?
C8B C9B 1.41(4) . ?
C9B C10B 1.41(4) . ?
N3 O5 0.64(4) 4_464 ?
N3 O5 1.28(3) . ?
N3 O7 1.28(3) . ?
N3 O6 1.28(3) . ?
N3 O6 1.31(5) 3_655 ?
N3 N3 1.897(10) 4_464 ?
N3 N3 1.897(10) 3_655 ?
O5 N3 0.64(4) 3_655 ?
O5 O6 0.98(4) 3_655 ?
O5 O7 1.30(6) 3_655 ?
O6 O5 0.98(4) 4_464 ?
O6 N3 1.31(5) 4_464 ?
O7 O5 1.30(6) 4_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
S1 Cu1 S1 106.30(3) 15_565 . ?
S1 Cu1 S1 116.01(7) 15_565 12_766 ?
S1 Cu1 S1 106.30(3) . 12_766 ?
S1 Cu1 S1 106.30(3) 15_565 6_564 ?
S1 Cu1 S1 116.01(7) . 6_564 ?
S1 Cu1 S1 106.30(3) 12_766 6_564 ?
N1B Cu2 N2A 64.6(8) . . ?
N1B Cu2 O4 147.8(7) . . ?
N2A Cu2 O4 94.8(3) . . ?
N1B Cu2 O1 102.8(8) . . ?
N2A Cu2 O1 163.3(3) . . ?
O4 Cu2 O1 91.37(17) . . ?
N1B Cu2 N1A 15.3(6) . . ?
N2A Cu2 N1A 79.4(4) . . ?
O4 Cu2 N1A 157.9(2) . . ?
O1 Cu2 N1A 89.1(3) . . ?
N1B Cu2 O2 96.6(7) . 12_766 ?
N2A Cu2 O2 97.5(3) . 12_766 ?
O4 Cu2 O2 111.01(16) . 12_766 ?
O1 Cu2 O2 94.74(17) . 12_766 ?
N1A Cu2 O2 91.0(2) . 12_766 ?
N1B Cu2 N2B 76.4(10) . . ?
N2A Cu2 N2B 12.1(6) . . ?
O4 Cu2 N2B 83.0(6) . . ?
O1 Cu2 N2B 166.0(6) . . ?
N1A Cu2 N2B 91.3(7) . . ?
O2 Cu2 N2B 99.2(5) 12_766 . ?
O2 S1 O3 107.6(2) . . ?
O2 S1 O4 105.3(2) . . ?
O3 S1 O4 104.7(2) . . ?
O2 S1 Cu1 109.26(16) . . ?
O3 S1 Cu1 114.73(17) . . ?
O4 S1 Cu1 114.62(17) . . ?
S1 O2 Cu2 128.5(3) . 15_565 ?
S1 O4 Cu2 128.8(2) . . ?
C5A N1A C1A 118.1(10) . . ?
C5A N1A Cu2 113.5(9) . . ?
C1A N1A Cu2 128.3(6) . . ?
C6A N2A C10A 119.1(10) . . ?
C6A N2A Cu2 118.3(8) . . ?
C10A N2A Cu2 122.5(7) . . ?
N1A C1A C2A 123.4(11) . . ?
C1A C2A C3A 118.2(11) . . ?
C2A C3A C4A 120.3(10) . . ?
C3A C4A C5A 117.8(10) . . ?
N1A C5A C4A 122.2(11) . . ?
N1A C5A C6A 113.7(9) . . ?
C4A C5A C6A 124.1(10) . . ?
N2A C6A C7A 121.7(13) . . ?
N2A C6A C5A 114.8(8) . . ?
C7A C6A C5A 123.5(10) . . ?
C8A C7A C6A 119.2(11) . . ?
C7A C8A C9A 120.5(10) . . ?
C8A C9A C10A 117.5(12) . . ?
N2A C10A C9A 122.2(11) . . ?
C1B N1B C5B 123(3) . . ?
C1B N1B Cu2 115(2) . . ?
C5B N1B Cu2 122(2) . . ?
C10B N2B C6B 119(3) . . ?
C10B N2B Cu2 129(2) . . ?
C6B N2B Cu2 111.7(19) . . ?
N1B C1B C2B 120(3) . . ?
C3B C2B C1B 114(3) . . ?
C2B C3B C4B 127(4) . . ?
C3B C4B C5B 117(3) . . ?
N1B C5B C6B 117(3) . . ?
N1B C5B C4B 118(3) . . ?
C6B C5B C4B 124(3) . . ?
C7B C6B N2B 122(3) . . ?
C7B C6B C5B 125(3) . . ?
N2B C6B C5B 112(3) . . ?
C6B C7B C8B 119(3) . . ?
C7B C8B C9B 120(3) . . ?
C10B C9B C8B 117(3) . . ?
N2B C10B C9B 122(3) . . ?
O5 N3 O5 153(6) 4_464 . ?
O5 N3 O7 77(6) 4_464 . ?
O5 N3 O7 121(4) . . ?
O5 N3 O6 48(4) 4_464 . ?
O5 N3 O6 117(4) . . ?
O7 N3 O6 121(5) . . ?
O5 N3 O6 157(5) 4_464 3_655 ?
O5 N3 O6 44(2) . 3_655 ?
O7 N3 O6 104(3) . 3_655 ?
O6 N3 O6 117(3) . 3_655 ?
O5 N3 N3 12(4) 4_464 4_464 ?
O5 N3 N3 159(3) . 4_464 ?
O7 N3 N3 78(4) . 4_464 ?
O6 N3 N3 44(2) . 4_464 ?
O6 N3 N3 144(3) 3_655 4_464 ?
O5 N3 N3 158(6) 4_464 3_655 ?
O5 N3 N3 6(2) . 3_655 ?
O7 N3 N3 115(4) . 3_655 ?
O6 N3 N3 123(3) . 3_655 ?
O6 N3 N3 42.3(13) 3_655 3_655 ?
N3 N3 N3 165(2) 4_464 3_655 ?
N3 O5 O6 103(5) 3_655 3_655 ?
N3 O5 N3 162(6) 3_655 . ?
O6 O5 N3 70(5) 3_655 . ?
N3 O5 O7 74(6) 3_655 3_655 ?
O6 O5 O7 157(5) 3_655 3_655 ?
N3 O5 O7 106(4) . 3_655 ?
O5 O6 N3 29(3) 4_464 . ?
O5 O6 N3 66(3) 4_464 4_464 ?
N3 O6 N3 94(2) . 4_464 ?
N3 O7 O5 28.7(19) . 4_464 ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        69.94
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.103

# Attachment '- fe32871m2final.cif'

data_fe32871m
_database_code_depnum_ccdc_archive 'CCDC 857017'
#TrackingRef '- fe32871m2final.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'(Cu S4 O12 7-)2, (Fe3 O4 H6 7+), (Fe H12 O6 2+)2, (Na3 H12 O6 3+), (H2 O)'
_chemical_formula_sum            'H44 Cu2 Fe5 Na3 O47 S8'
_chemical_formula_weight         1528.14

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Hexagonal
_symmetry_space_group_name_H-M   P63/m

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

_cell_length_a                   9.0550(3)
_cell_length_b                   9.0550(3)
_cell_length_c                   29.545(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     2097.9(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    6435
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.5

_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_colour            brown
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1534
_exptl_absorpt_coefficient_mu    3.238
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.722523
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
SHELDRICK G. M. SADABS
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker 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_%        1.000
_diffrn_reflns_number            12889
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1643
_reflns_number_gt                1600
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Water hydrogen atoms identified in the Fourier difference maps were
refined with restrained O-H distances and common isotropic displacement
parameters for each pair of hydrogen atoms.
The hydrogen atoms bound to atom O11 (the oxygen atom of an uncoordinated
water molecule) could not be unambiguously identified.

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^)+(0.0152P)^2^+25.4812P] 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         1643
_refine_ls_number_parameters     128
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1336
_refine_ls_wR_factor_gt          0.1330
_refine_ls_goodness_of_fit_ref   1.388
_refine_ls_restrained_S_all      1.385
_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
Cu1 Cu 0.6667 0.3333 0.14043(4) 0.0130(3) Uani 1 3 d S . .
Fe1 Fe 0.6667 0.3333 -0.09023(5) 0.0077(3) Uani 1 3 d S . .
Fe3 Fe 0.47847(16) 0.38677(15) 0.2500 0.0125(3) Uani 1 2 d S . .
S4 S 0.6667 0.3333 0.06429(8) 0.0101(5) Uani 1 3 d S . .
S5 S 0.40353(18) 0.13142(18) 0.16974(5) 0.0115(3) Uani 1 1 d . . .
O1 O 0.2618(6) 0.0225(6) 0.13882(15) 0.0165(9) Uani 1 1 d . . .
O2 O 0.3340(5) 0.2123(6) 0.20237(15) 0.0155(9) Uani 1 1 d . . .
O3 O 0.8336(5) 0.4661(6) 0.04447(15) 0.0161(9) Uani 1 1 d . . .
O4 O 0.1794(6) 0.1990(6) 0.05299(16) 0.0164(9) Uani 1 1 d D . .
O6 O 0.4310(6) 0.0059(6) 0.19943(15) 0.0153(9) Uani 1 1 d . . .
O7 O 0.8605(6) 0.5135(6) -0.04702(15) 0.0153(9) Uani 1 1 d D . .
O9 O 0.6667 0.3333 0.2500 0.017(2) Uani 1 6 d S . .
O10 O 0.2684(9) 0.4376(10) 0.2500 0.0213(14) Uani 1 2 d SD . .
O11 O 0.0000 0.0000 0.2500 0.046(4) Uani 1 6 d S . .
O12 O 0.6831(6) 0.5297(6) -0.13072(17) 0.0175(9) Uani 1 1 d D . .
Na2 Na 0.0000 0.0000 0.10797(15) 0.0139(8) Uani 1 3 d S . .
Na6 Na 0.0000 0.0000 0.0000 0.0087(11) Uani 1 6 d S . .
H41 H 0.171(11) 0.288(7) 0.049(3) 0.033(17) Uiso 1 1 d D . .
H42 H 0.287(3) 0.247(11) 0.058(3) 0.033(17) Uiso 1 1 d D . .
H71 H 0.961(4) 0.530(8) -0.050(2) 0.003(11) Uiso 1 1 d D . .
H72 H 0.848(8) 0.496(8) -0.0182(8) 0.003(11) Uiso 1 1 d D . .
H101 H 0.230(12) 0.443(13) 0.2239(16) 0.04(3) Uiso 1 1 d D . .
H121 H 0.785(5) 0.603(10) -0.139(3) 0.05(2) Uiso 1 1 d D . .
H122 H 0.637(12) 0.535(13) -0.1555(19) 0.05(2) Uiso 1 1 d D . .

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
Cu1 0.0135(4) 0.0135(4) 0.0120(6) 0.000 0.000 0.0067(2)
Fe1 0.0067(4) 0.0067(4) 0.0095(7) 0.000 0.000 0.0034(2)
Fe3 0.0128(6) 0.0108(6) 0.0119(6) 0.000 0.000 0.0044(5)
S4 0.0098(7) 0.0098(7) 0.0109(11) 0.000 0.000 0.0049(3)
S5 0.0102(7) 0.0108(7) 0.0131(7) -0.0003(5) -0.0005(5) 0.0050(5)
O1 0.016(2) 0.016(2) 0.016(2) -0.0023(18) -0.0044(18) 0.0075(18)
O2 0.013(2) 0.017(2) 0.018(2) -0.0010(18) 0.0023(17) 0.0080(18)
O3 0.009(2) 0.012(2) 0.021(2) 0.0006(18) 0.0005(17) 0.0008(17)
O4 0.012(2) 0.012(2) 0.026(2) -0.0010(18) -0.0023(18) 0.0072(18)
O6 0.018(2) 0.016(2) 0.016(2) 0.0045(17) 0.0005(17) 0.0110(19)
O7 0.015(2) 0.017(2) 0.016(2) 0.0026(18) 0.0018(18) 0.0085(19)
O9 0.020(3) 0.020(3) 0.010(5) 0.000 0.000 0.0102(17)
O10 0.024(4) 0.032(4) 0.013(3) 0.000 0.000 0.018(3)
O11 0.035(5) 0.035(5) 0.068(12) 0.000 0.000 0.018(3)
O12 0.016(2) 0.012(2) 0.024(2) 0.0015(19) -0.0016(19) 0.0062(18)
Na2 0.0124(12) 0.0124(12) 0.017(2) 0.000 0.000 0.0062(6)
Na6 0.0092(16) 0.0092(16) 0.008(3) 0.000 0.000 0.0046(8)

_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
Cu1 S4 2.250(3) . ?
Cu1 S5 2.3267(15) 2_655 ?
Cu1 S5 2.3267(15) . ?
Cu1 S5 2.3267(15) 3_665 ?
Fe3 O9 1.9907(13) . ?
Fe3 O2 2.030(5) . ?
Fe3 O2 2.030(5) 10_556 ?
Fe3 O6 2.068(4) 3_665 ?
Fe3 O6 2.068(4) 12_666 ?
Fe3 O10 2.169(7) . ?
S4 O3 1.502(4) 3_665 ?
S4 O3 1.502(4) . ?
S4 O3 1.502(4) 2_655 ?
S5 O1 1.480(4) . ?
S5 O2 1.524(4) . ?
S5 O6 1.551(4) . ?
O6 Fe3 2.068(4) 2_655 ?
O1 Na2 2.451(5) . ?
Fe1 O12 2.086(5) 3_665 ?
Fe1 O12 2.086(5) 2_655 ?
Fe1 O12 2.086(5) . ?
Fe1 O7 2.123(5) . ?
Fe1 O7 2.123(5) 3_665 ?
Fe1 O7 2.123(5) 2_655 ?
Na6 O4 2.326(5) 7 ?
Na6 O4 2.326(5) 9 ?
Na6 O4 2.326(5) 8 ?
Na6 O4 2.326(5) . ?
Na6 O4 2.326(5) 2 ?
Na6 O4 2.326(5) 3 ?
Na6 Na2 3.190(4) 7 ?
Na6 Na2 3.190(4) . ?
O4 Na2 2.366(6) . ?
Na2 O4 2.366(6) 2 ?
Na2 O4 2.366(6) 3 ?
Na2 O1 2.451(5) 3 ?
Na2 O1 2.451(5) 2 ?
O9 Fe3 1.9907(13) 2_655 ?
O9 Fe3 1.9907(13) 3_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
S4 Cu1 S5 111.85(5) . 2_655 ?
S4 Cu1 S5 111.85(5) . . ?
S5 Cu1 S5 106.99(5) 2_655 . ?
S4 Cu1 S5 111.85(5) . 3_665 ?
S5 Cu1 S5 106.99(5) 2_655 3_665 ?
S5 Cu1 S5 106.99(5) . 3_665 ?
O9 Fe3 O2 96.17(13) . . ?
O9 Fe3 O2 96.17(13) . 10_556 ?
O2 Fe3 O2 87.8(3) . 10_556 ?
O9 Fe3 O6 97.06(13) . 3_665 ?
O2 Fe3 O6 88.32(17) . 3_665 ?
O2 Fe3 O6 166.53(19) 10_556 3_665 ?
O9 Fe3 O6 97.06(13) . 12_666 ?
O2 Fe3 O6 166.53(18) . 12_666 ?
O2 Fe3 O6 88.32(17) 10_556 12_666 ?
O6 Fe3 O6 92.5(2) 3_665 12_666 ?
O9 Fe3 O10 178.4(2) . . ?
O2 Fe3 O10 82.71(19) . . ?
O2 Fe3 O10 82.71(19) 10_556 . ?
O6 Fe3 O10 84.01(19) 3_665 . ?
O6 Fe3 O10 84.01(19) 12_666 . ?
O3 S4 O3 105.8(2) 3_665 . ?
O3 S4 O3 105.8(2) 3_665 2_655 ?
O3 S4 O3 105.8(2) . 2_655 ?
O3 S4 Cu1 112.94(19) 3_665 . ?
O3 S4 Cu1 112.94(19) . . ?
O3 S4 Cu1 112.94(19) 2_655 . ?
O1 S5 O2 106.4(3) . . ?
O1 S5 O6 105.3(3) . . ?
O2 S5 O6 104.5(2) . . ?
O1 S5 Cu1 120.0(2) . . ?
O2 S5 Cu1 111.38(18) . . ?
O6 S5 Cu1 108.04(18) . . ?
S5 O2 Fe3 123.5(3) . . ?
S5 O6 Fe3 121.6(3) . 2_655 ?
S5 O1 Na2 140.0(3) . . ?
O12 Fe1 O12 90.38(19) 3_665 2_655 ?
O12 Fe1 O12 90.38(19) 3_665 . ?
O12 Fe1 O12 90.38(19) 2_655 . ?
O12 Fe1 O7 91.40(18) 3_665 . ?
O12 Fe1 O7 177.95(19) 2_655 . ?
O12 Fe1 O7 90.60(17) . . ?
O12 Fe1 O7 90.60(17) 3_665 3_665 ?
O12 Fe1 O7 91.40(18) 2_655 3_665 ?
O12 Fe1 O7 177.95(19) . 3_665 ?
O7 Fe1 O7 87.58(18) . 3_665 ?
O12 Fe1 O7 177.95(19) 3_665 2_655 ?
O12 Fe1 O7 90.60(17) 2_655 2_655 ?
O12 Fe1 O7 91.40(18) . 2_655 ?
O7 Fe1 O7 87.58(18) . 2_655 ?
O7 Fe1 O7 87.58(18) 3_665 2_655 ?
O4 Na6 O4 79.65(18) 7 9 ?
O4 Na6 O4 79.65(18) 7 8 ?
O4 Na6 O4 79.65(18) 9 8 ?
O4 Na6 O4 180.0(3) 7 . ?
O4 Na6 O4 100.35(18) 9 . ?
O4 Na6 O4 100.35(18) 8 . ?
O4 Na6 O4 100.35(18) 7 2 ?
O4 Na6 O4 100.35(18) 9 2 ?
O4 Na6 O4 180.00(18) 8 2 ?
O4 Na6 O4 79.65(18) . 2 ?
O4 Na6 O4 100.35(18) 7 3 ?
O4 Na6 O4 180.00(18) 9 3 ?
O4 Na6 O4 100.35(18) 8 3 ?
O4 Na6 O4 79.65(18) . 3 ?
O4 Na6 O4 79.65(18) 2 3 ?
O4 Na6 Na2 47.69(12) 7 7 ?
O4 Na6 Na2 47.69(12) 9 7 ?
O4 Na6 Na2 47.69(12) 8 7 ?
O4 Na6 Na2 132.31(12) . 7 ?
O4 Na6 Na2 132.31(12) 2 7 ?
O4 Na6 Na2 132.31(12) 3 7 ?
O4 Na6 Na2 132.31(12) 7 . ?
O4 Na6 Na2 132.31(12) 9 . ?
O4 Na6 Na2 132.31(12) 8 . ?
O4 Na6 Na2 47.69(12) . . ?
O4 Na6 Na2 47.69(12) 2 . ?
O4 Na6 Na2 47.69(12) 3 . ?
Na2 Na6 Na2 180.0 7 . ?
Na6 O4 Na2 85.68(17) . . ?
O4 Na2 O4 78.0(2) 2 3 ?
O4 Na2 O4 78.0(2) 2 . ?
O4 Na2 O4 78.0(2) 3 . ?
O4 Na2 O1 158.5(2) 2 . ?
O4 Na2 O1 84.90(15) 3 . ?
O4 Na2 O1 85.68(16) . . ?
O4 Na2 O1 84.90(15) 2 3 ?
O4 Na2 O1 85.68(16) 3 3 ?
O4 Na2 O1 158.5(2) . 3 ?
O1 Na2 O1 107.01(15) . 3 ?
O4 Na2 O1 85.68(15) 2 2 ?
O4 Na2 O1 158.5(2) 3 2 ?
O4 Na2 O1 84.90(15) . 2 ?
O1 Na2 O1 107.01(15) . 2 ?
O1 Na2 O1 107.01(15) 3 2 ?
O4 Na2 Na6 46.63(13) 2 . ?
O4 Na2 Na6 46.64(13) 3 . ?
O4 Na2 Na6 46.63(13) . . ?
O1 Na2 Na6 111.83(14) . . ?
O1 Na2 Na6 111.83(14) 3 . ?
O1 Na2 Na6 111.83(14) 2 . ?
Fe3 O9 Fe3 120.0 2_655 3_665 ?
Fe3 O9 Fe3 120.000(1) 2_655 . ?
Fe3 O9 Fe3 120.0 3_665 . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.175

# Attachment '- mn32081abs2.cif'

data_mn32081abs
_database_code_depnum_ccdc_archive 'CCDC 857018'
#TrackingRef '- mn32081abs2.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '(Cu1 S4 O12 7-)2, (Mn1 2+), (Na12 H16 O8 12+)'
_chemical_formula_sum            'H16 Cu2 Mn Na12 O32 S8'
_chemical_formula_weight         1242.51

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Mn Mn 0.3368 0.7283 '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'
Cu Cu 0.3201 1.2651 '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           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/n '

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

_cell_length_a                   9.6671(19)
_cell_length_b                   12.920(3)
_cell_length_c                   13.049(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.041(4)
_cell_angle_gamma                90.00
_cell_volume                     1629.5(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    130(2)
_cell_measurement_reflns_used    1205
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      24.97

_exptl_crystal_description       multifaceted
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1230
_exptl_absorpt_coefficient_mu    2.464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729131
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
SHELDRICK G. M. SADABS
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      130(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker 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            8196
_diffrn_reflns_av_R_equivalents  0.0637
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         25.17
_reflns_number_total             2896
_reflns_number_gt                2239
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
;
Water hydrogen atoms identified in the Fourier difference maps were
refined with restrained O-H distances and isotropic displacement
parameters.
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^)+(0.0434P)^2^+1.4894P] 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         2896
_refine_ls_number_parameters     273
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0481
_refine_ls_wR_factor_ref         0.1114
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.046
_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
Mn1 Mn 0.0000 0.5000 1.0000 0.0079(3) Uani 1 2 d S . .
Cu1 Cu 0.53014(7) 0.75102(5) 0.62574(6) 0.0089(2) Uani 1 1 d . . .
S1 S -0.11134(14) 0.74641(10) 0.98586(12) 0.0087(3) Uani 1 1 d . . .
S2 S 0.55890(14) 0.61400(11) 0.72649(11) 0.0083(3) Uani 1 1 d . . .
S3 S 0.04758(14) 0.38772(10) 0.77893(11) 0.0077(3) Uani 1 1 d . . .
S4 S 0.22465(14) 0.68681(10) 1.05655(11) 0.0082(3) Uani 1 1 d . . .
Na1 Na -0.3348(2) 0.54202(17) 0.92370(18) 0.0133(5) Uani 1 1 d . . .
Na2 Na 0.5181(2) 0.77494(17) 0.94956(18) 0.0126(5) Uani 1 1 d . . .
Na3 Na -0.0659(2) 0.65184(18) 0.76103(19) 0.0158(5) Uani 1 1 d . . .
Na4 Na -0.2814(2) 0.40614(17) 0.69930(18) 0.0129(5) Uani 1 1 d . . .
Na5 Na 0.1512(2) 0.88192(17) 0.88221(18) 0.0124(5) Uani 1 1 d . . .
Na6 Na 0.2784(2) 0.55648(19) 0.83089(19) 0.0180(6) Uani 1 1 d . . .
O1 O -0.2510(4) 0.7949(3) 1.0014(3) 0.0133(9) Uani 1 1 d . . .
O2 O -0.0578(4) 0.7928(3) 0.8880(3) 0.0113(9) Uani 1 1 d . . .
O3 O 0.4930(4) 0.5172(3) 0.6832(3) 0.0146(9) Uani 1 1 d . . .
O4 O 0.4965(4) 0.6328(3) 0.8295(3) 0.0116(9) Uani 1 1 d . . .
O5 O 0.1993(4) 0.3826(3) 0.7531(3) 0.0135(9) Uani 1 1 d . . .
O6 O 0.2861(4) 0.7563(3) 0.9790(3) 0.0121(9) Uani 1 1 d . . .
O7 O 0.1952(4) 0.5848(3) 1.0011(3) 0.0115(9) Uani 1 1 d . . .
O14 O 0.4132(4) 0.3991(3) 0.9212(4) 0.0184(10) Uani 1 1 d D . .
O16 O -0.1348(4) 0.6327(3) 0.9631(3) 0.0101(9) Uani 1 1 d . . .
O17 O 0.0305(4) 0.4900(3) 0.8352(3) 0.0098(9) Uani 1 1 d . . .
O18 O -0.0326(4) 0.3981(3) 0.6802(3) 0.0118(9) Uani 1 1 d . . .
O19 O -0.0374(4) 0.5949(3) 0.5830(3) 0.0134(9) Uani 1 1 d D . .
O20 O 0.1803(4) 0.6862(3) 0.7223(3) 0.0149(9) Uani 1 1 d D . .
O21 O -0.2928(4) 0.5852(3) 0.7487(3) 0.0086(8) Uiso 1 1 d . . .
O22 O 0.3347(4) 0.6602(3) 1.1366(3) 0.0131(9) Uani 1 1 d . . .
O23 O -0.1906(4) 1.0071(3) 0.9817(4) 0.0158(10) Uani 1 1 d . . .
H141 H 0.352(6) 0.356(5) 0.893(6) 0.047(17) Uiso 1 1 d D . .
H142 H 0.491(5) 0.377(5) 0.894(6) 0.047(17) Uiso 1 1 d D . .
H191 H -0.011(8) 0.531(3) 0.601(7) 0.07(2) Uiso 1 1 d D . .
H192 H -0.125(4) 0.598(6) 0.561(6) 0.07(2) Uiso 1 1 d D . .
H201 H 0.236(5) 0.741(3) 0.716(5) 0.028(14) Uiso 1 1 d D . .
H202 H 0.173(7) 0.682(5) 0.6537(17) 0.028(14) Uiso 1 1 d D . .
H231 H -0.128(6) 0.997(4) 0.941(5) 0.007(11) Uiso 1 1 d . . .
H232 H -0.208(6) 0.946(5) 0.997(5) 0.007(11) Uiso 1 1 d . . .

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
Mn1 0.0039(6) 0.0096(6) 0.0101(7) -0.0005(5) -0.0004(5) 0.0006(5)
Cu1 0.0059(4) 0.0109(4) 0.0097(4) 0.0007(3) -0.0007(3) 0.0001(3)
S1 0.0047(7) 0.0097(7) 0.0115(8) -0.0009(6) -0.0014(6) 0.0007(5)
S2 0.0050(7) 0.0107(7) 0.0093(8) -0.0010(6) -0.0022(6) -0.0002(5)
S3 0.0057(7) 0.0094(7) 0.0082(8) -0.0007(6) -0.0009(6) 0.0001(5)
S4 0.0040(7) 0.0106(7) 0.0099(8) 0.0002(6) -0.0016(6) -0.0003(5)
Na1 0.0089(11) 0.0187(12) 0.0122(13) 0.0031(10) -0.0042(10) 0.0008(9)
Na2 0.0074(11) 0.0175(12) 0.0129(13) 0.0005(10) -0.0013(10) 0.0008(9)
Na3 0.0086(12) 0.0199(13) 0.0189(14) -0.0027(11) -0.0012(10) -0.0019(10)
Na4 0.0105(12) 0.0144(12) 0.0137(13) 0.0015(10) -0.0025(10) 0.0003(9)
Na5 0.0079(11) 0.0142(12) 0.0151(14) 0.0010(10) 0.0009(10) 0.0010(9)
Na6 0.0102(12) 0.0258(14) 0.0180(14) 0.0031(11) -0.0009(10) -0.0046(10)
O1 0.007(2) 0.013(2) 0.020(3) -0.0040(18) -0.0023(18) 0.0040(16)
O2 0.012(2) 0.011(2) 0.012(2) 0.0028(17) -0.0001(18) -0.0005(16)
O3 0.013(2) 0.015(2) 0.016(2) -0.0033(18) -0.0030(18) -0.0024(17)
O4 0.009(2) 0.015(2) 0.011(2) 0.0036(18) 0.0002(17) -0.0013(16)
O5 0.003(2) 0.018(2) 0.020(3) -0.0006(19) 0.0019(18) 0.0029(16)
O6 0.0058(19) 0.017(2) 0.014(2) 0.0027(18) -0.0005(17) 0.0032(16)
O7 0.009(2) 0.012(2) 0.014(2) -0.0035(18) 0.0017(17) 0.0014(16)
O14 0.011(2) 0.026(3) 0.018(3) -0.004(2) 0.003(2) -0.0027(18)
O16 0.007(2) 0.009(2) 0.015(2) -0.0026(17) -0.0044(17) -0.0013(16)
O17 0.012(2) 0.0074(19) 0.010(2) -0.0035(17) -0.0017(17) -0.0011(16)
O18 0.012(2) 0.011(2) 0.012(2) 0.0002(17) -0.0026(18) 0.0012(16)
O19 0.011(2) 0.014(2) 0.015(2) 0.0050(19) -0.0017(19) 0.0034(18)
O20 0.014(2) 0.018(2) 0.012(2) 0.004(2) -0.0005(19) -0.0076(18)
O22 0.0035(19) 0.022(2) 0.013(2) 0.0026(19) -0.0004(17) 0.0038(17)
O23 0.015(2) 0.014(2) 0.019(3) 0.003(2) 0.000(2) 0.0014(19)

_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
Mn1 O17 2.179(4) . ?
Mn1 O17 2.179(4) 3_567 ?
Mn1 O7 2.182(4) . ?
Mn1 O7 2.182(4) 3_567 ?
Mn1 O16 2.202(4) 3_567 ?
Mn1 O16 2.202(4) . ?
Mn1 Na1 3.412(2) 3_567 ?
Mn1 Na1 3.412(2) . ?
Mn1 Na6 3.586(2) 3_567 ?
Mn1 Na6 3.586(2) . ?
Mn1 Na3 3.729(3) . ?
Mn1 Na3 3.729(3) 3_567 ?
Cu1 S2 2.2195(16) . ?
Cu1 S4 2.2490(15) 4_675 ?
Cu1 S1 2.2611(17) 4_675 ?
Cu1 S3 2.2946(16) 2_556 ?
S3 O18 1.498(4) . ?
S3 O5 1.513(4) . ?
S3 O17 1.523(4) . ?
S3 Cu1 2.2946(16) 2_546 ?
S3 Na6 3.184(3) . ?
S3 Na4 3.336(3) . ?
S3 Na2 3.369(3) 2_546 ?
S4 O6 1.485(4) . ?
S4 O22 1.517(4) . ?
S4 O7 1.528(4) . ?
S4 Cu1 2.2490(15) 4_576 ?
S4 Na1 3.151(3) 3_567 ?
S4 Na2 3.382(3) . ?
S2 O4 1.503(4) . ?
S2 O21 1.504(4) 1_655 ?
S2 O3 1.508(4) . ?
S2 Na1 2.906(3) 1_655 ?
S2 Na4 3.121(3) 1_655 ?
S2 Na6 3.146(3) . ?
S1 O1 1.506(4) . ?
S1 O2 1.510(4) . ?
S1 O16 1.515(4) . ?
S1 Cu1 2.2611(17) 4_576 ?
S1 Na3 3.216(3) . ?
S1 Na4 3.329(3) 2_456 ?
S1 Na5 3.386(3) . ?
Na1 O14 2.303(5) 3_567 ?
Na1 O16 2.310(4) . ?
Na1 O7 2.327(4) 3_567 ?
Na1 O4 2.340(4) 1_455 ?
Na1 O21 2.393(5) . ?
Na1 O22 2.729(5) 3_567 ?
Na1 S2 2.906(3) 1_455 ?
Na1 S4 3.151(3) 3_567 ?
Na1 Na2 3.348(3) 1_455 ?
Na1 Na4 3.461(3) . ?
Na1 Na6 3.480(3) 3_567 ?
Na5 O5 2.301(4) 2_556 ?
Na5 O23 2.308(5) 3_577 ?
Na5 O2 2.328(4) . ?
Na5 O3 2.385(4) 2_556 ?
Na5 O6 2.422(4) . ?
Na5 Na6 3.654(3) 2_556 ?
Na5 Na4 3.724(3) 2_456 ?
Na5 Na2 3.893(3) . ?
Na5 Na3 3.953(3) . ?
Na4 O22 2.372(5) 3_567 ?
Na4 O21 2.404(4) . ?
Na4 O2 2.407(4) 2_446 ?
Na4 O18 2.425(4) . ?
Na4 O3 2.616(4) 1_455 ?
Na4 O23 2.708(5) 2_446 ?
Na4 O1 3.009(5) 2_446 ?
Na4 S2 3.121(3) 1_455 ?
Na4 S1 3.329(3) 2_446 ?
Na4 Na3 3.643(3) 2_446 ?
Na3 O21 2.359(4) . ?
Na3 O19 2.458(5) . ?
Na3 O2 2.462(5) . ?
Na3 O17 2.479(4) . ?
Na3 O20 2.482(5) . ?
Na3 O16 2.742(5) . ?
Na3 Na4 3.643(3) 2_456 ?
Na3 Na6 3.649(3) . ?
Na2 O6 2.296(4) . ?
Na2 O18 2.329(5) 2_556 ?
Na2 O1 2.335(4) 1_655 ?
Na2 O4 2.420(5) . ?
Na2 O19 2.486(5) 4_676 ?
Na2 O14 2.881(5) 3_667 ?
Na2 Na1 3.348(3) 1_655 ?
Na2 S3 3.369(3) 2_556 ?
Na2 Na4 3.647(3) 2_556 ?
Na2 Na6 3.950(3) . ?
O3 Na5 2.385(4) 2_546 ?
O3 Na4 2.616(4) 1_655 ?
O3 Na6 2.902(5) . ?
O14 Na1 2.303(5) 3_567 ?
O14 Na6 2.677(5) . ?
O14 Na2 2.881(5) 3_667 ?
O4 Na6 2.328(4) . ?
O4 Na1 2.340(4) 1_655 ?
O7 Na1 2.327(4) 3_567 ?
O7 Na6 2.404(5) . ?
O5 Na5 2.301(4) 2_546 ?
O5 Na6 2.576(5) . ?
O1 Na2 2.335(4) 1_455 ?
O1 Na4 3.009(5) 2_456 ?
O2 Na4 2.407(4) 2_456 ?
Na6 O20 2.380(5) . ?
Na6 O17 2.547(4) . ?
Na6 Na1 3.480(3) 3_567 ?
O18 Na2 2.329(5) 2_546 ?
O19 Na2 2.486(5) 4_575 ?
O21 S2 1.504(4) 1_455 ?
O22 Na4 2.372(5) 3_567 ?
O22 Na1 2.729(5) 3_567 ?
O23 Na5 2.308(5) 3_577 ?
O23 Na4 2.708(5) 2_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
O17 Mn1 O17 180.000(1) . 3_567 ?
O17 Mn1 O7 84.49(14) . . ?
O17 Mn1 O7 95.51(14) 3_567 . ?
O17 Mn1 O7 95.51(14) . 3_567 ?
O17 Mn1 O7 84.49(14) 3_567 3_567 ?
O7 Mn1 O7 180.00(17) . 3_567 ?
O17 Mn1 O16 94.57(14) . 3_567 ?
O17 Mn1 O16 85.43(14) 3_567 3_567 ?
O7 Mn1 O16 83.15(13) . 3_567 ?
O7 Mn1 O16 96.85(13) 3_567 3_567 ?
O17 Mn1 O16 85.43(14) . . ?
O17 Mn1 O16 94.57(14) 3_567 . ?
O7 Mn1 O16 96.85(13) . . ?
O7 Mn1 O16 83.15(13) 3_567 . ?
O16 Mn1 O16 180.0(2) 3_567 . ?
O17 Mn1 Na1 97.70(10) . 3_567 ?
O17 Mn1 Na1 82.30(10) 3_567 3_567 ?
O7 Mn1 Na1 42.45(11) . 3_567 ?
O7 Mn1 Na1 137.55(11) 3_567 3_567 ?
O16 Mn1 Na1 42.07(10) 3_567 3_567 ?
O16 Mn1 Na1 137.93(10) . 3_567 ?
O17 Mn1 Na1 82.30(10) . . ?
O17 Mn1 Na1 97.70(10) 3_567 . ?
O7 Mn1 Na1 137.55(11) . . ?
O7 Mn1 Na1 42.45(11) 3_567 . ?
O16 Mn1 Na1 137.93(10) 3_567 . ?
O16 Mn1 Na1 42.07(10) . . ?
Na1 Mn1 Na1 180.0 3_567 . ?
O17 Mn1 Na6 135.36(10) . 3_567 ?
O17 Mn1 Na6 44.64(10) 3_567 3_567 ?
O7 Mn1 Na6 139.17(11) . 3_567 ?
O7 Mn1 Na6 40.83(11) 3_567 3_567 ?
O16 Mn1 Na6 98.91(11) 3_567 3_567 ?
O16 Mn1 Na6 81.09(11) . 3_567 ?
Na1 Mn1 Na6 120.43(6) 3_567 3_567 ?
Na1 Mn1 Na6 59.57(6) . 3_567 ?
O17 Mn1 Na6 44.64(10) . . ?
O17 Mn1 Na6 135.36(10) 3_567 . ?
O7 Mn1 Na6 40.83(11) . . ?
O7 Mn1 Na6 139.17(11) 3_567 . ?
O16 Mn1 Na6 81.09(11) 3_567 . ?
O16 Mn1 Na6 98.91(11) . . ?
Na1 Mn1 Na6 59.57(6) 3_567 . ?
Na1 Mn1 Na6 120.43(6) . . ?
Na6 Mn1 Na6 180.0 3_567 . ?
O17 Mn1 Na3 39.67(10) . . ?
O17 Mn1 Na3 140.33(10) 3_567 . ?
O7 Mn1 Na3 82.89(11) . . ?
O7 Mn1 Na3 97.11(11) 3_567 . ?
O16 Mn1 Na3 133.16(11) 3_567 . ?
O16 Mn1 Na3 46.84(11) . . ?
Na1 Mn1 Na3 118.33(5) 3_567 . ?
Na1 Mn1 Na3 61.67(5) . . ?
Na6 Mn1 Na3 120.19(5) 3_567 . ?
Na6 Mn1 Na3 59.81(5) . . ?
O17 Mn1 Na3 140.33(10) . 3_567 ?
O17 Mn1 Na3 39.67(10) 3_567 3_567 ?
O7 Mn1 Na3 97.11(11) . 3_567 ?
O7 Mn1 Na3 82.89(11) 3_567 3_567 ?
O16 Mn1 Na3 46.84(11) 3_567 3_567 ?
O16 Mn1 Na3 133.16(11) . 3_567 ?
Na1 Mn1 Na3 61.67(5) 3_567 3_567 ?
Na1 Mn1 Na3 118.33(5) . 3_567 ?
Na6 Mn1 Na3 59.81(5) 3_567 3_567 ?
Na6 Mn1 Na3 120.19(5) . 3_567 ?
Na3 Mn1 Na3 180.0 . 3_567 ?
S2 Cu1 S4 115.21(6) . 4_675 ?
S2 Cu1 S1 123.87(6) . 4_675 ?
S4 Cu1 S1 99.70(6) 4_675 4_675 ?
S2 Cu1 S3 109.36(6) . 2_556 ?
S4 Cu1 S3 103.13(6) 4_675 2_556 ?
S1 Cu1 S3 103.13(6) 4_675 2_556 ?
O18 S3 O5 107.5(2) . . ?
O18 S3 O17 106.2(2) . . ?
O5 S3 O17 105.1(2) . . ?
O18 S3 Cu1 111.48(16) . 2_546 ?
O5 S3 Cu1 114.56(17) . 2_546 ?
O17 S3 Cu1 111.54(16) . 2_546 ?
O18 S3 Na6 118.13(17) . . ?
O5 S3 Na6 53.06(16) . . ?
O17 S3 Na6 52.02(15) . . ?
Cu1 S3 Na6 130.30(8) 2_546 . ?
O18 S3 Na4 41.43(16) . . ?
O5 S3 Na4 148.91(19) . . ?
O17 S3 Na4 88.69(16) . . ?
Cu1 S3 Na4 84.50(6) 2_546 . ?
Na6 S3 Na4 132.67(7) . . ?
O18 S3 Na2 35.99(15) . 2_546 ?
O5 S3 Na2 87.22(17) . 2_546 ?
O17 S3 Na2 141.45(17) . 2_546 ?
Cu1 S3 Na2 95.08(6) 2_546 2_546 ?
Na6 S3 Na2 127.22(7) . 2_546 ?
Na4 S3 Na2 65.91(6) . 2_546 ?
O6 S4 O22 108.8(2) . . ?
O6 S4 O7 105.8(2) . . ?
O22 S4 O7 104.6(2) . . ?
O6 S4 Cu1 113.90(16) . 4_576 ?
O22 S4 Cu1 112.67(17) . 4_576 ?
O7 S4 Cu1 110.39(15) . 4_576 ?
O6 S4 Na1 118.98(16) . 3_567 ?
O22 S4 Na1 59.97(16) . 3_567 ?
O7 S4 Na1 44.67(16) . 3_567 ?
Cu1 S4 Na1 125.87(7) 4_576 3_567 ?
O6 S4 Na2 33.52(15) . . ?
O22 S4 Na2 77.14(16) . . ?
O7 S4 Na2 104.21(16) . . ?
Cu1 S4 Na2 139.40(7) 4_576 . ?
Na1 S4 Na2 93.72(6) 3_567 . ?
O4 S2 O21 105.3(2) . 1_655 ?
O4 S2 O3 107.2(2) . . ?
O21 S2 O3 105.1(2) 1_655 . ?
O4 S2 Cu1 110.65(16) . . ?
O21 S2 Cu1 114.85(15) 1_655 . ?
O3 S2 Cu1 113.09(18) . . ?
O4 S2 Na1 53.22(16) . 1_655 ?
O21 S2 Na1 55.24(16) 1_655 1_655 ?
O3 S2 Na1 101.90(18) . 1_655 ?
Cu1 S2 Na1 144.90(8) . 1_655 ?
O4 S2 Na4 116.64(16) . 1_655 ?
O21 S2 Na4 48.49(15) 1_655 1_655 ?
O3 S2 Na4 56.67(16) . 1_655 ?
Cu1 S2 Na4 132.52(7) . 1_655 ?
Na1 S2 Na4 69.98(7) 1_655 1_655 ?
O4 S2 Na6 44.58(16) . . ?
O21 S2 Na6 133.18(16) 1_655 . ?
O3 S2 Na6 66.71(16) . . ?
Cu1 S2 Na6 110.19(7) . . ?
Na1 S2 Na6 80.49(7) 1_655 . ?
Na4 S2 Na6 106.14(7) 1_655 . ?
O1 S1 O2 105.7(2) . . ?
O1 S1 O16 107.4(2) . . ?
O2 S1 O16 105.7(2) . . ?
O1 S1 Cu1 114.56(18) . 4_576 ?
O2 S1 Cu1 117.72(16) . 4_576 ?
O16 S1 Cu1 105.01(16) . 4_576 ?
O1 S1 Na3 114.77(18) . . ?
O2 S1 Na3 47.53(16) . . ?
O16 S1 Na3 58.34(16) . . ?
Cu1 S1 Na3 130.66(7) 4_576 . ?
O1 S1 Na4 64.64(17) . 2_456 ?
O2 S1 Na4 41.18(15) . 2_456 ?
O16 S1 Na4 114.53(17) . 2_456 ?
Cu1 S1 Na4 138.82(7) 4_576 2_456 ?
Na3 S1 Na4 67.62(6) . 2_456 ?
O1 S1 Na5 121.28(17) . . ?
O2 S1 Na5 35.54(16) . . ?
O16 S1 Na5 122.27(16) . . ?
Cu1 S1 Na5 82.42(6) 4_576 . ?
Na3 S1 Na5 73.52(6) . . ?
Na4 S1 Na5 67.37(6) 2_456 . ?
O14 Na1 O16 85.68(16) 3_567 . ?
O14 Na1 O7 93.43(17) 3_567 3_567 ?
O16 Na1 O7 77.70(15) . 3_567 ?
O14 Na1 O4 93.35(17) 3_567 1_455 ?
O16 Na1 O4 115.79(16) . 1_455 ?
O7 Na1 O4 165.33(17) 3_567 1_455 ?
O14 Na1 O21 145.69(17) 3_567 . ?
O16 Na1 O21 86.47(15) . . ?
O7 Na1 O21 117.33(16) 3_567 . ?
O4 Na1 O21 60.69(14) 1_455 . ?
O14 Na1 O22 124.84(16) 3_567 3_567 ?
O16 Na1 O22 123.03(15) . 3_567 ?
O7 Na1 O22 56.25(14) 3_567 3_567 ?
O4 Na1 O22 109.42(15) 1_455 3_567 ?
O21 Na1 O22 86.96(14) . 3_567 ?
O14 Na1 S2 123.74(14) 3_567 1_455 ?
O16 Na1 S2 108.41(13) . 1_455 ?
O7 Na1 S2 142.31(14) 3_567 1_455 ?
O4 Na1 S2 30.96(10) 1_455 1_455 ?
O21 Na1 S2 31.10(10) . 1_455 ?
O22 Na1 S2 93.04(11) 3_567 1_455 ?
O14 Na1 S4 110.74(14) 3_567 3_567 ?
O16 Na1 S4 100.23(12) . 3_567 ?
O7 Na1 S4 27.49(10) 3_567 3_567 ?
O4 Na1 S4 138.12(13) 1_455 3_567 ?
O21 Na1 S4 103.52(12) . 3_567 ?
O22 Na1 S4 28.76(9) 3_567 3_567 ?
S2 Na1 S4 119.09(9) 1_455 3_567 ?
O14 Na1 Na2 57.82(13) 3_567 1_455 ?
O16 Na1 Na2 82.92(12) . 1_455 ?
O7 Na1 Na2 146.52(14) 3_567 1_455 ?
O4 Na1 Na2 46.30(11) 1_455 1_455 ?
O21 Na1 Na2 88.08(11) . 1_455 ?
O22 Na1 Na2 153.14(12) 3_567 1_455 ?
S2 Na1 Na2 69.98(7) 1_455 1_455 ?
S4 Na1 Na2 168.09(9) 3_567 1_455 ?
O14 Na1 Mn1 97.01(13) 3_567 . ?
O16 Na1 Mn1 39.69(10) . . ?
O7 Na1 Mn1 39.25(10) 3_567 . ?
O4 Na1 Mn1 151.82(12) 1_455 . ?
O21 Na1 Mn1 98.00(11) . . ?
O22 Na1 Mn1 85.78(10) 3_567 . ?
S2 Na1 Mn1 128.87(8) 1_455 . ?
S4 Na1 Mn1 60.64(4) 3_567 . ?
Na2 Na1 Mn1 121.06(8) 1_455 . ?
O14 Na1 Na4 165.34(14) 3_567 . ?
O16 Na1 Na4 107.98(13) . . ?
O7 Na1 Na4 84.57(12) 3_567 . ?
O4 Na1 Na4 85.58(12) 1_455 . ?
O21 Na1 Na4 43.96(10) . . ?
O22 Na1 Na4 43.07(10) 3_567 . ?
S2 Na1 Na4 57.92(6) 1_455 . ?
S4 Na1 Na4 62.48(6) 3_567 . ?
Na2 Na1 Na4 127.69(9) 1_455 . ?
Mn1 Na1 Na4 90.63(6) . . ?
O14 Na1 Na6 50.27(13) 3_567 3_567 ?
O16 Na1 Na6 82.20(12) . 3_567 ?
O7 Na1 Na6 43.52(11) 3_567 3_567 ?
O4 Na1 Na6 139.72(13) 1_455 3_567 ?
O21 Na1 Na6 159.58(13) . 3_567 ?
O22 Na1 Na6 85.08(11) 3_567 3_567 ?
S2 Na1 Na6 168.19(9) 1_455 3_567 ?
S4 Na1 Na6 62.26(6) 3_567 3_567 ?
Na2 Na1 Na6 107.20(9) 1_455 3_567 ?
Mn1 Na1 Na6 62.70(5) . 3_567 ?
Na4 Na1 Na6 124.74(9) . 3_567 ?
O5 Na5 O23 119.38(18) 2_556 3_577 ?
O5 Na5 O2 125.75(17) 2_556 . ?
O23 Na5 O2 114.42(17) 3_577 . ?
O5 Na5 O3 95.38(16) 2_556 2_556 ?
O23 Na5 O3 84.70(16) 3_577 2_556 ?
O2 Na5 O3 82.65(15) . 2_556 ?
O5 Na5 O6 93.60(15) 2_556 . ?
O23 Na5 O6 86.29(16) 3_577 . ?
O2 Na5 O6 96.36(15) . . ?
O3 Na5 O6 169.57(18) 2_556 . ?
O5 Na5 S1 142.57(13) 2_556 . ?
O23 Na5 S1 97.37(14) 3_577 . ?
O2 Na5 S1 22.15(10) . . ?
O3 Na5 S1 94.84(12) 2_556 . ?
O6 Na5 S1 81.12(11) . . ?
O5 Na5 Na6 44.42(11) 2_556 2_556 ?
O23 Na5 Na6 99.89(14) 3_577 2_556 ?
O2 Na5 Na6 120.26(13) . 2_556 ?
O3 Na5 Na6 52.46(11) 2_556 2_556 ?
O6 Na5 Na6 134.77(12) . 2_556 ?
S1 Na5 Na6 140.77(8) . 2_556 ?
O5 Na5 Na4 113.17(13) 2_556 2_456 ?
O23 Na5 Na4 108.16(13) 3_577 2_456 ?
O2 Na5 Na4 38.90(11) . 2_456 ?
O3 Na5 Na4 44.28(10) 2_556 2_456 ?
O6 Na5 Na4 135.22(12) . 2_456 ?
S1 Na5 Na4 55.59(5) . 2_456 ?
Na6 Na5 Na4 85.52(7) 2_556 2_456 ?
O5 Na5 Na2 65.93(12) 2_556 . ?
O23 Na5 Na2 84.83(13) 3_577 . ?
O2 Na5 Na2 127.22(12) . . ?
O3 Na5 Na2 149.96(13) 2_556 . ?
O6 Na5 Na2 33.36(10) . . ?
S1 Na5 Na2 114.39(7) . . ?
Na6 Na5 Na2 102.09(7) 2_556 . ?
Na4 Na5 Na2 163.81(8) 2_456 . ?
O5 Na5 Na3 91.85(12) 2_556 . ?
O23 Na5 Na3 148.63(14) 3_577 . ?
O2 Na5 Na3 35.52(11) . . ?
O3 Na5 Na3 96.04(12) 2_556 . ?
O6 Na5 Na3 88.95(12) . . ?
S1 Na5 Na3 51.27(5) . . ?
Na6 Na5 Na3 105.35(8) 2_556 . ?
Na4 Na5 Na3 56.56(6) 2_456 . ?
Na2 Na5 Na3 107.37(7) . . ?
O22 Na4 O21 95.40(15) 3_567 . ?
O22 Na4 O2 93.35(15) 3_567 2_446 ?
O21 Na4 O2 132.84(16) . 2_446 ?
O22 Na4 O18 108.03(16) 3_567 . ?
O21 Na4 O18 96.83(14) . . ?
O2 Na4 O18 123.94(16) 2_446 . ?
O22 Na4 O3 94.38(15) 3_567 1_455 ?
O21 Na4 O3 56.74(13) . 1_455 ?
O2 Na4 O3 76.46(14) 2_446 1_455 ?
O18 Na4 O3 147.38(15) . 1_455 ?
O22 Na4 O23 160.38(16) 3_567 2_446 ?
O21 Na4 O23 76.46(15) . 2_446 ?
O2 Na4 O23 80.03(15) 2_446 2_446 ?
O18 Na4 O23 90.82(15) . 2_446 ?
O3 Na4 O23 66.17(14) 1_455 2_446 ?
O22 Na4 O1 129.87(15) 3_567 2_446 ?
O21 Na4 O1 134.32(15) . 2_446 ?
O2 Na4 O1 51.24(12) 2_446 2_446 ?
O18 Na4 O1 76.75(13) . 2_446 ?
O3 Na4 O1 106.98(14) 1_455 2_446 ?
O23 Na4 O1 58.73(13) 2_446 2_446 ?
O22 Na4 S2 95.31(12) 3_567 1_455 ?
O21 Na4 S2 27.94(9) . 1_455 ?
O2 Na4 S2 105.13(12) 2_446 1_455 ?
O18 Na4 S2 122.82(12) . 1_455 ?
O3 Na4 S2 28.80(9) 1_455 1_455 ?
O23 Na4 S2 69.07(11) 2_446 1_455 ?
O1 Na4 S2 124.71(11) 2_446 1_455 ?
O22 Na4 S1 111.18(13) 3_567 2_446 ?
O21 Na4 S1 140.88(13) . 2_446 ?
O2 Na4 S1 24.40(9) 2_446 2_446 ?
O18 Na4 S1 101.26(12) . 2_446 ?
O3 Na4 S1 91.94(11) 1_455 2_446 ?
O23 Na4 S1 68.94(11) 2_446 2_446 ?
O1 Na4 S1 26.89(7) 2_446 2_446 ?
S2 Na4 S1 117.89(8) 1_455 2_446 ?
O22 Na4 S3 85.09(11) 3_567 . ?
O21 Na4 S3 91.90(11) . . ?
O2 Na4 S3 135.04(12) 2_446 . ?
O18 Na4 S3 24.12(10) . . ?
O3 Na4 S3 148.50(12) 1_455 . ?
O23 Na4 S3 112.68(12) 2_446 . ?
O1 Na4 S3 97.08(9) 2_446 . ?
S2 Na4 S3 119.78(8) 1_455 . ?
S1 Na4 S3 117.67(7) 2_446 . ?
O22 Na4 Na1 51.79(11) 3_567 . ?
O21 Na4 Na1 43.69(10) . . ?
O2 Na4 Na1 127.18(12) 2_446 . ?
O18 Na4 Na1 105.79(12) . . ?
O3 Na4 Na1 69.67(11) 1_455 . ?
O23 Na4 Na1 118.66(13) 2_446 . ?
O1 Na4 Na1 176.63(11) 2_446 . ?
S2 Na4 Na1 52.10(6) 1_455 . ?
S1 Na4 Na1 151.57(8) 2_446 . ?
S3 Na4 Na1 85.90(7) . . ?
O22 Na4 Na3 56.66(11) 3_567 2_446 ?
O21 Na4 Na3 144.01(12) . 2_446 ?
O2 Na4 Na3 42.16(11) 2_446 2_446 ?
O18 Na4 Na3 112.41(12) . 2_446 ?
O3 Na4 Na3 99.61(11) 1_455 2_446 ?
O23 Na4 Na3 121.62(12) 2_446 2_446 ?
O1 Na4 Na3 75.04(9) 2_446 2_446 ?
S2 Na4 Na3 123.88(8) 1_455 2_446 ?
S1 Na4 Na3 54.71(6) 2_446 2_446 ?
S3 Na4 Na3 106.12(7) . 2_446 ?
Na1 Na4 Na3 105.68(8) . 2_446 ?
O21 Na3 O19 86.91(15) . . ?
O21 Na3 O2 109.53(15) . . ?
O19 Na3 O2 148.75(17) . . ?
O21 Na3 O17 93.51(14) . . ?
O19 Na3 O17 93.95(15) . . ?
O2 Na3 O17 110.71(16) . . ?
O21 Na3 O20 160.94(18) . . ?
O19 Na3 O20 74.74(15) . . ?
O2 Na3 O20 89.18(15) . . ?
O17 Na3 O20 82.83(14) . . ?
O21 Na3 O16 77.94(14) . . ?
O19 Na3 O16 156.26(16) . . ?
O2 Na3 O16 54.90(13) . . ?
O17 Na3 O16 69.18(13) . . ?
O20 Na3 O16 117.53(16) . . ?
O21 Na3 S1 93.38(12) . . ?
O19 Na3 S1 174.82(13) . . ?
O2 Na3 S1 26.90(9) . . ?
O17 Na3 S1 91.19(12) . . ?
O20 Na3 S1 105.36(13) . . ?
O16 Na3 S1 28.05(8) . . ?
O21 Na3 Na4 87.74(11) . 2_456 ?
O19 Na3 Na4 117.20(13) . 2_456 ?
O2 Na3 Na4 41.01(10) . 2_456 ?
O17 Na3 Na4 148.84(13) . 2_456 ?
O20 Na3 Na4 105.07(12) . 2_456 ?
O16 Na3 Na4 80.71(10) . 2_456 ?
S1 Na3 Na4 57.67(6) . 2_456 ?
O21 Na3 Na6 137.42(13) . . ?
O19 Na3 Na6 91.02(12) . . ?
O2 Na3 Na6 93.65(12) . . ?
O17 Na3 Na6 44.18(10) . . ?
O20 Na3 Na6 40.32(11) . . ?
O16 Na3 Na6 88.04(11) . . ?
S1 Na3 Na6 92.25(7) . . ?
Na4 Na3 Na6 129.72(8) 2_456 . ?
O21 Na3 Na1 39.76(11) . . ?
O19 Na3 Na1 121.58(13) . . ?
O2 Na3 Na1 84.89(11) . . ?
O17 Na3 Na1 73.34(11) . . ?
O20 Na3 Na1 151.45(14) . . ?
O16 Na3 Na1 38.95(9) . . ?
S1 Na3 Na1 60.62(6) . . ?
Na4 Na3 Na1 88.49(7) 2_456 . ?
Na6 Na3 Na1 112.16(8) . . ?
O21 Na3 Mn1 90.55(12) . . ?
O19 Na3 Mn1 127.79(12) . . ?
O2 Na3 Mn1 79.83(11) . . ?
O17 Na3 Mn1 34.14(9) . . ?
O20 Na3 Mn1 96.56(12) . . ?
O16 Na3 Mn1 35.85(8) . . ?
S1 Na3 Mn1 57.39(5) . . ?
Na4 Na3 Mn1 114.78(7) 2_456 . ?
Na6 Na3 Mn1 58.15(5) . . ?
Na1 Na3 Mn1 54.91(5) . . ?
O21 Na3 Na4 35.98(10) . . ?
O19 Na3 Na4 68.11(11) . . ?
O2 Na3 Na4 139.15(12) . . ?
O17 Na3 Na4 65.61(10) . . ?
O20 Na3 Na4 128.19(13) . . ?
O16 Na3 Na4 89.25(10) . . ?
S1 Na3 Na4 114.79(7) . . ?
Na4 Na3 Na4 123.44(6) 2_456 . ?
Na6 Na3 Na4 105.06(7) . . ?
Na1 Na3 Na4 54.53(6) . . ?
Mn1 Na3 Na4 79.97(6) . . ?
O6 Na2 O18 105.34(16) . 2_556 ?
O6 Na2 O1 153.52(18) . 1_655 ?
O18 Na2 O1 93.76(16) 2_556 1_655 ?
O6 Na2 O4 87.44(15) . . ?
O18 Na2 O4 93.06(16) 2_556 . ?
O1 Na2 O4 110.04(15) 1_655 . ?
O6 Na2 O19 74.31(15) . 4_676 ?
O18 Na2 O19 93.62(16) 2_556 4_676 ?
O1 Na2 O19 86.55(15) 1_655 4_676 ?
O4 Na2 O19 161.65(16) . 4_676 ?
O6 Na2 O14 92.05(14) . 3_667 ?
O18 Na2 O14 160.46(15) 2_556 3_667 ?
O1 Na2 O14 73.02(14) 1_655 3_667 ?
O4 Na2 O14 78.64(14) . 3_667 ?
O19 Na2 O14 99.71(16) 4_676 3_667 ?
O6 Na2 Na1 109.93(13) . 1_655 ?
O18 Na2 Na1 120.64(13) 2_556 1_655 ?
O1 Na2 Na1 73.93(12) 1_655 1_655 ?
O4 Na2 Na1 44.34(10) . 1_655 ?
O19 Na2 Na1 140.91(14) 4_676 1_655 ?
O14 Na2 Na1 42.58(10) 3_667 1_655 ?
O6 Na2 S3 91.38(12) . 2_556 ?
O18 Na2 S3 22.20(10) 2_556 2_556 ?
O1 Na2 S3 111.88(13) 1_655 2_556 ?
O4 Na2 S3 75.07(11) . 2_556 ?
O19 Na2 S3 106.70(13) 4_676 2_556 ?
O14 Na2 S3 153.30(12) 3_667 2_556 ?
Na1 Na2 S3 111.91(8) 1_655 2_556 ?
O6 Na2 S4 20.94(10) . . ?
O18 Na2 S4 126.28(12) 2_556 . ?
O1 Na2 S4 136.24(14) 1_655 . ?
O4 Na2 S4 87.05(11) . . ?
O19 Na2 S4 75.23(11) 4_676 . ?
O14 Na2 S4 71.43(10) 3_667 . ?
Na1 Na2 S4 95.74(7) 1_655 . ?
S3 Na2 S4 111.39(7) 2_556 . ?
O6 Na2 Na4 146.22(14) . 2_556 ?
O18 Na2 Na4 40.88(10) 2_556 2_556 ?
O1 Na2 Na4 55.28(12) 1_655 2_556 ?
O4 Na2 Na4 93.48(11) . 2_556 ?
O19 Na2 Na4 102.73(12) 4_676 2_556 ?
O14 Na2 Na4 121.27(11) 3_667 2_556 ?
Na1 Na2 Na4 93.57(7) 1_655 2_556 ?
S3 Na2 Na4 56.62(6) 2_556 2_556 ?
S4 Na2 Na4 167.15(8) . 2_556 ?
O6 Na2 Na5 35.47(11) . . ?
O18 Na2 Na5 70.10(11) 2_556 . ?
O1 Na2 Na5 152.69(13) 1_655 . ?
O4 Na2 Na5 93.18(11) . . ?
O19 Na2 Na5 73.15(11) 4_676 . ?
O14 Na2 Na5 127.48(11) 3_667 . ?
Na1 Na2 Na5 133.11(8) 1_655 . ?
S3 Na2 Na5 59.34(5) 2_556 . ?
S4 Na2 Na5 56.28(5) . . ?
Na4 Na2 Na5 110.89(8) 2_556 . ?
O6 Na2 Na6 54.72(11) . . ?
O18 Na2 Na6 104.22(13) 2_556 . ?
O1 Na2 Na6 138.05(13) 1_655 . ?
O4 Na2 Na6 32.97(10) . . ?
O19 Na2 Na6 128.68(12) 4_676 . ?
O14 Na2 Na6 78.40(11) 3_667 . ?
Na1 Na2 Na6 64.25(6) 1_655 . ?
S3 Na2 Na6 82.08(7) 2_556 . ?
S4 Na2 Na6 55.29(5) . . ?
Na4 Na2 Na6 122.24(8) 2_556 . ?
Na5 Na2 Na6 68.86(6) . . ?
S2 O3 Na5 169.1(2) . 2_546 ?
S2 O3 Na4 94.54(19) . 1_655 ?
Na5 O3 Na4 96.18(15) 2_546 1_655 ?
S2 O3 Na6 84.77(18) . . ?
Na5 O3 Na6 86.87(13) 2_546 . ?
Na4 O3 Na6 130.38(17) 1_655 . ?
Na1 O14 Na6 88.31(16) 3_567 . ?
Na1 O14 Na2 79.60(15) 3_567 3_667 ?
Na6 O14 Na2 162.87(18) . 3_667 ?
S4 O6 Na2 125.5(2) . . ?
S4 O6 Na5 122.8(2) . . ?
Na2 O6 Na5 111.17(17) . . ?
S2 O4 Na6 108.5(2) . . ?
S2 O4 Na1 95.82(19) . 1_655 ?
Na6 O4 Na1 113.97(17) . 1_655 ?
S2 O4 Na2 132.1(2) . . ?
Na6 O4 Na2 112.58(17) . . ?
Na1 O4 Na2 89.36(16) 1_655 . ?
S4 O7 Mn1 126.1(2) . . ?
S4 O7 Na1 107.8(2) . 3_567 ?
Mn1 O7 Na1 98.29(16) . 3_567 ?
S4 O7 Na6 120.4(2) . . ?
Mn1 O7 Na6 102.78(16) . . ?
Na1 O7 Na6 94.68(15) 3_567 . ?
S3 O5 Na5 142.8(3) . 2_546 ?
S3 O5 Na6 98.96(19) . . ?
Na5 O5 Na6 96.88(15) 2_546 . ?
S1 O1 Na2 140.3(2) . 1_455 ?
S1 O1 Na4 88.48(18) . 2_456 ?
Na2 O1 Na4 85.10(14) 1_455 2_456 ?
S1 O2 Na5 122.3(2) . . ?
S1 O2 Na4 114.4(2) . 2_456 ?
Na5 O2 Na4 103.70(16) . 2_456 ?
S1 O2 Na3 105.6(2) . . ?
Na5 O2 Na3 111.16(17) . . ?
Na4 O2 Na3 96.83(16) 2_456 . ?
O4 Na6 O20 92.75(16) . . ?
O4 Na6 O7 105.13(16) . . ?
O20 Na6 O7 107.86(17) . . ?
O4 Na6 O17 174.58(16) . . ?
O20 Na6 O17 83.45(15) . . ?
O7 Na6 O17 72.56(14) . . ?
O4 Na6 O5 128.95(16) . . ?
O20 Na6 O5 105.51(16) . . ?
O7 Na6 O5 113.28(15) . . ?
O17 Na6 O5 56.10(12) . . ?
O4 Na6 O14 83.76(15) . . ?
O20 Na6 O14 169.20(18) . . ?
O7 Na6 O14 82.93(15) . . ?
O17 Na6 O14 100.67(14) . . ?
O5 Na6 O14 69.51(14) . . ?
O4 Na6 O3 53.85(13) . . ?
O20 Na6 O3 90.56(15) . . ?
O7 Na6 O3 153.54(16) . . ?
O17 Na6 O3 129.81(15) . . ?
O5 Na6 O3 78.25(13) . . ?
O14 Na6 O3 79.12(14) . . ?
O4 Na6 S2 26.94(11) . . ?
O20 Na6 S2 85.01(12) . . ?
O7 Na6 S2 132.03(13) . . ?
O17 Na6 S2 155.23(14) . . ?
O5 Na6 S2 106.69(12) . . ?
O14 Na6 S2 87.32(11) . . ?
O3 Na6 S2 28.51(8) . . ?
O4 Na6 S3 156.88(14) . . ?
O20 Na6 S3 94.90(13) . . ?
O7 Na6 S3 93.22(11) . . ?
O17 Na6 S3 28.11(9) . . ?
O5 Na6 S3 27.99(9) . . ?
O14 Na6 S3 84.69(11) . . ?
O3 Na6 S3 104.22(11) . . ?
S2 Na6 S3 132.52(9) . . ?
O4 Na6 Na1 92.03(13) . 3_567 ?
O20 Na6 Na1 149.24(15) . 3_567 ?
O7 Na6 Na1 41.81(10) . 3_567 ?
O17 Na6 Na1 89.32(12) . 3_567 ?
O5 Na6 Na1 94.84(12) . 3_567 ?
O14 Na6 Na1 41.42(11) . 3_567 ?
O3 Na6 Na1 116.43(11) . 3_567 ?
S2 Na6 Na1 111.29(8) . 3_567 ?
S3 Na6 Na1 92.47(7) . 3_567 ?
O4 Na6 Mn1 141.35(14) . . ?
O20 Na6 Mn1 102.38(12) . . ?
O7 Na6 Mn1 36.40(9) . . ?
O17 Na6 Mn1 36.96(9) . . ?
O5 Na6 Mn1 81.06(10) . . ?
O14 Na6 Mn1 86.53(11) . . ?
O3 Na6 Mn1 157.92(11) . . ?
S2 Na6 Mn1 167.68(9) . . ?
S3 Na6 Mn1 57.38(4) . . ?
Na1 Na6 Mn1 57.73(5) 3_567 . ?
O4 Na6 Na3 132.62(13) . . ?
O20 Na6 Na3 42.44(11) . . ?
O7 Na6 Na3 82.00(11) . . ?
O17 Na6 Na3 42.71(9) . . ?
O5 Na6 Na3 86.17(11) . . ?
O14 Na6 Na3 143.23(12) . . ?
O3 Na6 Na3 123.58(12) . . ?
S2 Na6 Na3 126.98(9) . . ?
S3 Na6 Na3 62.97(6) . . ?
Na1 Na6 Na3 118.71(8) 3_567 . ?
Mn1 Na6 Na3 62.04(5) . . ?
S3 O18 Na2 121.8(2) . 2_546 ?
S3 O18 Na4 114.5(2) . . ?
Na2 O18 Na4 100.17(16) 2_546 . ?
S3 O17 Mn1 123.0(2) . . ?
S3 O17 Na3 126.0(2) . . ?
Mn1 O17 Na3 106.19(15) . . ?
S3 O17 Na6 99.88(19) . . ?
Mn1 O17 Na6 98.40(15) . . ?
Na3 O17 Na6 93.11(14) . . ?
Na3 O19 Na2 119.26(18) . 4_575 ?
Na6 O20 Na3 97.24(16) . . ?
S1 O16 Mn1 128.8(2) . . ?
S1 O16 Na1 131.1(2) . . ?
Mn1 O16 Na1 98.24(15) . . ?
S1 O16 Na3 93.61(18) . . ?
Mn1 O16 Na3 97.32(14) . . ?
Na1 O16 Na3 92.79(15) . . ?
S2 O21 Na3 143.5(2) 1_455 . ?
S2 O21 Na1 93.66(18) 1_455 . ?
Na3 O21 Na1 101.16(17) . . ?
S2 O21 Na4 103.57(19) 1_455 . ?
Na3 O21 Na4 108.82(16) . . ?
Na1 O21 Na4 92.35(15) . . ?
S4 O22 Na4 122.9(2) . 3_567 ?
S4 O22 Na1 91.27(19) . 3_567 ?
Na4 O22 Na1 85.14(14) 3_567 3_567 ?
Na5 O23 Na4 169.3(2) 3_577 2_456 ?

_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_theta_full        25.17
_diffrn_measured_fraction_theta_full 0.989
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.156