Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001


data_global

_journal_coden_Cambridge      186

loop_
_publ_author_name
_publ_author_address

'Blake, Alexander J.'              
; 
School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England  UK
; 

'Doble, Dan M.J.'          
; 
School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England  UK
; 

'Li,Wan-Sheung'               
; 
School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England  UK
;

'Schroder, Martin'               
; 
School of Chemistry
The University of Nottingham
University Park
Nottingham  NG7 2RD
England  UK
;


# SUBMISSION DETAILS 

_publ_contact_author_name            'Prof Martin Schroder' 
_publ_contact_author_address
;
School of Chemistry
University of Nottingham
University Park
Nottingham
NG7 2RD
UNITED KINGDOM
;
_publ_contact_author_email         M.SCHRODER@NOTTINGHAM.AC.UK
_publ_contact_author_fax          '0115 951 3563'
_publ_contact_author_phone        '0115 951 3488'
_publ_requested_journal           'JCS Dalton Transactions' 

#============================================================================== 

# TITLE AND AUTHOR LIST 

_publ_section_title 
;
Na^+^-Mediated Aggregation of Imino-carboxylate Transition Metal Complexes
; 

# The loop structure below should contain the names and addresses of all 
# authors, in the required order of publication. Repeat as necessary. 



## Data blocks for individual structures follow. These are to be 
## separated by a line containing only the string #=== END
## The file should also be terminated by the same string.
## ===========================================================


data_2

_database_code_CSD	171265

# Code MNTRAM

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum            'C30 H68 Cl2 Mn2 N8 Na4 O25' 
_chemical_formula_weight          1213.66 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Na'  'Na'   0.0362   0.0249 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Mn'  'Mn'   0.3368   0.7283 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Cl'  'Cl'   0.1484   0.1585 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Trigonal 
_symmetry_space_group_name_H-M    P-3 

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

_cell_length_a                    9.004(5) 
_cell_length_b                    9.004(5) 
_cell_length_c                    18.119(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      1272.1(13) 
_cell_formula_units_Z             1 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     26
_cell_measurement_theta_min       15
_cell_measurement_theta_max       17

_exptl_crystal_description        'equant block'
_exptl_crystal_colour             'yellow'
_exptl_crystal_size_max           0.51 
_exptl_crystal_size_mid           0.51 
_exptl_crystal_size_min           0.38 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.584 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              632 
_exptl_absorpt_coefficient_mu     0.725 
_exptl_absorpt_correction_type    'psi scans' 
_exptl_absorpt_correction_T_min   0.709 
_exptl_absorpt_correction_T_max   0.770 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(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   'Stoe Stadi-4 four-circle'
_diffrn_measurement_method        omega-theta 
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         5
_diffrn_reflns_number             3076 
_diffrn_reflns_av_R_equivalents   0.0179 
_diffrn_reflns_av_sigmaI/netI     0.0191 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        10 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          2.61 
_diffrn_reflns_theta_max          24.98 
_reflns_number_total              1513 
_reflns_number_gt                 1353 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'STADI-4 (Stoe & Cie, 1996a)' 
_computing_cell_refinement        'STADI-4 (Stoe & Cie, 1996a)' 
_computing_data_reduction         'X-RED (Stoe & Cie, 1996b)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 


_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.1834P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'Patterson' 
_atom_sites_solution_secondary    'difference fourier synthesis'
_atom_sites_solution_hydrogens    
'Me and water Hs found in delta-F, others placed geometrically'
_refine_ls_hydrogen_treatment     'riding model' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          1513 
_refine_ls_number_parameters      176 
_refine_ls_number_restraints      19 
_refine_ls_R_factor_all           0.0403 
_refine_ls_R_factor_gt            0.0345 
_refine_ls_wR_factor_ref          0.0935 
_refine_ls_wR_factor_gt           0.0879 
_refine_ls_goodness_of_fit_ref    1.084 
_refine_ls_restrained_S_all       1.082 
_refine_ls_shift/su_max           0.098 
_refine_ls_shift/su_mean          0.002 

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_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Mn Mn 0.3333 0.6667 0.30781(3) 0.0238(2) Uani 1 d S . . 
Na1 Na 1.0000 1.0000 0.5000 0.0188(4) Uani 1 d S . . 
Na2 Na 0.6686(3) 0.6131(3) 0.45863(12) 0.0290(5) Uani 0.50 d P . 1 
O1W O 0.5803(6) 0.5420(5) 0.4694(2) 0.0326(9) Uani 0.50 d PD . 2 
H1WA H 0.588(5) 0.628(3) 0.446(2) 0.039 Uiso 0.50 d PD A 2 
H1WB H 0.656(6) 0.584(5) 0.503(2) 0.039 Uiso 0.50 d PD B 2 
N N 0.3333 0.6667 0.16447(18) 0.0272(7) Uani 1 d SD . . 
C1 C 0.3928(6) 0.8447(5) 0.1468(2) 0.0241(9) Uani 0.50 d PD C 1 
H1A H 0.3001 0.8698 0.1584 0.029 Uiso 0.50 calc PR C 1 
H1B H 0.4148 0.8613 0.0931 0.029 Uiso 0.50 calc PR C 1 
C1' C 0.4869(7) 0.8219(6) 0.1352(3) 0.0376(12) Uani 0.50 d PD C 2 
H1A' H 0.5797 0.7952 0.1266 0.045 Uiso 0.50 calc PR C 2 
H1B' H 0.4579 0.8535 0.0872 0.045 Uiso 0.50 calc PR C 2 
C2 C 0.5491(4) 0.9691(3) 0.18624(14) 0.0378(6) Uani 1 d D . . 
H2A H 0.652(3) 0.973(5) 0.164(3) 0.045 Uiso 0.50 d PD D 1 
H2B H 0.569(6) 1.088(2) 0.186(3) 0.045 Uiso 0.50 d PD E 1 
H2A' H 0.441(3) 0.973(5) 0.191(3) 0.045 Uiso 0.50 d PD F 2 
H2B' H 0.641(4) 1.086(3) 0.172(3) 0.045 Uiso 0.50 d PD G 2 
N3 N 0.5523(2) 0.9153(2) 0.26217(10) 0.0267(4) Uani 1 d . . . 
C4 C 0.6833(3) 1.0003(3) 0.30245(13) 0.0301(5) Uani 1 d . . . 
C5 C 0.6766(3) 0.9231(3) 0.37806(13) 0.0319(6) Uani 1 d . . . 
O6 O 0.5529(2) 0.7740(2) 0.38894(9) 0.0411(5) Uani 1 d . . . 
O7 O 0.7917(2) 1.0096(3) 0.42298(10) 0.0449(5) Uani 1 d . . . 
C8 C 0.8416(4) 1.1635(4) 0.28180(19) 0.0551(8) Uani 1 d . . . 
H8A H 0.8972 1.1427 0.2397 0.083 Uiso 1 calc R . . 
H8B H 0.9207 1.2049 0.3238 0.083 Uiso 1 calc R . . 
H8C H 0.8107 1.2500 0.2683 0.083 Uiso 1 calc R . . 
Cl1 Cl 0.0000 1.0000 0.1395(6) 0.0318(18) Uani 0.30 d SP H 1 
O2W O 0.0000 1.0000 0.1399(12) 0.077(5) Uani 0.70 d SPD I 2 
H2WA H -0.097(6) 0.913(8) 0.149(6) 0.093 Uiso 0.47 d PD J 2 
Cl2 Cl -0.1380(11) 0.1854(11) 0.0492(7) 0.060(2) Uani 0.20 d P K 1 
O3W O -0.1320(11) 0.1784(12) 0.0355(5) 0.105(3) Uani 0.80 d PD L 2 
H3WA H -0.112(4) 0.131(6) 0.071(2) 0.126 Uiso 0.80 d PD M 2 
H3WB H -0.200(8) 0.209(9) 0.053(3) 0.126 Uiso 0.80 d PD N 2 
Cl3 Cl -0.3333 0.3333 0.0761(13) 0.031(5) Uani 0.10 d SP O 1 
O4W O -0.3333 0.3333 0.0710(6) 0.083(4) Uani 0.90 d SPD P 2 
H4WB H -0.249(4) 0.320(6) 0.0588(6) 0.099 Uiso 0.45 d PD Q 2 
H4WA H -0.3333 0.3333 0.1179(6) 0.099 Uiso 0.45 d SPD R 2 
O5W O -0.3333 0.3333 0.40044(15) 0.0301(6) Uani 1 d SD . . 
H5WA H -0.240(3) 0.354(5) 0.4205(19) 0.036 Uiso 0.67 d PD . . 

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 
Mn 0.0256(2) 0.0256(2) 0.0203(3) 0.000 0.000 0.01279(12) 
Na1 0.0176(6) 0.0176(6) 0.0211(9) 0.000 0.000 0.0088(3) 
Na2 0.0319(13) 0.0227(11) 0.0298(11) -0.0010(9) 0.0001(10) 0.0116(10) 
O1W 0.023(2) 0.031(2) 0.036(2) -0.0021(18) -0.0084(19) 0.0079(17) 
N 0.0258(10) 0.0258(10) 0.0301(17) 0.000 0.000 0.0129(5) 
C1 0.027(2) 0.028(2) 0.020(2) 0.0047(17) 0.0009(18) 0.016(2) 
C1' 0.040(3) 0.037(3) 0.026(2) 0.007(2) 0.002(2) 0.013(3) 
C2 0.0456(15) 0.0279(13) 0.0321(13) 0.0069(10) 0.0006(11) 0.0125(12) 
N3 0.0286(10) 0.0243(10) 0.0273(9) -0.0015(8) -0.0032(8) 0.0132(8) 
C4 0.0283(12) 0.0262(12) 0.0395(13) -0.0080(10) -0.0058(10) 0.0163(10) 
C5 0.0320(13) 0.0403(14) 0.0352(13) -0.0103(11) -0.0086(10) 0.0269(12) 
O6 0.0418(10) 0.0476(11) 0.0297(9) 0.0036(8) -0.0063(8) 0.0194(9) 
O7 0.0416(11) 0.0586(12) 0.0461(11) -0.0210(9) -0.0243(9) 0.0336(10) 
C8 0.0365(16) 0.0349(15) 0.074(2) -0.0002(14) -0.0135(14) 0.0032(13) 
Cl1 0.031(2) 0.031(2) 0.034(5) 0.000 0.000 0.0153(12) 
O2W 0.088(7) 0.088(7) 0.057(12) 0.000 0.000 0.044(3) 
Cl2 0.033(3) 0.041(3) 0.096(4) 0.004(3) 0.023(3) 0.011(2) 
O3W 0.098(5) 0.101(5) 0.144(7) 0.024(4) 0.005(4) 0.070(4) 
Cl3 0.028(6) 0.028(6) 0.035(11) 0.000 0.000 0.014(3) 
O4W 0.091(5) 0.091(5) 0.067(7) 0.000 0.000 0.045(2) 
O5W 0.0340(10) 0.0340(10) 0.0224(14) 0.000 0.000 0.0170(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 
Mn O6 2.257(2) 2_665 ? 
Mn O6 2.257(2) . y 
Mn O6 2.257(2) 3_565 ? 
Mn N3 2.273(2) 2_665 ? 
Mn N3 2.273(2) . y 
Mn N3 2.273(2) 3_565 ? 
Mn N 2.597(4) . y 
Na1 O7 2.3736(19) 5_566 ? 
Na1 O7 2.374(2) . y 
Na1 O7 2.374(2) 6_656 ? 
Na1 O7 2.374(2) 4_776 ? 
Na1 O7 2.374(2) 3_675 ? 
Na1 O7 2.374(2) 2_765 ? 
Na1 Na2 3.348(3) 4_776 ? 
Na1 Na2 3.348(3) . ? 
Na1 Na2 3.348(3) 5_566 ? 
Na1 Na2 3.348(3) 3_675 ? 
Na1 Na2 3.348(3) 2_765 ? 
Na1 Na2 3.348(3) 6_656 ? 
Na2 O6 2.508(3) . y 
Na2 O7 2.567(3) 6_656 y 
Na2 O7 2.592(3) 2_765 y 
Na2 O5W 2.723(3) 1_655 y 
Na2 C5 3.038(4) 6_656 ? 
Na2 Na2 3.070(5) 4_666 ? 
Na2 C5 3.119(4) . ? 
Na2 Na2 3.591(3) 5_566 ? 
Na2 Na2 3.591(3) 6_656 ? 
O1W O1W 1.672(10) 4_666 ? 
N C1 1.449(4) . ? 
N C1 1.449(4) 2_665 ? 
N C1 1.449(4) 3_565 ? 
N C1' 1.488(5) 2_665 ? 
N C1' 1.488(5) . ? 
N C1' 1.488(5) 3_565 ? 
C1 C2 1.473(5) . ? 
C1' C2 1.477(5) . ? 
C2 N3 1.464(3) . ? 
N3 C4 1.268(3) . ? 
C4 C8 1.496(4) . ? 
C4 C5 1.524(4) . ? 
C5 O7 1.239(3) . ? 
C5 O6 1.260(3) . ? 
C5 Na2 3.038(4) 5_566 ? 
O7 Na2 2.567(3) 5_566 ? 
O7 Na2 2.592(3) 3_675 ? 
O5W Na2 2.723(3) 3_565 ? 
O5W Na2 2.723(3) 2 ? 
O5W Na2 2.722(3) 1_455 ? 

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 
O6 Mn O6 82.15(8) 2_665 . y 
O6 Mn O6 82.15(8) 2_665 3_565 ? 
O6 Mn O6 82.15(8) . 3_565 ? 
O6 Mn N3 70.90(7) 2_665 2_665 ? 
O6 Mn N3 152.58(7) . 2_665 ? 
O6 Mn N3 98.66(7) 3_565 2_665 ? 
O6 Mn N3 98.66(7) 2_665 . y 
O6 Mn N3 70.90(7) . . y 
O6 Mn N3 152.58(7) 3_565 . ? 
N3 Mn N3 107.55(5) 2_665 . ? 
O6 Mn N3 152.58(7) 2_665 3_565 ? 
O6 Mn N3 98.66(7) . 3_565 ? 
O6 Mn N3 70.90(7) 3_565 3_565 ? 
N3 Mn N3 107.55(5) 2_665 3_565 ? 
N3 Mn N3 107.55(5) . 3_565 ? 
O6 Mn N 130.65(5) 2_665 . ? 
O6 Mn N 130.65(5) . . y 
O6 Mn N 130.65(5) 3_565 . ? 
N3 Mn N 68.67(5) 2_665 . ? 
N3 Mn N 68.67(5) . . y 
N3 Mn N 68.67(5) 3_565 . ? 
O7 Na1 O7 91.06(8) 5_566 . ? 
O7 Na1 O7 88.94(7) 5_566 6_656 ? 
O7 Na1 O7 91.06(8) . 6_656 ? 
O7 Na1 O7 88.94(8) 5_566 4_776 ? 
O7 Na1 O7 180.0 . 4_776 ? 
O7 Na1 O7 88.94(8) 6_656 4_776 ? 
O7 Na1 O7 91.06(8) 5_566 3_675 ? 
O7 Na1 O7 88.94(8) . 3_675 ? 
O7 Na1 O7 180.0 6_656 3_675 ? 
O7 Na1 O7 91.06(8) 4_776 3_675 ? 
O7 Na1 O7 180.0 5_566 2_765 ? 
O7 Na1 O7 88.94(8) . 2_765 ? 
O7 Na1 O7 91.06(8) 6_656 2_765 ? 
O7 Na1 O7 91.06(8) 4_776 2_765 ? 
O7 Na1 O7 88.94(8) 3_675 2_765 ? 
O7 Na1 Na2 50.44(6) 5_566 4_776 ? 
O7 Na1 Na2 113.78(6) . 4_776 ? 
O7 Na1 Na2 130.17(7) 6_656 4_776 ? 
O7 Na1 Na2 66.22(6) 4_776 4_776 ? 
O7 Na1 Na2 49.83(7) 3_675 4_776 ? 
O7 Na1 Na2 129.56(6) 2_765 4_776 ? 
O7 Na1 Na2 129.56(6) 5_566 . ? 
O7 Na1 Na2 66.22(6) . . ? 
O7 Na1 Na2 49.83(7) 6_656 . ? 
O7 Na1 Na2 113.78(6) 4_776 . ? 
O7 Na1 Na2 130.17(7) 3_675 . ? 
O7 Na1 Na2 50.44(6) 2_765 . ? 
Na2 Na1 Na2 180.0 4_776 . ? 
O7 Na1 Na2 66.22(6) 5_566 5_566 ? 
O7 Na1 Na2 49.83(7) . 5_566 ? 
O7 Na1 Na2 50.44(6) 6_656 5_566 ? 
O7 Na1 Na2 130.17(7) 4_776 5_566 ? 
O7 Na1 Na2 129.56(6) 3_675 5_566 ? 
O7 Na1 Na2 113.78(6) 2_765 5_566 ? 
Na2 Na1 Na2 115.14(3) 4_776 5_566 ? 
Na2 Na1 Na2 64.86(3) . 5_566 ? 
O7 Na1 Na2 49.83(7) 5_566 3_675 ? 
O7 Na1 Na2 50.44(6) . 3_675 ? 
O7 Na1 Na2 113.78(6) 6_656 3_675 ? 
O7 Na1 Na2 129.56(6) 4_776 3_675 ? 
O7 Na1 Na2 66.22(6) 3_675 3_675 ? 
O7 Na1 Na2 130.17(7) 2_765 3_675 ? 
Na2 Na1 Na2 64.86(3) 4_776 3_675 ? 
Na2 Na1 Na2 115.14(3) . 3_675 ? 
Na2 Na1 Na2 64.86(3) 5_566 3_675 ? 
O7 Na1 Na2 113.78(6) 5_566 2_765 ? 
O7 Na1 Na2 130.17(7) . 2_765 ? 
O7 Na1 Na2 129.56(6) 6_656 2_765 ? 
O7 Na1 Na2 49.83(7) 4_776 2_765 ? 
O7 Na1 Na2 50.44(6) 3_675 2_765 ? 
O7 Na1 Na2 66.22(6) 2_765 2_765 ? 
Na2 Na1 Na2 64.86(3) 4_776 2_765 ? 
Na2 Na1 Na2 115.14(3) . 2_765 ? 
Na2 Na1 Na2 180.0 5_566 2_765 ? 
Na2 Na1 Na2 115.14(3) 3_675 2_765 ? 
O7 Na1 Na2 130.17(7) 5_566 6_656 ? 
O7 Na1 Na2 129.56(6) . 6_656 ? 
O7 Na1 Na2 66.22(6) 6_656 6_656 ? 
O7 Na1 Na2 50.44(6) 4_776 6_656 ? 
O7 Na1 Na2 113.78(6) 3_675 6_656 ? 
O7 Na1 Na2 49.83(7) 2_765 6_656 ? 
Na2 Na1 Na2 115.14(3) 4_776 6_656 ? 
Na2 Na1 Na2 64.86(3) . 6_656 ? 
Na2 Na1 Na2 115.14(3) 5_566 6_656 ? 
Na2 Na1 Na2 180.0 3_675 6_656 ? 
Na2 Na1 Na2 64.86(3) 2_765 6_656 ? 
O6 Na2 O7 102.07(10) . 6_656 ? 
O6 Na2 O7 101.57(10) . 2_765 ? 
O7 Na2 O7 82.08(11) 6_656 2_765 ? 
O6 Na2 O5W 121.82(11) . 1_655 ? 
O7 Na2 O5W 136.02(11) 6_656 1_655 ? 
O7 Na2 O5W 86.27(8) 2_765 1_655 ? 
O6 Na2 C5 121.32(10) . 6_656 ? 
O7 Na2 C5 91.70(9) 2_765 6_656 ? 
O5W Na2 C5 115.84(10) 1_655 6_656 ? 
O6 Na2 Na2 94.04(12) . 4_666 ? 
O7 Na2 Na2 87.67(10) 6_656 4_666 ? 
O7 Na2 Na2 162.80(14) 2_765 4_666 ? 
O5W Na2 Na2 91.66(10) 1_655 4_666 ? 
C5 Na2 Na2 73.84(9) 6_656 4_666 ? 
O7 Na2 C5 90.38(9) 6_656 . ? 
O7 Na2 C5 80.73(9) 2_765 . ? 
O5W Na2 C5 129.29(11) 1_655 . ? 
C5 Na2 C5 113.35(10) 6_656 . ? 
Na2 Na2 C5 113.26(12) 4_666 . ? 
O6 Na2 Na1 85.59(8) . . ? 
O5W Na2 Na1 129.75(9) 1_655 . ? 
C5 Na2 Na1 64.94(6) 6_656 . ? 
Na2 Na2 Na1 130.69(10) 4_666 . ? 
C5 Na2 Na1 64.13(6) . . ? 
O6 Na2 Na2 57.28(8) . 5_566 ? 
O7 Na2 Na2 46.19(7) 6_656 5_566 ? 
O7 Na2 Na2 101.26(5) 2_765 5_566 ? 
O5W Na2 Na2 172.47(9) 1_655 5_566 ? 
C5 Na2 Na2 64.11(8) 6_656 5_566 ? 
Na2 Na2 Na2 81.08(11) 4_666 5_566 ? 
C5 Na2 Na2 53.29(7) . 5_566 ? 
Na1 Na2 Na2 57.569(14) . 5_566 ? 
O6 Na2 Na2 141.65(8) . 6_656 ? 
O7 Na2 Na2 60.60(7) 6_656 6_656 ? 
O5W Na2 Na2 81.22(8) 1_655 6_656 ? 
C5 Na2 Na2 55.37(8) 6_656 6_656 ? 
Na2 Na2 Na2 117.21(14) 4_666 6_656 ? 
C5 Na2 Na2 118.96(6) . 6_656 ? 
Na1 Na2 Na2 57.569(14) . 6_656 ? 
Na2 Na2 Na2 103.80(8) 5_566 6_656 ? 
C1 N C1 115.28(15) . 2_665 ? 
C1 N C1 115.28(15) . 3_565 ? 
C1 N C1 115.28(15) 2_665 3_565 ? 
C1' N C1' 108.0(2) 2_665 . ? 
C1 N Mn 102.7(2) . . ? 
C1 N Mn 102.7(2) 2_665 . ? 
C1 N Mn 102.7(2) 3_565 . ? 
C1' N Mn 110.9(2) 2_665 . ? 
C1' N Mn 110.9(2) . . ? 
C1' N Mn 110.9(2) 3_565 . ? 
N C1 C2 114.7(3) . . ? 
C2 C1' N 112.2(3) . . ? 
N3 C2 C1 111.9(2) . . ? 
N3 C2 C1' 110.7(3) . . ? 
C4 N3 C2 120.5(2) . . ? 
C4 N3 Mn 118.16(16) . . ? 
C2 N3 Mn 121.15(15) . . ? 
N3 C4 C8 126.2(2) . . ? 
N3 C4 C5 115.5(2) . . ? 
C8 C4 C5 118.3(2) . . ? 
O7 C5 O6 125.7(2) . . ? 
O7 C5 C4 118.3(2) . . ? 
O6 C5 C4 116.0(2) . . ? 
O7 C5 Na2 56.31(14) . 5_566 ? 
O6 C5 Na2 79.68(15) . 5_566 ? 
C4 C5 Na2 144.32(16) . 5_566 ? 
O7 C5 Na2 83.86(16) . . ? 
O6 C5 Na2 50.25(13) . . ? 
C4 C5 Na2 143.82(15) . . ? 
Na2 C5 Na2 71.34(8) 5_566 . ? 
C5 O6 Mn 118.23(15) . . ? 
C5 O6 Na2 107.04(16) . . ? 
Mn O6 Na2 127.49(10) . . ? 
C5 O7 Na1 142.26(17) . . ? 
C5 O7 Na2 100.01(18) . 5_566 ? 
Na1 O7 Na2 85.22(9) . 5_566 ? 
C5 O7 Na2 132.52(17) . 3_675 ? 
Na1 O7 Na2 84.66(7) . 3_675 ? 
Na2 O7 Na2 88.21(7) 5_566 3_675 ? 
Na2 O5W Na2 105.96(8) 3_565 2 ? 
Na2 O5W Na2 105.96(8) 3_565 1_455 ? 
Na2 O5W Na2 105.96(8) 2 1_455 ? 

_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              24.98 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.68 
_refine_diff_density_min   -0.26 
_refine_diff_density_rms    0.05 

#===END

data_3

_database_code_CSD	171266

# Code MNTRIC

_refine_special_details 
; 
One MeOH was found to be disordered over three equally-occupied sites. 
; 

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ?
_chemical_formula_sum            'C36 H66 Mn2 N8 Na2 O18' 
_chemical_formula_weight          1054.82

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Na'  'Na'   0.0362   0.0249 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Mn'  'Mn'   0.3368   0.7283 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            triclinic
_symmetry_space_group_name_H-M    'P -1'

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

_cell_length_a                    10.094(3) 
_cell_length_b                    11.423(5) 
_cell_length_c                    12.613(3) 
_cell_angle_alpha                 104.16(4) 
_cell_angle_beta                  107.27(3) 
_cell_angle_gamma                 106.27(3) 
_cell_volume                      1245.0(7) 
_cell_formula_units_Z             1
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     28 
_cell_measurement_theta_min       15 
_cell_measurement_theta_max       17 

_exptl_crystal_description        'trigonal prism' 
_exptl_crystal_colour             'pale yellow' 
_exptl_crystal_size_max           0.78 
_exptl_crystal_size_mid           0.62 
_exptl_crystal_size_min           0.46 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.407 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              554 
_exptl_absorpt_coefficient_mu     0.600 
_exptl_absorpt_correction_type    'Psi scans'
_exptl_absorpt_correction_T_min   0.543
_exptl_absorpt_correction_T_max   0.615 

_diffrn_ambient_temperature       150(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   'Stoe Stadi-4 four-circle'
_diffrn_measurement_method        '\w-\q profile fitting'
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         'variation +/- 2'
_diffrn_reflns_number             4395 
_diffrn_reflns_av_R_equivalents   0.0123 
_diffrn_reflns_av_sigmaI/netI     0.0106 
_diffrn_reflns_limit_h_min        -12 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -13 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        15 
_diffrn_reflns_theta_min          2.88 
_diffrn_reflns_theta_max          25.05 
_reflns_number_total              4402
_reflns_number_gt                 4058 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'Stadi4 (Stoe & Cie, 1997a)'
_computing_cell_refinement        'Stadi4 (Stoe & Cie, 1997a)'
_computing_data_reduction         'X-RED (Stoe & Cie, 1997b)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC version 5.03 (Sheldrick, 1995)'
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)'


_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+2.4064P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'direct methods'
_atom_sites_solution_secondary    'difference-Fourier' 
_atom_sites_solution_hydrogens     
;
all carbon bonded H-atoms were placed at calculated positions, and the
hydroxyl H-atom on the two non-disorder methanol molecules were located
from a difference-Fourier map. No H-atoms were calculated for the disordered
methanol molecule.
;
_refine_ls_hydrogen_treatment     
;
riding model for the C-bonded H-atoms; isotropic refinement for the hydroxyl
H-atoms
;
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4381 
_refine_ls_number_parameters      312 
_refine_ls_number_restraints      7 
_refine_ls_R_factor_all           0.0533 
_refine_ls_R_factor_gt            0.0494 
_refine_ls_wR_factor_ref          0.1366 
_refine_ls_wR_factor_gt           0.1310 
_refine_ls_goodness_of_fit_ref    1.068 
_refine_ls_restrained_S_all       1.068 
_refine_ls_shift/su_max           0.002 
_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_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Mn Mn 0.35016(4) 0.84862(4) 0.67436(4) 0.01954(15) Uani 1 d . . . 
Na Na -0.04731(13) 0.92377(11) 0.60125(10) 0.0262(3) Uani 1 d . . . 
N N 0.5167(3) 0.7048(2) 0.6869(2) 0.0207(5) Uani 1 d . . . 
C1A C 0.4257(3) 0.5792(3) 0.6866(3) 0.0232(6) Uani 1 d . . . 
H1AA H 0.4926 0.5388 0.7236 0.028 Uiso 1 calc R . . 
H1AB H 0.3619 0.5195 0.6036 0.028 Uiso 1 calc R . . 
C2A C 0.3266(3) 0.5983(3) 0.7550(3) 0.0233(6) Uani 1 d . . . 
H2AA H 0.2613 0.5128 0.7504 0.028 Uiso 1 calc R . . 
H2AB H 0.3894 0.6523 0.8397 0.028 Uiso 1 calc R . . 
N3A N 0.2351(3) 0.6639(2) 0.7007(2) 0.0200(5) Uani 1 d . . . 
C4A C 0.0934(3) 0.6224(3) 0.6692(3) 0.0241(6) Uani 1 d . . . 
C5A C 0.0173(3) 0.7024(3) 0.6103(3) 0.0253(6) Uani 1 d . . . 
O6A O 0.1023(2) 0.79422(19) 0.59320(18) 0.0248(4) Uani 1 d . . . 
O7A O -0.1190(2) 0.6731(2) 0.5844(2) 0.0378(6) Uani 1 d . . . 
C8A C -0.0034(4) 0.5084(4) 0.6859(4) 0.0409(8) Uani 1 d . . . 
H8AA H 0.0588 0.4664 0.7241 0.061 Uiso 1 calc R . . 
H8AB H -0.0789 0.4455 0.6083 0.061 Uiso 1 calc R . . 
H8AC H -0.0537 0.5387 0.7361 0.061 Uiso 1 calc R . . 
C1B C 0.5572(3) 0.6903(3) 0.5832(3) 0.0239(6) Uani 1 d . . . 
H1BA H 0.5896 0.6157 0.5693 0.029 Uiso 1 calc R . . 
H1BB H 0.6422 0.7702 0.5989 0.029 Uiso 1 calc R . . 
C2B C 0.4241(3) 0.6674(3) 0.4726(3) 0.0264(6) Uani 1 d . . . 
H2BA H 0.4543 0.6636 0.4043 0.032 Uiso 1 calc R . . 
H2BB H 0.3414 0.5837 0.4519 0.032 Uiso 1 calc R . . 
N3B N 0.3752(3) 0.7760(2) 0.4995(2) 0.0221(5) Uani 1 d . . . 
C4B C 0.3312(3) 0.8258(3) 0.4227(2) 0.0219(6) Uani 1 d . . . 
C5B C 0.2955(3) 0.9454(3) 0.4691(3) 0.0226(6) Uani 1 d . . . 
O6B O 0.3392(2) 0.99361(19) 0.58154(17) 0.0242(4) Uani 1 d . . . 
O7B O 0.2282(2) 0.9850(2) 0.39578(19) 0.0298(5) Uani 1 d . . . 
C8B C 0.3115(4) 0.7798(3) 0.2951(3) 0.0307(7) Uani 1 d . . . 
H8BA H 0.3382 0.7031 0.2779 0.046 Uiso 1 calc R . . 
H8BB H 0.3768 0.8497 0.2801 0.046 Uiso 1 calc R . . 
H8BC H 0.2067 0.7565 0.2438 0.046 Uiso 1 calc R . . 
C1C C 0.6509(3) 0.7758(3) 0.7989(3) 0.0241(6) Uani 1 d . . . 
H1CA H 0.7322 0.7458 0.7925 0.029 Uiso 1 calc R . . 
H1CB H 0.6271 0.7564 0.8649 0.029 Uiso 1 calc R . . 
C2C C 0.7044(3) 0.9227(3) 0.8261(3) 0.0241(6) Uani 1 d . . . 
H2CA H 0.7886 0.9695 0.9049 0.029 Uiso 1 calc R . . 
H2CB H 0.7399 0.9442 0.7654 0.029 Uiso 1 calc R . . 
N3C N 0.5782(3) 0.9620(2) 0.8252(2) 0.0211(5) Uani 1 d . . . 
C4C C 0.5955(3) 1.0674(3) 0.9023(2) 0.0214(6) Uani 1 d . . . 
C5C C 0.4505(3) 1.0908(3) 0.8910(2) 0.0242(6) Uani 1 d . . . 
O6C O 0.3305(2) 0.9975(2) 0.81589(18) 0.0268(5) Uani 1 d . . . 
O7C O 0.4602(3) 1.1958(2) 0.9553(2) 0.0412(6) Uani 1 d . . . 
C8C C 0.7390(4) 1.1669(3) 0.9997(3) 0.0324(7) Uani 1 d . . . 
H8CA H 0.8221 1.1399 0.9966 0.049 Uiso 1 calc R . . 
H8CB H 0.7318 1.1745 1.0767 0.049 Uiso 1 calc R . . 
H8CC H 0.7569 1.2516 0.9896 0.049 Uiso 1 calc R . . 
C1M C 0.2128(5) 1.2396(3) 0.6830(3) 0.0445(9) Uani 1 d D . . 
H1MA H 0.2884 1.2877 0.6589 0.067 Uiso 1 calc R . . 
H1MB H 0.2611 1.2455 0.7651 0.067 Uiso 1 calc R . . 
H1MC H 0.1362 1.2775 0.6779 0.067 Uiso 1 calc R . . 
O1M O 0.1447(2) 1.1069(2) 0.60678(19) 0.0276(5) Uani 1 d D . . 
H1MO H 0.211(3) 1.077(3) 0.609(4) 0.058(13) Uiso 1 d D . . 
C2M C 0.0756(4) 1.1190(4) 0.8835(3) 0.0367(7) Uani 1 d D . . 
H2MA H 0.1213 1.1317 0.9678 0.055 Uiso 1 calc R . . 
H2MB H -0.0233 1.1245 0.8658 0.055 Uiso 1 calc R . . 
H2MC H 0.1398 1.1870 0.8659 0.055 Uiso 1 calc R . . 
O2M O 0.0597(3) 0.9946(2) 0.8129(2) 0.0352(5) Uani 1 d D . . 
H2MO H 0.144(3) 0.994(3) 0.820(4) 0.060(14) Uiso 1 d D . . 
C3M C 0.165(3) 0.440(3) 0.081(2) 0.132(9) Uiso 0.33 d PD A 1 
O3M O 0.0611(19) 0.4664(17) 0.0028(15) 0.118(5) Uiso 0.33 d PD . 1 
C4M C 0.322(2) 0.480(2) 0.0359(19) 0.092(5) Uiso 0.33 d PD B 2 
O4M O 0.4435(19) 0.4621(18) 0.0041(17) 0.127(6) Uiso 0.33 d PD . 2 
C5M C 0.282(3) 0.549(4) 0.009(3) 0.160(12) Uiso 0.33 d PD C 3 
O5M O 0.426(2) 0.5769(19) 0.1034(17) 0.129(6) Uiso 0.33 d PD C 3 

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 
Mn 0.0198(2) 0.0181(2) 0.0212(2) 0.00469(17) 0.00773(18) 0.01046(18) 
Na 0.0268(6) 0.0280(6) 0.0289(6) 0.0104(5) 0.0117(5) 0.0166(5) 
N 0.0207(12) 0.0183(11) 0.0228(12) 0.0048(9) 0.0077(10) 0.0099(9) 
C1A 0.0242(14) 0.0165(13) 0.0286(15) 0.0064(11) 0.0087(12) 0.0106(11) 
C2A 0.0235(14) 0.0199(13) 0.0282(15) 0.0086(12) 0.0100(12) 0.0111(11) 
N3A 0.0227(12) 0.0164(11) 0.0210(11) 0.0053(9) 0.0083(9) 0.0092(9) 
C4A 0.0223(14) 0.0226(14) 0.0256(14) 0.0051(12) 0.0098(12) 0.0087(12) 
C5A 0.0222(15) 0.0266(15) 0.0244(14) 0.0035(12) 0.0072(12) 0.0124(12) 
O6A 0.0216(10) 0.0232(10) 0.0309(11) 0.0096(9) 0.0101(9) 0.0109(8) 
O7A 0.0220(11) 0.0447(14) 0.0504(14) 0.0203(12) 0.0133(10) 0.0161(10) 
C8A 0.0262(17) 0.0403(19) 0.060(2) 0.0275(18) 0.0153(16) 0.0108(15) 
C1B 0.0248(14) 0.0222(14) 0.0290(15) 0.0058(12) 0.0136(12) 0.0147(12) 
C2B 0.0345(16) 0.0253(14) 0.0253(14) 0.0062(12) 0.0140(13) 0.0199(13) 
N3B 0.0242(12) 0.0217(12) 0.0233(12) 0.0071(10) 0.0101(10) 0.0130(10) 
C4B 0.0191(13) 0.0230(14) 0.0231(14) 0.0067(11) 0.0089(11) 0.0080(11) 
C5B 0.0177(13) 0.0235(14) 0.0296(15) 0.0106(12) 0.0113(11) 0.0090(11) 
O6B 0.0254(10) 0.0232(10) 0.0252(10) 0.0072(8) 0.0089(8) 0.0133(8) 
O7B 0.0338(12) 0.0387(12) 0.0311(11) 0.0189(10) 0.0166(10) 0.0240(10) 
C8B 0.0397(18) 0.0324(16) 0.0247(15) 0.0114(13) 0.0141(13) 0.0179(14) 
C1C 0.0201(14) 0.0234(14) 0.0280(15) 0.0067(12) 0.0059(12) 0.0130(12) 
C2C 0.0193(14) 0.0221(14) 0.0278(15) 0.0059(12) 0.0067(11) 0.0089(11) 
N3C 0.0239(12) 0.0159(11) 0.0253(12) 0.0083(10) 0.0099(10) 0.0089(9) 
C4C 0.0268(15) 0.0182(13) 0.0208(13) 0.0090(11) 0.0107(11) 0.0076(11) 
C5C 0.0327(16) 0.0236(14) 0.0199(13) 0.0078(12) 0.0113(12) 0.0146(13) 
O6C 0.0263(11) 0.0239(10) 0.0299(11) 0.0044(9) 0.0109(9) 0.0137(9) 
O7C 0.0425(14) 0.0333(13) 0.0364(13) -0.0056(10) 0.0076(11) 0.0224(11) 
C8C 0.0317(17) 0.0262(15) 0.0303(16) 0.0013(13) 0.0106(13) 0.0074(13) 
C1M 0.057(2) 0.0248(17) 0.045(2) 0.0032(15) 0.0187(18) 0.0148(16) 
O1M 0.0276(11) 0.0226(10) 0.0310(11) 0.0050(9) 0.0093(9) 0.0135(9) 
C2M 0.0283(16) 0.045(2) 0.0351(17) 0.0098(15) 0.0115(14) 0.0166(15) 
O2M 0.0280(12) 0.0443(14) 0.0342(12) 0.0095(10) 0.0118(10) 0.0192(11) 

_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 
Mn O6A 2.234(2) . y 
Mn O6C 2.244(2) . y 
Mn O6B 2.258(2) . y 
Mn N3A 2.260(2) . y 
Mn N3C 2.263(3) . y 
Mn N3B 2.274(2) . y 
Na O7B 2.348(2) 2_576 y 
Na O2M 2.385(3) . y 
Na O1M 2.390(3) . y 
Na O6A 2.398(2) . y 
Na O1M 2.408(3) 2_576 y 
Na O7A 2.686(3) . y 
Na C5A 2.803(3) . y 
Na Na 3.628(3) 2_576 y 
N C1A 1.468(4) . ? 
N C1B 1.469(4) . ? 
N C1C 1.476(4) . ? 
C1A C2A 1.529(4) . ? 
C2A N3A 1.465(3) . ? 
N3A C4A 1.272(4) . ? 
C4A C8A 1.496(4) . ? 
C4A C5A 1.538(4) . ? 
C5A O7A 1.239(4) . ? 
C5A O6A 1.265(4) . ? 
C1B C2B 1.526(4) . ? 
C2B N3B 1.462(4) . ? 
N3B C4B 1.270(4) . ? 
C4B C8B 1.498(4) . ? 
C4B C5B 1.532(4) . ? 
C5B O7B 1.235(4) . ? 
C5B O6B 1.272(4) . ? 
O7B Na 2.348(2) 2_576 ? 
C1C C2C 1.525(4) . ? 
C2C N3C 1.462(4) . ? 
N3C C4C 1.278(4) . ? 
C4C C8C 1.496(4) . ? 
C4C C5C 1.533(4) . ? 
C5C O7C 1.232(4) . ? 
C5C O6C 1.266(4) . ? 
C1M O1M 1.416(4) . ? 
O1M Na 2.408(3) 2_576 ? 
C2M O2M 1.417(4) . ? 
C3M O3M 1.37(2) . ? 
O3M O3M 1.62(3) 2_565 ? 
C4M O4M 1.45(2) . ? 
O4M O4M 1.27(3) 2_665 ? 
C5M O5M 1.47(2) . ? 

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 
O6A Mn O6C 81.58(9) . . y 
O6A Mn O6B 79.48(8) . . y 
O6C Mn O6B 82.66(8) . . y 
O6A Mn N3A 71.39(9) . . y 
O6C Mn N3A 100.34(9) . . y 
O6B Mn N3A 149.82(8) . . y 
O6A Mn N3C 152.35(8) . . y 
O6C Mn N3C 71.03(9) . . y 
O6B Mn N3C 100.18(9) . . y 
N3A Mn N3C 109.24(9) . . y 
O6A Mn N3B 95.66(9) . . y 
O6C Mn N3B 153.09(8) . . y 
O6B Mn N3B 70.55(8) . . y 
N3A Mn N3B 104.11(9) . . y 
N3C Mn N3B 110.43(9) . . y 
O7B Na O2M 91.88(9) 2_576 . y 
O7B Na O1M 98.94(9) 2_576 . y 
O2M Na O1M 90.38(10) . . y 
O7B Na O6A 169.47(9) 2_576 . y 
O2M Na O6A 89.09(9) . . y 
O1M Na O6A 91.53(9) . . y 
O7B Na O1M 82.89(8) 2_576 2_576 y 
O2M Na O1M 169.75(9) . 2_576 y 
O1M Na O1M 81.77(10) . 2_576 y 
O6A Na O1M 97.66(9) . 2_576 y 
O7B Na O7A 117.89(9) 2_576 . y 
O2M Na O7A 90.72(10) . . y 
O1M Na O7A 143.09(9) . . y 
O6A Na O7A 51.60(7) . . y 
O1M Na O7A 99.52(10) 2_576 . y 
O7B Na C5A 143.05(10) 2_576 . ? 
O2M Na C5A 84.37(10) . . ? 
O1M Na C5A 117.78(9) . . ? 
O1M Na C5A 105.10(10) 2_576 . ? 
O7B Na Na 91.16(7) 2_576 2_576 ? 
O2M Na Na 131.11(9) . 2_576 ? 
O6A Na Na 96.10(7) . 2_576 ? 
O7A Na Na 129.54(8) . 2_576 ? 
C5A Na Na 118.69(8) . 2_576 ? 
C1A N C1B 112.5(2) . . ? 
C1A N C1C 111.0(2) . . ? 
C1B N C1C 111.3(2) . . ? 
N C1A C2A 110.7(2) . . ? 
N3A C2A C1A 107.5(2) . . ? 
C4A N3A C2A 122.7(2) . . ? 
C4A N3A Mn 118.42(19) . . ? 
C2A N3A Mn 118.84(18) . . ? 
N3A C4A C8A 127.3(3) . . ? 
N3A C4A C5A 114.8(3) . . ? 
C8A C4A C5A 117.9(3) . . ? 
O7A C5A O6A 125.8(3) . . ? 
O7A C5A C4A 118.5(3) . . ? 
O6A C5A C4A 115.8(2) . . ? 
O7A C5A Na 71.77(18) . . ? 
O6A C5A Na 58.51(15) . . ? 
C4A C5A Na 155.6(2) . . ? 
C5A O6A Mn 118.84(18) . . ? 
C5A O6A Na 94.77(17) . . ? 
Mn O6A Na 131.24(10) . . ? 
C5A O7A Na 82.26(19) . . ? 
N C1B C2B 110.8(2) . . ? 
N3B C2B C1B 107.5(2) . . ? 
C4B N3B C2B 121.9(2) . . ? 
C4B N3B Mn 116.72(19) . . ? 
C2B N3B Mn 121.08(18) . . ? 
N3B C4B C8B 126.9(3) . . ? 
N3B C4B C5B 114.7(2) . . ? 
C8B C4B C5B 118.3(2) . . ? 
O7B C5B O6B 126.6(3) . . ? 
O7B C5B C4B 118.1(3) . . ? 
O6B C5B C4B 115.3(2) . . ? 
C5B O6B Mn 114.70(18) . . ? 
C5B O7B Na 129.52(19) . 2_576 ? 
N C1C C2C 111.0(2) . . ? 
N3C C2C C1C 108.0(2) . . ? 
C4C N3C C2C 121.6(2) . . ? 
C4C N3C Mn 117.6(2) . . ? 
C2C N3C Mn 120.48(18) . . ? 
N3C C4C C8C 127.3(3) . . ? 
N3C C4C C5C 114.7(3) . . ? 
C8C C4C C5C 118.0(2) . . ? 
O7C C5C O6C 126.2(3) . . ? 
O7C C5C C4C 118.2(3) . . ? 
O6C C5C C4C 115.6(2) . . ? 
C5C O6C Mn 117.21(18) . . ? 
C1M O1M Na 131.9(2) . . ? 
C1M O1M Na 113.8(2) . 2_576 ? 
Na O1M Na 98.23(10) . 2_576 ? 
C2M O2M Na 120.6(2) . . ? 
C3M O3M O3M 141(2) . 2_565 ? 
O4M O4M C4M 134(2) 2_665 . ? 

_diffrn_measured_fraction_theta_max    0.995 
_diffrn_reflns_theta_full              25.05 
_diffrn_measured_fraction_theta_full   0.995 
_refine_diff_density_max    0.85
_refine_diff_density_min   -0.53 
_refine_diff_density_rms    0.08 

#===END


data_4

_database_code_CSD	171267

# Code MNHTRA 

_refine_special_details
;
O2W, O2W' and O2W" represent disorder of a water molecule over three
sites: a similarity restraint was applied to the three corresponding
Na---O distances. All solvent water molecules were refined at half
occupancy.
;

_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum            'C30 H62 Mn2 N8 Na2 O22' 
_chemical_formula_weight          1042.74 

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'H'  'H'   0.0000   0.0000 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Na'  'Na'   0.0362   0.0249 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'Mn'  'Mn'   0.3368   0.7283 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1

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

_cell_length_a                    10.062(4) 
_cell_length_b                    11.572(4) 
_cell_length_c                    12.334(10) 
_cell_angle_alpha                 65.02(4) 
_cell_angle_beta                  66.08(4) 
_cell_angle_gamma                 71.21(3) 
_cell_volume                      1170.1(11) 
_cell_formula_units_Z             1
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     19 
_cell_measurement_theta_min       12.5
_cell_measurement_theta_max       13.85

_exptl_crystal_description        'irregular block' 
_exptl_crystal_colour             colourless
_exptl_crystal_size_max           0.67 
_exptl_crystal_size_mid           0.54 
_exptl_crystal_size_min           0.43 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.480 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              546 
_exptl_absorpt_coefficient_mu     0.643 
_exptl_absorpt_correction_type    none
_exptl_absorpt_correction_T_min   ?
_exptl_absorpt_correction_T_max   ?


_diffrn_ambient_temperature       150(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   'Stoe Stadi-4 four-circle'
_diffrn_measurement_method        omega-theta
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          2
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             4691 
_diffrn_reflns_av_R_equivalents   0.0330 
_diffrn_reflns_av_sigmaI/netI     0.0124 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        13 
_diffrn_reflns_limit_l_min        -9 
_diffrn_reflns_limit_l_max        14 
_diffrn_reflns_theta_min          2.71 
_diffrn_reflns_theta_max          25.06 
_reflns_number_total              4001 
_reflns_number_gt                 3589 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'STADI-4 (Stoe & Cie, 1996a)'
_computing_cell_refinement        'STADI-4 (Stoe & Cie, 1996a)' 
_computing_data_reduction         'X-RED (Stoe & Cie, 1996b)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 


_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0880P)^2^+2.8778P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'direct methods'
_atom_sites_solution_secondary    'difference Fourier synthesis'
_atom_sites_solution_hydrogens     
'Me Hs found in delta-F, water Hs not located, others placed geometrically'
_refine_ls_hydrogen_treatment     'riding model' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          4001 
_refine_ls_number_parameters      321 
_refine_ls_number_restraints      4 
_refine_ls_R_factor_all           0.0679 
_refine_ls_R_factor_gt            0.0605 
_refine_ls_wR_factor_ref          0.1697 
_refine_ls_wR_factor_gt           0.1589 
_refine_ls_goodness_of_fit_ref    1.060 
_refine_ls_restrained_S_all       1.061 
_refine_ls_shift/su_max           0.069 
_refine_ls_shift/su_mean          0.001 

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_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Mn Mn 0.71881(6) 0.65675(5) 0.67334(5) 0.0300(2) Uani 1 d . . . 
Na Na 0.56919(19) 0.47864(16) 0.61457(16) 0.0451(4) Uani 1 d D . . 
N N 0.8311(3) 0.7931(3) 0.7229(3) 0.0334(7) Uani 1 d . . . 
C1A C 0.9786(4) 0.8037(4) 0.6311(4) 0.0406(9) Uani 1 d . . . 
H1AA H 1.0481 0.7221 0.6563 0.049 Uiso 1 calc R . . 
H1AB H 1.0136 0.8749 0.6302 0.049 Uiso 1 calc R . . 
C2A C 0.9781(4) 0.8301(4) 0.4986(4) 0.0365(9) Uani 1 d . . . 
H2AA H 0.9209 0.9176 0.4673 0.044 Uiso 1 calc R . . 
H2AB H 1.0805 0.8263 0.4400 0.044 Uiso 1 calc R . . 
N3A N 0.9107(3) 0.7315(3) 0.5052(3) 0.0299(7) Uani 1 d . . . 
C4A C 0.9499(4) 0.6944(3) 0.4113(3) 0.0288(7) Uani 1 d . . . 
C5A C 0.8770(4) 0.5838(3) 0.4371(4) 0.0312(8) Uani 1 d . . . 
O6A O 0.8099(3) 0.5282(2) 0.5501(2) 0.0322(6) Uani 1 d . . . 
O7A O 0.8914(3) 0.5558(3) 0.3456(3) 0.0410(7) Uani 1 d . . . 
C8A C 1.0542(4) 0.7490(4) 0.2857(4) 0.0386(9) Uani 1 d . . . 
H8A1 H 1.0154 0.8409 0.2487 0.058 Uiso 1 calc R . . 
H8A2 H 1.0662 0.7022 0.2310 0.058 Uiso 1 calc R . . 
H8A3 H 1.1502 0.7399 0.2940 0.058 Uiso 1 calc R . . 
C1C C 0.8405(5) 0.7262(4) 0.8515(4) 0.0437(10) Uani 1 d . . . 
H1CA H 0.7440 0.7474 0.9125 0.052 Uiso 1 calc R . . 
H1CB H 0.9156 0.7568 0.8603 0.052 Uiso 1 calc R . . 
C2C C 0.8822(5) 0.5796(4) 0.8809(4) 0.0422(10) Uani 1 d . . . 
H2CA H 0.9846 0.5563 0.8286 0.051 Uiso 1 calc R . . 
H2CB H 0.8764 0.5353 0.9707 0.051 Uiso 1 calc R . . 
N3C N 0.7790(4) 0.5398(3) 0.8536(3) 0.0343(7) Uani 1 d . . . 
C4C C 0.7206(4) 0.4409(3) 0.9276(3) 0.0324(8) Uani 1 d . . . 
C5C C 0.6109(4) 0.4159(3) 0.8873(3) 0.0332(8) Uani 1 d . . . 
O6C O 0.5840(3) 0.4995(3) 0.7897(3) 0.0379(6) Uani 1 d . . . 
O7C O 0.5576(4) 0.3151(3) 0.9523(3) 0.0480(7) Uani 1 d . . . 
C8C C 0.7489(5) 0.3490(5) 1.0492(4) 0.0501(11) Uani 1 d . . . 
H8C1 H 0.8556 0.3196 1.0343 0.075 Uiso 1 calc R . . 
H8C2 H 0.7015 0.2740 1.0812 0.075 Uiso 1 calc R . . 
H8C3 H 0.7080 0.3934 1.1113 0.075 Uiso 1 calc R . . 
C1B C 0.7344(5) 0.9216(4) 0.7123(4) 0.0398(9) Uani 1 d . . . 
H1BA H 0.7585 0.9784 0.6229 0.048 Uiso 1 calc R . . 
H1BB H 0.7517 0.9621 0.7606 0.048 Uiso 1 calc R . . 
C2B C 0.5732(4) 0.9081(4) 0.7625(4) 0.0382(9) Uani 1 d . . . 
H2BA H 0.5457 0.8585 0.8540 0.046 Uiso 1 calc R . . 
H2BB H 0.5091 0.9948 0.7495 0.046 Uiso 1 calc R . . 
N3B N 0.5533(3) 0.8404(3) 0.6954(3) 0.0329(7) Uani 1 d . . . 
C4B C 0.4416(4) 0.8748(4) 0.6570(4) 0.0356(9) Uani 1 d . . . 
C5B C 0.4439(4) 0.7963(4) 0.5830(4) 0.0388(9) Uani 1 d . . . 
O6B O 0.5558(3) 0.7098(3) 0.5655(3) 0.0378(6) Uani 1 d . . . 
O7B O 0.3358(3) 0.8234(3) 0.5455(3) 0.0517(8) Uani 1 d . . . 
C8B C 0.3124(5) 0.9817(4) 0.6785(5) 0.0523(12) Uani 1 d . . . 
H8B1 H 0.2400 0.9489 0.7610 0.078 Uiso 1 calc R . . 
H8B2 H 0.2662 1.0127 0.6125 0.078 Uiso 1 calc R . . 
H8B3 H 0.3465 1.0533 0.6762 0.078 Uiso 1 calc R . . 
O1W O 0.3388(4) 0.5574(4) 0.5881(4) 0.0677(11) Uani 1 d . . . 
O2W O 0.6263(9) 0.2470(5) 0.6609(6) 0.039(2) Uiso 0.469(14) d PD A 1 
O2W' O 0.5438(14) 0.2506(8) 0.6992(10) 0.054(4) Uiso 0.365(15) d PD A 2 
O2W" O 0.4382(18) 0.3187(15) 0.7926(14) 0.044(6) Uiso 0.166(10) d PD A 3 
O3W O 0.9079(12) 0.9512(7) 0.9742(8) 0.135(4) Uani 0.855(14) d P B 1 
O3W' O 0.783(2) 1.020(2) 0.9913(18) 0.039(8) Uiso 0.145(14) d P B 2 
O4W O 0.6273(10) 0.0784(6) 0.9212(5) 0.068(2) Uani 0.50 d P . . 
O5W O 0.8671(8) 0.7069(10) 0.1106(9) 0.051(2) Uani 0.50 d P . . 
O6W O 0.781(2) 0.7267(12) 0.1486(11) 0.116(5) Uani 0.50 d P . . 
O7W O 0.4299(13) 0.1762(12) 0.8969(11) 0.108(3) Uani 0.50 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 
Mn 0.0305(3) 0.0256(3) 0.0352(3) 0.0008(2) -0.0184(2) -0.0114(2) 
Na 0.0518(10) 0.0432(9) 0.0514(10) -0.0013(7) -0.0298(8) -0.0249(7) 
N 0.0337(16) 0.0285(15) 0.0413(17) -0.0051(13) -0.0203(14) -0.0078(13) 
C1A 0.036(2) 0.034(2) 0.061(3) -0.0153(18) -0.0224(19) -0.0106(16) 
C2A 0.0328(19) 0.0285(18) 0.050(2) -0.0093(17) -0.0109(17) -0.0162(15) 
N3A 0.0287(15) 0.0245(14) 0.0376(17) -0.0025(12) -0.0155(13) -0.0103(12) 
C4A 0.0284(17) 0.0244(17) 0.0341(18) -0.0025(14) -0.0189(15) -0.0037(13) 
C5A 0.0314(18) 0.0239(17) 0.041(2) -0.0015(15) -0.0243(16) -0.0041(14) 
O6A 0.0358(14) 0.0246(12) 0.0422(15) -0.0048(11) -0.0214(12) -0.0099(10) 
O7A 0.0449(16) 0.0447(16) 0.0454(16) -0.0132(13) -0.0241(13) -0.0128(13) 
C8A 0.038(2) 0.036(2) 0.038(2) -0.0056(16) -0.0130(17) -0.0107(16) 
C1C 0.053(2) 0.040(2) 0.051(2) -0.0112(19) -0.033(2) -0.0077(18) 
C2C 0.050(2) 0.037(2) 0.047(2) -0.0038(18) -0.032(2) -0.0093(18) 
N3C 0.0363(17) 0.0280(15) 0.0394(17) -0.0050(13) -0.0206(14) -0.0041(13) 
C4C 0.0314(19) 0.0266(18) 0.0295(18) -0.0041(15) -0.0095(15) -0.0008(14) 
C5C 0.0320(18) 0.0267(18) 0.0328(19) -0.0084(15) -0.0027(15) -0.0071(14) 
O6C 0.0392(15) 0.0346(14) 0.0392(15) 0.0016(12) -0.0178(12) -0.0180(11) 
O7C 0.0583(19) 0.0334(15) 0.0459(16) 0.0000(13) -0.0137(14) -0.0223(13) 
C8C 0.056(3) 0.048(2) 0.035(2) 0.0052(19) -0.0199(19) -0.014(2) 
C1B 0.044(2) 0.0304(19) 0.050(2) -0.0102(17) -0.0214(19) -0.0093(16) 
C2B 0.037(2) 0.034(2) 0.043(2) -0.0107(17) -0.0165(17) -0.0042(16) 
N3B 0.0318(16) 0.0302(15) 0.0344(16) -0.0006(13) -0.0146(13) -0.0113(13) 
C4B 0.0282(18) 0.0305(19) 0.039(2) 0.0031(15) -0.0136(16) -0.0110(15) 
C5B 0.035(2) 0.0291(18) 0.050(2) 0.0062(17) -0.0247(18) -0.0155(16) 
O6B 0.0369(14) 0.0318(14) 0.0502(16) -0.0029(12) -0.0276(12) -0.0100(11) 
O7B 0.0470(17) 0.0362(15) 0.083(2) -0.0034(15) -0.0468(17) -0.0092(13) 
C8B 0.036(2) 0.042(2) 0.073(3) -0.008(2) -0.027(2) -0.0015(18) 
O1W 0.0403(18) 0.072(2) 0.121(3) -0.053(2) -0.032(2) -0.0104(16) 
O3W 0.206(11) 0.072(4) 0.145(7) -0.004(4) -0.081(7) -0.058(6) 
O4W 0.133(7) 0.048(4) 0.023(3) -0.010(3) 0.004(3) -0.057(4) 
O5W 0.040(4) 0.065(5) 0.048(5) -0.021(4) -0.016(3) -0.006(3) 
O6W 0.225(17) 0.077(8) 0.061(7) 0.014(6) -0.075(10) -0.058(11) 
O7W 0.118(9) 0.113(8) 0.094(7) -0.028(6) -0.026(6) -0.044(7) 

_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 
Mn O6C 2.240(3) . ? 
Mn N3A 2.256(3) . ? 
Mn N3C 2.272(4) . ? 
Mn N3B 2.281(3) . ? 
Mn O6B 2.295(3) . ? 
Mn O6A 2.295(3) . ? 
Mn Na 3.3445(19) . ? 
Na O1W 2.305(4) . ? 
Na O6C 2.339(4) . ? 
Na O6A 2.403(3) . ? 
Na O2W" 2.404(13) . ? 
Na O2W 2.413(6) . ? 
Na O6B 2.451(3) . ? 
Na O1W 2.457(5) 2_666 ? 
Na O2W' 2.452(9) . ? 
Na Na 3.426(4) 2_666 ? 
N C1A 1.462(5) . ? 
N C1C 1.470(5) . ? 
N C1B 1.477(5) . ? 
C1A C2A 1.532(6) . ? 
C2A N3A 1.464(4) . ? 
N3A C4A 1.274(5) . ? 
C4A C8A 1.478(5) . ? 
C4A C5A 1.532(5) . ? 
C5A O7A 1.243(5) . ? 
C5A O6A 1.254(5) . ? 
C1C C2C 1.526(6) . ? 
C2C N3C 1.459(5) . ? 
N3C C4C 1.266(5) . ? 
C4C C8C 1.505(5) . ? 
C4C C5C 1.525(6) . ? 
C5C O7C 1.247(5) . ? 
C5C O6C 1.252(5) . ? 
C1B C2B 1.518(6) . ? 
C2B N3B 1.457(5) . ? 
N3B C4B 1.277(5) . ? 
C4B C8B 1.501(6) . ? 
C4B C5B 1.526(6) . ? 
C5B O7B 1.249(5) . ? 
C5B O6B 1.255(5) . ? 
O1W Na 2.457(5) 2_666 ? 
O2W" O7W 1.610(18) . ? 
O5W O6W 0.809(17) . ? 

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 
O6C Mn N3A 148.25(12) . . ? 
O6C Mn N3C 70.85(11) . . ? 
N3A Mn N3C 113.64(12) . . ? 
O6C Mn N3B 103.69(11) . . ? 
N3A Mn N3B 103.85(12) . . ? 
N3C Mn N3B 109.54(13) . . ? 
O6C Mn O6B 78.07(11) . . ? 
N3A Mn O6B 97.09(12) . . ? 
N3C Mn O6B 147.84(11) . . ? 
N3B Mn O6B 69.69(11) . . ? 
O6C Mn O6A 78.44(11) . . ? 
N3A Mn O6A 70.22(11) . . ? 
N3C Mn O6A 107.59(12) . . ? 
N3B Mn O6A 141.26(11) . . ? 
O6B Mn O6A 73.11(11) . . ? 
O1W Na O6C 114.29(15) . . ? 
O1W Na O6A 144.48(14) . . ? 
O6C Na O6A 74.40(11) . . ? 
O1W Na O2W" 81.1(4) . . ? 
O6C Na O2W" 75.3(4) . . ? 
O6A Na O2W" 133.2(4) . . ? 
O1W Na O2W 109.0(2) . . ? 
O6C Na O2W 102.91(17) . . ? 
O6A Na O2W 101.6(2) . . ? 
O2W" Na O2W 52.5(5) . . ? 
O1W Na O6B 80.87(12) . . ? 
O6C Na O6B 73.17(11) . . ? 
O6A Na O6B 68.54(10) . . ? 
O2W" Na O6B 132.8(4) . . ? 
O2W Na O6B 170.0(2) . . ? 
O1W Na O1W 88.04(15) . 2_666 ? 
O6C Na O1W 156.91(13) . 2_666 ? 
O6A Na O1W 83.98(12) . 2_666 ? 
O2W" Na O1W 116.0(4) . 2_666 ? 
O2W Na O1W 73.3(2) . 2_666 ? 
O6B Na O1W 106.60(14) . 2_666 ? 
O1W Na O2W' 94.5(3) . . ? 
O6C Na O2W' 100.3(2) . . ? 
O6A Na O2W' 118.6(3) . . ? 
O6B Na O2W' 169.2(3) . . ? 
O1W Na O2W' 82.8(3) 2_666 . ? 
O1W Na Na 45.79(12) . 2_666 ? 
O6C Na Na 159.47(13) . 2_666 ? 
O6A Na Na 118.19(11) . 2_666 ? 
O2W" Na Na 102.1(4) . 2_666 ? 
O2W Na Na 90.75(17) . 2_666 ? 
O6B Na Na 95.64(10) . 2_666 ? 
O2W' Na Na 87.8(2) . 2_666 ? 
Mn Na Na 136.08(8) . 2_666 ? 
C1A N C1C 110.5(3) . . ? 
C1A N C1B 111.5(3) . . ? 
C1C N C1B 110.4(3) . . ? 
N C1A C2A 111.3(3) . . ? 
N3A C2A C1A 108.3(3) . . ? 
C4A N3A C2A 120.7(3) . . ? 
C4A N3A Mn 118.0(2) . . ? 
C2A N3A Mn 121.0(3) . . ? 
N3A C4A C8A 125.9(3) . . ? 
N3A C4A C5A 114.0(3) . . ? 
C8A C4A C5A 120.1(3) . . ? 
O7A C5A O6A 126.0(3) . . ? 
O7A C5A C4A 117.7(3) . . ? 
O6A C5A C4A 116.3(3) . . ? 
C5A O6A Mn 114.1(2) . . ? 
C5A O6A Na 122.0(2) . . ? 
Mn O6A Na 90.74(11) . . ? 
N C1C C2C 110.9(3) . . ? 
N3C C2C C1C 108.0(3) . . ? 
C4C N3C C2C 122.1(3) . . ? 
C4C N3C Mn 118.1(3) . . ? 
C2C N3C Mn 119.9(2) . . ? 
N3C C4C C8C 126.3(4) . . ? 
N3C C4C C5C 115.3(3) . . ? 
C8C C4C C5C 118.3(3) . . ? 
O7C C5C O6C 126.1(4) . . ? 
O7C C5C C4C 117.9(3) . . ? 
O6C C5C C4C 116.0(3) . . ? 
C5C O6C Mn 119.2(2) . . ? 
C5C O6C Na 131.2(3) . . ? 
Mn O6C Na 93.80(12) . . ? 
N C1B C2B 110.3(3) . . ? 
N3B C2B C1B 108.4(3) . . ? 
C4B N3B C2B 122.4(3) . . ? 
C4B N3B Mn 119.2(3) . . ? 
C2B N3B Mn 118.2(2) . . ? 
N3B C4B C8B 126.5(4) . . ? 
N3B C4B C5B 114.8(3) . . ? 
C8B C4B C5B 118.8(3) . . ? 
O7B C5B O6B 126.1(4) . . ? 
O7B C5B C4B 117.7(4) . . ? 
O6B C5B C4B 116.2(3) . . ? 
C5B O6B Mn 118.7(3) . . ? 
C5B O6B Na 129.0(2) . . ? 
Mn O6B Na 89.55(10) . . ? 
Na O1W Na 91.96(15) . 2_666 ? 
O7W O2W" Na 152.8(11) . . ? 

_diffrn_measured_fraction_theta_max    0.965 
_diffrn_reflns_theta_full              25.06 
_diffrn_measured_fraction_theta_full   0.965 
_refine_diff_density_max    1.00 
_refine_diff_density_min   -0.73 
_refine_diff_density_rms    0.09 

#===END 


data_5

_database_code_CSD	171268

# Code NIN4PV 

_refine_special_details 
; 
Disorder was identified in the BF4- anions and in the arms of the tripodal
ligand. In both circumstances extensive similarity restraints were applied
to distances and angles.
Merohedral twinning was found to be present: it was accounted for using the
twin law (100/010/00-1) and the unequal components 0.577(7) and 0.423(7) 
were established by refinement.
; 



_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum            'C30 H42 B2 F8 N8 Na4 Ni2 O12' 
_chemical_formula_weight          1089.72 

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' 
'B'  'B'   0.0013   0.0007 
'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' 
'F'  'F'   0.0171   0.0103 
'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' 
'Ni'  'Ni'   0.3393   1.1124 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Trigonal 
_symmetry_space_group_name_H-M    P31c

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

_cell_length_a                    9.369(3) 
_cell_length_b                    9.369(3) 
_cell_length_c                    28.603(6) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 120.00 
_cell_volume                      2174.3(11) 
_cell_formula_units_Z             2 
_cell_measurement_temperature     150(2) 
_cell_measurement_reflns_used     54 
_cell_measurement_theta_min       14.05
_cell_measurement_theta_max       15.9

_exptl_crystal_description        'hexagonal plate' 
_exptl_crystal_colour             blue
_exptl_crystal_size_max           0.58 
_exptl_crystal_size_mid           0.44 
_exptl_crystal_size_min           0.29 
_exptl_crystal_density_meas       'not measured' 
_exptl_crystal_density_diffrn     1.664 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1112 
_exptl_absorpt_coefficient_mu     1.007 
_exptl_absorpt_correction_type    'psi scans' 
_exptl_absorpt_correction_T_min   0.593 
_exptl_absorpt_correction_T_max   0.759 

_exptl_special_details 
; 
? 
; 

_diffrn_ambient_temperature       150(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   'Stoe Stadi-4 four-circle' 
_diffrn_measurement_method        omega-theta 
_diffrn_detector_area_resol_mean  ? 
_diffrn_standards_number          3 
_diffrn_standards_interval_count  ? 
_diffrn_standards_interval_time   60 
_diffrn_standards_decay_%         5.5 
_diffrn_reflns_number             4781 
_diffrn_reflns_av_R_equivalents   0.1106 
_diffrn_reflns_av_sigmaI/netI     0.0643 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -9 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        0 
_diffrn_reflns_limit_l_max        34 
_diffrn_reflns_theta_min          2.61 
_diffrn_reflns_theta_max          25.01 
_reflns_number_total              1284 
_reflns_number_gt                 1111 
_reflns_threshold_expression      >2sigma(I) 

_computing_data_collection        'STADI-4 (Stoe & Cie, 1996a)' 
_computing_cell_refinement        'STADI-4 (Stoe & Cie, 1996a)' 
_computing_data_reduction         'X-RED (Stoe & Cie, 1996b)' 
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'SHELXTL/PC (Sheldrick, 1994)' 
_computing_publication_material   'SHELXL-97 (Sheldrick, 1997)' 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.1128P)^2^+3.7435P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      'direct methods'
_atom_sites_solution_secondary    'difference Fourier synthesis'
_atom_sites_solution_hydrogens    
'Me Hs found in delta-F, -CH2- placed geometrically'
_refine_ls_hydrogen_treatment     'riding model' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_abs_structure_details 
'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.07(8) 
_refine_ls_number_reflns          1284 
_refine_ls_number_parameters      198 
_refine_ls_number_restraints      16 
_refine_ls_R_factor_all           0.0801 
_refine_ls_R_factor_gt            0.0694 
_refine_ls_wR_factor_ref          0.1885 
_refine_ls_wR_factor_gt           0.1749 
_refine_ls_goodness_of_fit_ref    1.056 
_refine_ls_restrained_S_all       1.050 
_refine_ls_shift/su_max           0.007 
_refine_ls_shift/su_mean          0.001 

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_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_assembly 
_atom_site_disorder_group 
Ni1 Ni 0.0000 1.0000 0.03694(9) 0.0333(6) Uani 1 d S . . 
Ni2 Ni -0.3333 0.3333 0.24041(8) 0.0414(8) Uani 1 d S . . 
Na1 Na 0.0000 1.0000 0.1457(3) 0.033(2) Uani 1 d S . . 
Na2 Na -0.3591(19) 0.536(3) 0.1319(5) 0.054(4) Uiso 0.58(4) d P . 1 
Na2' Na -0.3566(19) 0.588(3) 0.1270(5) 0.035(5) Uiso 0.42(4) d P . 2 
N0A N 0.0000 1.0000 -0.0732(7) 0.027(4) Uani 1 d S . . 
C1A C 0.0602(19) 0.885(2) -0.0799(5) 0.035(3) Uani 1 d . . . 
H1A1 H 0.1303 0.9172 -0.1082 0.042 Uiso 1 calc R . . 
H1A2 H -0.0347 0.7733 -0.0851 0.042 Uiso 1 calc R . . 
C2A C 0.157(2) 0.882(2) -0.0392(4) 0.040(4) Uani 1 d . . . 
H2A1 H 0.1909 0.7992 -0.0450 0.047 Uiso 1 calc R . . 
H2A2 H 0.2579 0.9910 -0.0363 0.047 Uiso 1 calc R . . 
N3A N 0.0665(15) 0.8433(15) 0.0042(5) 0.034(3) Uani 1 d . . . 
C4A C 0.011(2) 0.703(2) 0.0252(6) 0.039(4) Uani 1 d . . . 
C5A C -0.092(2) 0.677(2) 0.0686(5) 0.045(4) Uani 1 d . . . 
O6A O -0.1226(18) 0.7928(16) 0.0783(3) 0.049(3) Uani 1 d . . . 
O7A O -0.1371(18) 0.5465(17) 0.0900(4) 0.057(3) Uani 1 d . . . 
C8A C 0.032(3) 0.560(3) 0.0091(6) 0.061(6) Uani 1 d . . . 
H8A1 H 0.0282 0.5542 -0.0251 0.091 Uiso 1 calc R . . 
H8A2 H -0.0564 0.4569 0.0221 0.091 Uiso 1 calc R . . 
H8A3 H 0.1389 0.5773 0.0199 0.091 Uiso 1 calc R . . 
N0B N -0.3333 0.3333 0.3482(6) 0.021(3) Uani 1 d S . . 
C1B C -0.1598(17) 0.436(3) 0.3570(4) 0.038(4) Uani 1 d . . . 
H1B1 H -0.1288 0.3925 0.3843 0.045 Uiso 1 calc R . . 
H1B2 H -0.1366 0.5488 0.3649 0.045 Uiso 1 calc R . . 
C2B C -0.0561(18) 0.4455(18) 0.3158(5) 0.031(3) Uani 1 d . . . 
H2B1 H 0.0609 0.5268 0.3221 0.038 Uiso 1 calc R . . 
H2B2 H -0.0653 0.3367 0.3107 0.038 Uiso 1 calc R . . 
N3B N -0.1110(18) 0.4940(17) 0.2741(4) 0.040(3) Uani 1 d . . . 
C4B C -0.017(4) 0.633(3) 0.2559(13) 0.026(7) Uiso 0.58(4) d PD . 1 
C5B C -0.087(5) 0.665(3) 0.2120(9) 0.038(7) Uiso 0.58(4) d PD . 1 
O6B O -0.238(3) 0.556(3) 0.2029(6) 0.034(5) Uiso 0.58(4) d PD . 1 
O7B O -0.012(4) 0.796(2) 0.1899(7) 0.042(6) Uiso 0.58(4) d PD . 1 
C8B C 0.154(5) 0.762(4) 0.2677(13) 0.060(11) Uiso 0.58(4) d PD . 1 
H8B1 H 0.1567 0.8014 0.2997 0.090 Uiso 0.58(4) calc PR . 1 
H8B2 H 0.1902 0.8548 0.2458 0.090 Uiso 0.58(4) calc PR . 1 
H8B3 H 0.2274 0.7166 0.2653 0.090 Uiso 0.58(4) calc PR . 1 
C4B' C -0.053(7) 0.617(5) 0.2461(18) 0.053(17) Uiso 0.42(4) d PD . 2 
C5B' C -0.149(6) 0.639(4) 0.2066(10) 0.028(9) Uiso 0.42(4) d PD . 2 
O6B' O -0.274(4) 0.502(4) 0.1928(10) 0.048(9) Uiso 0.42(4) d PD . 2 
O7B' O -0.095(6) 0.771(3) 0.1856(8) 0.050(8) Uiso 0.42(4) d PD . 2 
C8B' C 0.101(7) 0.765(6) 0.2618(17) 0.059(14) Uiso 0.42(4) d PD . 2 
H8B4 H 0.0994 0.7748 0.2959 0.088 Uiso 0.42(4) calc PR . 2 
H8B5 H 0.1088 0.8639 0.2473 0.088 Uiso 0.42(4) calc PR . 2 
H8B6 H 0.1964 0.7554 0.2525 0.088 Uiso 0.42(4) calc PR . 2 
B1 B 0.3333 0.6667 0.4089(7) 0.036(5) Uani 1 d SD . . 
F1 F 0.3333 0.6667 0.3633(8) 0.142(13) Uani 1 d SD . . 
F2 F 0.240(3) 0.5117(18) 0.4180(9) 0.184(11) Uani 1 d D . . 
B2 B 0.3333 0.6667 0.1376(12) 0.062(9) Uani 1 d SD . . 
F3 F 0.3333 0.6667 0.0926(12) 0.26(3) Uani 1 d SD . . 
F4 F 0.456(3) 0.649(5) 0.1479(15) 0.28(2) Uani 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 
Ni1 0.0356(9) 0.0356(9) 0.0287(11) 0.000 0.000 0.0178(4) 
Ni2 0.0497(12) 0.0497(12) 0.0248(11) 0.000 0.000 0.0249(6) 
Na1 0.036(4) 0.036(4) 0.027(4) 0.000 0.000 0.0180(18) 
N0A 0.028(7) 0.028(7) 0.026(9) 0.000 0.000 0.014(3) 
C1A 0.030(8) 0.041(9) 0.037(6) -0.012(6) 0.004(6) 0.020(8) 
C2A 0.033(9) 0.064(12) 0.037(6) -0.018(8) -0.015(7) 0.036(9) 
N3A 0.026(7) 0.031(7) 0.044(6) 0.002(6) -0.008(5) 0.013(6) 
C4A 0.040(9) 0.032(8) 0.045(10) -0.003(7) -0.020(6) 0.018(7) 
C5A 0.048(10) 0.042(9) 0.036(7) 0.012(7) -0.007(7) 0.015(8) 
O6A 0.066(9) 0.051(7) 0.030(4) 0.004(4) -0.003(5) 0.029(7) 
O7A 0.067(8) 0.044(7) 0.048(6) 0.014(5) 0.023(6) 0.020(6) 
C8A 0.099(17) 0.051(11) 0.046(8) 0.006(7) 0.015(10) 0.048(11) 
N0B 0.012(5) 0.012(5) 0.038(8) 0.000 0.000 0.006(2) 
C1B 0.032(7) 0.051(11) 0.024(5) -0.005(7) -0.005(5) 0.016(7) 
C2B 0.023(6) 0.029(8) 0.040(6) 0.001(6) -0.002(5) 0.011(6) 
N3B 0.040(7) 0.042(8) 0.037(6) 0.010(5) 0.015(5) 0.019(6) 
B1 0.029(8) 0.029(8) 0.051(13) 0.000 0.000 0.014(4) 
F1 0.15(2) 0.15(2) 0.13(3) 0.000 0.000 0.075(10) 
F2 0.12(2) 0.046(8) 0.37(3) 0.045(13) -0.02(2) 0.031(13) 
B2 0.053(13) 0.053(13) 0.08(2) 0.000 0.000 0.026(6) 
F3 0.30(5) 0.30(5) 0.16(4) 0.000 0.000 0.15(3) 
F4 0.15(3) 0.24(3) 0.52(6) -0.21(4) -0.13(3) 0.15(3) 

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

loop_ 
_geom_bond_atom_site_label_1 
_geom_bond_atom_site_label_2 
_geom_bond_distance 
_geom_bond_site_symmetry_2 
_geom_bond_publ_flag 
Ni1 O6A 2.063(12) 3_465 ? 
Ni1 O6A 2.063(12) 2_675 ? 
Ni1 O6A 2.063(12) . y 
Ni1 N3A 2.082(14) 3_465 ? 
Ni1 N3A 2.082(14) 2_675 ? 
Ni1 N3A 2.082(14) . y 
Ni1 Na1 3.112(9) . ? 
Ni1 N0A 3.15(2) . y 
Ni2 O6B' 1.95(3) 3_455 ? 
Ni2 O6B' 1.95(3) 2_565 ? 
Ni2 O6B' 1.95(3) . y 
Ni2 N3B 2.098(15) 3_455 ? 
Ni2 N3B 2.098(15) . y 
Ni2 N3B 2.098(15) 2_565 ? 
Ni2 O6B 2.11(2) 3_455 ? 
Ni2 O6B 2.11(2) 2_565 ? 
Ni2 O6B 2.11(2) . y 
Ni2 N0B 3.084(18) . ? 
Na1 O7B' 2.19(2) 2_675 ? 
Na1 O7B' 2.19(2) 3_465 ? 
Na1 O7B' 2.19(2) . y 
Na1 O7B 2.25(2) 2_675 ? 
Na1 O7B 2.25(2) 3_465 ? 
Na1 O7B 2.25(2) . y 
Na1 O6A 2.564(14) . y 
Na1 O6A 2.564(13) 3_465 ? 
Na1 O6A 2.564(14) 2_675 ? 
Na1 Na2' 3.67(2) . ? 
Na1 Na2' 3.669(19) 3_465 ? 
Na2 O7A 2.27(2) 2_565 ? 
Na2 O6B 2.29(2) . y 
Na2 O7A 2.36(2) . y 
Na2 F4 2.48(3) 1_455 y 
Na2 O6A 2.78(2) . y 
Na2 C5A 2.83(2) . ? 
Na2 Na2 3.51(4) 2_565 ? 
Na2 Na2 3.51(4) 3_455 ? 
Na2' F4 2.18(3) 1_455 y 
Na2' O6B' 2.32(3) . y 
Na2' O7A 2.50(2) 2_565 y 
Na2' O6A 2.50(2) . y 
Na2' O7A 2.51(2) . y 
Na2' O7B' 2.75(4) . y 
Na2' C5A 2.75(2) . ? 
Na2' C5B' 2.88(4) . ? 
N0A C1A 1.455(14) 3_465 ? 
N0A C1A 1.455(14) 2_675 ? 
N0A C1A 1.455(14) . ? 
C1A C2A 1.484(19) . ? 
C2A N3A 1.444(19) . ? 
N3A C4A 1.29(2) . ? 
C4A C5A 1.51(3) . ? 
C4A C8A 1.52(3) . ? 
C5A O7A 1.24(2) . ? 
C5A O6A 1.29(2) . ? 
O7A Na2 2.27(2) 3_455 y 
O7A Na2' 2.50(2) 3_455 y 
N0B C1B 1.438(14) 3_455 ? 
N0B C1B 1.438(14) . ? 
N0B C1B 1.438(14) 2_565 ? 
C1B C2B 1.50(2) . ? 
C2B N3B 1.46(2) . ? 
N3B C4B 1.26(3) . ? 
N3B C4B' 1.28(4) . ? 
C4B C8B 1.48(5) . ? 
C4B C5B 1.52(4) . ? 
C5B O7B 1.24(3) . ? 
C5B O6B 1.29(4) . ? 
C4B' C8B' 1.49(5) . ? 
C4B' C5B' 1.52(4) . ? 
C5B' O7B' 1.24(3) . ? 
C5B' O6B' 1.29(4) . ? 
B1 F2 1.292(14) 3_565 ? 
B1 F2 1.292(14) . ? 
B1 F2 1.292(14) 2_665 ? 
B1 F1 1.305(19) . ? 
B2 F4 1.280(16) 2_665 ? 
B2 F4 1.280(16) 3_565 ? 
B2 F4 1.280(16) . ? 
B2 F3 1.29(2) . ? 
F4 Na2' 2.18(3) 1_655 ? 
F4 Na2 2.48(3) 1_655 ? 

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 
O6A Ni1 O6A 90.4(4) 3_465 2_675 ? 
O6A Ni1 O6A 90.4(4) 3_465 . y 
O6A Ni1 O6A 90.4(4) 2_675 . ? 
O6A Ni1 N3A 79.4(5) 3_465 3_465 ? 
O6A Ni1 N3A 169.7(5) 2_675 3_465 ? 
O6A Ni1 N3A 88.4(5) . 3_465 y 
O6A Ni1 N3A 88.4(5) 3_465 2_675 ? 
O6A Ni1 N3A 79.4(5) 2_675 2_675 ? 
O6A Ni1 N3A 169.7(5) . 2_675 y 
N3A Ni1 N3A 101.4(4) 3_465 2_675 ? 
O6A Ni1 N3A 169.7(5) 3_465 . ? 
O6A Ni1 N3A 88.4(5) 2_675 . ? 
O6A Ni1 N3A 79.4(5) . . y 
N3A Ni1 N3A 101.4(4) 3_465 . ? 
N3A Ni1 N3A 101.4(4) 2_675 . ? 
O6A Ni1 Na1 55.0(3) 3_465 . ? 
O6A Ni1 Na1 55.0(3) 2_675 . ? 
O6A Ni1 Na1 55.0(3) . . ? 
N3A Ni1 Na1 116.7(4) 3_465 . ? 
N3A Ni1 Na1 116.7(4) 2_675 . ? 
N3A Ni1 Na1 116.7(4) . . ? 
O6A Ni1 N0A 125.0(3) 3_465 . ? 
O6A Ni1 N0A 125.0(3) 2_675 . ? 
O6A Ni1 N0A 125.0(3) . . ? 
N3A Ni1 N0A 63.3(4) 3_465 . ? 
N3A Ni1 N0A 63.3(4) 2_675 . ? 
N3A Ni1 N0A 63.3(4) . . ? 
Na1 Ni1 N0A 180 . . ? 
O6B' Ni2 O6B' 76.5(17) 3_455 2_565 ? 
O6B' Ni2 O6B' 76.5(17) 3_455 . ? 
O6B' Ni2 O6B' 76.5(17) 2_565 . y 
O6B' Ni2 N3B 87.8(11) 3_455 3_455 ? 
O6B' Ni2 N3B 92.8(10) 2_565 3_455 ? 
O6B' Ni2 N3B 162.6(11) . 3_455 y 
O6B' Ni2 N3B 92.8(10) 3_455 . y 
O6B' Ni2 N3B 162.6(11) 2_565 . ? 
O6B' Ni2 N3B 87.8(11) . . y 
N3B Ni2 N3B 100.5(4) 3_455 . ? 
O6B' Ni2 N3B 162.6(11) 3_455 2_565 ? 
O6B' Ni2 N3B 87.8(11) 2_565 2_565 ? 
O6B' Ni2 N3B 92.8(10) . 2_565 ? 
N3B Ni2 N3B 100.5(4) 3_455 2_565 ? 
N3B Ni2 N3B 100.5(4) . 2_565 y 
N3B Ni2 O6B 75.3(8) 3_455 3_455 ? 
N3B Ni2 O6B 88.2(7) . 3_455 y 
N3B Ni2 O6B 170.9(7) 2_565 3_455 ? 
N3B Ni2 O6B 88.2(7) 3_455 2_565 ? 
N3B Ni2 O6B 170.9(6) . 2_565 ? 
N3B Ni2 O6B 75.3(8) 2_565 2_565 ? 
O6B Ni2 O6B 96.4(9) 3_455 2_565 ? 
N3B Ni2 O6B 170.9(6) 3_455 . ? 
N3B Ni2 O6B 75.3(8) . . ? 
N3B Ni2 O6B 88.2(7) 2_565 . ? 
O6B Ni2 O6B 96.4(9) 3_455 . ? 
O6B Ni2 O6B 96.4(9) 2_565 . ? 
O6B' Ni2 N0B 134.4(11) 3_455 . ? 
O6B' Ni2 N0B 134.4(11) 2_565 . ? 
O6B' Ni2 N0B 134.4(11) . . ? 
N3B Ni2 N0B 62.6(3) 3_455 . ? 
N3B Ni2 N0B 62.6(3) . . ? 
N3B Ni2 N0B 62.6(3) 2_565 . ? 
O6B Ni2 N0B 120.6(7) 3_455 . ? 
O6B Ni2 N0B 120.6(7) 2_565 . ? 
O6B Ni2 N0B 120.6(7) . . ? 
O7B' Na1 O7B' 95.3(9) 2_675 3_465 ? 
O7B' Na1 O7B' 95.3(9) 2_675 . ? 
O7B' Na1 O7B' 95.3(9) 3_465 . ? 
O7B' Na1 O7B 79.2(9) 3_465 2_675 ? 
O7B' Na1 O7B 105.0(9) . 2_675 ? 
O7B' Na1 O7B 105.0(9) 2_675 3_465 ? 
O7B' Na1 O7B 79.2(9) . 3_465 ? 
O7B  Na1 O7B 91.6(8) 2_675 3_465 ? 
O7B' Na1 O7B 79.2(9) 2_675 . ? 
O7B' Na1 O7B 105.0(9) 3_465 . ? 
O7B Na1 O7B 91.6(8) 2_675 . ? 
O7B Na1 O7B 91.6(8) 3_465 . ? 
O7B' Na1 O6A 140.0(12) 2_675 . ? 
O7B' Na1 O6A 124.7(11) 3_465 . ? 
O7B' Na1 O6A 80.9(8) . . ? 
O7B Na1 O6A 155.3(8) 2_675 . ? 
O7B Na1 O6A 113.1(7) 3_465 . ? 
O7B Na1 O6A 88.0(7) . . ? 
O7B' Na1 O6A 124.7(11) 2_675 3_465 ? 
O7B' Na1 O6A 80.9(8) 3_465 3_465 ? 
O7B' Na1 O6A 140.0(12) . 3_465 ? 
O7B Na1 O6A 113.1(7) 2_675 3_465 ? 
O7B Na1 O6A 88.0(6) 3_465 3_465 ? 
O7B Na1 O6A 155.3(8) . 3_465 ? 
O6A Na1 O6A 69.6(4) . 3_465 ? 
O7B' Na1 O6A 80.9(8) 2_675 2_675 ? 
O7B' Na1 O6A 140.0(12) 3_465 2_675 ? 
O7B' Na1 O6A 124.7(11) . 2_675 ? 
O7B Na1 O6A 88.0(7) 2_675 2_675 ? 
O7B Na1 O6A 155.3(8) 3_465 2_675 ? 
O7B Na1 O6A 113.1(7) . 2_675 ? 
O6A Na1 O6A 69.6(4) . 2_675 ? 
O6A Na1 O6A 69.6(4) 3_465 2_675 ? 
O7B' Na1 Ni1 121.4(7) 2_675 . ? 
O7B' Na1 Ni1 121.4(7) 3_465 . ? 
O7B' Na1 Ni1 121.4(7) . . ? 
O7B Na1 Ni1 124.1(6) 2_675 . ? 
O7B Na1 Ni1 124.1(6) 3_465 . ? 
O7B Na1 Ni1 124.1(6) . . ? 
O6A Na1 Ni1 41.2(3) . . ? 
O6A Na1 Ni1 41.2(3) 3_465 . ? 
O6A Na1 Ni1 41.2(3) 2_675 . ? 
O7B' Na1 Na2' 142.7(10) 2_675 . ? 
O7B' Na1 Na2' 95.7(12) 3_465 . ? 
O7B' Na1 Na2' 48.2(10) . . ? 
O7B Na1 Na2' 152.6(6) 2_675 . ? 
O7B Na1 Na2' 78.7(7) 3_465 . ? 
O7B Na1 Na2' 63.5(7) . . ? 
O6A Na1 Na2' 42.8(3) . . ? 
O6A Na1 Na2' 92.2(5) 3_465 . ? 
O6A Na1 Na2' 111.5(4) 2_675 . ? 
Ni1 Na1 Na2' 81.6(3) . . ? 
O7B' Na1 Na2' 95.7(12) 2_675 3_465 ? 
O7B' Na1 Na2' 48.2(10) 3_465 3_465 ? 
O7B' Na1 Na2' 142.7(10) . 3_465 ? 
O7B Na1 Na2' 78.7(7) 2_675 3_465 ? 
O7B Na1 Na2' 63.5(7) 3_465 3_465 ? 
O7B Na1 Na2' 152.6(6) . 3_465 ? 
O6A Na1 Na2' 111.5(4) . 3_465 ? 
O6A Na1 Na2' 42.8(3) 3_465 3_465 ? 
O6A Na1 Na2' 92.2(5) 2_675 3_465 ? 
Ni1 Na1 Na2' 81.6(3) . 3_465 ? 
Na2' Na1 Na2' 117.91(14) . 3_465 ? 
O7A Na2 O6B 132.2(16) 2_565 . ? 
O7A Na2 O7A 92.1(10) 2_565 . ? 
O6B Na2 O7A 93.3(8) . . ? 
O7A Na2 F4 95.5(10) 2_565 1_455 ? 
O6B Na2 F4 103.0(12) . 1_455 ? 
O7A Na2 F4 149.7(16) . 1_455 ? 
O7A Na2 O6A 114.5(7) 2_565 . ? 
O6B Na2 O6A 105.7(9) . . ? 
O7A Na2 O6A 51.6(6) . . ? 
F4 Na2 O6A 99.0(14) 1_455 . ? 
O7A Na2 C5A 100.8(7) 2_565 . ? 
O6B Na2 C5A 104.1(8) . . ? 
F4 Na2 C5A 124.2(15) 1_455 . ? 
O7A Na2 Na2 41.6(8) 2_565 2_565 ? 
O6B Na2 Na2 91.4(10) . 2_565 ? 
O7A Na2 Na2 87.0(6) . 2_565 ? 
F4 Na2 Na2 117.5(13) 1_455 2_565 ? 
O6A Na2 Na2 135.1(5) . 2_565 ? 
C5A Na2 Na2 109.6(6) . 2_565 ? 
O7A Na2 Na2 88.4(7) 2_565 3_455 ? 
O6B Na2 Na2 67.3(8) . 3_455 ? 
O7A Na2 Na2 39.6(7) . 3_455 ? 
F4 Na2 Na2 169.2(11) 1_455 3_455 ? 
O6A Na2 Na2 88.5(7) . 3_455 ? 
C5A Na2 Na2 64.5(7) . 3_455 ? 
Na2 Na2 Na2 60  2_565 3_455 ? 
O7A Na2 Na1 153.4(8) 2_565 . ? 
O6B Na2 Na1 73.0(9) . . ? 
O7A Na2 Na1 76.0(6) . . ? 
F4 Na2 Na1 84.5(11) 1_455 . ? 
O6A Na2 Na1 40.0(4) . . ? 
C5A Na2 Na1 59.0(5) . . ? 
Na2 Na2 Na1 155.9(6) 2_565 . ? 
Na2 Na2 Na1 96.5(6) 3_455 . ? 
F4 Na2' O6B' 108.5(14) 1_455 . ? 
F4 Na2' O7A 97.3(11) 1_455 2_565 ? 
O6B' Na2' O7A 100.5(16) . 2_565 ? 
F4 Na2' O6A 117.6(16) 1_455 . ? 
O6B' Na2' O6A 113.7(9) . . ? 
O7A Na2' O6A 116.9(7) 2_565 . ? 
F4 Na2' O7A 169.7(16) 1_455 . ? 
O6B' Na2' O7A 81.3(11) . . ? 
O7A Na2' O7A 83.4(9) 2_565 . ? 
O6A Na2' O7A 53.9(6) . . ? 
F4 Na2' O7B' 104.5(12) 1_455 . ? 
O6B' Na2' O7B' 51.4(9) . . ? 
O7A Na2' O7B' 148.7(11) 2_565 . ? 
O6A Na2' O7B' 72.1(8) . . ? 
O7A Na2' O7B' 79.1(9) . . ? 
F4 Na2' C5A 143.8(17) 1_455 . ? 
O6B' Na2' C5A 101.1(10) . . ? 
O7A Na2' C5A 97.3(7) 2_565 . ? 
O6A Na2' C5A 27.8(5) . . ? 
O7A Na2' C5A 26.7(5) . . ? 
O7B' Na2' C5A 78.1(9) . . ? 
F4 Na2' C5B' 107.8(13) 1_455 . ? 
O6B' Na2' C5B' 26.1(8) . . ? 
O7A Na2' C5B' 125.7(13) 2_565 . ? 
O6A Na2' C5B' 93.1(10) . . ? 
O7A Na2' C5B' 79.7(9) . . ? 
O7B' Na2' C5B' 25.3(7) . . ? 
C5A Na2' C5B' 89.9(9) . . ? 
F4 Na2' Na1 96.4(12) 1_455 . ? 
O6B' Na2' Na1 87.7(10) . . ? 
O7A Na2' Na1 160.8(6) 2_565 . ? 
O6A Na2' Na1 44.3(4) . . ? 
O7A Na2' Na1 80.7(5) . . ? 
O7B' Na2' Na1 36.4(5) . . ? 
C5A Na2' Na1 64.0(5) . . ? 
C5B' Na2' Na1 61.7(8) . . ? 
C1A N0A C1A 118.3(4) 3_465 2_675 ? 
C1A N0A C1A 118.3(4) 3_465 . ? 
C1A N0A C1A 118.3(4) 2_675 . ? 
C1A N0A Ni1 97.6(10) 3_465 . ? 
C1A N0A Ni1 97.6(10) 2_675 . ? 
C1A N0A Ni1 97.6(10) . . ? 
N0A C1A C2A 112.2(13) . . ? 
N3A C2A C1A 113.2(12) . . ? 
C4A N3A C2A 122.8(15) . . ? 
C4A N3A Ni1 113.4(12) . . ? 
C2A N3A Ni1 123.6(11) . . ? 
N3A C4A C5A 116.4(16) . . ? 
N3A C4A C8A 126.1(17) . . ? 
C5A C4A C8A 117.4(16) . . ? 
O7A C5A O6A 128.0(16) . . ? 
O7A C5A C4A 116.3(18) . . ? 
O6A C5A C4A 115.7(14) . . ? 
O7A C5A Na2' 65.6(11) . . ? 
O6A C5A Na2' 64.9(11) . . ? 
C4A C5A Na2' 162.0(12) . . ? 
O7A C5A Na2 55.6(11) . . ? 
O6A C5A Na2 74.7(11) . . ? 
C4A C5A Na2 160.8(12) . . ? 
C5A O6A Ni1 114.6(11) . . ? 
C5A O6A Na2' 87.3(11) . . ? 
Ni1 O6A Na2' 155.0(9) . . ? 
C5A O6A Na1 126.7(10) . . ? 
Ni1 O6A Na1 83.8(5) . . ? 
Na2' O6A Na1 93.0(5) . . ? 
C5A O6A Na2 78.8(10) . . ? 
Ni1 O6A Na2 163.6(9) . . ? 
Na1 O6A Na2 95.9(5) . . ? 
C5A O7A Na2 156.1(15) . 3_455 ? 
C5A O7A Na2 98.8(14) . . ? 
Na2 O7A Na2 98.8(13) 3_455 . ? 
C5A O7A Na2' 147.0(15) . 3_455 ? 
Na2 O7A Na2' 109.4(11) . 3_455 ? 
C5A O7A Na2' 87.7(13) . . ? 
Na2 O7A Na2' 109.4(12) 3_455 . ? 
Na2' O7A Na2' 119.8(12) 3_455 . ? 
C1B N0B C1B 117.0(5) 3_455 . ? 
C1B N0B C1B 117.0(5) 3_455 2_565 ? 
C1B N0B C1B 117.0(5) . 2_565 ? 
C1B N0B Ni2 100.1(9) 3_455 . ? 
C1B N0B Ni2 100.1(9) . . ? 
C1B N0B Ni2 100.1(9) 2_565 . ? 
N0B C1B C2B 112.5(12) . . ? 
N3B C2B C1B 109.9(12) . . ? 
C4B N3B C2B 119(2) . . ? 
C4B' N3B C2B 137(2) . . ? 
C4B N3B Ni2 118.7(19) . . ? 
C4B' N3B Ni2 100(2) . . ? 
C2B N3B Ni2 122.1(9) . . ? 
N3B C4B C8B 131(3) . . ? 
N3B C4B C5B 113(3) . . ? 
C8B C4B C5B 115(3) . . ? 
O7B C5B O6B 123(3) . . ? 
O7B C5B C4B 122(3) . . ? 
O6B C5B C4B 114.9(19) . . ? 
C5B O6B Ni2 116.0(15) . . ? 
C5B O6B Na2 123.0(16) . . ? 
Ni2 O6B Na2 115.0(16) . . ? 
C5B O7B Na1 153(3) . . ? 
N3B C4B' C8B' 115(4) . . ? 
N3B C4B' C5B' 125(4) . . ? 
C8B' C4B' C5B' 118(3) . . ? 
O7B' C5B' O6B' 124(3) . . ? 
O7B' C5B' C4B' 122(4) . . ? 
O6B' C5B' C4B' 114(2) . . ? 
O7B' C5B' Na2' 72(2) . . ? 
O6B' C5B' Na2' 52.3(18) . . ? 
C4B' C5B' Na2' 164(2) . . ? 
C5B' O6B' Ni2 110(2) . . ? 
C5B' O6B' Na2' 102(2) . . ? 
Ni2 O6B' Na2' 147.0(19) . . ? 
C5B' O7B' Na1 178(2) . . ? 
C5B' O7B' Na2' 83(2) . . ? 
Na1 O7B' Na2' 95.4(11) . . ? 
F2 B1 F2 116.0(9) 3_565 . ? 
F2 B1 F2 116.0(9) 3_565 2_665 ? 
F2 B1 F2 116.0(9) . 2_665 ? 
F2 B1 F1 101.6(14) 3_565 . ? 
F2 B1 F1 101.6(14) . . ? 
F2 B1 F1 101.6(14) 2_665 . ? 
F4 B2 F4 114.9(14) 2_665 3_565 ? 
F4 B2 F4 114.9(14) 2_665 . ? 
F4 B2 F4 114.9(14) 3_565 . ? 
F4 B2 F3 103.3(19) 2_665 . ? 
F4 B2 F3 103.3(19) 3_565 . ? 
F4 B2 F3 103.3(19) . . ? 
B2 F4 Na2' 150(2) . 1_655 ? 
B2 F4 Na2 152(2) . 1_655 ? 


_diffrn_measured_fraction_theta_max    0.994 
_diffrn_reflns_theta_full              25.01 
_diffrn_measured_fraction_theta_full   0.994 
_refine_diff_density_max    1.17 
_refine_diff_density_min   -0.47 
_refine_diff_density_rms    0.10 

#===END