# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010


data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Enrique Colacio'
_publ_contact_author_address     
;

;

_publ_contact_author_email       ecolacio@ugr.es
_publ_requested_category         ?
loop_
_publ_author_name
'Jesus E. Perea-Buceta'
'Antonio Mota'
'Jean-Pierre Costes'
'Reijo Sillanpaa'
'J. Krzystek'
;
E.Colacio
;
'N.De Kimpe'

#This CIF-file is done by R.Sillanpaa

data_jp453
_database_code_depnum_ccdc_archive 'CCDC 779232'
#TrackingRef '- newMn3cif.cif'

_audit_creation_date             2009-10-28T12:36:47-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#

_chemical_name_systematic        ?
_chemical_formula_moiety         'C30 H33 Mn3 N12 O12, 6(H2 O), 3(Cl)'
_chemical_formula_sum            'C30 H45 Cl3 Mn3 N12 O18'
_chemical_compound_source        'synthesis as described'
_chemical_formula_weight         1132.95

#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_H-M   'R 3'
_symmetry_Int_Tables_number      146
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  'R 3'

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

_cell_length_a                   20.0110(6)
_cell_length_b                   20.0110(6)
_cell_length_c                   10.0549(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3486.95(18)
_cell_formula_units_Z            3
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    16483
_cell_measurement_theta_min      0.407
_cell_measurement_theta_max      28.283
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_diffrn_ambient_temperature      123(2)
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1737
_exptl_special_details           
;
?
;

#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_T_max  0.746
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073

#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#

_diffrn_source                   'Enraf Nonius FR590'
_diffrn_radiation_monochromator  graphite
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_number            11352
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.1
_diffrn_reflns_theta_max         27
_diffrn_reflns_theta_full        27
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             3245
_reflns_number_gt                3095
_reflns_threshold_expression     >2\s(I)

#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#

_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction        
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_solution    'SIR97 (Giacovazzo et al, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

#----------------------------------------------------------------------------#
# STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#

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

The hydrogen atoms of the water molecules were refined with geometrical
restraints (DFIX and DANG).
;
_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^)+(0.0000P)^2^+24.3601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3245
_refine_ls_number_parameters     224
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0477
_refine_ls_wR_factor_ref         0.1058
_refine_ls_wR_factor_gt          0.104
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_restrained_S_all      1.127
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(3)
_refine_diff_density_max         0.874
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.079

#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#

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 0 '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 0.006 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.59562(4) 0.18042(3) 0.87270(8) 0.02691(15) Uani 1 1 d . . .
Cl1 Cl 0.75261(10) 0.25086(8) 0.23539(15) 0.0552(4) Uani 1 1 d . . .
O1 O 0.71795(18) 0.27759(17) 0.8624(3) 0.0277(7) Uani 1 1 d . . .
O2 O 0.8419(2) 0.3167(2) 0.8961(4) 0.0399(9) Uani 1 1 d . . .
O3 O 0.5984(2) 0.1899(2) 1.0873(4) 0.0424(9) Uani 1 1 d D . .
H3A H 0.562(3) 0.199(3) 1.130(5) 0.051 Uiso 1 1 d D . .
H3B H 0.634(3) 0.192(4) 1.146(5) 0.051 Uiso 1 1 d D . .
O4 O 0.5759(2) 0.1567(2) 0.6635(4) 0.0375(8) Uani 1 1 d D . .
H4A H 0.566(3) 0.1134(18) 0.620(5) 0.045 Uiso 1 1 d D . .
H4B H 0.613(3) 0.2018(16) 0.635(6) 0.045 Uiso 1 1 d D . .
O5 O 0.6063(3) 0.2306(5) 0.4305(7) 0.102(2) Uani 1 1 d D . .
H5A H 0.565(3) 0.226(5) 0.379(7) 0.122 Uiso 1 1 d D . .
H5B H 0.652(2) 0.256(5) 0.381(7) 0.122 Uiso 1 1 d D . .
O6 O 0.5450(2) 0.0175(2) 0.5793(4) 0.0484(10) Uani 1 1 d D . .
H6A H 0.5922(16) 0.022(3) 0.579(6) 0.058 Uiso 1 1 d D . .
H6B H 0.502(2) -0.0314(18) 0.578(6) 0.058 Uiso 1 1 d D . .
N1 N 0.6769(2) 0.1319(2) 0.8945(4) 0.0249(8) Uani 1 1 d . . .
N5 N 0.6955(2) 0.0249(2) 0.9197(4) 0.0311(8) Uani 1 1 d . . .
N8 N 0.5367(2) -0.0706(2) 0.9071(4) 0.0333(9) Uani 1 1 d . . .
N12 N 0.5252(2) 0.0421(2) 0.8934(4) 0.0285(8) Uani 1 1 d . . .
C2 C 0.7532(3) 0.1813(2) 0.9023(4) 0.0263(9) Uani 1 1 d . . .
C3 C 0.8046(3) 0.1547(3) 0.9220(5) 0.0293(9) Uani 1 1 d . . .
C4 C 0.7718(3) 0.0757(3) 0.9292(5) 0.0309(10) Uani 1 1 d . . .
H4 H 0.8054 0.0555 0.9417 0.037 Uiso 1 1 calc R . .
C6 C 0.6513(2) 0.0564(2) 0.9043(5) 0.0265(9) Uani 1 1 d . . .
C7 C 0.5655(3) 0.0057(2) 0.9005(4) 0.0256(9) Uani 1 1 d . . .
C9 C 0.4602(3) -0.1129(3) 0.9050(6) 0.0378(11) Uani 1 1 d . . .
H9 H 0.4368 -0.1675 0.9079 0.045 Uiso 1 1 calc R . .
C10 C 0.4129(3) -0.0802(3) 0.8987(6) 0.0401(12) Uani 1 1 d . . .
H10 H 0.3583 -0.1115 0.8994 0.048 Uiso 1 1 calc R . .
C11 C 0.4485(3) -0.0005(3) 0.8913(5) 0.0354(11) Uani 1 1 d . . .
H11 H 0.4182 0.0237 0.8848 0.042 Uiso 1 1 calc R . .
C13 C 0.7726(3) 0.2634(3) 0.8851(5) 0.0291(10) Uani 1 1 d . . .
C14 C 0.8902(3) 0.2051(3) 0.9373(6) 0.0387(11) Uani 1 1 d . . .
H14A H 0.9116 0.2367 0.8572 0.058 Uiso 1 1 calc R . .
H14B H 0.9137 0.1727 0.9498 0.058 Uiso 1 1 calc R . .
H14C H 0.9013 0.2387 1.0147 0.058 Uiso 1 1 calc R . .

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 0.0217(3) 0.0177(3) 0.0426(3) 0.0039(3) 0.0073(3) 0.0109(3)
Cl1 0.0808(11) 0.0370(7) 0.0509(8) 0.0040(6) -0.0188(8) 0.0318(7)
O1 0.0204(15) 0.0193(15) 0.0443(19) 0.0058(13) 0.0032(13) 0.0105(13)
O2 0.0271(18) 0.0260(17) 0.066(2) 0.0084(17) -0.0005(16) 0.0129(15)
O3 0.047(2) 0.047(2) 0.046(2) 0.0084(17) 0.0141(17) 0.0330(19)
O4 0.0298(18) 0.040(2) 0.047(2) -0.0035(17) -0.0014(16) 0.0215(17)
O5 0.051(3) 0.137(6) 0.103(5) 0.033(4) 0.014(3) 0.036(4)
O6 0.034(2) 0.052(2) 0.069(3) -0.019(2) -0.0089(19) 0.0288(19)
N1 0.0235(18) 0.0242(18) 0.034(2) 0.0017(15) 0.0020(15) 0.0174(16)
N5 0.033(2) 0.0220(18) 0.041(2) 0.0067(15) 0.0049(16) 0.0157(17)
N8 0.038(2) 0.0197(18) 0.044(2) 0.0040(16) 0.0015(18) 0.0159(17)
N12 0.0256(19) 0.0168(17) 0.041(2) 0.0043(15) 0.0062(16) 0.0094(15)
C2 0.024(2) 0.022(2) 0.036(2) 0.0011(17) 0.0034(17) 0.0133(18)
C3 0.026(2) 0.025(2) 0.037(2) 0.0085(18) 0.0080(18) 0.0132(19)
C4 0.031(2) 0.028(2) 0.039(3) 0.0013(19) -0.0002(19) 0.019(2)
C6 0.022(2) 0.020(2) 0.034(2) 0.0029(17) 0.0020(17) 0.0073(17)
C7 0.028(2) 0.0169(19) 0.031(2) 0.0014(16) 0.0045(17) 0.0112(18)
C9 0.035(3) 0.014(2) 0.058(3) 0.002(2) -0.005(2) 0.0077(19)
C10 0.031(3) 0.024(2) 0.053(3) 0.001(2) -0.004(2) 0.005(2)
C11 0.029(2) 0.021(2) 0.053(3) 0.004(2) 0.011(2) 0.010(2)
C13 0.030(2) 0.021(2) 0.042(3) 0.0064(18) 0.0060(19) 0.017(2)
C14 0.032(3) 0.032(3) 0.057(3) 0.004(2) -0.003(2) 0.021(2)

#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#

_geom_special_details            
;
All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell s.u.'s are taken
into account individually in the estimation of s.u.'s in distances, angles
and torsion angles; correlations between s.u.'s in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Mn1 O4 2.149(4) . ?
Mn1 O3 2.165(4) . ?
Mn1 O2 2.241(3) 3_665 ?
Mn1 O1 2.241(3) . ?
Mn1 N1 2.284(3) . ?
Mn1 N12 2.406(4) . ?
Mn1 O1 2.476(3) 3_665 ?
O1 C13 1.280(5) . ?
O1 Mn1 2.476(3) 2_655 ?
O2 C13 1.262(6) . ?
O2 Mn1 2.241(3) 2_655 ?
O3 H3A 0.93(2) . ?
O3 H3B 0.91(2) . ?
O4 H4A 0.901(19) . ?
O4 H4B 0.882(19) . ?
O5 H5A 0.94(2) . ?
O5 H5B 0.94(2) . ?
O6 H6A 0.905(19) . ?
O6 H6B 0.925(19) . ?
N1 C6 1.334(6) . ?
N1 C2 1.344(6) . ?
N5 C6 1.329(6) . ?
N5 C4 1.350(6) . ?
N8 C9 1.329(6) . ?
N8 C7 1.337(5) . ?
N12 C11 1.331(6) . ?
N12 C7 1.334(6) . ?
C2 C3 1.387(6) . ?
C2 C13 1.499(6) . ?
C3 C4 1.378(6) . ?
C3 C14 1.499(7) . ?
C4 H4 0.95 . ?
C6 C7 1.495(6) . ?
C9 C10 1.394(7) . ?
C9 H9 0.95 . ?
C10 C11 1.386(7) . ?
C10 H10 0.95 . ?
C11 H11 0.95 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?

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
O4 Mn1 O3 171.50(16) . . ?
O4 Mn1 O2 89.87(14) . 3_665 ?
O3 Mn1 O2 83.72(15) . 3_665 ?
O4 Mn1 O1 98.43(14) . . ?
O3 Mn1 O1 90.05(14) . . ?
O2 Mn1 O1 141.19(11) 3_665 . ?
O4 Mn1 N1 95.26(13) . . ?
O3 Mn1 N1 87.08(14) . . ?
O2 Mn1 N1 146.33(13) 3_665 . ?
O1 Mn1 N1 70.85(12) . . ?
O4 Mn1 N12 83.89(15) . . ?
O3 Mn1 N12 89.39(15) . . ?
O2 Mn1 N12 78.96(12) 3_665 . ?
O1 Mn1 N12 139.42(12) . . ?
N1 Mn1 N12 68.60(13) . . ?
O4 Mn1 O1 92.50(12) . 3_665 ?
O3 Mn1 O1 88.55(13) . 3_665 ?
O2 Mn1 O1 55.94(12) 3_665 3_665 ?
O1 Mn1 O1 85.73(15) . 3_665 ?
N1 Mn1 O1 156.15(12) . 3_665 ?
N12 Mn1 O1 134.81(12) . 3_665 ?
C13 O1 Mn1 118.9(3) . . ?
C13 O1 Mn1 85.5(2) . 2_655 ?
Mn1 O1 Mn1 153.69(15) . 2_655 ?
C13 O2 Mn1 96.7(3) . 2_655 ?
Mn1 O3 H3A 120(4) . . ?
Mn1 O3 H3B 129(4) . . ?
H3A O3 H3B 111(6) . . ?
Mn1 O4 H4A 128(4) . . ?
Mn1 O4 H4B 97(4) . . ?
H4A O4 H4B 119(4) . . ?
H5A O5 H5B 109(4) . . ?
H6A O6 H6B 119(4) . . ?
C6 N1 C2 118.7(4) . . ?
C6 N1 Mn1 122.4(3) . . ?
C2 N1 Mn1 118.9(3) . . ?
C6 N5 C4 114.9(4) . . ?
C9 N8 C7 115.3(4) . . ?
C11 N12 C7 118.0(4) . . ?
C11 N12 Mn1 124.1(3) . . ?
C7 N12 Mn1 117.8(3) . . ?
N1 C2 C3 121.0(4) . . ?
N1 C2 C13 112.0(4) . . ?
C3 C2 C13 127.0(4) . . ?
C4 C3 C2 115.3(4) . . ?
C4 C3 C14 119.7(4) . . ?
C2 C3 C14 125.0(4) . . ?
N5 C4 C3 124.9(4) . . ?
N5 C4 H4 117.6 . . ?
C3 C4 H4 117.6 . . ?
N5 C6 N1 125.2(4) . . ?
N5 C6 C7 119.4(4) . . ?
N1 C6 C7 115.4(4) . . ?
N12 C7 N8 126.4(4) . . ?
N12 C7 C6 115.7(4) . . ?
N8 C7 C6 117.9(4) . . ?
N8 C9 C10 122.6(4) . . ?
N8 C9 H9 118.7 . . ?
C10 C9 H9 118.7 . . ?
C11 C10 C9 117.6(5) . . ?
C11 C10 H10 121.2 . . ?
C9 C10 H10 121.2 . . ?
N12 C11 C10 120.1(5) . . ?
N12 C11 H11 120 . . ?
C10 C11 H11 120 . . ?
O2 C13 O1 121.9(4) . . ?
O2 C13 C2 119.3(4) . . ?
O1 C13 C2 118.8(4) . . ?
C3 C14 H14A 109.5 . . ?
C3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O3 H3A Cl1 0.93(2) 2.23(2) 3.140(4) 167(5) 3_666
O3 H3B Cl1 0.91(2) 2.24(3) 3.076(5) 152(6) 1_556
O4 H4A O6 0.901(19) 1.79(2) 2.672(5) 164(5) .
O4 H4B O5 0.882(19) 2.15(6) 2.673(7) 117(5) .
O5 H5A Cl1 0.94(2) 2.15(3) 3.059(6) 162(7) 3_665
O5 H5B O5 0.94(2) 2.42(7) 3.099(13) 129(7) 2_655
O5 H5B Cl1 0.94(2) 2.53(5) 3.377(6) 150(8) .
O6 H6A N5 0.905(19) 2.11(4) 2.932(5) 151(5) 9_654
O6 H6A N8 0.905(19) 2.46(4) 3.167(6) 135(5) 9_654
O6 H6B Cl1 0.925(19) 2.35(3) 3.253(4) 166(5) 5_545

# END of CIF