# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_1166
_database_code_depnum_ccdc_archive 'CCDC 1041650'
_audit_update_record             
;
2015-06-04 deposited with the CCDC.
2015-06-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        unk
_chemical_name_common            ?
_chemical_formula_moiety         'C30 H48 Mn4 N4 O26, 8(H2 O)'
_chemical_formula_sum            'C30 H64 Mn4 N4 O34'
_chemical_compound_source        synthesis
_exptl_crystal_recrystallization_method water
_chemical_melting_point          ?

_exptl_crystal_description       plates
_exptl_crystal_colour            colourless

_diffrn_ambient_temperature      293(2)
_chemical_formula_weight         1244.61

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'
Mn Mn 0.3368 0.7283 '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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  '-P 1'

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

_cell_length_a                   10.4029(8)
_cell_length_b                   11.7222(8)
_cell_length_c                   11.8865(7)
_cell_angle_alpha                71.602(6)
_cell_angle_beta                 64.303(7)
_cell_angle_gamma                77.400(6)
_cell_volume                     1233.77(15)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2865
_cell_measurement_theta_min      2.9795
_cell_measurement_theta_max      28.5760
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             644
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_T_max  0.767
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6911
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.99
_diffrn_reflns_theta_max         25.00
_reflns_number_total             3840
_reflns_number_gt                3039
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0380P)²+0.2337P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3840
_refine_ls_number_parameters     324
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0423
_refine_ls_wR_factor_ref         0.1012
_refine_ls_wR_factor_gt          0.0890
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.017
_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 0.84366(5) 0.30404(5) 0.65131(5) 0.02153(16) Uani 1 1 d . . .
Mn2 Mn 0.50547(5) 0.74205(5) 0.56894(5) 0.02314(17) Uani 1 1 d . . .
O8 O 0.5447(2) 0.1424(2) 0.5953(2) 0.0269(6) Uani 1 1 d . . .
O1 O 0.7158(3) 0.4818(2) 0.6229(2) 0.0313(7) Uani 1 1 d . . .
O4 O 0.9719(4) 0.4435(3) 0.8740(3) 0.0674(10) Uani 1 1 d . . .
O2 O 0.5609(3) 0.6187(2) 0.7230(2) 0.0334(7) Uani 1 1 d . . .
O6 O 1.1676(2) 0.0136(2) 0.5953(2) 0.0364(7) Uani 1 1 d . . .
O5 O 1.0390(2) 0.1822(2) 0.6452(2) 0.0309(7) Uani 1 1 d . . .
O13 O 0.7251(2) 0.6932(2) 0.4334(2) 0.0329(7) Uani 1 1 d . . .
H13A H 0.7578 0.6242 0.4677 0.049 Uiso 1 1 d R . .
H13B H 0.7800 0.7460 0.4168 0.049 Uiso 1 1 d R . .
O12 O 0.5869(2) 0.8955(2) 0.5743(2) 0.0324(7) Uani 1 1 d . . .
H12A H 0.5223 0.9550 0.5802 0.049 Uiso 1 1 d R . .
H12B H 0.6606 0.9154 0.5052 0.049 Uiso 1 1 d R . .
O3 O 0.9518(3) 0.4101(2) 0.7088(2) 0.0320(6) Uani 1 1 d . . .
O10 O 0.4177(3) 0.5891(2) 0.5630(2) 0.0342(7) Uani 1 1 d . . .
H10A H 0.3589 0.6164 0.5263 0.051 Uiso 1 1 d R . .
H10B H 0.3744 0.5484 0.6397 0.051 Uiso 1 1 d R . .
O9 O 0.9674(3) 0.3672(2) 0.4445(2) 0.0468(8) Uani 1 1 d . . .
H9A H 1.0503 0.3285 0.4244 0.070 Uiso 1 1 d R . .
H9B H 0.9759 0.4423 0.4262 0.070 Uiso 1 1 d R . .
O11 O 0.2951(3) 0.7978(2) 0.6993(2) 0.0385(7) Uani 1 1 d . . .
H11A H 0.2435 0.7383 0.7373 0.058 Uiso 1 1 d R . .
H11B H 0.2544 0.8550 0.6567 0.058 Uiso 1 1 d R . .
N2 N 0.7885(3) 0.0751(3) 0.7544(2) 0.0210(7) Uani 1 1 d . . .
C13 C 1.0519(4) 0.0770(3) 0.6329(3) 0.0246(9) Uani 1 1 d . . .
O7 O 0.6963(3) 0.2516(2) 0.5925(3) 0.0371(7) Uani 1 1 d . . .
C11 C 0.9132(4) 0.3998(3) 0.8269(4) 0.0345(10) Uani 1 1 d . . .
N1 N 0.6939(3) 0.3160(3) 0.8622(3) 0.0266(8) Uani 1 1 d . . .
C1 C 0.7804(3) 0.0307(3) 0.8850(3) 0.0222(8) Uani 1 1 d . . .
C9 C 0.6300(4) 0.5155(3) 0.7225(3) 0.0258(9) Uani 1 1 d . . .
C12 C 0.9164(3) 0.0281(3) 0.6570(3) 0.0263(9) Uani 1 1 d . . .
H12C H 0.9031 0.0494 0.5767 0.032 Uiso 1 1 calc R . .
H12D H 0.9272 -0.0593 0.6854 0.032 Uiso 1 1 calc R . .
C15 C 0.6313(4) 0.1585(3) 0.6343(3) 0.0240(9) Uani 1 1 d . . .
C8 C 0.5990(5) 0.4291(4) 0.8513(4) 0.0520(14) Uani 1 1 d . . .
H8A H 0.5995 0.4717 0.9091 0.062 Uiso 1 1 calc R . .
H8B H 0.5023 0.4075 0.8832 0.062 Uiso 1 1 calc R . .
C14 C 0.6593(3) 0.0591(3) 0.7411(3) 0.0240(9) Uani 1 1 d . . .
H14A H 0.5772 0.0591 0.8220 0.029 Uiso 1 1 calc R . .
H14B H 0.6714 -0.0184 0.7228 0.029 Uiso 1 1 calc R . .
C6 C 0.6885(3) 0.0951(3) 0.9766(3) 0.0231(8) Uani 1 1 d . . .
C5 C 0.6828(4) 0.0516(4) 1.1016(3) 0.0343(10) Uani 1 1 d . . .
H5 H 0.6220 0.0935 1.1630 0.041 Uiso 1 1 calc R . .
C7 C 0.6035(4) 0.2140(3) 0.9443(3) 0.0287(9) Uani 1 1 d . . .
H7A H 0.5488 0.2043 0.8999 0.034 Uiso 1 1 calc R . .
H7B H 0.5358 0.2345 1.0239 0.034 Uiso 1 1 calc R . .
C3 C 0.8537(5) -0.1122(4) 1.0483(4) 0.0485(13) Uani 1 1 d . . .
H3 H 0.9100 -0.1810 1.0717 0.058 Uiso 1 1 calc R . .
C2 C 0.8622(4) -0.0729(3) 0.9222(4) 0.0371(11) Uani 1 1 d . . .
H2 H 0.9232 -0.1163 0.8623 0.044 Uiso 1 1 calc R . .
C4 C 0.7637(5) -0.0509(4) 1.1377(4) 0.0453(12) Uani 1 1 d . . .
H4 H 0.7570 -0.0781 1.2223 0.054 Uiso 1 1 calc R . .
C10 C 0.7907(5) 0.3247(4) 0.9197(4) 0.0408(11) Uani 1 1 d . . .
H10C H 0.8294 0.2439 0.9515 0.049 Uiso 1 1 calc R . .
H10D H 0.7356 0.3594 0.9929 0.049 Uiso 1 1 calc R . .
O14 O 0.2085(3) 0.2489(2) 0.2826(2) 0.0599(10) Uani 1 1 d G . .
H14C H 0.1475 0.3106 0.2838 0.090 Uiso 1 1 d G . .
H14D H 0.2687 0.2523 0.2056 0.090 Uiso 1 1 d G . .
O15 O 0.2466(3) 0.3647(3) 0.0295(2) 0.0936(14) Uani 1 1 d G . .
H15A H 0.1611 0.3968 0.0583 0.140 Uiso 1 1 d G . .
H15B H 0.2648 0.3493 -0.0415 0.140 Uiso 1 1 d G . .
O16 O 0.0974(4) 0.6425(3) 0.8566(2) 0.0873(13) Uani 1 1 d G . .
H16A H 0.0886 0.6095 0.9340 0.131 Uiso 1 1 d G . .
H16B H 0.0685 0.5973 0.8304 0.131 Uiso 1 1 d G . .
O17 O 0.3041(3) 0.3858(3) 0.7651(2) 0.137(2) Uani 1 1 d G . .
H17A H 0.3753 0.3540 0.7854 0.206 Uiso 1 1 d G . .
H17B H 0.2888 0.3410 0.7290 0.206 Uiso 1 1 d G . .


_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 O9 2.184(2) . ?
Mn1 O7 2.197(3) . ?
Mn1 O5 2.201(2) . ?
Mn1 O1 2.228(2) . ?
Mn1 O3 2.257(3) . ?
Mn1 N1 2.339(3) . ?
Mn2 O2 2.159(2) . ?
Mn2 O11 2.166(2) . ?
Mn2 O12 2.177(3) . ?
Mn2 O8 2.197(2) 2_666 ?
Mn2 O10 2.214(3) . ?
Mn2 O13 2.228(2) . ?
O8 C15 1.247(4) . ?
O8 Mn2 2.197(2) 2_666 ?
O1 C9 1.257(4) . ?
O4 C11 1.250(5) . ?
O2 C9 1.265(4) . ?
O6 C13 1.246(4) . ?
O5 C13 1.260(4) . ?
O3 C11 1.253(4) . ?
N2 C1 1.444(4) . ?
N2 C12 1.470(4) . ?
N2 C14 1.476(4) . ?
C13 C12 1.515(5) . ?
O7 C15 1.258(4) . ?
C11 C10 1.508(6) . ?
N1 C10 1.476(5) . ?
N1 C8 1.477(4) . ?
N1 C7 1.491(5) . ?
C1 C2 1.390(5) . ?
C1 C6 1.403(5) . ?
C9 C8 1.487(5) . ?
C15 C14 1.514(5) . ?
C6 C5 1.389(5) . ?
C6 C7 1.514(5) . ?
C5 C4 1.372(5) . ?
C3 C4 1.359(6) . ?
C3 C2 1.390(5) . ?

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
O9 Mn1 O7 84.92(11) . . ?
O9 Mn1 O5 83.45(10) . . ?
O7 Mn1 O5 117.33(10) . . ?
O9 Mn1 O1 83.33(9) . . ?
O7 Mn1 O1 81.66(10) . . ?
O5 Mn1 O1 155.67(10) . . ?
O9 Mn1 O3 94.68(10) . . ?
O7 Mn1 O3 162.78(9) . . ?
O5 Mn1 O3 79.63(10) . . ?
O1 Mn1 O3 81.19(10) . . ?
O9 Mn1 N1 158.08(10) . . ?
O7 Mn1 N1 101.19(11) . . ?
O5 Mn1 N1 111.36(10) . . ?
O1 Mn1 N1 76.86(9) . . ?
O3 Mn1 N1 73.26(10) . . ?
O2 Mn2 O11 93.40(10) . . ?
O2 Mn2 O12 94.13(10) . . ?
O11 Mn2 O12 88.98(10) . . ?
O2 Mn2 O8 175.96(9) . 2_666 ?
O11 Mn2 O8 89.47(9) . 2_666 ?
O12 Mn2 O8 88.77(10) . 2_666 ?
O2 Mn2 O10 86.97(10) . . ?
O11 Mn2 O10 89.95(10) . . ?
O12 Mn2 O10 178.51(9) . . ?
O8 Mn2 O10 90.19(9) 2_666 . ?
O2 Mn2 O13 87.41(9) . . ?
O11 Mn2 O13 177.27(10) . . ?
O12 Mn2 O13 88.36(10) . . ?
O8 Mn2 O13 89.85(9) 2_666 . ?
O10 Mn2 O13 92.70(10) . . ?
C15 O8 Mn2 127.3(2) . 2_666 ?
C9 O1 Mn1 117.1(2) . . ?
C9 O2 Mn2 127.1(2) . . ?
C13 O5 Mn1 120.7(2) . . ?
C11 O3 Mn1 117.6(3) . . ?
C1 N2 C12 115.3(3) . . ?
C1 N2 C14 113.3(3) . . ?
C12 N2 C14 109.3(3) . . ?
O6 C13 O5 125.1(4) . . ?
O6 C13 C12 118.0(3) . . ?
O5 C13 C12 116.8(3) . . ?
C15 O7 Mn1 131.6(2) . . ?
O4 C11 O3 125.0(4) . . ?
O4 C11 C10 117.3(4) . . ?
O3 C11 C10 117.7(4) . . ?
C10 N1 C8 110.0(3) . . ?
C10 N1 C7 110.3(3) . . ?
C8 N1 C7 108.7(3) . . ?
C10 N1 Mn1 105.1(2) . . ?
C8 N1 Mn1 106.4(2) . . ?
C7 N1 Mn1 116.2(2) . . ?
C2 C1 C6 119.1(3) . . ?
C2 C1 N2 121.9(3) . . ?
C6 C1 N2 119.0(3) . . ?
O1 C9 O2 125.0(3) . . ?
O1 C9 C8 119.6(3) . . ?
O2 C9 C8 115.3(3) . . ?
N2 C12 C13 112.6(3) . . ?
O8 C15 O7 125.0(3) . . ?
O8 C15 C14 117.6(3) . . ?
O7 C15 C14 117.5(3) . . ?
N1 C8 C9 118.7(3) . . ?
N2 C14 C15 111.5(3) . . ?
C5 C6 C1 118.2(3) . . ?
C5 C6 C7 118.2(3) . . ?
C1 C6 C7 123.5(3) . . ?
C4 C5 C6 122.4(4) . . ?
N1 C7 C6 113.7(3) . . ?
C4 C3 C2 120.6(4) . . ?
C1 C2 C3 120.6(4) . . ?
C3 C4 C5 119.2(4) . . ?
N1 C10 C11 113.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.883
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.883
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.070

