# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C3 H8 Co N3 O7 P'
_chemical_formula_weight         288.02

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   8.8749(3)
_cell_length_b                   7.4104(2)
_cell_length_c                   15.2333(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.172(3)
_cell_angle_gamma                90.00
_cell_volume                     979.32(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1980
_cell_measurement_theta_min      3.6000
_cell_measurement_theta_max      28.7130

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             580
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.92226
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, 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            3900
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         25.00
_reflns_number_total             1721
_reflns_number_gt                1532
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0317P)²+0.3993P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1721
_refine_ls_number_parameters     137
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0689
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.78969(4) 0.52945(5) 0.10589(2) 0.01859(13) Uani 1 1 d . . .
P1 P 0.87064(8) 0.88556(10) 0.23356(5) 0.02382(19) Uani 1 1 d . . .
H1 H 0.996(3) 0.9454(13) 0.2845(11) 0.036 Uiso 1 1 calc R . .
O1 O 0.8181(3) 1.0285(3) 0.15844(15) 0.0516(7) Uani 1 1 d . . .
H2 H 0.7999 1.1242 0.1812 0.077 Uiso 1 1 calc R . .
O2 O 0.7534(2) 0.8644(3) 0.29171(11) 0.0246(4) Uani 1 1 d . . .
O3 O 0.91137(19) 0.7165(3) 0.19059(11) 0.0251(4) Uani 1 1 d . . .
O4 O 0.65498(19) 0.3515(3) 0.01205(12) 0.0288(5) Uani 1 1 d . . .
O5 O 0.42537(19) 0.3388(2) -0.08106(11) 0.0248(4) Uani 1 1 d . . .
O6 O 0.99412(19) 0.3878(3) 0.10056(11) 0.0239(4) Uani 1 1 d . . .
O7 O 1.1516(2) 0.3483(3) 0.00600(12) 0.0301(5) Uani 1 1 d . . .
N1 N 0.2349(3) 0.9795(4) 0.05964(17) 0.0503(8) Uani 1 1 d . . .
H3 H 0.2637 0.8926 0.0295 0.060 Uiso 1 1 calc R . .
H4 H 0.1597 1.0481 0.0350 0.060 Uiso 1 1 calc R . .
N2 N 0.4206(3) 0.9032(4) 0.18116(17) 0.0428(7) Uani 1 1 d . . .
H5 H 0.4493 0.8163 0.1510 0.051 Uiso 1 1 calc R . .
H6 H 0.4670 0.9215 0.2359 0.051 Uiso 1 1 calc R . .
N3 N 0.2584(3) 1.1362(4) 0.19118(16) 0.0426(7) Uani 1 1 d . . .
H7 H 0.3025 1.1512 0.2466 0.051 Uiso 1 1 calc R . .
H8 H 0.1832 1.2050 0.1667 0.051 Uiso 1 1 calc R . .
C1 C 0.5230(3) 0.4103(4) -0.01968(17) 0.0211(6) Uani 1 1 d . . .
C2 C 1.0417(3) 0.4245(4) 0.03060(16) 0.0195(6) Uani 1 1 d . . .
C3 C 0.3062(3) 1.0075(4) 0.14367(19) 0.0280(6) Uani 1 1 d . . .


_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
Co1 O3 2.0408(18) . ?
Co1 O2 2.0800(17) 2_645 ?
Co1 O7 2.0911(18) 3_765 ?
Co1 O5 2.1057(17) 3_665 ?
Co1 O6 2.1123(17) . ?
Co1 O4 2.1191(18) . ?
P1 O3 1.4928(19) . ?
P1 O2 1.5102(18) . ?
P1 O1 1.557(2) . ?
P1 H1 1.2921 . ?
O1 H2 0.8200 . ?
O2 Co1 2.0800(17) 2_655 ?
O4 C1 1.248(3) . ?
O5 C1 1.250(3) . ?
O5 Co1 2.1057(17) 3_665 ?
O6 C2 1.256(3) . ?
O7 C2 1.250(3) . ?
O7 Co1 2.0911(18) 3_765 ?
N1 C3 1.319(4) . ?
N1 H3 0.8600 . ?
N1 H4 0.8600 . ?
N2 C3 1.307(4) . ?
N2 H5 0.8600 . ?
N2 H6 0.8600 . ?
N3 C3 1.320(4) . ?
N3 H7 0.8600 . ?
N3 H8 0.8600 . ?
C1 C1 1.549(5) 3_665 ?
C2 C2 1.542(5) 3_765 ?

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
O3 Co1 O2 94.68(7) . 2_645 ?
O3 Co1 O7 91.80(8) . 3_765 ?
O2 Co1 O7 169.39(7) 2_645 3_765 ?
O3 Co1 O5 97.90(7) . 3_665 ?
O2 Co1 O5 95.98(7) 2_645 3_665 ?
O7 Co1 O5 91.44(7) 3_765 3_665 ?
O3 Co1 O6 91.00(7) . . ?
O2 Co1 O6 91.83(7) 2_645 . ?
O7 Co1 O6 79.64(7) 3_765 . ?
O5 Co1 O6 167.62(6) 3_665 . ?
O3 Co1 O4 175.70(7) . . ?
O2 Co1 O4 88.47(7) 2_645 . ?
O7 Co1 O4 85.53(8) 3_765 . ?
O5 Co1 O4 78.83(7) 3_665 . ?
O6 Co1 O4 91.83(7) . . ?
O3 P1 O2 115.51(11) . . ?
O3 P1 O1 108.15(11) . . ?
O2 P1 O1 111.39(12) . . ?
O3 P1 H1 107.1 . . ?
O2 P1 H1 107.1 . . ?
O1 P1 H1 107.1 . . ?
P1 O1 H2 109.5 . . ?
P1 O2 Co1 129.59(11) . 2_655 ?
P1 O3 Co1 134.63(11) . . ?
C1 O4 Co1 113.22(16) . . ?
C1 O5 Co1 113.39(16) . 3_665 ?
C2 O6 Co1 111.74(15) . . ?
C2 O7 Co1 113.12(16) . 3_765 ?
C3 N1 H3 120.0 . . ?
C3 N1 H4 120.0 . . ?
H3 N1 H4 120.0 . . ?
C3 N2 H5 120.0 . . ?
C3 N2 H6 120.0 . . ?
H5 N2 H6 120.0 . . ?
C3 N3 H7 120.0 . . ?
C3 N3 H8 120.0 . . ?
H7 N3 H8 120.0 . . ?
O4 C1 O5 126.0(2) . . ?
O4 C1 C1 116.9(3) . 3_665 ?
O5 C1 C1 117.1(3) . 3_665 ?
O7 C2 O6 125.4(2) . . ?
O7 C2 C2 116.9(3) . 3_765 ?
O6 C2 C2 117.7(3) . 3_765 ?
N2 C3 N1 120.0(3) . . ?
N2 C3 N3 119.8(3) . . ?
N1 C3 N3 120.2(3) . . ?

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
O1 H2 O2 0.82 1.91 2.716(3) 167.8 2_655
N1 H3 O4 0.86 2.09 2.935(3) 165.4 3_665
N1 H4 O7 0.86 2.27 2.903(3) 130.9 1_465
N2 H5 O5 0.86 2.05 2.879(3) 162.3 3_665
N3 H8 O6 0.86 2.23 3.086(3) 178.0 1_465

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.072
_database_code_depnum_ccdc_archive 'CCDC 982206'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H17 Mn2.50 N6 O15 P'
_chemical_formula_weight         593.59

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'
P P 0.1023 0.0942 '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                   9.7205(6)
_cell_length_b                   9.7468(6)
_cell_length_c                   10.8926(5)
_cell_angle_alpha                83.989(4)
_cell_angle_beta                 75.467(5)
_cell_angle_gamma                78.545(5)
_cell_volume                     977.45(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    3161
_cell_measurement_theta_min      3.2650
_cell_measurement_theta_max      28.4810

_exptl_crystal_description       block
_exptl_crystal_colour            light-pink
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             597
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.87191
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'Xcalibur, 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            7356
_diffrn_reflns_av_R_equivalents  0.0254
_diffrn_reflns_av_sigmaI/netI    0.0425
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         24.99
_reflns_number_total             3448
_reflns_number_gt                2942
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0477P)²+0.9206P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3448
_refine_ls_number_parameters     306
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0874
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_restrained_S_all      0.981
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.5000 0.0000 1.0000 0.02089(18) Uani 1 2 d S . .
Mn2 Mn 0.36465(5) 0.25534(5) 0.52307(5) 0.01836(15) Uani 1 1 d . . .
Mn3 Mn 0.24086(5) 0.55013(5) 0.28165(5) 0.01894(15) Uani 1 1 d . . .
P1 P 0.47556(9) -0.02251(8) 0.69689(8) 0.0184(2) Uani 1 1 d . . .
H1 H 0.593(3) 0.0421(16) 0.6686(7) 0.028 Uiso 1 1 calc R . .
O1 O 0.4174(3) -0.0237(3) 0.8398(2) 0.0292(6) Uani 1 1 d . . .
O2 O 0.3679(2) 0.0608(2) 0.6254(2) 0.0241(5) Uani 1 1 d . . .
O3 O 0.5276(3) -0.1717(2) 0.6539(2) 0.0312(6) Uani 1 1 d . . .
O4 O 0.7021(2) 0.0461(2) 0.8782(2) 0.0238(5) Uani 1 1 d . . .
O5 O 0.8004(2) 0.2221(2) 0.7697(2) 0.0318(6) Uani 1 1 d . . .
O6 O 0.4571(2) 0.2323(2) 0.9679(2) 0.0262(6) Uani 1 1 d . . .
O7 O 0.5654(2) 0.4039(2) 0.8580(2) 0.0298(6) Uani 1 1 d . . .
O8 O 0.0299(2) 0.5540(3) 0.2417(2) 0.0290(6) Uani 1 1 d . . .
O9 O -0.2046(2) 0.6386(3) 0.3111(2) 0.0305(6) Uani 1 1 d . . .
O10 O 0.0802(2) 0.6259(2) 0.4553(2) 0.0237(5) Uani 1 1 d . . .
O11 O -0.1545(2) 0.7089(2) 0.5247(2) 0.0263(6) Uani 1 1 d . . .
O12 O 0.3755(2) 0.4724(2) 0.4186(2) 0.0205(5) Uani 1 1 d . . .
O13 O 0.4643(2) 0.6651(2) 0.4237(2) 0.0256(5) Uani 1 1 d . . .
OW1 O 0.3056(3) 0.3448(2) 0.2029(2) 0.0289(6) Uani 1 1 d . . .
H2 H 0.3523 0.2809 0.2436 0.043 Uiso 1 1 d R . .
H3 H 0.3404 0.3288 0.1253 0.043 Uiso 1 1 d R . .
OW2 O 0.1399(4) 0.1712(5) 0.9369(4) 0.1081(17) Uani 1 1 d . . .
H5 H 0.1496 0.2526 0.9484 0.162 Uiso 1 1 d R . .
H4 H 0.2035 0.1488 0.8548 0.162 Uiso 1 1 d R . .
N1 N 0.9253(3) -0.0261(3) 0.2926(3) 0.0399(8) Uani 1 1 d . . .
H6 H 0.9965 -0.0750 0.2423 0.048 Uiso 1 1 calc R . .
H7 H 0.8406 -0.0474 0.3085 0.048 Uiso 1 1 calc R . .
N2 N 0.8354(4) 0.1583(4) 0.4202(3) 0.0485(10) Uani 1 1 d . . .
H8 H 0.8482 0.2299 0.4530 0.058 Uiso 1 1 calc R . .
H9 H 0.7508 0.1368 0.4359 0.058 Uiso 1 1 calc R . .
N3 N 1.0750(3) 0.1137(4) 0.3212(4) 0.0463(9) Uani 1 1 d . . .
H10 H 1.1463 0.0649 0.2708 0.056 Uiso 1 1 calc R . .
H11 H 1.0885 0.1839 0.3557 0.056 Uiso 1 1 calc R . .
N4 N 0.2951(9) -0.4228(12) 0.8127(9) 0.078(3) Uani 0.613(9) 1 d P A 1
N5 N 0.0503(7) -0.3575(7) 0.8947(6) 0.054(2) Uani 0.613(9) 1 d P A 1
N4' N 0.3512(11) -0.3668(11) 0.8225(12) 0.043(3) Uani 0.387(9) 1 d P A 2
N5' N 0.1686(10) -0.4568(10) 0.9693(10) 0.055(4) Uani 0.387(9) 1 d P A 2
N6 N 0.1854(6) -0.2191(5) 0.9238(4) 0.0769(14) Uani 1 1 d . A .
H12 H 0.2563 -0.1742 0.8996 0.092 Uiso 1 1 calc R . .
H13 H 0.1066 -0.1819 0.9741 0.092 Uiso 1 1 calc R . .
C1 C 0.6998(3) 0.1731(3) 0.8432(3) 0.0209(7) Uani 1 1 d . . .
C2 C 0.5608(4) 0.2792(3) 0.8937(3) 0.0214(7) Uani 1 1 d . . .
C3 C -0.0765(3) 0.6107(3) 0.3219(3) 0.0205(7) Uani 1 1 d . . .
C4 C -0.0472(3) 0.6511(3) 0.4452(3) 0.0193(7) Uani 1 1 d . . .
C5 C 0.4536(3) 0.5411(3) 0.4547(3) 0.0177(7) Uani 1 1 d . . .
C6 C 0.9459(4) 0.0812(4) 0.3454(4) 0.0303(8) Uani 1 1 d . . .
C7 C 0.1970(6) -0.3384(5) 0.8857(5) 0.0684(17) Uani 1 1 d . . .


_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 O1 2.146(2) 2_657 ?
Mn1 O1 2.146(2) . ?
Mn1 O4 2.177(2) . ?
Mn1 O4 2.177(2) 2_657 ?
Mn1 O6 2.226(2) . ?
Mn1 O6 2.226(2) 2_657 ?
Mn2 O2 2.095(2) . ?
Mn2 O3 2.111(2) 2_656 ?
Mn2 O11 2.186(2) 2_566 ?
Mn2 O13 2.189(2) 2_666 ?
Mn2 O9 2.257(2) 2_566 ?
Mn2 O12 2.304(2) . ?
Mn3 OW1 2.174(2) . ?
Mn3 O8 2.193(2) . ?
Mn3 O7 2.195(2) 2_666 ?
Mn3 O12 2.205(2) . ?
Mn3 O5 2.214(2) 2_666 ?
Mn3 O10 2.217(2) . ?
P1 O2 1.516(2) . ?
P1 O1 1.517(2) . ?
P1 O3 1.523(2) . ?
P1 H1 1.3687 . ?
O3 Mn2 2.111(2) 2_656 ?
O4 C1 1.254(4) . ?
O5 C1 1.240(4) . ?
O5 Mn3 2.214(2) 2_666 ?
O6 C2 1.255(4) . ?
O7 C2 1.242(4) . ?
O7 Mn3 2.195(2) 2_666 ?
O8 C3 1.248(4) . ?
O9 C3 1.253(4) . ?
O9 Mn2 2.257(2) 2_566 ?
O10 C4 1.244(4) . ?
O11 C4 1.253(4) . ?
O11 Mn2 2.186(2) 2_566 ?
O12 C5 1.259(4) . ?
O13 C5 1.238(4) . ?
O13 Mn2 2.189(2) 2_666 ?
OW1 H2 0.8496 . ?
OW1 H3 0.8467 . ?
OW2 H5 0.8427 . ?
OW2 H4 0.9692 . ?
N1 C6 1.316(5) . ?
N1 H6 0.8600 . ?
N1 H7 0.8600 . ?
N2 C6 1.323(5) . ?
N2 H8 0.8600 . ?
N2 H9 0.8600 . ?
N3 C6 1.311(5) . ?
N3 H10 0.8600 . ?
N3 H11 0.8600 . ?
N4 C7 1.289(9) . ?
N5 C7 1.451(8) . ?
N4' C7 1.468(11) . ?
N5' C7 1.420(11) . ?
N6 C7 1.251(6) . ?
N6 H12 0.8600 . ?
N6 H13 0.8600 . ?
C1 C2 1.545(4) . ?
C3 C4 1.546(5) . ?
C5 C5 1.557(6) 2_666 ?

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
O1 Mn1 O1 180.000(1) 2_657 . ?
O1 Mn1 O4 87.90(9) 2_657 . ?
O1 Mn1 O4 92.10(9) . . ?
O1 Mn1 O4 92.10(9) 2_657 2_657 ?
O1 Mn1 O4 87.90(9) . 2_657 ?
O4 Mn1 O4 180.00(8) . 2_657 ?
O1 Mn1 O6 89.13(9) 2_657 . ?
O1 Mn1 O6 90.87(9) . . ?
O4 Mn1 O6 76.35(8) . . ?
O4 Mn1 O6 103.65(8) 2_657 . ?
O1 Mn1 O6 90.87(9) 2_657 2_657 ?
O1 Mn1 O6 89.13(9) . 2_657 ?
O4 Mn1 O6 103.65(8) . 2_657 ?
O4 Mn1 O6 76.35(8) 2_657 2_657 ?
O6 Mn1 O6 180.0 . 2_657 ?
O2 Mn2 O3 95.24(9) . 2_656 ?
O2 Mn2 O11 102.18(9) . 2_566 ?
O3 Mn2 O11 92.39(9) 2_656 2_566 ?
O2 Mn2 O13 101.92(9) . 2_666 ?
O3 Mn2 O13 102.18(10) 2_656 2_666 ?
O11 Mn2 O13 150.44(9) 2_566 2_666 ?
O2 Mn2 O9 90.76(9) . 2_566 ?
O3 Mn2 O9 166.05(9) 2_656 2_566 ?
O11 Mn2 O9 74.01(9) 2_566 2_566 ?
O13 Mn2 O9 88.83(9) 2_666 2_566 ?
O2 Mn2 O12 175.23(9) . . ?
O3 Mn2 O12 86.20(9) 2_656 . ?
O11 Mn2 O12 82.28(8) 2_566 . ?
O13 Mn2 O12 73.31(8) 2_666 . ?
O9 Mn2 O12 88.86(9) 2_566 . ?
OW1 Mn3 O8 86.56(9) . . ?
OW1 Mn3 O7 83.57(9) . 2_666 ?
O8 Mn3 O7 125.59(9) . 2_666 ?
OW1 Mn3 O12 88.16(9) . . ?
O8 Mn3 O12 144.05(9) . . ?
O7 Mn3 O12 88.97(9) 2_666 . ?
OW1 Mn3 O5 143.39(9) . 2_666 ?
O8 Mn3 O5 84.43(10) . 2_666 ?
O7 Mn3 O5 73.33(8) 2_666 2_666 ?
O12 Mn3 O5 118.71(10) . 2_666 ?
OW1 Mn3 O10 131.58(9) . . ?
O8 Mn3 O10 74.92(9) . . ?
O7 Mn3 O10 143.07(9) 2_666 . ?
O12 Mn3 O10 82.38(8) . . ?
O5 Mn3 O10 79.61(9) 2_666 . ?
O2 P1 O1 112.59(14) . . ?
O2 P1 O3 111.81(14) . . ?
O1 P1 O3 110.48(13) . . ?
O2 P1 H1 107.2 . . ?
O1 P1 H1 107.2 . . ?
O3 P1 H1 107.2 . . ?
P1 O1 Mn1 135.80(15) . . ?
P1 O2 Mn2 131.16(14) . . ?
P1 O3 Mn2 133.15(14) . 2_656 ?
C1 O4 Mn1 114.4(2) . . ?
C1 O5 Mn3 116.8(2) . 2_666 ?
C2 O6 Mn1 113.2(2) . . ?
C2 O7 Mn3 117.6(2) . 2_666 ?
C3 O8 Mn3 115.3(2) . . ?
C3 O9 Mn2 114.8(2) . 2_566 ?
C4 O10 Mn3 114.5(2) . . ?
C4 O11 Mn2 117.6(2) . 2_566 ?
C5 O12 Mn3 125.70(19) . . ?
C5 O12 Mn2 114.06(18) . . ?
Mn3 O12 Mn2 120.01(10) . . ?
C5 O13 Mn2 117.47(19) . 2_666 ?
Mn3 OW1 H2 116.7 . . ?
Mn3 OW1 H3 126.0 . . ?
H2 OW1 H3 105.4 . . ?
H5 OW2 H4 105.1 . . ?
C6 N1 H6 120.0 . . ?
C6 N1 H7 120.0 . . ?
H6 N1 H7 120.0 . . ?
C6 N2 H8 120.0 . . ?
C6 N2 H9 120.0 . . ?
H8 N2 H9 120.0 . . ?
C6 N3 H10 120.0 . . ?
C6 N3 H11 120.0 . . ?
H10 N3 H11 120.0 . . ?
C7 N6 H12 120.0 . . ?
C7 N6 H13 120.0 . . ?
H12 N6 H13 120.0 . . ?
O5 C1 O4 125.4(3) . . ?
O5 C1 C2 116.3(3) . . ?
O4 C1 C2 118.3(3) . . ?
O7 C2 O6 126.7(3) . . ?
O7 C2 C1 115.7(3) . . ?
O6 C2 C1 117.6(3) . . ?
O8 C3 O9 126.0(3) . . ?
O8 C3 C4 117.0(3) . . ?
O9 C3 C4 117.1(3) . . ?
O10 C4 O11 126.2(3) . . ?
O10 C4 C3 117.3(3) . . ?
O11 C4 C3 116.5(3) . . ?
O13 C5 O12 126.3(3) . . ?
O13 C5 C5 118.0(4) . 2_666 ?
O12 C5 C5 115.7(3) . 2_666 ?
N3 C6 N1 120.0(4) . . ?
N3 C6 N2 120.1(4) . . ?
N1 C6 N2 119.8(3) . . ?
N6 C7 N4 136.3(8) . . ?
N6 C7 N5' 122.9(6) . . ?
N4 C7 N5' 87.5(7) . . ?
N6 C7 N5 105.6(5) . . ?
N4 C7 N5 114.4(7) . . ?
N5' C7 N5 71.0(5) . . ?
N6 C7 N4' 100.8(7) . . ?
N4 C7 N4' 36.3(5) . . ?
N5' C7 N4' 106.8(7) . . ?
N5 C7 N4' 149.6(7) . . ?

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
OW1 H2 O3 0.85 1.91 2.746(3) 167.1 2_656
OW1 H3 O6 0.85 2.01 2.824(3) 160.6 1_554
OW2 H4 O1 0.97 2.38 2.993(4) 120.5 .
N1 H6 O5 0.86 2.18 2.926(4) 144.7 2_756
N1 H7 O2 0.86 2.00 2.842(4) 166.3 2_656
N2 H8 O10 0.86 2.12 2.963(5) 167.0 2_666
N2 H9 O2 0.86 2.65 3.332(5) 137.0 2_656
N3 H10 O4 0.86 2.12 2.974(4) 169.4 2_756
N3 H11 O11 0.86 2.04 2.862(4) 159.0 2_666
N6 H12 O1 0.86 2.29 3.139(6) 171.0 .
N6 H13 OW2 0.86 2.33 3.110(7) 150.3 2_557

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.109
_database_code_depnum_ccdc_archive 'CCDC 982207'
