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


#######################################################################
#
#                 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 
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#  except for the purpose of generating routine backup copies 
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#  data retrieval see:
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data_f1
_database_code_depnum_ccdc_archive 'CCDC 896253'
#TrackingRef '1.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H104 Cd7 N12 O50 P6'
_chemical_formula_weight         2694.11

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'
Cd Cd -0.8075 1.2024 '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'

_symmetry_cell_setting           Rhombohedral
_symmetry_space_group_name_H-M   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'
'-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                   22.891(2)
_cell_length_b                   22.891(2)
_cell_length_c                   13.1165(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5952.2(9)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4647
_cell_measurement_theta_min      3.1311
_cell_measurement_theta_max      27.4934

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4014
_exptl_absorpt_coefficient_mu    2.080
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8683
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15274
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0314
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.08
_diffrn_reflns_theta_max         27.46
_reflns_number_total             3027
_reflns_number_gt                2766
_reflns_threshold_expression     >2sigma(I)

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+61.7094P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3027
_refine_ls_number_parameters     195
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0443
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1088
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_restrained_S_all      1.148
_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
Cd1 Cd 0.054643(16) -0.121987(16) 0.13530(3) 0.02249(13) Uani 1 1 d . . .
Cd2 Cd 0.0000 0.0000 0.0000 0.01679(18) Uani 1 6 d S . .
P1 P 0.15010(6) 0.04401(6) 0.11891(10) 0.0212(3) Uani 1 1 d . . .
O1 O 0.07808(17) -0.01186(16) 0.0954(3) 0.0260(8) Uani 1 1 d . . .
O2 O 0.1495(2) 0.1011(2) 0.1765(4) 0.0460(12) Uani 1 1 d . . .
O3 O 0.1971(2) 0.0660(2) 0.0291(3) 0.0413(10) Uani 1 1 d . . .
O4 O 0.0621(2) -0.1129(3) 0.3188(4) 0.0512(13) Uani 1 1 d . . .
O5 O 0.1224(2) -0.1173(2) 0.4476(3) 0.0460(11) Uani 1 1 d . . .
O6 O 0.36328(12) 0.62981(12) 0.09290(18) 0.0032(5) Uani 1 1 d . . .
O7 O 0.32115(17) 0.58524(18) 0.0097(3) 0.0247(7) Uani 1 1 d . . .
O8 O 0.2709(3) 0.5300(3) 0.0830(5) 0.0743(17) Uani 1 1 d . . .
O9 O 0.3333 0.6667 -0.0543(6) 0.066(3) Uani 1 3 d S . .
N1 N 0.16996(19) -0.05953(19) 0.1900(3) 0.0198(8) Uani 1 1 d . . .
N2 N 0.4295(2) 0.0696(2) 0.1687(4) 0.0328(10) Uani 1 1 d . . .
C1 C 0.1810(2) 0.0086(2) 0.2131(4) 0.0229(10) Uani 1 1 d . . .
H2 H 0.2290 0.0390 0.2217 0.027 Uiso 1 1 calc R . .
H1 H 0.1595 0.0066 0.2777 0.027 Uiso 1 1 calc R . .
C2 C 0.1147(3) -0.1085(3) 0.3569(4) 0.0294(11) Uani 1 1 d . . .
C3 C 0.1734(2) -0.0921(3) 0.2853(4) 0.0263(10) Uani 1 1 d . . .
H4 H 0.2155 -0.0624 0.3200 0.032 Uiso 1 1 calc R . .
H3 H 0.1734 -0.1334 0.2687 0.032 Uiso 1 1 calc R . .
C4 C 0.2165(2) -0.0597(2) 0.1104(4) 0.0231(10) Uani 1 1 d . . .
H5 H 0.2062 -0.0456 0.0464 0.028 Uiso 1 1 calc R . .
H6 H 0.2070 -0.1057 0.1016 0.028 Uiso 1 1 calc R . .
C5 C 0.2910(2) -0.0155(2) 0.1314(4) 0.0243(10) Uani 1 1 d . . .
C6 C 0.3300(3) -0.0397(3) 0.1749(4) 0.0301(11) Uani 1 1 d . . .
H7 H 0.3106 -0.0850 0.1921 0.036 Uiso 1 1 calc R . .
C7 C 0.3983(3) 0.0042(3) 0.1927(5) 0.0323(12) Uani 1 1 d . . .
H8 H 0.4234 -0.0129 0.2229 0.039 Uiso 1 1 calc R . .
C8 C 0.3234(3) 0.0524(3) 0.1072(5) 0.0346(13) Uani 1 1 d . . .
H9 H 0.2992 0.0709 0.0781 0.042 Uiso 1 1 calc R . .
C9 C 0.3914(3) 0.0927(3) 0.1261(6) 0.0422(15) Uani 1 1 d . . .
H10 H 0.4120 0.1381 0.1087 0.051 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
Cd1 0.01575(18) 0.01692(18) 0.0338(2) 0.00099(13) -0.00268(13) 0.00739(13)
Cd2 0.0135(2) 0.0135(2) 0.0233(4) 0.000 0.000 0.00677(11)
P1 0.0170(5) 0.0138(5) 0.0324(7) -0.0006(5) -0.0055(5) 0.0075(4)
O1 0.0207(16) 0.0175(16) 0.038(2) 0.0038(14) -0.0080(14) 0.0083(13)
O2 0.049(3) 0.027(2) 0.074(3) -0.020(2) -0.027(2) 0.0280(19)
O3 0.027(2) 0.056(3) 0.038(2) 0.021(2) 0.0004(17) 0.0183(19)
O4 0.032(2) 0.088(4) 0.041(3) 0.022(2) 0.0081(18) 0.035(2)
O5 0.055(3) 0.064(3) 0.028(2) 0.008(2) -0.0012(19) 0.037(2)
O6 0.0032(11) 0.0022(10) 0.0036(12) -0.0018(9) -0.0018(9) 0.0010(9)
O7 0.0239(17) 0.0304(18) 0.0239(18) -0.0078(14) -0.0043(14) 0.0166(15)
O8 0.082(4) 0.064(4) 0.068(4) 0.014(3) 0.004(3) 0.030(3)
O9 0.082(4) 0.082(4) 0.033(5) 0.000 0.000 0.041(2)
N1 0.0192(18) 0.0178(18) 0.025(2) 0.0021(15) -0.0014(15) 0.0110(15)
N2 0.018(2) 0.029(2) 0.049(3) -0.005(2) -0.0035(19) 0.0104(18)
C1 0.023(2) 0.022(2) 0.028(3) -0.0054(19) -0.0055(19) 0.0139(19)
C2 0.032(3) 0.027(3) 0.031(3) 0.002(2) -0.001(2) 0.016(2)
C3 0.025(2) 0.031(3) 0.031(3) 0.005(2) -0.005(2) 0.019(2)
C4 0.016(2) 0.025(2) 0.028(3) 0.0006(19) -0.0001(18) 0.0103(19)
C5 0.018(2) 0.025(2) 0.029(3) -0.0014(19) 0.0006(19) 0.0096(19)
C6 0.023(2) 0.024(2) 0.045(3) -0.004(2) -0.002(2) 0.014(2)
C7 0.025(3) 0.030(3) 0.046(3) -0.003(2) -0.004(2) 0.017(2)
C8 0.020(2) 0.025(3) 0.054(4) 0.009(2) -0.004(2) 0.008(2)
C9 0.023(3) 0.027(3) 0.070(4) 0.006(3) -0.008(3) 0.007(2)

_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
Cd1 O2 2.183(4) 3 ?
Cd1 O3 2.194(4) 11 ?
Cd1 O1 2.359(3) . ?
Cd1 N1 2.399(4) . ?
Cd1 N2 2.412(4) 15_445 ?
Cd1 O4 2.415(5) . ?
Cd2 O1 2.306(3) 10 ?
Cd2 O1 2.306(3) . ?
Cd2 O1 2.306(3) 2 ?
Cd2 O1 2.306(3) 3 ?
Cd2 O1 2.306(3) 12 ?
Cd2 O1 2.306(3) 11 ?
P1 O3 1.502(4) . ?
P1 O2 1.516(4) . ?
P1 O1 1.530(3) . ?
P1 C1 1.806(5) . ?
O2 Cd1 2.183(4) 2 ?
O3 Cd1 2.194(4) 12 ?
O4 C2 1.261(7) . ?
O5 C2 1.234(7) . ?
O6 O7 1.475(4) . ?
O7 O8 1.547(7) . ?
N1 C3 1.478(6) . ?
N1 C1 1.480(6) . ?
N1 C4 1.492(6) . ?
N2 C7 1.335(7) . ?
N2 C9 1.347(7) . ?
N2 Cd1 2.412(4) 14 ?
C2 C3 1.524(7) . ?
C4 C5 1.511(6) . ?
C5 C8 1.383(7) . ?
C5 C6 1.388(7) . ?
C6 C7 1.393(7) . ?
C8 C9 1.379(7) . ?

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
O2 Cd1 O3 112.22(18) 3 11 ?
O2 Cd1 O1 89.91(14) 3 . ?
O3 Cd1 O1 84.78(14) 11 . ?
O2 Cd1 N1 143.70(17) 3 . ?
O3 Cd1 N1 101.73(15) 11 . ?
O1 Cd1 N1 80.50(12) . . ?
O2 Cd1 N2 89.23(16) 3 15_445 ?
O3 Cd1 N2 91.87(16) 11 15_445 ?
O1 Cd1 N2 175.94(14) . 15_445 ?
N1 Cd1 N2 102.48(14) . 15_445 ?
O2 Cd1 O4 78.30(16) 3 . ?
O3 Cd1 O4 168.88(14) 11 . ?
O1 Cd1 O4 99.21(16) . . ?
N1 Cd1 O4 68.98(14) . . ?
N2 Cd1 O4 84.50(18) 15_445 . ?
O1 Cd2 O1 180.0(2) 10 . ?
O1 Cd2 O1 86.65(13) 10 2 ?
O1 Cd2 O1 93.35(13) . 2 ?
O1 Cd2 O1 86.65(13) 10 3 ?
O1 Cd2 O1 93.35(13) . 3 ?
O1 Cd2 O1 93.35(13) 2 3 ?
O1 Cd2 O1 93.35(13) 10 12 ?
O1 Cd2 O1 86.65(13) . 12 ?
O1 Cd2 O1 86.65(13) 2 12 ?
O1 Cd2 O1 180.0(2) 3 12 ?
O1 Cd2 O1 93.35(13) 10 11 ?
O1 Cd2 O1 86.65(13) . 11 ?
O1 Cd2 O1 180.0(2) 2 11 ?
O1 Cd2 O1 86.65(13) 3 11 ?
O1 Cd2 O1 93.35(13) 12 11 ?
O3 P1 O2 114.6(3) . . ?
O3 P1 O1 114.4(2) . . ?
O2 P1 O1 110.5(2) . . ?
O3 P1 C1 108.2(2) . . ?
O2 P1 C1 102.8(2) . . ?
O1 P1 C1 105.2(2) . . ?
P1 O1 Cd2 125.84(18) . . ?
P1 O1 Cd1 115.03(17) . . ?
Cd2 O1 Cd1 118.08(14) . . ?
P1 O2 Cd1 133.6(3) . 2 ?
P1 O3 Cd1 131.0(2) . 12 ?
C2 O4 Cd1 115.1(4) . . ?
O6 O7 O8 93.9(3) . . ?
C3 N1 C1 109.5(4) . . ?
C3 N1 C4 111.9(4) . . ?
C1 N1 C4 113.6(4) . . ?
C3 N1 Cd1 105.8(3) . . ?
C1 N1 Cd1 104.3(3) . . ?
C4 N1 Cd1 111.3(3) . . ?
C7 N2 C9 116.8(5) . . ?
C7 N2 Cd1 129.8(4) . 14 ?
C9 N2 Cd1 113.3(4) . 14 ?
N1 C1 P1 115.7(3) . . ?
O5 C2 O4 125.3(5) . . ?
O5 C2 C3 116.9(5) . . ?
O4 C2 C3 117.8(5) . . ?
N1 C3 C2 112.4(4) . . ?
N1 C4 C5 116.0(4) . . ?
C8 C5 C6 116.9(5) . . ?
C8 C5 C4 120.2(4) . . ?
C6 C5 C4 122.9(4) . . ?
C5 C6 C7 119.8(5) . . ?
N2 C7 C6 123.2(5) . . ?
C9 C8 C5 120.2(5) . . ?
N2 C9 C8 123.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.080
_refine_diff_density_rms         0.157


data_2
_database_code_depnum_ccdc_archive 'CCDC 896254'
#TrackingRef '2.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C54 H106 Mn7 N12 O51 P6'
_chemical_formula_weight         2309.91

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           rhombohedral
_symmetry_space_group_name_H-M   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'
'-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                   22.5060(13)
_cell_length_b                   22.5060(13)
_cell_length_c                   13.2344(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     5805.4(7)
_cell_formula_units_Z            3
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4372
_cell_measurement_theta_min      3.1356
_cell_measurement_theta_max      27.4624

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.982
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3561
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9213
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15196
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.60
_diffrn_reflns_theta_max         27.46
_reflns_number_total             2954
_reflns_number_gt                2405
_reflns_threshold_expression     >2sigma(I)

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0866P)^2^+85.3069P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2954
_refine_ls_number_parameters     197
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0747
_refine_ls_wR_factor_ref         0.1957
_refine_ls_wR_factor_gt          0.1814
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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 0.21314(4) -0.27962(4) 0.03036(7) 0.0261(3) Uani 1 1 d . . .
Mn2 Mn 0.3333 -0.3333 0.1667 0.0236(4) Uani 1 6 d S . .
P1 P 0.37730(6) -0.18331(7) 0.05652(11) 0.0243(3) Uani 1 1 d . . .
O1 O 0.32038(17) -0.25813(17) 0.0723(3) 0.0257(8) Uani 1 1 d . . .
O2 O 0.4389(2) -0.1799(2) 0.0066(4) 0.0488(13) Uani 1 1 d . . .
O3 O 0.3939(2) -0.1388(2) 0.1494(3) 0.0390(10) Uani 1 1 d . . .
O4 O 0.2255(3) -0.2726(2) -0.1424(4) 0.0539(13) Uani 1 1 d . . .
O5 O 0.2170(3) -0.2157(3) -0.2739(4) 0.0575(14) Uani 1 1 d . . .
O6 O 0.3333 -0.3333 -0.3333 0.164(12) Uani 1 6 d S . .
O7 O 0.3652(3) -0.2678(3) -0.4144(5) 0.0735(17) Uani 1 1 d . . .
O8 O 0.3148(13) -0.2681(17) -0.4961(17) 0.74(5) Uani 1 1 d . . .
O9 O 0.2738(4) -0.2621(4) -0.4133(7) 0.102(2) Uani 1 1 d . . .
O10 O 0.3333 -0.3333 -0.5934(13) 0.085(5) Uani 1 3 d S . .
N1 N 0.2728(2) -0.1642(2) -0.0176(3) 0.0243(9) Uani 1 1 d . . .
N2 N 0.4030(3) 0.1003(2) 0.0049(4) 0.0376(12) Uani 1 1 d . . .
C1 C 0.3437(3) -0.1501(3) -0.0386(4) 0.0273(11) Uani 1 1 d . . .
H2 H 0.3739 -0.1009 -0.0438 0.033 Uiso 1 1 calc R . .
H1 H 0.3441 -0.1701 -0.1034 0.033 Uiso 1 1 calc R . .
C2 C 0.2275(3) -0.2211(3) -0.1829(5) 0.0399(14) Uani 1 1 d . . .
C3 C 0.2412(3) -0.1613(3) -0.1137(4) 0.0330(12) Uani 1 1 d . . .
H4 H 0.2715 -0.1184 -0.1477 0.040 Uiso 1 1 calc R . .
H3 H 0.1984 -0.1624 -0.0998 0.040 Uiso 1 1 calc R . .
C4 C 0.2704(3) -0.1180(3) 0.0606(4) 0.0306(12) Uani 1 1 d . . .
H5 H 0.2838 -0.1286 0.1248 0.037 Uiso 1 1 calc R . .
H6 H 0.2233 -0.1282 0.0673 0.037 Uiso 1 1 calc R . .
C5 C 0.3156(3) -0.0414(3) 0.0410(4) 0.0305(12) Uani 1 1 d . . .
C6 C 0.2919(3) -0.0019(3) -0.0046(5) 0.0374(13) Uani 1 1 d . . .
H7 H 0.2463 -0.0218 -0.0242 0.045 Uiso 1 1 calc R . .
C7 C 0.3368(3) 0.0679(3) -0.0212(5) 0.0393(14) Uani 1 1 d . . .
H8 H 0.3195 0.0932 -0.0521 0.047 Uiso 1 1 calc R . .
C8 C 0.3842(3) -0.0079(3) 0.0691(5) 0.0409(15) Uani 1 1 d . . .
H9 H 0.4025 -0.0320 0.1006 0.049 Uiso 1 1 calc R . .
C9 C 0.4253(3) 0.0615(3) 0.0500(6) 0.0450(16) Uani 1 1 d . . .
H10 H 0.4711 0.0826 0.0696 0.054 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 0.0221(4) 0.0179(4) 0.0373(5) 0.0029(3) -0.0009(3) 0.0093(3)
Mn2 0.0174(5) 0.0174(5) 0.0360(11) 0.000 0.000 0.0087(3)
P1 0.0172(6) 0.0192(6) 0.0369(8) 0.0062(5) 0.0018(5) 0.0093(5)
O1 0.0187(16) 0.0198(17) 0.037(2) 0.0053(14) -0.0006(14) 0.0082(14)
O2 0.032(2) 0.043(2) 0.084(4) 0.032(2) 0.025(2) 0.028(2)
O3 0.047(3) 0.025(2) 0.042(2) 0.0008(17) -0.0175(19) 0.0160(19)
O4 0.075(4) 0.039(3) 0.051(3) -0.007(2) -0.018(3) 0.030(3)
O5 0.069(4) 0.060(3) 0.044(3) -0.002(2) -0.015(2) 0.032(3)
O6 0.235(19) 0.235(19) 0.022(9) 0.000 0.000 0.117(9)
O7 0.075(4) 0.072(4) 0.076(4) -0.006(3) -0.003(3) 0.039(3)
O8 0.31(3) 0.86(7) 0.34(3) 0.45(4) -0.21(3) -0.23(4)
O9 0.106(6) 0.093(6) 0.089(6) 0.006(4) 0.019(5) 0.037(5)
O10 0.018(2) 0.018(2) 0.219(17) 0.000 0.000 0.0091(12)
N1 0.019(2) 0.021(2) 0.034(2) 0.0038(17) -0.0014(17) 0.0103(17)
N2 0.032(3) 0.023(2) 0.053(3) 0.005(2) 0.006(2) 0.010(2)
C1 0.024(2) 0.025(2) 0.033(3) 0.009(2) 0.007(2) 0.012(2)
C2 0.037(3) 0.041(3) 0.043(4) 0.000(3) -0.008(3) 0.021(3)
C3 0.031(3) 0.029(3) 0.039(3) 0.008(2) -0.007(2) 0.015(2)
C4 0.026(3) 0.025(3) 0.039(3) 0.003(2) 0.002(2) 0.011(2)
C5 0.031(3) 0.025(3) 0.036(3) 0.001(2) 0.003(2) 0.014(2)
C6 0.029(3) 0.029(3) 0.057(4) 0.000(3) -0.001(3) 0.016(2)
C7 0.042(3) 0.031(3) 0.052(4) 0.008(3) 0.004(3) 0.023(3)
C8 0.034(3) 0.025(3) 0.058(4) 0.005(3) -0.012(3) 0.011(2)
C9 0.034(3) 0.027(3) 0.066(5) 0.008(3) -0.005(3) 0.010(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
Mn1 O2 2.042(4) 2_545 ?
Mn1 O3 2.074(4) 15_445 ?
Mn1 O1 2.280(3) . ?
Mn1 O4 2.299(5) . ?
Mn1 N1 2.337(4) . ?
Mn1 N2 2.370(5) 11 ?
Mn2 O1 2.237(3) . ?
Mn2 O1 2.237(3) 15_445 ?
Mn2 O1 2.237(3) 14 ?
Mn2 O1 2.237(3) 13_545 ?
Mn2 O1 2.237(3) 2_545 ?
Mn2 O1 2.237(3) 3_655 ?
P1 O2 1.504(4) . ?
P1 O3 1.510(5) . ?
P1 O1 1.537(4) . ?
P1 C1 1.810(5) . ?
O2 Mn1 2.042(4) 3_655 ?
O3 Mn1 2.074(4) 14 ?
O4 C2 1.259(8) . ?
O5 C2 1.244(8) . ?
O6 O7 1.668(7) 15_444 ?
O6 O7 1.668(7) . ?
O6 O7 1.668(7) 2_545 ?
O6 O7 1.668(7) 14_554 ?
O6 O7 1.668(7) 13_544 ?
O6 O7 1.668(7) 3_655 ?
O7 O8 1.57(2) . ?
O8 O9 1.48(4) . ?
N1 C3 1.473(7) . ?
N1 C4 1.488(7) . ?
N1 C1 1.490(6) . ?
N2 C7 1.337(8) . ?
N2 C9 1.345(8) . ?
N2 Mn1 2.370(5) 12 ?
C2 C3 1.526(9) . ?
C4 C5 1.524(7) . ?
C5 C6 1.381(8) . ?
C5 C8 1.389(8) . ?
C6 C7 1.396(8) . ?
C8 C9 1.383(8) . ?

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
O2 Mn1 O3 104.5(2) 2_545 15_445 ?
O2 Mn1 O1 91.79(15) 2_545 . ?
O3 Mn1 O1 85.85(15) 15_445 . ?
O2 Mn1 O4 83.52(19) 2_545 . ?
O3 Mn1 O4 170.83(17) 15_445 . ?
O1 Mn1 O4 98.55(17) . . ?
O2 Mn1 N1 152.5(2) 2_545 . ?
O3 Mn1 N1 102.00(16) 15_445 . ?
O1 Mn1 N1 82.63(13) . . ?
O4 Mn1 N1 70.80(16) . . ?
O2 Mn1 N2 88.39(17) 2_545 11 ?
O3 Mn1 N2 91.46(18) 15_445 11 ?
O1 Mn1 N2 177.26(17) . 11 ?
O4 Mn1 N2 84.19(19) . 11 ?
N1 Mn1 N2 98.45(16) . 11 ?
O1 Mn2 O1 88.16(14) . 15_445 ?
O1 Mn2 O1 88.16(14) . 14 ?
O1 Mn2 O1 91.84(14) 15_445 14 ?
O1 Mn2 O1 180.0 . 13_545 ?
O1 Mn2 O1 91.84(14) 15_445 13_545 ?
O1 Mn2 O1 91.84(14) 14 13_545 ?
O1 Mn2 O1 91.84(14) . 2_545 ?
O1 Mn2 O1 88.16(14) 15_445 2_545 ?
O1 Mn2 O1 179.997(1) 14 2_545 ?
O1 Mn2 O1 88.16(14) 13_545 2_545 ?
O1 Mn2 O1 91.84(14) . 3_655 ?
O1 Mn2 O1 180.0 15_445 3_655 ?
O1 Mn2 O1 88.16(14) 14 3_655 ?
O1 Mn2 O1 88.16(14) 13_545 3_655 ?
O1 Mn2 O1 91.84(14) 2_545 3_655 ?
O2 P1 O3 114.1(3) . . ?
O2 P1 O1 110.9(2) . . ?
O3 P1 O1 114.3(2) . . ?
O2 P1 C1 103.8(3) . . ?
O3 P1 C1 107.9(2) . . ?
O1 P1 C1 104.8(2) . . ?
P1 O1 Mn2 123.5(2) . . ?
P1 O1 Mn1 114.41(18) . . ?
Mn2 O1 Mn1 119.99(15) . . ?
P1 O2 Mn1 139.3(3) . 3_655 ?
P1 O3 Mn1 133.1(2) . 14 ?
C2 O4 Mn1 115.8(4) . . ?
O7 O6 O7 96.9(3) 15_444 . ?
O7 O6 O7 96.9(3) 15_444 2_545 ?
O7 O6 O7 83.1(3) . 2_545 ?
O7 O6 O7 83.1(3) 15_444 14_554 ?
O7 O6 O7 96.9(3) . 14_554 ?
O7 O6 O7 179.996(1) 2_545 14_554 ?
O7 O6 O7 83.1(3) 15_444 13_544 ?
O7 O6 O7 179.996(1) . 13_544 ?
O7 O6 O7 96.9(3) 2_545 13_544 ?
O7 O6 O7 83.1(3) 14_554 13_544 ?
O7 O6 O7 179.999(1) 15_444 3_655 ?
O7 O6 O7 83.1(3) . 3_655 ?
O7 O6 O7 83.1(3) 2_545 3_655 ?
O7 O6 O7 96.9(3) 14_554 3_655 ?
O7 O6 O7 96.9(3) 13_544 3_655 ?
O8 O7 O6 116.7(8) . . ?
O9 O8 O7 88.4(12) . . ?
C3 N1 C4 112.5(4) . . ?
C3 N1 C1 108.6(4) . . ?
C4 N1 C1 112.9(4) . . ?
C3 N1 Mn1 105.2(3) . . ?
C4 N1 Mn1 112.7(3) . . ?
C1 N1 Mn1 104.3(3) . . ?
C7 N2 C9 115.9(5) . . ?
C7 N2 Mn1 130.9(4) . 12 ?
C9 N2 Mn1 112.9(4) . 12 ?
N1 C1 P1 114.0(3) . . ?
O5 C2 O4 125.5(6) . . ?
O5 C2 C3 117.5(6) . . ?
O4 C2 C3 117.0(6) . . ?
N1 C3 C2 111.7(4) . . ?
N1 C4 C5 115.9(5) . . ?
C6 C5 C8 116.7(5) . . ?
C6 C5 C4 123.3(5) . . ?
C8 C5 C4 120.0(5) . . ?
C5 C6 C7 119.9(6) . . ?
N2 C7 C6 123.7(6) . . ?
C9 C8 C5 119.9(6) . . ?
N2 C9 C8 123.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.139


data_3
_database_code_depnum_ccdc_archive 'CCDC 896255'
#TrackingRef '3.CIF'


_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H17 Co N2 O8 P'
_chemical_formula_weight         371.15

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                   9.484(6)
_cell_length_b                   8.377(5)
_cell_length_c                   18.414(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 103.319(12)
_cell_angle_gamma                90.00
_cell_volume                     1423.6(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2824
_cell_measurement_theta_min      2.6839
_cell_measurement_theta_max      27.4817

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.1000
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.732
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9171
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?

_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  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10687
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.68
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3109
_reflns_number_gt                2407
_reflns_threshold_expression     >2sigma(I)

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+4.0158P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3109
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0682
_refine_ls_wR_factor_ref         0.1786
_refine_ls_wR_factor_gt          0.1635
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_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
Co1 Co -0.78359(7) -0.13931(8) 0.33720(4) 0.0223(2) Uani 1 1 d . . .
P1 P -0.67124(15) -0.48014(16) 0.33127(7) 0.0256(3) Uani 1 1 d . . .
O1 O -0.8070(4) -0.3837(4) 0.3214(2) 0.0286(8) Uani 1 1 d . . .
O2 O -0.6796(4) -0.6178(4) 0.27828(19) 0.0285(8) Uani 1 1 d . . .
O3 O -0.6312(5) -0.5402(5) 0.4138(2) 0.0361(9) Uani 1 1 d . . .
H1 H -0.5649 -0.6051 0.4189 0.054 Uiso 1 1 calc R . .
O4 O -0.7304(4) -0.1646(5) 0.4509(2) 0.0374(10) Uani 1 1 d . . .
O5 O -0.5690(5) -0.2572(6) 0.5485(2) 0.0470(12) Uani 1 1 d . . .
O6 O -0.7532(5) 0.1107(5) 0.3539(3) 0.0373(10) Uani 1 1 d . . .
H3 H -0.711(7) 0.178(8) 0.331(4) 0.042(19) Uiso 1 1 d . . .
H2 H -0.805(9) 0.181(10) 0.368(5) 0.06(3) Uiso 1 1 d . . .
O7 O -0.9481(11) 0.3495(14) 0.3982(7) 0.177(5) Uani 1 1 d . . .
O8 O -0.8076(13) -0.4591(18) 0.5653(7) 0.202(6) Uani 1 1 d . . .
N1 N -0.5416(4) -0.1895(5) 0.3561(2) 0.0237(9) Uani 1 1 d . . .
N2 N -0.0084(5) -0.1146(5) 0.3344(3) 0.0289(10) Uani 1 1 d . . .
C1 C -0.5302(5) -0.3443(6) 0.3193(3) 0.0265(11) Uani 1 1 d . . .
H5 H -0.4363 -0.3915 0.3403 0.032 Uiso 1 1 calc R . .
H4 H -0.5376 -0.3269 0.2665 0.032 Uiso 1 1 calc R . .
C2 C -0.6059(6) -0.2156(7) 0.4808(3) 0.0341(13) Uani 1 1 d . . .
C3 C -0.4866(6) -0.2026(7) 0.4373(3) 0.0324(12) Uani 1 1 d . . .
H7 H -0.4275 -0.1097 0.4549 0.039 Uiso 1 1 calc R . .
H6 H -0.4247 -0.2959 0.4480 0.039 Uiso 1 1 calc R . .
C4 C -0.4658(5) -0.0600(6) 0.3242(3) 0.0295(12) Uani 1 1 d . . .
H9 H -0.4778 0.0388 0.3495 0.035 Uiso 1 1 calc R . .
H8 H -0.5143 -0.0468 0.2721 0.035 Uiso 1 1 calc R . .
C5 C -0.3053(6) -0.0834(7) 0.3287(3) 0.0300(12) Uani 1 1 d . . .
C6 C -0.2017(6) -0.0255(8) 0.3886(4) 0.0421(15) Uani 1 1 d . . .
H10 H -0.2294 0.0258 0.4279 0.051 Uiso 1 1 calc R . .
C7 C -0.0566(7) -0.0447(9) 0.3893(4) 0.0435(15) Uani 1 1 d . . .
H11 H 0.0115 -0.0067 0.4304 0.052 Uiso 1 1 calc R . .
C8 C -0.1094(6) -0.1722(8) 0.2779(3) 0.0381(14) Uani 1 1 d . . .
H12 H -0.0789 -0.2223 0.2391 0.046 Uiso 1 1 calc R . .
C9 C -0.2552(6) -0.1620(8) 0.2734(3) 0.0377(14) Uani 1 1 d . . .
H13 H -0.3205 -0.2077 0.2332 0.045 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
Co1 0.0169(4) 0.0255(4) 0.0249(4) 0.0015(3) 0.0057(3) 0.0016(3)
P1 0.0253(7) 0.0240(6) 0.0277(7) -0.0007(5) 0.0062(5) -0.0005(5)
O1 0.0202(18) 0.0251(18) 0.041(2) 0.0003(15) 0.0071(16) -0.0025(14)
O2 0.031(2) 0.0301(19) 0.0252(18) -0.0048(15) 0.0074(16) -0.0053(16)
O3 0.041(2) 0.037(2) 0.030(2) 0.0062(16) 0.0075(17) 0.0065(18)
O4 0.031(2) 0.056(3) 0.0266(19) 0.0057(18) 0.0099(17) 0.0145(19)
O5 0.050(3) 0.064(3) 0.027(2) 0.007(2) 0.0079(19) 0.021(2)
O6 0.041(3) 0.027(2) 0.047(3) 0.0024(18) 0.017(2) -0.0024(19)
O7 0.122(8) 0.157(10) 0.275(15) 0.031(9) 0.094(9) -0.021(7)
O8 0.150(10) 0.271(16) 0.195(12) 0.046(11) 0.062(9) -0.052(10)
N1 0.018(2) 0.025(2) 0.028(2) -0.0023(17) 0.0047(17) -0.0010(17)
N2 0.019(2) 0.037(2) 0.032(2) -0.0012(19) 0.0096(19) 0.0037(19)
C1 0.021(3) 0.030(3) 0.029(3) -0.006(2) 0.006(2) 0.003(2)
C2 0.029(3) 0.052(3) 0.022(3) 0.002(2) 0.007(2) 0.010(3)
C3 0.024(3) 0.039(3) 0.031(3) -0.005(2) -0.002(2) 0.003(2)
C4 0.018(3) 0.027(3) 0.044(3) 0.000(2) 0.009(2) -0.003(2)
C5 0.028(3) 0.030(3) 0.032(3) 0.002(2) 0.007(2) -0.001(2)
C6 0.027(3) 0.061(4) 0.042(3) -0.020(3) 0.013(3) -0.002(3)
C7 0.025(3) 0.067(4) 0.036(3) -0.009(3) 0.003(3) -0.005(3)
C8 0.024(3) 0.054(4) 0.040(3) -0.011(3) 0.015(3) -0.006(3)
C9 0.023(3) 0.052(4) 0.039(3) -0.012(3) 0.008(2) -0.009(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
Co1 O4 2.049(4) . ?
Co1 O1 2.072(4) . ?
Co1 O2 2.082(4) 2_355 ?
Co1 O6 2.127(4) . ?
Co1 N2 2.131(5) 1_455 ?
Co1 N1 2.280(4) . ?
P1 O1 1.495(4) . ?
P1 O2 1.501(4) . ?
P1 O3 1.562(4) . ?
P1 C1 1.808(6) . ?
O2 Co1 2.082(4) 2_345 ?
O4 C2 1.257(6) . ?
O5 C2 1.264(7) . ?
N1 C3 1.471(7) . ?
N1 C1 1.478(6) . ?
N1 C4 1.494(7) . ?
N2 C8 1.332(7) . ?
N2 C7 1.337(8) . ?
N2 Co1 2.131(5) 1_655 ?
C2 C3 1.532(8) . ?
C4 C5 1.518(7) . ?
C5 C6 1.385(8) . ?
C5 C9 1.387(8) . ?
C6 C7 1.382(9) . ?
C8 C9 1.369(8) . ?

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 Co1 O1 91.96(16) . . ?
O4 Co1 O2 175.41(15) . 2_355 ?
O1 Co1 O2 87.42(15) . 2_355 ?
O4 Co1 O6 87.75(18) . . ?
O1 Co1 O6 178.41(16) . . ?
O2 Co1 O6 92.74(16) 2_355 . ?
O4 Co1 N2 92.52(17) . 1_455 ?
O1 Co1 N2 91.04(16) . 1_455 ?
O2 Co1 N2 92.04(16) 2_355 1_455 ?
O6 Co1 N2 90.54(18) . 1_455 ?
O4 Co1 N1 79.80(15) . . ?
O1 Co1 N1 84.89(14) . . ?
O2 Co1 N1 95.61(15) 2_355 . ?
O6 Co1 N1 93.52(17) . . ?
N2 Co1 N1 171.15(17) 1_455 . ?
O1 P1 O2 114.9(2) . . ?
O1 P1 O3 107.6(2) . . ?
O2 P1 O3 110.5(2) . . ?
O1 P1 C1 106.6(2) . . ?
O2 P1 C1 109.5(2) . . ?
O3 P1 C1 107.5(2) . . ?
P1 O1 Co1 117.1(2) . . ?
P1 O2 Co1 134.6(2) . 2_345 ?
C2 O4 Co1 117.9(4) . . ?
C3 N1 C1 110.8(4) . . ?
C3 N1 C4 111.3(4) . . ?
C1 N1 C4 111.3(4) . . ?
C3 N1 Co1 106.1(3) . . ?
C1 N1 Co1 105.6(3) . . ?
C4 N1 Co1 111.4(3) . . ?
C8 N2 C7 116.1(5) . . ?
C8 N2 Co1 121.3(4) . 1_655 ?
C7 N2 Co1 122.6(4) . 1_655 ?
N1 C1 P1 111.2(4) . . ?
O4 C2 O5 122.9(5) . . ?
O4 C2 C3 118.7(5) . . ?
O5 C2 C3 117.7(5) . . ?
N1 C3 C2 113.9(4) . . ?
N1 C4 C5 116.8(4) . . ?
C6 C5 C9 116.8(5) . . ?
C6 C5 C4 121.2(5) . . ?
C9 C5 C4 122.0(5) . . ?
C7 C6 C5 119.3(6) . . ?
N2 C7 C6 123.8(6) . . ?
N2 C8 C9 124.1(6) . . ?
C8 C9 C5 119.8(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
O6 H2 O7 0.85(9) 2.12(9) 2.963(13) 176(8) .
O6 H3 O2 0.86(7) 2.02(7) 2.837(6) 159(6) 1_565
O3 H1 O5 0.82 1.72 2.522(6) 166.0 3_446

_diffrn_measured_fraction_theta_max 0.951
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.951
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.126