# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012


data_global
_journal_name_full               'New J.Chem.'
_journal_coden_cambridge         0440
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_name        'Zhen-Gang Sun'
_publ_contact_author_email       szg188@163.com
loop_
_publ_author_name
'Hui Tian'
'Yanyu Zhu'
'Zhen-Gang Sun'
'Fei Tong'
'Jiang Zhu'
'Wei Chu'
'Shou-Hui Sun'
'Ming-Jing Zheng'

data_0910i
_database_code_depnum_ccdc_archive 'CCDC 875544'
#TrackingRef 'szg184(875544).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H58 Mn N4 O24 P6'
_chemical_formula_weight         919.41

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-3c '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   16.6808(8)
_cell_length_b                   16.6808(8)
_cell_length_c                   52.257(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12592.5(15)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2546
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      19.89

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.36
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5796
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7666
_exptl_absorpt_correction_T_max  0.8084
_exptl_absorpt_process_details   sadabs

_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  'Smart Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            19187
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_theta_min         2.10
_diffrn_reflns_theta_max         24.62
_reflns_number_total             2362
_reflns_number_gt                1706
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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          
;
OMIT -3 53
ISOR 0.01 C5

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^)+(0.1014P)^2^+50.5415P] 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         2362
_refine_ls_number_parameters     151
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0549
_refine_ls_wR_factor_ref         0.1747
_refine_ls_wR_factor_gt          0.1507
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.003
_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 0.3333 0.6667 0.04543(2) 0.0340(3) Uani 1 3 d S . .
P1 P 0.44780(9) 0.55686(9) 0.02688(3) 0.0483(4) Uani 1 1 d . . .
P2 P 0.52728(8) 0.68517(8) 0.07306(2) 0.0427(4) Uani 1 1 d . . .
O1 O 0.3786(3) 0.5886(3) 0.02376(6) 0.0575(9) Uani 1 1 d . . .
O2 O 0.3979(2) 0.4512(2) 0.02091(7) 0.0656(11) Uani 1 1 d . . .
H2A H 0.4299 0.4404 0.0112 0.098 Uiso 1 1 calc R . .
O3 O 0.5346(3) 0.6090(2) 0.01092(7) 0.0613(10) Uani 1 1 d . . .
O4 O 0.3964(2) 0.5058(2) 0.07484(6) 0.0510(9) Uani 1 1 d . . .
H4D H 0.4083 0.4793 0.0861 0.077 Uiso 1 1 calc R . .
O5 O 0.6060(2) 0.7493(2) 0.05461(6) 0.0517(9) Uani 1 1 d . . .
H5D H 0.6558 0.7589 0.0604 0.077 Uiso 1 1 calc R . .
O6 O 0.5628(2) 0.6882(2) 0.09990(6) 0.0545(9) Uani 1 1 d . . .
O7 O 0.4503(2) 0.7071(2) 0.07165(6) 0.0456(8) Uani 1 1 d . . .
C1 C 0.4798(3) 0.5664(3) 0.06093(10) 0.0466(12) Uani 1 1 d . . .
C2 C 0.5484(4) 0.5320(4) 0.06518(13) 0.0708(17) Uani 1 1 d . . .
H2B H 0.5226 0.4702 0.0586 0.106 Uiso 1 1 calc R . .
H2C H 0.5603 0.5322 0.0832 0.106 Uiso 1 1 calc R . .
H2D H 0.6052 0.5720 0.0564 0.106 Uiso 1 1 calc R . .
C3 C 0.5222(8) 0.7650(7) -0.02405(17) 0.126(3) Uani 1 1 d . . .
H3A H 0.4595 0.7174 -0.0205 0.190 Uiso 1 1 d R . .
H3B H 0.5484 0.7434 -0.0371 0.190 Uiso 1 1 d R . .
H3C H 0.5225 0.8196 -0.0303 0.190 Uiso 1 1 d R . .
C4 C 0.6694(7) 0.8579(6) -0.0025(2) 0.143(4) Uani 1 1 d . . .
H4A H 0.7013 0.8703 0.0138 0.214 Uiso 1 1 d R . .
H4B H 0.6714 0.9134 -0.0087 0.214 Uiso 1 1 d R . .
H4C H 0.6989 0.8381 -0.0150 0.214 Uiso 1 1 d R . .
C5 C 0.4254(10) 0.7653(8) 0.13107(19) 0.175(5) Uani 1 1 d U . .
H5A H 0.4797 0.7638 0.1255 0.262 Uiso 1 1 d R . .
H5B H 0.4247 0.7680 0.1497 0.262 Uiso 1 1 d R . .
H5C H 0.4264 0.8191 0.1239 0.262 Uiso 1 1 d R . .
N1 N 0.5722(4) 0.7867(4) -0.00027(11) 0.0807(16) Uani 1 1 d . . .
H1B H 0.5709 0.7350 0.0055 0.097 Uiso 1 1 d R . .
H1A H 0.5463 0.8060 0.0118 0.097 Uiso 1 1 d R . .
N2 N 0.3333 0.6667 0.11999(19) 0.119(4) Uani 1 3 d S . .
H2F H 0.3333 0.6667 0.1025 0.143 Uiso 1 3 d SR . .
O1W O 0.3642(5) 0.3910(4) 0.11813(13) 0.150(3) Uani 1 1 d . . .
H1WA H 0.3178 0.3372 0.1158 0.225 Uiso 1 1 d R . .
H1WB H 0.4138 0.3903 0.1147 0.225 Uiso 1 1 d 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 0.0313(4) 0.0313(4) 0.0393(6) 0.000 0.000 0.0156(2)
P1 0.0451(8) 0.0396(7) 0.0618(8) -0.0071(6) 0.0110(6) 0.0223(6)
P2 0.0315(6) 0.0395(7) 0.0562(8) 0.0006(5) -0.0041(5) 0.0171(5)
O1 0.067(2) 0.072(2) 0.0485(19) -0.0142(17) -0.0036(17) 0.046(2)
O2 0.052(2) 0.043(2) 0.093(3) -0.0131(19) 0.0248(19) 0.0166(17)
O3 0.063(2) 0.0392(19) 0.075(2) -0.0038(17) 0.0264(19) 0.0206(18)
O4 0.0433(19) 0.0436(19) 0.068(2) 0.0185(16) 0.0053(16) 0.0229(16)
O5 0.0348(17) 0.051(2) 0.063(2) 0.0107(16) -0.0007(15) 0.0167(16)
O6 0.0402(19) 0.058(2) 0.058(2) 0.0086(17) -0.0086(16) 0.0192(17)
O7 0.0360(17) 0.0413(18) 0.063(2) -0.0090(15) -0.0092(15) 0.0217(15)
C1 0.034(2) 0.044(3) 0.067(3) 0.004(2) 0.004(2) 0.023(2)
C2 0.051(3) 0.060(4) 0.114(5) 0.014(3) 0.004(3) 0.037(3)
C3 0.163(10) 0.135(8) 0.104(7) 0.033(6) 0.045(7) 0.091(7)
C4 0.111(7) 0.092(6) 0.189(10) 0.015(6) 0.057(7) 0.024(6)
C5 0.194(8) 0.167(8) 0.098(6) -0.010(6) 0.008(6) 0.041(6)
N1 0.092(4) 0.073(4) 0.087(4) 0.019(3) 0.033(3) 0.049(3)
N2 0.153(7) 0.153(7) 0.051(6) 0.000 0.000 0.076(4)
O1W 0.156(6) 0.103(4) 0.148(5) 0.039(4) -0.038(5) 0.033(4)

_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 2.129(3) 3_565 ?
Mn1 O1 2.129(3) 2_665 ?
Mn1 O1 2.129(3) . ?
Mn1 O7 2.196(3) 2_665 ?
Mn1 O7 2.196(3) 3_565 ?
Mn1 O7 2.196(3) . ?
P1 O1 1.500(4) . ?
P1 O3 1.514(4) . ?
P1 O2 1.558(4) . ?
P1 C1 1.841(5) . ?
P2 O7 1.503(3) . ?
P2 O6 1.514(3) . ?
P2 O5 1.547(3) . ?
P2 C1 1.840(5) . ?
O2 H2A 0.8200 . ?
O4 C1 1.441(6) . ?
O4 H4D 0.8200 . ?
O5 H5D 0.8200 . ?
C1 C2 1.531(7) . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C3 N1 1.438(11) . ?
C3 H3A 0.9631 . ?
C3 H3B 0.9696 . ?
C3 H3C 0.9643 . ?
C4 N1 1.459(10) . ?
C4 H4A 0.9732 . ?
C4 H4B 0.9641 . ?
C4 H4C 0.9686 . ?
C5 N2 1.696(12) . ?
C5 H5A 0.9642 . ?
C5 H5B 0.9760 . ?
C5 H5C 0.9647 . ?
N1 H1B 0.9040 . ?
N1 H1A 0.9081 . ?
N2 C5 1.696(12) 2_665 ?
N2 C5 1.696(12) 3_565 ?
N2 H2F 0.9150 . ?
O1W H1WA 0.8525 . ?
O1W H1WB 0.8529 . ?

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 94.35(13) 3_565 2_665 ?
O1 Mn1 O1 94.35(13) 3_565 . ?
O1 Mn1 O1 94.35(13) 2_665 . ?
O1 Mn1 O7 90.84(13) 3_565 2_665 ?
O1 Mn1 O7 89.27(12) 2_665 2_665 ?
O1 Mn1 O7 173.42(14) . 2_665 ?
O1 Mn1 O7 89.27(12) 3_565 3_565 ?
O1 Mn1 O7 173.42(14) 2_665 3_565 ?
O1 Mn1 O7 90.84(13) . 3_565 ?
O7 Mn1 O7 85.18(13) 2_665 3_565 ?
O1 Mn1 O7 173.42(14) 3_565 . ?
O1 Mn1 O7 90.84(13) 2_665 . ?
O1 Mn1 O7 89.27(12) . . ?
O7 Mn1 O7 85.18(13) 2_665 . ?
O7 Mn1 O7 85.18(13) 3_565 . ?
O1 P1 O3 114.9(2) . . ?
O1 P1 O2 107.9(2) . . ?
O3 P1 O2 110.89(18) . . ?
O1 P1 C1 108.4(2) . . ?
O3 P1 C1 109.3(2) . . ?
O2 P1 C1 105.0(2) . . ?
O7 P2 O6 113.9(2) . . ?
O7 P2 O5 109.54(19) . . ?
O6 P2 O5 111.79(18) . . ?
O7 P2 C1 106.56(19) . . ?
O6 P2 C1 107.8(2) . . ?
O5 P2 C1 106.8(2) . . ?
P1 O1 Mn1 136.8(2) . . ?
P1 O2 H2A 109.5 . . ?
C1 O4 H4D 109.5 . . ?
P2 O5 H5D 109.5 . . ?
P2 O7 Mn1 133.76(19) . . ?
O4 C1 C2 107.7(4) . . ?
O4 C1 P2 109.1(3) . . ?
C2 C1 P2 110.7(4) . . ?
O4 C1 P1 106.9(3) . . ?
C2 C1 P1 110.2(4) . . ?
P2 C1 P1 112.1(3) . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2B C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N1 C3 H3A 107.2 . . ?
N1 C3 H3B 112.8 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 108.9 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 108.9 . . ?
N1 C4 H4A 111.7 . . ?
N1 C4 H4B 107.4 . . ?
H4A C4 H4B 109.7 . . ?
N1 C4 H4C 108.9 . . ?
H4A C4 H4C 110.1 . . ?
H4B C4 H4C 108.9 . . ?
N2 C5 H5A 106.2 . . ?
N2 C5 H5B 111.1 . . ?
H5A C5 H5B 109.7 . . ?
N2 C5 H5C 110.9 . . ?
H5A C5 H5C 109.2 . . ?
H5B C5 H5C 109.8 . . ?
C4 N1 C3 113.8(7) . . ?
C4 N1 H1B 106.9 . . ?
C3 N1 H1B 108.4 . . ?
C4 N1 H1A 107.4 . . ?
C3 N1 H1A 111.6 . . ?
H1B N1 H1A 108.4 . . ?
C5 N2 C5 109.0(5) 2_665 . ?
C5 N2 C5 109.0(5) 2_665 3_565 ?
C5 N2 C5 109.0(5) . 3_565 ?
C5 N2 H2F 110.0 2_665 . ?
C5 N2 H2F 110.0 . . ?
C5 N2 H2F 110.0 3_565 . ?
H1WA O1W H1WB 109.4 . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.62
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.949
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.076

# Attachment 'szg185(875545).cif'

data_0924i
_database_code_depnum_ccdc_archive 'CCDC 875545'
#TrackingRef 'szg185(875545).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H58 Co N4 O24 P6'
_chemical_formula_weight         923.40

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           Rhombohedral
_symmetry_space_group_name_H-M   'R-3c '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   16.6483(6)
_cell_length_b                   16.6483(6)
_cell_length_c                   51.521(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12366.7(10)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    6260
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      26.70

_exptl_crystal_description       block
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5820
_exptl_absorpt_coefficient_mu    0.731
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7439
_exptl_absorpt_correction_T_max  0.8315
_exptl_absorpt_process_details   sadabs

_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  'Smart Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            22102
_diffrn_reflns_av_R_equivalents  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0203
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         26.50
_reflns_number_total             2863
_reflns_number_gt                2251
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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          
;
OMIT -3 53
ISOR 0.01 O1W
ISOR 0.005 C5
DFIX 1.50 0.01 N2 C5
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^)+(0.1035P)^2^+33.7728P] 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         2863
_refine_ls_number_parameters     151
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0636
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1724
_refine_ls_wR_factor_gt          0.1578
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.158
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.3333 0.6667 0.045813(15) 0.0270(2) Uani 1 3 d S . .
P1 P 0.44574(6) 0.55891(6) 0.02632(2) 0.0384(3) Uani 1 1 d . . .
P2 P 0.52640(6) 0.68765(6) 0.072835(19) 0.0355(3) Uani 1 1 d . . .
O1 O 0.3763(2) 0.5910(2) 0.02364(5) 0.0449(7) Uani 1 1 d . . .
O2 O 0.39419(19) 0.45252(19) 0.02031(6) 0.0530(8) Uani 1 1 d . . .
H2A H 0.4260 0.4410 0.0105 0.080 Uiso 1 1 calc R . .
O3 O 0.5317(2) 0.60964(19) 0.00947(6) 0.0505(8) Uani 1 1 d . . .
O4 O 0.39795(18) 0.50733(18) 0.07520(5) 0.0447(7) Uani 1 1 d . . .
H4D H 0.4112 0.4812 0.0865 0.067 Uiso 1 1 calc R . .
O5 O 0.60506(18) 0.75251(18) 0.05405(5) 0.0442(7) Uani 1 1 d . . .
H5D H 0.6551 0.7623 0.0598 0.066 Uiso 1 1 calc R . .
O6 O 0.56240(18) 0.6919(2) 0.10005(5) 0.0480(7) Uani 1 1 d . . .
O7 O 0.44806(17) 0.70860(17) 0.07125(5) 0.0369(6) Uani 1 1 d . . .
C1 C 0.4799(3) 0.5683(3) 0.06061(8) 0.0390(8) Uani 1 1 d . . .
C2 C 0.5499(3) 0.5357(3) 0.06444(11) 0.0594(12) Uani 1 1 d . . .
H2B H 0.5245 0.4736 0.0579 0.089 Uiso 1 1 calc R . .
H2C H 0.5633 0.5366 0.0826 0.089 Uiso 1 1 calc R . .
H2D H 0.6059 0.5762 0.0552 0.089 Uiso 1 1 calc R . .
C3 C 0.5153(6) 0.7628(5) -0.02660(15) 0.102(2) Uani 1 1 d . . .
H3A H 0.4527 0.7153 -0.0231 0.153 Uiso 1 1 d R . .
H3B H 0.5416 0.7413 -0.0396 0.153 Uiso 1 1 d R . .
H3C H 0.5157 0.8174 -0.0328 0.153 Uiso 1 1 d R . .
C4 C 0.6659(6) 0.8581(5) -0.00533(19) 0.129(3) Uani 1 1 d . . .
H4A H 0.6978 0.8705 0.0110 0.193 Uiso 1 1 d R . .
H4B H 0.6679 0.9136 -0.0115 0.193 Uiso 1 1 d R . .
H4C H 0.6954 0.8383 -0.0178 0.193 Uiso 1 1 d R . .
C5 C 0.4265(7) 0.7586(6) 0.13114(18) 0.147(3) Uani 1 1 d DU . .
H5A H 0.4808 0.7570 0.1256 0.220 Uiso 1 1 d R . .
H5B H 0.4258 0.7612 0.1498 0.220 Uiso 1 1 d R . .
H5C H 0.4275 0.8124 0.1240 0.220 Uiso 1 1 d R . .
N1 N 0.5698(4) 0.7858(3) -0.00266(10) 0.0716(13) Uani 1 1 d . . .
H1B H 0.5685 0.7341 0.0032 0.086 Uiso 1 1 d R . .
H1A H 0.5439 0.8051 0.0094 0.086 Uiso 1 1 d R . .
N2 N 0.3333 0.6667 0.12125(17) 0.108(4) Uani 1 3 d SD . .
H2F H 0.3333 0.6667 0.1037 0.130 Uiso 1 3 d SR . .
O1W O 0.3627(4) 0.3891(4) 0.11834(12) 0.144(2) Uani 1 1 d U . .
H1WA H 0.3162 0.3353 0.1160 0.216 Uiso 1 1 d R . .
H1WB H 0.4123 0.3884 0.1149 0.216 Uiso 1 1 d 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 0.0242(3) 0.0242(3) 0.0327(4) 0.000 0.000 0.01209(15)
P1 0.0337(5) 0.0305(5) 0.0517(6) -0.0037(4) 0.0088(4) 0.0166(4)
P2 0.0260(5) 0.0318(5) 0.0471(6) 0.0018(4) -0.0050(4) 0.0133(4)
O1 0.0503(16) 0.0533(16) 0.0417(15) -0.0113(12) -0.0030(12) 0.0338(14)
O2 0.0420(15) 0.0339(14) 0.076(2) -0.0094(13) 0.0200(14) 0.0136(12)
O3 0.0488(17) 0.0344(14) 0.0632(18) -0.0026(12) 0.0207(14) 0.0170(13)
O4 0.0379(14) 0.0382(14) 0.0607(17) 0.0186(12) 0.0069(12) 0.0210(12)
O5 0.0301(13) 0.0423(15) 0.0543(16) 0.0072(12) -0.0033(11) 0.0137(12)
O6 0.0352(14) 0.0511(16) 0.0500(16) 0.0079(13) -0.0081(12) 0.0158(13)
O7 0.0314(13) 0.0332(13) 0.0481(15) -0.0075(11) -0.0093(11) 0.0177(11)
C1 0.0279(17) 0.0317(18) 0.059(2) 0.0053(16) 0.0049(16) 0.0164(14)
C2 0.042(2) 0.054(3) 0.095(4) 0.011(2) 0.003(2) 0.033(2)
C3 0.132(7) 0.103(5) 0.089(5) 0.023(4) 0.035(5) 0.072(5)
C4 0.095(6) 0.083(5) 0.182(10) 0.018(5) 0.054(6) 0.024(4)
C5 0.165(5) 0.139(5) 0.108(4) -0.013(4) 0.016(4) 0.054(4)
N1 0.084(3) 0.062(3) 0.082(3) 0.020(2) 0.037(3) 0.047(2)
N2 0.140(6) 0.140(6) 0.045(5) 0.000 0.000 0.070(3)
O1W 0.131(5) 0.103(4) 0.149(4) 0.050(3) -0.032(4) 0.021(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 O1 2.074(3) 3_565 ?
Co1 O1 2.074(3) 2_665 ?
Co1 O1 2.074(3) . ?
Co1 O7 2.126(2) 2_665 ?
Co1 O7 2.126(2) 3_565 ?
Co1 O7 2.126(2) . ?
P1 O1 1.503(3) . ?
P1 O3 1.518(3) . ?
P1 O2 1.565(3) . ?
P1 C1 1.838(4) . ?
P2 O7 1.511(3) . ?
P2 O6 1.513(3) . ?
P2 O5 1.550(3) . ?
P2 C1 1.846(4) . ?
O2 H2A 0.8200 . ?
O4 C1 1.439(5) . ?
O4 H4D 0.8200 . ?
O5 H5D 0.8200 . ?
C1 C2 1.525(5) . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C3 N1 1.464(10) . ?
C3 H3A 0.9607 . ?
C3 H3B 0.9620 . ?
C3 H3C 0.9611 . ?
C4 N1 1.450(8) . ?
C4 H4A 0.9622 . ?
C4 H4B 0.9610 . ?
C4 H4C 0.9614 . ?
C5 N2 1.623(8) . ?
C5 H5A 0.9613 . ?
C5 H5B 0.9623 . ?
C5 H5C 0.9610 . ?
N1 H1B 0.9010 . ?
N1 H1A 0.9010 . ?
N2 C5 1.623(8) 2_665 ?
N2 C5 1.623(8) 3_565 ?
N2 H2F 0.9021 . ?
O1W H1WA 0.8507 . ?
O1W H1WB 0.8507 . ?

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 Co1 O1 92.59(11) 3_565 2_665 ?
O1 Co1 O1 92.59(11) 3_565 . ?
O1 Co1 O1 92.59(11) 2_665 . ?
O1 Co1 O7 90.51(11) 3_565 2_665 ?
O1 Co1 O7 90.73(10) 2_665 2_665 ?
O1 Co1 O7 175.34(11) . 2_665 ?
O1 Co1 O7 90.73(10) 3_565 3_565 ?
O1 Co1 O7 175.34(11) 2_665 3_565 ?
O1 Co1 O7 90.51(11) . 3_565 ?
O7 Co1 O7 85.98(11) 2_665 3_565 ?
O1 Co1 O7 175.34(11) 3_565 . ?
O1 Co1 O7 90.51(11) 2_665 . ?
O1 Co1 O7 90.73(10) . . ?
O7 Co1 O7 85.98(11) 2_665 . ?
O7 Co1 O7 85.98(11) 3_565 . ?
O1 P1 O3 115.35(18) . . ?
O1 P1 O2 107.50(17) . . ?
O3 P1 O2 110.34(16) . . ?
O1 P1 C1 108.53(16) . . ?
O3 P1 C1 109.68(18) . . ?
O2 P1 C1 104.90(18) . . ?
O7 P2 O6 113.99(16) . . ?
O7 P2 O5 109.36(15) . . ?
O6 P2 O5 111.66(15) . . ?
O7 P2 C1 106.50(15) . . ?
O6 P2 C1 108.06(18) . . ?
O5 P2 C1 106.90(17) . . ?
P1 O1 Co1 136.52(17) . . ?
P1 O2 H2A 109.5 . . ?
C1 O4 H4D 109.5 . . ?
P2 O5 H5D 109.5 . . ?
P2 O7 Co1 134.00(15) . . ?
O4 C1 C2 107.8(3) . . ?
O4 C1 P2 108.7(3) . . ?
C2 C1 P2 110.8(3) . . ?
O4 C1 P1 107.4(3) . . ?
C2 C1 P1 110.7(3) . . ?
P2 C1 P1 111.40(19) . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2B C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 110.3 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 108.9 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.4 . . ?
N1 C4 H4A 110.9 . . ?
N1 C4 H4B 108.9 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 108.6 . . ?
H4A C4 H4C 109.6 . . ?
H4B C4 H4C 109.4 . . ?
N2 C5 H5A 110.5 . . ?
N2 C5 H5B 109.2 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 108.7 . . ?
H5A C5 H5C 109.4 . . ?
H5B C5 H5C 109.5 . . ?
C4 N1 C3 114.8(6) . . ?
C4 N1 H1B 108.3 . . ?
C3 N1 H1B 108.4 . . ?
C4 N1 H1A 107.1 . . ?
C3 N1 H1A 109.2 . . ?
H1B N1 H1A 108.9 . . ?
C5 N2 C5 110.6(4) 2_665 . ?
C5 N2 C5 110.6(4) 2_665 3_565 ?
C5 N2 C5 110.6(4) . 3_565 ?
C5 N2 H2F 108.3 2_665 . ?
C5 N2 H2F 108.3 . . ?
C5 N2 H2F 108.3 3_565 . ?
H1WA O1W H1WB 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.632
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.088

# Attachment 'szg186(875546).cif'

data_0924f
_database_code_depnum_ccdc_archive 'CCDC 875546'
#TrackingRef 'szg186(875546).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H58 N4 Ni O24 P6'
_chemical_formula_weight         923.18

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'
Ni Ni 0.3393 1.1124 '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-3c '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   16.6093(7)
_cell_length_b                   16.6093(7)
_cell_length_c                   51.213(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12235.4(12)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5264
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      26.40

_exptl_crystal_description       block
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.36
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5832
_exptl_absorpt_coefficient_mu    0.794
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.7179
_exptl_absorpt_correction_T_max  0.7620
_exptl_absorpt_process_details   sadabs

_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  'Smart Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            21856
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         26.48
_reflns_number_total             2832
_reflns_number_gt                2190
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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          
;
OMIT -3 53
ISOR 0.01 C5 O1W
DFIX 1.45 0.01 N2 C5
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^)+(0.0905P)^2^+70.6740P] 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         2832
_refine_ls_number_parameters     151
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.1666
_refine_ls_wR_factor_gt          0.1496
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.007
_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
Ni1 Ni 0.3333 0.6667 0.046036(16) 0.0254(2) Uani 1 3 d S . .
P1 P 0.44478(7) 0.55991(7) 0.02606(2) 0.0356(3) Uani 1 1 d . . .
P2 P 0.52578(7) 0.68874(7) 0.07271(2) 0.0336(3) Uani 1 1 d . . .
O1 O 0.3755(2) 0.5925(2) 0.02348(6) 0.0406(7) Uani 1 1 d . . .
O2 O 0.3926(2) 0.4530(2) 0.02007(7) 0.0491(8) Uani 1 1 d . . .
H2A H 0.4243 0.4412 0.0103 0.074 Uiso 1 1 calc R . .
O3 O 0.5308(2) 0.6100(2) 0.00901(6) 0.0466(8) Uani 1 1 d . . .
O4 O 0.3985(2) 0.5081(2) 0.07528(6) 0.0428(7) Uani 1 1 d . . .
H4D H 0.4122 0.4820 0.0866 0.064 Uiso 1 1 calc R . .
O5 O 0.6046(2) 0.7542(2) 0.05371(6) 0.0425(7) Uani 1 1 d . . .
H5D H 0.6549 0.7640 0.0594 0.064 Uiso 1 1 calc R . .
O6 O 0.5624(2) 0.6940(2) 0.10008(6) 0.0457(8) Uani 1 1 d . . .
O7 O 0.44680(19) 0.70902(19) 0.07115(5) 0.0348(6) Uani 1 1 d . . .
C1 C 0.4800(3) 0.5694(3) 0.06056(9) 0.0372(9) Uani 1 1 d . . .
C2 C 0.5506(3) 0.5371(4) 0.06427(12) 0.0576(13) Uani 1 1 d . . .
H2B H 0.5253 0.4749 0.0577 0.086 Uiso 1 1 calc R . .
H2C H 0.5645 0.5383 0.0825 0.086 Uiso 1 1 calc R . .
H2D H 0.6066 0.5779 0.0549 0.086 Uiso 1 1 calc R . .
C3 C 0.5135(7) 0.7625(6) -0.02760(16) 0.100(3) Uani 1 1 d . . .
H3A H 0.4508 0.7149 -0.0241 0.149 Uiso 1 1 d R . .
H3B H 0.5397 0.7409 -0.0406 0.149 Uiso 1 1 d R . .
H3C H 0.5138 0.8171 -0.0338 0.149 Uiso 1 1 d R . .
C4 C 0.6654(6) 0.8584(6) -0.0068(2) 0.124(4) Uani 1 1 d . . .
H4A H 0.6973 0.8707 0.0096 0.186 Uiso 1 1 d R . .
H4B H 0.6674 0.9138 -0.0129 0.186 Uiso 1 1 d R . .
H4C H 0.6950 0.8385 -0.0192 0.186 Uiso 1 1 d R . .
C5 C 0.4260(8) 0.7575(7) 0.13141(18) 0.155(4) Uani 1 1 d DU . .
H5A H 0.4803 0.7559 0.1258 0.232 Uiso 1 1 d R . .
H5B H 0.4252 0.7601 0.1501 0.232 Uiso 1 1 d R . .
H5C H 0.4270 0.8113 0.1243 0.232 Uiso 1 1 d R . .
N1 N 0.5697(4) 0.7859(3) -0.00361(11) 0.0710(15) Uani 1 1 d . . .
H1B H 0.5684 0.7342 0.0022 0.085 Uiso 1 1 d R . .
H1A H 0.5438 0.8052 0.0084 0.085 Uiso 1 1 d R . .
N2 N 0.3333 0.6667 0.12154(19) 0.103(4) Uani 1 3 d SD . .
H2F H 0.3333 0.6667 0.1040 0.124 Uiso 1 3 d SR . .
O1W O 0.3627(5) 0.3874(5) 0.11785(14) 0.152(3) Uani 1 1 d U . .
H1WA H 0.3162 0.3336 0.1155 0.229 Uiso 1 1 d R . .
H1WB H 0.4123 0.3867 0.1144 0.229 Uiso 1 1 d 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
Ni1 0.0224(3) 0.0224(3) 0.0313(4) 0.000 0.000 0.01121(15)
P1 0.0313(5) 0.0277(5) 0.0487(6) -0.0029(4) 0.0079(4) 0.0155(4)
P2 0.0247(5) 0.0304(5) 0.0444(6) 0.0023(4) -0.0044(4) 0.0127(4)
O1 0.0448(17) 0.0464(17) 0.0398(16) -0.0091(13) -0.0018(13) 0.0297(15)
O2 0.0387(17) 0.0291(15) 0.074(2) -0.0079(14) 0.0190(15) 0.0126(13)
O3 0.0446(18) 0.0322(16) 0.0599(19) -0.0012(13) 0.0202(15) 0.0170(14)
O4 0.0361(16) 0.0374(16) 0.0567(18) 0.0180(14) 0.0082(14) 0.0199(13)
O5 0.0291(14) 0.0406(17) 0.0510(17) 0.0075(13) -0.0017(12) 0.0123(13)
O6 0.0341(16) 0.0480(18) 0.0470(17) 0.0062(14) -0.0075(13) 0.0146(14)
O7 0.0291(14) 0.0319(14) 0.0455(16) -0.0061(12) -0.0070(12) 0.0167(12)
C1 0.0272(19) 0.032(2) 0.055(2) 0.0070(18) 0.0040(18) 0.0164(17)
C2 0.042(3) 0.052(3) 0.091(4) 0.009(3) 0.003(3) 0.032(2)
C3 0.134(8) 0.103(6) 0.081(5) 0.026(4) 0.032(5) 0.074(6)
C4 0.090(6) 0.082(5) 0.177(10) 0.017(6) 0.056(6) 0.025(5)
C5 0.206(9) 0.130(7) 0.088(5) -0.014(5) 0.037(6) 0.054(6)
N1 0.081(4) 0.059(3) 0.085(4) 0.021(3) 0.036(3) 0.044(3)
N2 0.132(7) 0.132(7) 0.045(5) 0.000 0.000 0.066(3)
O1W 0.135(5) 0.107(5) 0.163(5) 0.052(4) -0.036(4) 0.022(4)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 2.051(3) 3_565 ?
Ni1 O1 2.051(3) 2_665 ?
Ni1 O1 2.051(3) . ?
Ni1 O7 2.092(3) 2_665 ?
Ni1 O7 2.092(3) 3_565 ?
Ni1 O7 2.092(3) . ?
P1 O1 1.502(3) . ?
P1 O3 1.519(3) . ?
P1 O2 1.568(3) . ?
P1 C1 1.843(5) . ?
P2 O6 1.513(3) . ?
P2 O7 1.511(3) . ?
P2 O5 1.556(3) . ?
P2 C1 1.841(4) . ?
O2 H2A 0.8200 . ?
O4 C1 1.435(5) . ?
O4 H4D 0.8200 . ?
O5 H5D 0.8200 . ?
C1 C2 1.525(6) . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C3 N1 1.473(10) . ?
C3 H3A 0.9584 . ?
C3 H3B 0.9580 . ?
C3 H3C 0.9585 . ?
C4 N1 1.446(9) . ?
C4 H4A 0.9573 . ?
C4 H4B 0.9583 . ?
C4 H4C 0.9576 . ?
C5 N2 1.606(8) . ?
C5 H5A 0.9587 . ?
C5 H5B 0.9565 . ?
C5 H5C 0.9583 . ?
N1 H1B 0.8985 . ?
N1 H1A 0.8974 . ?
N2 C5 1.606(8) 2_665 ?
N2 C5 1.606(8) 3_565 ?
N2 H2F 0.8967 . ?
O1W H1WA 0.8486 . ?
O1W H1WB 0.8486 . ?

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 Ni1 O1 91.37(12) 3_565 2_665 ?
O1 Ni1 O1 91.37(12) 3_565 . ?
O1 Ni1 O1 91.37(12) 2_665 . ?
O1 Ni1 O7 90.80(12) 3_565 2_665 ?
O1 Ni1 O7 91.56(11) 2_665 2_665 ?
O1 Ni1 O7 176.31(12) . 2_665 ?
O1 Ni1 O7 91.56(11) 3_565 3_565 ?
O1 Ni1 O7 176.31(12) 2_665 3_565 ?
O1 Ni1 O7 90.80(12) . 3_565 ?
O7 Ni1 O7 86.16(12) 2_665 3_565 ?
O1 Ni1 O7 176.31(12) 3_565 . ?
O1 Ni1 O7 90.80(12) 2_665 . ?
O1 Ni1 O7 91.56(11) . . ?
O7 Ni1 O7 86.16(12) 2_665 . ?
O7 Ni1 O7 86.16(12) 3_565 . ?
O1 P1 O3 115.60(19) . . ?
O1 P1 O2 107.53(18) . . ?
O3 P1 O2 110.10(17) . . ?
O1 P1 C1 108.74(18) . . ?
O3 P1 C1 109.43(19) . . ?
O2 P1 C1 104.9(2) . . ?
O6 P2 O7 113.91(18) . . ?
O6 P2 O5 111.44(17) . . ?
O7 P2 O5 109.44(17) . . ?
O6 P2 C1 108.22(19) . . ?
O7 P2 C1 106.58(17) . . ?
O5 P2 C1 106.90(19) . . ?
P1 O1 Ni1 136.07(19) . . ?
P1 O2 H2A 109.5 . . ?
C1 O4 H4D 109.5 . . ?
P2 O5 H5D 109.5 . . ?
P2 O7 Ni1 133.98(17) . . ?
O4 C1 C2 107.7(3) . . ?
O4 C1 P2 108.8(3) . . ?
C2 C1 P2 111.1(3) . . ?
O4 C1 P1 107.2(3) . . ?
C2 C1 P1 110.9(3) . . ?
P2 C1 P1 111.0(2) . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2B C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N1 C3 H3A 110.0 . . ?
N1 C3 H3B 109.4 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.0 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.9 . . ?
N1 C4 H4B 109.4 . . ?
H4A C4 H4B 109.4 . . ?
N1 C4 H4C 109.1 . . ?
H4A C4 H4C 109.4 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 110.7 . . ?
N2 C5 H5B 109.2 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 108.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.4 . . ?
C4 N1 C3 114.4(6) . . ?
C4 N1 H1B 108.9 . . ?
C3 N1 H1B 108.4 . . ?
C4 N1 H1A 107.7 . . ?
C3 N1 H1A 108.3 . . ?
H1B N1 H1A 109.1 . . ?
C5 N2 C5 110.6(5) 2_665 . ?
C5 N2 C5 110.6(5) 2_665 3_565 ?
C5 N2 C5 110.6(5) . 3_565 ?
C5 N2 H2F 108.3 2_665 . ?
C5 N2 H2F 108.3 . . ?
C5 N2 H2F 108.3 3_565 . ?
H1WA O1W H1WB 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        26.48
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.739
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.090

# Attachment 'szg186(875547).cif'

data_0827g
_database_code_depnum_ccdc_archive 'CCDC 875547'
#TrackingRef 'szg186(875547).cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15 H58 N4 O24 P6 Zn'
_chemical_formula_weight         929.84

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'
Zn Zn 0.2839 1.4301 '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-3c '

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'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'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'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'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-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'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-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'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'

_cell_length_a                   16.6344(15)
_cell_length_b                   16.6344(15)
_cell_length_c                   51.382(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     12313(2)
_cell_formula_units_Z            12
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2418
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      20.11

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5856
_exptl_absorpt_coefficient_mu    0.915
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.6804
_exptl_absorpt_correction_T_max  0.7766
_exptl_absorpt_process_details   sadabs

_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  'Smart Apex II CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            17851
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_theta_min         2.12
_diffrn_reflns_theta_max         24.56
_reflns_number_total             2300
_reflns_number_gt                1659
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_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          
;
OMIT -3 53
ISOR 0.01 C5 O1W
DFIX 1.45 0.01 N2 C5
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^)+(0.0742P)^2^+99.2249P] 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         2300
_refine_ls_number_parameters     151
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0531
_refine_ls_wR_factor_ref         0.1617
_refine_ls_wR_factor_gt          0.1458
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.129
_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
Zn1 Zn 0.3333 0.6667 0.045296(19) 0.0301(3) Uani 1 3 d S . .
P1 P 0.44577(10) 0.55930(10) 0.02621(3) 0.0400(4) Uani 1 1 d . . .
P2 P 0.52614(10) 0.68782(10) 0.07285(3) 0.0377(4) Uani 1 1 d . . .
O1 O 0.3772(3) 0.5923(3) 0.02340(7) 0.0461(10) Uani 1 1 d . . .
O2 O 0.3936(3) 0.4530(3) 0.02019(8) 0.0542(12) Uani 1 1 d . . .
H2A H 0.4252 0.4411 0.0104 0.081 Uiso 1 1 calc R . .
O3 O 0.5318(3) 0.6100(3) 0.00935(8) 0.0511(11) Uani 1 1 d . . .
O4 O 0.3978(3) 0.5079(3) 0.07508(8) 0.0459(10) Uani 1 1 d . . .
H4D H 0.4107 0.4816 0.0864 0.069 Uiso 1 1 calc R . .
O5 O 0.6050(3) 0.7529(3) 0.05397(7) 0.0448(10) Uani 1 1 d . . .
H5D H 0.6551 0.7627 0.0597 0.067 Uiso 1 1 calc R . .
O6 O 0.5628(3) 0.6925(3) 0.10003(7) 0.0494(11) Uani 1 1 d . . .
O7 O 0.4476(3) 0.7084(2) 0.07132(7) 0.0386(9) Uani 1 1 d . . .
C1 C 0.4799(4) 0.5689(4) 0.06071(12) 0.0399(13) Uani 1 1 d . . .
C2 C 0.5495(5) 0.5360(5) 0.06450(15) 0.0621(19) Uani 1 1 d . . .
H2B H 0.5239 0.4739 0.0579 0.093 Uiso 1 1 calc R . .
H2C H 0.5630 0.5368 0.0827 0.093 Uiso 1 1 calc R . .
H2D H 0.6056 0.5764 0.0553 0.093 Uiso 1 1 calc R . .
C3 C 0.5157(8) 0.7633(7) -0.02666(19) 0.107(3) Uani 1 1 d . . .
H3A H 0.4530 0.7158 -0.0231 0.160 Uiso 1 1 d R . .
H3B H 0.5419 0.7418 -0.0397 0.160 Uiso 1 1 d R . .
H3C H 0.5160 0.8179 -0.0329 0.160 Uiso 1 1 d R . .
C4 C 0.6676(7) 0.8585(7) -0.0060(2) 0.129(4) Uani 1 1 d . . .
H4A H 0.6995 0.8709 0.0103 0.194 Uiso 1 1 d R . .
H4B H 0.6696 0.9140 -0.0122 0.194 Uiso 1 1 d R . .
H4C H 0.6971 0.8387 -0.0185 0.194 Uiso 1 1 d R . .
C5 C 0.4236(9) 0.7571(8) 0.1310(2) 0.165(5) Uani 1 1 d DU . .
H5A H 0.4779 0.7555 0.1254 0.247 Uiso 1 1 d R . .
H5B H 0.4229 0.7597 0.1497 0.247 Uiso 1 1 d R . .
H5C H 0.4246 0.8109 0.1239 0.247 Uiso 1 1 d R . .
N1 N 0.5716(5) 0.7872(4) -0.00269(14) 0.0743(19) Uani 1 1 d . . .
H1B H 0.5703 0.7356 0.0031 0.089 Uiso 1 1 d R . .
H1A H 0.5457 0.8065 0.0093 0.089 Uiso 1 1 d R . .
N2 N 0.3333 0.6667 0.1214(2) 0.105(5) Uani 1 3 d SD . .
H2F H 0.3333 0.6667 0.1039 0.125 Uiso 1 3 d SR . .
O1W O 0.3627(6) 0.3876(5) 0.11785(15) 0.152(3) Uani 1 1 d U . .
H1WA H 0.3163 0.3337 0.1155 0.227 Uiso 1 1 d R . .
H1WB H 0.4124 0.3869 0.1144 0.227 Uiso 1 1 d 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
Zn1 0.0276(4) 0.0276(4) 0.0351(6) 0.000 0.000 0.0138(2)
P1 0.0352(8) 0.0325(8) 0.0529(10) -0.0034(7) 0.0088(7) 0.0173(7)
P2 0.0293(8) 0.0345(8) 0.0484(9) 0.0019(6) -0.0046(6) 0.0152(7)
O1 0.052(3) 0.053(3) 0.044(2) -0.0108(19) -0.0037(18) 0.035(2)
O2 0.041(2) 0.036(2) 0.078(3) -0.009(2) 0.020(2) 0.014(2)
O3 0.051(3) 0.037(2) 0.063(3) 0.0001(19) 0.022(2) 0.020(2)
O4 0.042(2) 0.041(2) 0.057(2) 0.0183(19) 0.0078(19) 0.022(2)
O5 0.031(2) 0.043(2) 0.054(2) 0.0080(19) -0.0027(18) 0.0138(18)
O6 0.038(2) 0.052(3) 0.050(2) 0.0059(19) -0.0084(18) 0.016(2)
O7 0.032(2) 0.035(2) 0.050(2) -0.0071(17) -0.0093(17) 0.0187(17)
C1 0.027(3) 0.034(3) 0.060(4) 0.006(3) 0.006(3) 0.016(3)
C2 0.050(4) 0.052(4) 0.098(5) 0.007(4) 0.001(4) 0.035(3)
C3 0.136(9) 0.112(8) 0.091(7) 0.021(6) 0.033(7) 0.076(8)
C4 0.095(8) 0.084(7) 0.179(12) 0.018(7) 0.044(8) 0.023(6)
C5 0.201(10) 0.151(9) 0.097(7) -0.007(6) 0.029(7) 0.054(7)
N1 0.089(5) 0.059(4) 0.086(5) 0.020(3) 0.037(4) 0.045(4)
N2 0.138(8) 0.138(8) 0.037(6) 0.000 0.000 0.069(4)
O1W 0.140(6) 0.114(5) 0.155(6) 0.046(5) -0.031(5) 0.029(5)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.057(4) 3_565 ?
Zn1 O1 2.057(4) 2_665 ?
Zn1 O1 2.057(4) . ?
Zn1 O7 2.137(4) 2_665 ?
Zn1 O7 2.136(4) 3_565 ?
Zn1 O7 2.137(4) . ?
P1 O1 1.499(4) . ?
P1 O3 1.517(4) . ?
P1 O2 1.562(4) . ?
P1 C1 1.844(6) . ?
P2 O7 1.509(4) . ?
P2 O6 1.510(4) . ?
P2 O5 1.554(4) . ?
P2 C1 1.837(6) . ?
O2 H2A 0.8200 . ?
O4 C1 1.433(6) . ?
O4 H4D 0.8200 . ?
O5 H5D 0.8200 . ?
C1 C2 1.521(8) . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2 H2D 0.9600 . ?
C3 N1 1.473(12) . ?
C3 H3A 0.9599 . ?
C3 H3B 0.9603 . ?
C3 H3C 0.9601 . ?
C4 N1 1.447(11) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9598 . ?
C5 N2 1.582(9) . ?
C5 H5A 0.9603 . ?
C5 H5B 0.9597 . ?
C5 H5C 0.9600 . ?
N1 H1B 0.9000 . ?
N1 H1A 0.8995 . ?
N2 C5 1.582(9) 2_665 ?
N2 C5 1.582(9) 3_565 ?
N2 H2F 0.8997 . ?
O1W H1WA 0.8499 . ?
O1W H1WB 0.8500 . ?

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 Zn1 O1 92.94(16) 3_565 2_665 ?
O1 Zn1 O1 92.94(16) 3_565 . ?
O1 Zn1 O1 92.94(16) 2_665 . ?
O1 Zn1 O7 91.12(15) 3_565 2_665 ?
O1 Zn1 O7 90.70(14) 2_665 2_665 ?
O1 Zn1 O7 174.40(16) . 2_665 ?
O1 Zn1 O7 90.70(14) 3_565 3_565 ?
O1 Zn1 O7 174.40(16) 2_665 3_565 ?
O1 Zn1 O7 91.12(15) . 3_565 ?
O7 Zn1 O7 84.97(15) 2_665 3_565 ?
O1 Zn1 O7 174.40(16) 3_565 . ?
O1 Zn1 O7 91.12(15) 2_665 . ?
O1 Zn1 O7 90.70(14) . . ?
O7 Zn1 O7 84.97(15) 2_665 . ?
O7 Zn1 O7 84.97(15) 3_565 . ?
O1 P1 O3 114.8(2) . . ?
O1 P1 O2 107.5(2) . . ?
O3 P1 O2 110.6(2) . . ?
O1 P1 C1 108.6(2) . . ?
O3 P1 C1 109.7(3) . . ?
O2 P1 C1 105.1(2) . . ?
O7 P2 O6 114.2(2) . . ?
O7 P2 O5 109.5(2) . . ?
O6 P2 O5 111.3(2) . . ?
O7 P2 C1 106.4(2) . . ?
O6 P2 C1 108.1(3) . . ?
O5 P2 C1 107.0(2) . . ?
P1 O1 Zn1 137.0(2) . . ?
P1 O2 H2A 109.5 . . ?
C1 O4 H4D 109.5 . . ?
P2 O5 H5D 109.5 . . ?
P2 O7 Zn1 133.6(2) . . ?
O4 C1 C2 107.9(5) . . ?
O4 C1 P2 109.0(4) . . ?
C2 C1 P2 111.1(4) . . ?
O4 C1 P1 106.9(4) . . ?
C2 C1 P1 110.4(4) . . ?
P2 C1 P1 111.4(3) . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2 H2D 109.5 . . ?
H2B C2 H2D 109.5 . . ?
H2C C2 H2D 109.5 . . ?
N1 C3 H3A 110.0 . . ?
N1 C3 H3B 109.9 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 108.6 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.4 . . ?
N1 C4 H4A 109.7 . . ?
N1 C4 H4B 108.7 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 110.0 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C5 H5A 109.9 . . ?
N2 C5 H5B 109.2 . . ?
H5A C5 H5B 109.5 . . ?
N2 C5 H5C 109.4 . . ?
H5A C5 H5C 109.4 . . ?
H5B C5 H5C 109.5 . . ?
C4 N1 C3 114.3(8) . . ?
C4 N1 H1B 108.2 . . ?
C3 N1 H1B 108.0 . . ?
C4 N1 H1A 108.6 . . ?
C3 N1 H1A 108.7 . . ?
H1B N1 H1A 109.0 . . ?
C5 N2 C5 110.7(6) 2_665 . ?
C5 N2 C5 110.7(6) 2_665 3_565 ?
C5 N2 C5 110.7(6) . 3_565 ?
C5 N2 H2F 108.2 2_665 . ?
C5 N2 H2F 108.2 . . ?
C5 N2 H2F 108.2 3_565 . ?
H1WA O1W H1WB 109.5 . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        24.56
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.412
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.089