# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1508118'
_audit_update_record             
;
2016-10-04 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 N7 O9 P3 Zn3'
_chemical_formula_weight         765.47

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           triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   8.621(5)
_cell_length_b                   15.529(8)
_cell_length_c                   16.001(7)
_cell_angle_alpha                62.121(12)
_cell_angle_beta                 76.294(19)
_cell_angle_gamma                88.84(2)
_cell_volume                     1829.3(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    566(2)
_cell_measurement_reflns_used    5158
_cell_measurement_theta_min      3.1
_cell_measurement_theta_max      27.5

_exptl_crystal_description       rod-shape
_exptl_crystal_colour            light-yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_exptl_absorpt_coefficient_mu    2.127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.671
_exptl_absorpt_correction_T_max  0.758
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      566(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  'XtaLABmini: Fixed Chi 2 circle'
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19235
_diffrn_reflns_av_R_equivalents  0.1196
_diffrn_reflns_av_sigmaI/netI    0.1143
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.05
_diffrn_reflns_theta_max         27.55
_reflns_number_total             8365
_reflns_number_gt                6773
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0385P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8365
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1132
_refine_ls_wR_factor_gt          0.1071
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_restrained_S_all      1.015
_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
C1 C 0.4109(3) 0.2669(2) 0.5693(2) 0.0209(6) Uani 1 1 d . . .
H1A H 0.3818 0.2188 0.6381 0.025 Uiso 1 1 calc R . .
H1B H 0.4038 0.3315 0.5644 0.025 Uiso 1 1 calc R . .
C2 C 0.1526(3) 0.3015(2) 0.5271(2) 0.0220(6) Uani 1 1 d . . .
H2A H 0.1211 0.2985 0.5908 0.026 Uiso 1 1 calc R . .
H2B H 0.0650 0.2693 0.5201 0.026 Uiso 1 1 calc R . .
C3 C 0.2566(3) 0.1445(2) 0.5585(2) 0.0220(6) Uani 1 1 d . . .
H3A H 0.1667 0.1199 0.6161 0.026 Uiso 1 1 calc R . .
H3B H 0.3477 0.1097 0.5773 0.026 Uiso 1 1 calc R . .
C4 C 0.6233(3) 0.5780(3) 0.2994(2) 0.0317(7) Uani 1 1 d . . .
H4 H 0.5245 0.5664 0.3439 0.038 Uiso 1 1 calc R . .
C5 C 0.6541(3) 0.6363(3) 0.2016(2) 0.0362(8) Uani 1 1 d . . .
H5 H 0.5825 0.6727 0.1667 0.043 Uiso 1 1 calc R . .
C6 C 0.8732(3) 0.5724(3) 0.2397(2) 0.0325(7) Uani 1 1 d . . .
H6 H 0.9791 0.5578 0.2343 0.039 Uiso 1 1 calc R . .
C7 C 1.4092(5) 0.5432(3) -0.1264(3) 0.0505(11) Uani 1 1 d . . .
H7 H 1.4651 0.4887 -0.1156 0.061 Uiso 1 1 calc R . .
C8 C 1.2856(5) 0.5491(3) -0.0587(3) 0.0554(12) Uani 1 1 d . . .
H8 H 1.2418 0.5006 0.0053 0.067 Uiso 1 1 calc R . .
C9 C 1.3339(4) 0.6851(3) -0.1954(2) 0.0359(8) Uani 1 1 d . . .
H9 H 1.3261 0.7487 -0.2418 0.043 Uiso 1 1 calc R . .
C10 C 0.7906(6) 1.0353(4) -0.2407(3) 0.0689(15) Uani 1 1 d . . .
H10 H 0.7428 1.0926 -0.2520 0.083 Uiso 1 1 calc R . .
C11 C 0.8197(6) 0.9706(4) -0.1552(3) 0.0675(14) Uani 1 1 d . . .
H11 H 0.7960 0.9752 -0.0977 0.081 Uiso 1 1 calc R . .
C12 C 0.9028(4) 0.9211(3) -0.2623(2) 0.0373(8) Uani 1 1 d . . .
H12 H 0.9491 0.8835 -0.2909 0.045 Uiso 1 1 calc R . .
C13 C 1.1096(3) 0.6831(3) -0.0670(2) 0.0298(7) Uani 1 1 d . . .
C14 C 1.0674(4) 0.7719(3) -0.1327(2) 0.0368(8) Uani 1 1 d . . .
H14 H 1.1258 0.8044 -0.1978 0.044 Uiso 1 1 calc R . .
C15 C 0.9380(4) 0.8103(3) -0.0991(2) 0.0357(8) Uani 1 1 d . . .
C16 C 0.8526(4) 0.7660(3) -0.0010(2) 0.0357(8) Uani 1 1 d . . .
H16 H 0.7672 0.7942 0.0210 0.043 Uiso 1 1 calc R . .
C17 C 0.8990(4) 0.6792(3) 0.0624(2) 0.0325(8) Uani 1 1 d . . .
C18 C 1.0270(4) 0.6354(3) 0.0316(2) 0.0334(7) Uani 1 1 d . . .
H18 H 1.0562 0.5765 0.0753 0.040 Uiso 1 1 calc R . .
N1 N 0.7612(3) 0.5384(2) 0.32264(17) 0.0255(5) Uani 1 1 d . . .
N2 N 1.4390(3) 0.6291(2) -0.21264(18) 0.0288(6) Uani 1 1 d . . .
N3 N 0.8424(3) 1.0035(2) -0.30892(19) 0.0332(6) Uani 1 1 d . . .
N4 N 0.8141(3) 0.6310(2) 0.16388(18) 0.0302(6) Uani 1 1 d . . .
N5 N 1.2394(3) 0.6412(2) -0.10426(18) 0.0316(6) Uani 1 1 d . . .
N6 N 0.8897(3) 0.8977(2) -0.16836(19) 0.0359(7) Uani 1 1 d . . .
N7 N 0.2968(2) 0.25070(18) 0.52008(17) 0.0187(5) Uani 1 1 d . . .
O1 O 0.6494(2) 0.15043(16) 0.55953(17) 0.0279(5) Uani 1 1 d . . .
O2 O 0.7266(2) 0.31723(16) 0.53357(15) 0.0266(5) Uani 1 1 d . . .
O3 O 0.6266(2) 0.30056(18) 0.40482(15) 0.0280(5) Uani 1 1 d . . .
O4 O 0.2327(3) 0.01661(18) 0.49253(19) 0.0363(6) Uani 1 1 d . . .
O5 O 0.0300(2) 0.14143(17) 0.46329(15) 0.0282(5) Uani 1 1 d . . .
O6 O 0.3214(2) 0.19515(18) 0.36873(16) 0.0310(5) Uani 1 1 d . . .
O7 O 0.0364(2) 0.47052(17) 0.41235(15) 0.0285(5) Uani 1 1 d . . .
O8 O 0.2832(2) 0.48604(16) 0.46433(15) 0.0257(5) Uani 1 1 d . . .
O9 O 0.2983(2) 0.42767(16) 0.34012(14) 0.0251(4) Uani 1 1 d . . .
P1 P 0.61696(8) 0.25692(6) 0.51338(5) 0.01901(15) Uani 1 1 d . . .
P2 P 0.20503(8) 0.12303(6) 0.46496(6) 0.02242(17) Uani 1 1 d . . .
P3 P 0.19245(8) 0.42996(5) 0.43104(5) 0.01859(15) Uani 1 1 d . . .
Zn1 Zn 0.80531(3) 0.45544(2) 0.45335(2) 0.01935(9) Uani 1 1 d . . .
Zn2 Zn 0.42854(3) 0.31814(3) 0.35522(2) 0.01969(9) Uani 1 1 d . . .
Zn3 Zn 0.82266(4) 0.07120(2) 0.55355(2) 0.02142(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N7 1.488(3) . ?
C1 P1 1.830(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N7 1.469(4) . ?
C2 P3 1.836(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N7 1.481(4) . ?
C3 P2 1.827(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.351(4) . ?
C4 N1 1.377(4) . ?
C4 H4 0.9300 . ?
C5 N4 1.387(4) . ?
C5 H5 0.9300 . ?
C6 N1 1.315(4) . ?
C6 N4 1.342(4) . ?
C6 H6 0.9300 . ?
C7 C8 1.364(5) . ?
C7 N2 1.369(5) . ?
C7 H7 0.9300 . ?
C8 N5 1.369(5) . ?
C8 H8 0.9300 . ?
C9 N2 1.315(4) . ?
C9 N5 1.336(4) . ?
C9 H9 0.9300 . ?
C10 C11 1.346(6) . ?
C10 N3 1.378(5) . ?
C10 H10 0.9300 . ?
C11 N6 1.351(5) . ?
C11 H11 0.9300 . ?
C12 N3 1.314(5) . ?
C12 N6 1.348(4) . ?
C12 H12 0.9300 . ?
C13 C18 1.392(4) . ?
C13 C14 1.395(5) . ?
C13 N5 1.431(4) . ?
C14 C15 1.369(5) . ?
C14 H14 0.9300 . ?
C15 C16 1.394(4) . ?
C15 N6 1.426(4) . ?
C16 C17 1.378(5) . ?
C16 H16 0.9300 . ?
C17 C18 1.396(4) . ?
C17 N4 1.433(4) . ?
C18 H18 0.9300 . ?
N1 Zn1 2.004(3) . ?
N2 Zn2 2.058(3) 2_765 ?
N3 Zn3 1.996(3) 1_564 ?
N7 Zn2 2.322(3) . ?
O1 P1 1.515(2) . ?
O1 Zn3 1.929(2) . ?
O2 P1 1.529(2) . ?
O2 Zn1 1.945(2) . ?
O3 P1 1.522(2) . ?
O3 Zn2 2.010(2) . ?
O4 P2 1.528(3) . ?
O4 Zn3 1.940(2) 2_656 ?
O5 P2 1.534(2) . ?
O5 Zn3 1.963(2) 1_455 ?
O6 P2 1.527(2) . ?
O6 Zn2 2.034(2) . ?
O7 P3 1.509(2) . ?
O7 Zn1 1.926(2) 1_455 ?
O8 P3 1.521(2) . ?
O8 Zn1 1.938(2) 2_666 ?
O9 P3 1.539(2) . ?
O9 Zn2 1.970(2) . ?
Zn1 O7 1.926(2) 1_655 ?
Zn1 O8 1.938(2) 2_666 ?
Zn2 N2 2.058(3) 2_765 ?
Zn3 O4 1.940(2) 2_656 ?
Zn3 O5 1.963(2) 1_655 ?
Zn3 N3 1.996(3) 1_546 ?

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
N7 C1 P1 110.86(18) . . ?
N7 C1 H1A 109.5 . . ?
P1 C1 H1A 109.5 . . ?
N7 C1 H1B 109.5 . . ?
P1 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N7 C2 P3 110.16(19) . . ?
N7 C2 H2A 109.6 . . ?
P3 C2 H2A 109.6 . . ?
N7 C2 H2B 109.6 . . ?
P3 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N7 C3 P2 109.82(19) . . ?
N7 C3 H3A 109.7 . . ?
P2 C3 H3A 109.7 . . ?
N7 C3 H3B 109.7 . . ?
P2 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 C4 N1 109.3(3) . . ?
C5 C4 H4 125.3 . . ?
N1 C4 H4 125.3 . . ?
C4 C5 N4 106.0(3) . . ?
C4 C5 H5 127.0 . . ?
N4 C5 H5 127.0 . . ?
N1 C6 N4 110.9(3) . . ?
N1 C6 H6 124.5 . . ?
N4 C6 H6 124.5 . . ?
C8 C7 N2 110.2(4) . . ?
C8 C7 H7 124.9 . . ?
N2 C7 H7 124.9 . . ?
C7 C8 N5 105.8(3) . . ?
C7 C8 H8 127.1 . . ?
N5 C8 H8 127.1 . . ?
N2 C9 N5 112.9(3) . . ?
N2 C9 H9 123.5 . . ?
N5 C9 H9 123.5 . . ?
C11 C10 N3 109.5(4) . . ?
C11 C10 H10 125.2 . . ?
N3 C10 H10 125.2 . . ?
C10 C11 N6 107.3(4) . . ?
C10 C11 H11 126.4 . . ?
N6 C11 H11 126.4 . . ?
N3 C12 N6 112.1(3) . . ?
N3 C12 H12 123.9 . . ?
N6 C12 H12 123.9 . . ?
C18 C13 C14 121.4(3) . . ?
C18 C13 N5 120.7(3) . . ?
C14 C13 N5 117.9(3) . . ?
C15 C14 C13 118.5(3) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 122.2(3) . . ?
C14 C15 N6 117.9(3) . . ?
C16 C15 N6 119.9(3) . . ?
C17 C16 C15 117.8(3) . . ?
C17 C16 H16 121.1 . . ?
C15 C16 H16 121.1 . . ?
C16 C17 C18 122.3(3) . . ?
C16 C17 N4 119.6(3) . . ?
C18 C17 N4 118.0(3) . . ?
C13 C18 C17 117.7(3) . . ?
C13 C18 H18 121.2 . . ?
C17 C18 H18 121.2 . . ?
C6 N1 C4 106.5(3) . . ?
C6 N1 Zn1 123.0(2) . . ?
C4 N1 Zn1 130.3(2) . . ?
C9 N2 C7 104.5(3) . . ?
C9 N2 Zn2 116.4(2) . 2_765 ?
C7 N2 Zn2 138.4(3) . 2_765 ?
C12 N3 C10 104.7(3) . . ?
C12 N3 Zn3 129.7(2) . 1_564 ?
C10 N3 Zn3 125.6(3) . 1_564 ?
C6 N4 C5 107.3(2) . . ?
C6 N4 C17 126.9(3) . . ?
C5 N4 C17 125.8(3) . . ?
C9 N5 C8 106.6(3) . . ?
C9 N5 C13 124.9(3) . . ?
C8 N5 C13 128.4(3) . . ?
C12 N6 C11 106.4(3) . . ?
C12 N6 C15 124.6(3) . . ?
C11 N6 C15 129.0(3) . . ?
C2 N7 C3 112.0(2) . . ?
C2 N7 C1 112.3(2) . . ?
C3 N7 C1 110.3(2) . . ?
C2 N7 Zn2 107.06(17) . . ?
C3 N7 Zn2 108.15(16) . . ?
C1 N7 Zn2 106.81(16) . . ?
P1 O1 Zn3 139.69(13) . . ?
P1 O2 Zn1 127.65(13) . . ?
P1 O3 Zn2 121.80(11) . . ?
P2 O4 Zn3 132.98(15) . 2_656 ?
P2 O5 Zn3 133.46(14) . 1_455 ?
P2 O6 Zn2 120.60(12) . . ?
P3 O7 Zn1 148.41(15) . 1_455 ?
P3 O8 Zn1 127.84(12) . 2_666 ?
P3 O9 Zn2 120.09(13) . . ?
O1 P1 O3 113.04(13) . . ?
O1 P1 O2 110.51(13) . . ?
O3 P1 O2 112.06(13) . . ?
O1 P1 C1 109.45(13) . . ?
O3 P1 C1 104.87(12) . . ?
O2 P1 C1 106.52(13) . . ?
O6 P2 O4 112.16(14) . . ?
O6 P2 O5 111.44(13) . . ?
O4 P2 O5 111.83(13) . . ?
O6 P2 C3 105.19(13) . . ?
O4 P2 C3 105.68(14) . . ?
O5 P2 C3 110.15(13) . . ?
O7 P3 O8 112.18(13) . . ?
O7 P3 O9 110.86(12) . . ?
O8 P3 O9 110.84(11) . . ?
O7 P3 C2 109.80(13) . . ?
O8 P3 C2 107.82(14) . . ?
O9 P3 C2 105.03(13) . . ?
O7 Zn1 O8 114.22(9) 1_655 2_666 ?
O7 Zn1 O2 109.91(10) 1_655 . ?
O8 Zn1 O2 104.46(10) 2_666 . ?
O7 Zn1 N1 98.73(10) 1_655 . ?
O8 Zn1 N1 107.33(11) 2_666 . ?
O2 Zn1 N1 122.60(10) . . ?
O9 Zn2 O3 122.99(9) . . ?
O9 Zn2 O6 117.80(10) . . ?
O3 Zn2 O6 115.61(10) . . ?
O9 Zn2 N2 99.69(10) . 2_765 ?
O3 Zn2 N2 92.43(10) . 2_765 ?
O6 Zn2 N2 96.78(10) . 2_765 ?
O9 Zn2 N7 84.72(8) . . ?
O3 Zn2 N7 83.37(8) . . ?
O6 Zn2 N7 82.88(8) . . ?
N2 Zn2 N7 175.12(9) 2_765 . ?
O1 Zn3 O4 109.37(10) . 2_656 ?
O1 Zn3 O5 116.42(10) . 1_655 ?
O4 Zn3 O5 104.28(11) 2_656 1_655 ?
O1 Zn3 N3 102.87(11) . 1_546 ?
O4 Zn3 N3 114.14(12) 2_656 1_546 ?
O5 Zn3 N3 110.14(10) 1_655 1_546 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C4 C5 N4 1.1(4) . . . . ?
N2 C7 C8 N5 -0.5(5) . . . . ?
N3 C10 C11 N6 0.0(6) . . . . ?
C18 C13 C14 C15 -2.4(6) . . . . ?
N5 C13 C14 C15 176.6(3) . . . . ?
C13 C14 C15 C16 3.2(6) . . . . ?
C13 C14 C15 N6 -175.9(3) . . . . ?
C14 C15 C16 C17 -2.1(6) . . . . ?
N6 C15 C16 C17 177.0(3) . . . . ?
C15 C16 C17 C18 0.2(5) . . . . ?
C15 C16 C17 N4 -179.7(3) . . . . ?
C14 C13 C18 C17 0.6(5) . . . . ?
N5 C13 C18 C17 -178.4(3) . . . . ?
C16 C17 C18 C13 0.5(5) . . . . ?
N4 C17 C18 C13 -179.6(3) . . . . ?
N4 C6 N1 C4 -0.8(4) . . . . ?
N4 C6 N1 Zn1 -175.9(2) . . . . ?
C5 C4 N1 C6 -0.2(4) . . . . ?
C5 C4 N1 Zn1 174.4(3) . . . . ?
N5 C9 N2 C7 0.2(4) . . . . ?
N5 C9 N2 Zn2 172.4(2) . . . 2_765 ?
C8 C7 N2 C9 0.2(5) . . . . ?
C8 C7 N2 Zn2 -169.2(3) . . . 2_765 ?
N6 C12 N3 C10 1.2(4) . . . . ?
N6 C12 N3 Zn3 -178.0(2) . . . 1_564 ?
C11 C10 N3 C12 -0.7(5) . . . . ?
C11 C10 N3 Zn3 178.5(3) . . . 1_564 ?
N1 C6 N4 C5 1.4(4) . . . . ?
N1 C6 N4 C17 -178.4(3) . . . . ?
C4 C5 N4 C6 -1.5(4) . . . . ?
C4 C5 N4 C17 178.3(3) . . . . ?
C16 C17 N4 C6 -151.7(4) . . . . ?
C18 C17 N4 C6 28.4(5) . . . . ?
C16 C17 N4 C5 28.6(5) . . . . ?
C18 C17 N4 C5 -151.4(4) . . . . ?
N2 C9 N5 C8 -0.5(5) . . . . ?
N2 C9 N5 C13 -176.7(3) . . . . ?
C7 C8 N5 C9 0.6(5) . . . . ?
C7 C8 N5 C13 176.6(4) . . . . ?
C18 C13 N5 C9 -174.1(3) . . . . ?
C14 C13 N5 C9 6.8(5) . . . . ?
C18 C13 N5 C8 10.5(6) . . . . ?
C14 C13 N5 C8 -168.6(4) . . . . ?
N3 C12 N6 C11 -1.2(5) . . . . ?
N3 C12 N6 C15 177.0(3) . . . . ?
C10 C11 N6 C12 0.7(6) . . . . ?
C10 C11 N6 C15 -177.4(4) . . . . ?
C14 C15 N6 C12 32.8(5) . . . . ?
C16 C15 N6 C12 -146.3(4) . . . . ?
C14 C15 N6 C11 -149.4(5) . . . . ?
C16 C15 N6 C11 31.5(6) . . . . ?
P3 C2 N7 C3 -152.26(19) . . . . ?
P3 C2 N7 C1 83.0(2) . . . . ?
P3 C2 N7 Zn2 -33.9(2) . . . . ?
P2 C3 N7 C2 82.0(2) . . . . ?
P2 C3 N7 C1 -152.16(18) . . . . ?
P2 C3 N7 Zn2 -35.7(2) . . . . ?
P1 C1 N7 C2 -152.7(2) . . . . ?
P1 C1 N7 C3 81.7(2) . . . . ?
P1 C1 N7 Zn2 -35.6(2) . . . . ?
Zn3 O1 P1 O3 66.2(2) . . . . ?
Zn3 O1 P1 O2 -60.3(2) . . . . ?
Zn3 O1 P1 C1 -177.27(19) . . . . ?
Zn2 O3 P1 O1 101.42(16) . . . . ?
Zn2 O3 P1 O2 -132.90(15) . . . . ?
Zn2 O3 P1 C1 -17.74(19) . . . . ?
Zn1 O2 P1 O1 151.45(15) . . . . ?
Zn1 O2 P1 O3 24.4(2) . . . . ?
Zn1 O2 P1 C1 -89.75(18) . . . . ?
N7 C1 P1 O1 -85.5(2) . . . . ?
N7 C1 P1 O3 36.1(2) . . . . ?
N7 C1 P1 O2 155.03(19) . . . . ?
Zn2 O6 P2 O4 -136.96(15) . . . . ?
Zn2 O6 P2 O5 96.79(16) . . . . ?
Zn2 O6 P2 C3 -22.56(19) . . . . ?
Zn3 O4 P2 O6 -77.1(2) 2_656 . . . ?
Zn3 O4 P2 O5 48.9(2) 2_656 . . . ?
Zn3 O4 P2 C3 168.78(18) 2_656 . . . ?
Zn3 O5 P2 O6 173.03(16) 1_455 . . . ?
Zn3 O5 P2 O4 46.6(2) 1_455 . . . ?
Zn3 O5 P2 C3 -70.6(2) 1_455 . . . ?
N7 C3 P2 O6 38.7(2) . . . . ?
N7 C3 P2 O4 157.54(18) . . . . ?
N7 C3 P2 O5 -81.5(2) . . . . ?
Zn1 O7 P3 O8 -107.6(3) 1_455 . . . ?
Zn1 O7 P3 O9 127.9(3) 1_455 . . . ?
Zn1 O7 P3 C2 12.3(3) 1_455 . . . ?
Zn1 O8 P3 O7 35.4(2) 2_666 . . . ?
Zn1 O8 P3 O9 159.95(15) 2_666 . . . ?
Zn1 O8 P3 C2 -85.60(19) 2_666 . . . ?
Zn2 O9 P3 O7 -142.69(13) . . . . ?
Zn2 O9 P3 O8 92.04(16) . . . . ?
Zn2 O9 P3 C2 -24.15(16) . . . . ?
N7 C2 P3 O7 158.02(18) . . . . ?
N7 C2 P3 O8 -79.5(2) . . . . ?
N7 C2 P3 O9 38.8(2) . . . . ?
P1 O2 Zn1 O7 -119.32(16) . . . 1_655 ?
P1 O2 Zn1 O8 117.72(17) . . . 2_666 ?
P1 O2 Zn1 N1 -4.3(2) . . . . ?
C6 N1 Zn1 O7 9.9(3) . . . 1_655 ?
C4 N1 Zn1 O7 -163.9(3) . . . 1_655 ?
C6 N1 Zn1 O8 128.8(3) . . . 2_666 ?
C4 N1 Zn1 O8 -45.0(3) . . . 2_666 ?
C6 N1 Zn1 O2 -110.5(3) . . . . ?
C4 N1 Zn1 O2 75.6(3) . . . . ?
P3 O9 Zn2 O3 -72.32(16) . . . . ?
P3 O9 Zn2 O6 85.33(15) . . . . ?
P3 O9 Zn2 N2 -171.65(14) . . . 2_765 ?
P3 O9 Zn2 N7 6.25(13) . . . . ?
P1 O3 Zn2 O9 79.36(18) . . . . ?
P1 O3 Zn2 O6 -78.73(17) . . . . ?
P1 O3 Zn2 N2 -177.43(17) . . . 2_765 ?
P1 O3 Zn2 N7 0.07(16) . . . . ?
P2 O6 Zn2 O9 -76.01(18) . . . . ?
P2 O6 Zn2 O3 83.27(17) . . . . ?
P2 O6 Zn2 N2 179.25(16) . . . 2_765 ?
P2 O6 Zn2 N7 4.16(15) . . . . ?
C2 N7 Zn2 O9 18.39(17) . . . . ?
C3 N7 Zn2 O9 139.27(17) . . . . ?
C1 N7 Zn2 O9 -102.05(18) . . . . ?
C2 N7 Zn2 O3 142.53(18) . . . . ?
C3 N7 Zn2 O3 -96.59(17) . . . . ?
C1 N7 Zn2 O3 22.09(18) . . . . ?
C2 N7 Zn2 O6 -100.53(18) . . . . ?
C3 N7 Zn2 O6 20.35(17) . . . . ?
C1 N7 Zn2 O6 139.03(18) . . . . ?
C2 N7 Zn2 N2 173.2(11) . . . 2_765 ?
C3 N7 Zn2 N2 -65.9(12) . . . 2_765 ?
C1 N7 Zn2 N2 52.8(12) . . . 2_765 ?
P1 O1 Zn3 O4 -116.8(2) . . . 2_656 ?
P1 O1 Zn3 O5 1.0(3) . . . 1_655 ?
P1 O1 Zn3 N3 121.5(2) . . . 1_546 ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        27.55
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.677
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.135
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.012 0.000 0.000 672 167 ' '
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F² was
written to a new HKL file. The number of located electrons, 
in one void per unit cell is 167.There are two formula units 
in one unit cell. On base of charge balance considerations, 
volume/count_electrons analysis, TG analyses and elemental analyses, 
this residual electron density was assigned to nine water molecules.  
So SQUEEZE removed these disordered units per unit cell. 
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1508119'
_audit_update_record             
;
2016-10-04 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H18 Co3 N7 O9 P3'
_chemical_formula_weight         746.09

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           Triclinic
_symmetry_space_group_name_H-M   'P -1'

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

_cell_length_a                   8.645(4)
_cell_length_b                   15.658(7)
_cell_length_c                   15.977(6)
_cell_angle_alpha                62.066(13)
_cell_angle_beta                 76.251(17)
_cell_angle_gamma                88.765(19)
_cell_volume                     1845.8(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    566(2)
_cell_measurement_reflns_used    4341
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.5

_exptl_crystal_description       rod-shape
_exptl_crystal_colour            pink
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             746
_exptl_absorpt_coefficient_mu    1.507
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_T_max  0.810
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      566(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  'XtaLABmini: Fixed Chi 2 circle'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            19386
_diffrn_reflns_av_R_equivalents  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         27.49
_reflns_number_total             8420
_reflns_number_gt                6344
_reflns_threshold_expression     >2sigma(I)

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

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0421P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8420
_refine_ls_number_parameters     361
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1105
_refine_ls_wR_factor_gt          0.1014
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_restrained_S_all      0.975
_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
C1 C -0.2427(4) 0.1436(2) 0.5582(2) 0.0264(7) Uani 1 1 d . . .
H1A H -0.3324 0.1194 0.6159 0.032 Uiso 1 1 calc R . .
H1B H -0.1520 0.1089 0.5770 0.032 Uiso 1 1 calc R . .
C2 C -0.0910(4) 0.2664(2) 0.5707(2) 0.0235(7) Uani 1 1 d . . .
H2A H -0.1213 0.2188 0.6397 0.028 Uiso 1 1 calc R . .
H2B H -0.0993 0.3305 0.5654 0.028 Uiso 1 1 calc R . .
C3 C -0.3484(3) 0.3005(2) 0.5259(2) 0.0235(7) Uani 1 1 d . . .
H3A H -0.3820 0.2969 0.5900 0.028 Uiso 1 1 calc R . .
H3B H -0.4346 0.2689 0.5176 0.028 Uiso 1 1 calc R . .
C4 C 0.1263(4) 0.5776(3) 0.2996(2) 0.0328(8) Uani 1 1 d . . .
H4 H 0.0276 0.5660 0.3442 0.039 Uiso 1 1 calc R . .
C5 C 0.1560(4) 0.6359(3) 0.2023(3) 0.0377(9) Uani 1 1 d . . .
H5 H 0.0842 0.6723 0.1679 0.045 Uiso 1 1 calc R . .
C6 C 0.3744(4) 0.5713(3) 0.2403(2) 0.0340(8) Uani 1 1 d . . .
H6 H 0.4796 0.5561 0.2350 0.041 Uiso 1 1 calc R . .
C7 C 0.4010(4) 0.6791(3) 0.0626(2) 0.0334(8) Uani 1 1 d . . .
C8 C 0.5285(4) 0.6355(3) 0.0312(2) 0.0359(9) Uani 1 1 d . . .
H8 H 0.5577 0.5770 0.0749 0.043 Uiso 1 1 calc R . .
C9 C 0.6100(4) 0.6829(3) -0.0677(2) 0.0325(8) Uani 1 1 d . . .
C10 C 0.7843(5) 0.5492(3) -0.0606(3) 0.0589(13) Uani 1 1 d . . .
H10 H 0.7407 0.5002 0.0031 0.071 Uiso 1 1 calc R . .
C11 C 0.9059(5) 0.5444(3) -0.1289(3) 0.0531(12) Uani 1 1 d . . .
H11 H 0.9603 0.4900 -0.1193 0.064 Uiso 1 1 calc R . .
C12 C 0.8346(4) 0.6861(3) -0.1963(3) 0.0392(9) Uani 1 1 d . . .
H12 H 0.8283 0.7497 -0.2423 0.047 Uiso 1 1 calc R . .
C13 C 0.5661(4) 0.7703(3) -0.1322(3) 0.0386(9) Uani 1 1 d . . .
H13 H 0.6234 0.8022 -0.1977 0.046 Uiso 1 1 calc R . .
C14 C 0.4375(4) 0.8098(3) -0.0992(2) 0.0342(8) Uani 1 1 d . . .
C15 C 0.3540(4) 0.7658(3) -0.0012(2) 0.0369(9) Uani 1 1 d . . .
H15 H 0.2690 0.7937 0.0212 0.044 Uiso 1 1 calc R . .
C16 C 0.3217(7) 0.9687(4) -0.1543(3) 0.0757(17) Uani 1 1 d . . .
H16 H 0.3011 0.9734 -0.0968 0.091 Uiso 1 1 calc R . .
C17 C 0.2901(7) 1.0332(4) -0.2399(3) 0.0713(16) Uani 1 1 d . . .
H17 H 0.2407 1.0894 -0.2504 0.086 Uiso 1 1 calc R . .
C18 C 0.4006(5) 0.9209(3) -0.2626(3) 0.0386(9) Uani 1 1 d . . .
H18 H 0.4454 0.8837 -0.2917 0.046 Uiso 1 1 calc R . .
Co1 Co -0.07157(5) 0.31478(3) 0.35860(3) 0.02105(11) Uani 1 1 d . . .
Co2 Co 0.32232(5) 0.07187(3) 0.55203(3) 0.02356(11) Uani 1 1 d . . .
Co3 Co 0.30596(5) 0.45513(3) 0.45540(3) 0.02143(11) Uani 1 1 d . . .
N1 N -0.2019(3) 0.24955(17) 0.51970(18) 0.0191(5) Uani 1 1 d . . .
N2 N 0.2619(3) 0.5380(2) 0.32361(19) 0.0277(6) Uani 1 1 d . . .
N3 N 0.3152(3) 0.6308(2) 0.16331(19) 0.0320(7) Uani 1 1 d . . .
N4 N 0.7383(3) 0.6418(2) -0.1047(2) 0.0329(7) Uani 1 1 d . . .
N5 N 0.9378(3) 0.6308(2) -0.21404(19) 0.0310(6) Uani 1 1 d . . .
N6 N 0.3889(4) 0.8967(2) -0.1687(2) 0.0387(8) Uani 1 1 d . . .
N7 N 0.3419(4) 1.0028(2) -0.3084(2) 0.0351(7) Uani 1 1 d . . .
O1 O -0.4676(3) 0.13976(17) 0.46388(17) 0.0316(5) Uani 1 1 d . . .
O2 O -0.2644(3) 0.01709(17) 0.49228(19) 0.0386(6) Uani 1 1 d . . .
O3 O -0.1784(3) 0.19454(18) 0.36973(17) 0.0346(6) Uani 1 1 d . . .
O4 O 0.1505(3) 0.15076(16) 0.56318(18) 0.0324(5) Uani 1 1 d . . .
O5 O 0.2222(3) 0.31826(16) 0.53531(17) 0.0308(5) Uani 1 1 d . . .
O6 O 0.1255(3) 0.29821(17) 0.40738(16) 0.0304(5) Uani 1 1 d . . .
O7 O -0.4632(3) 0.46681(17) 0.41230(17) 0.0333(6) Uani 1 1 d . . .
O8 O -0.2179(3) 0.48373(16) 0.46450(17) 0.0301(5) Uani 1 1 d . . .
O9 O -0.2009(3) 0.42521(15) 0.34027(16) 0.0261(5) Uani 1 1 d . . .
P1 P -0.29391(10) 0.12218(6) 0.46559(6) 0.02509(19) Uani 1 1 d . . .
P2 P 0.11523(9) 0.25651(6) 0.51617(6) 0.02140(17) Uani 1 1 d . . .
P3 P -0.30726(9) 0.42790(6) 0.43061(6) 0.02152(17) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.490(4) . ?
C1 P1 1.811(3) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 N1 1.495(4) . ?
C2 P2 1.827(3) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.491(4) . ?
C3 P3 1.831(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.345(5) . ?
C4 N2 1.366(4) . ?
C4 H4 0.9300 . ?
C5 N3 1.386(4) . ?
C5 H5 0.9300 . ?
C6 N2 1.322(4) . ?
C6 N3 1.359(4) . ?
C6 H6 0.9300 . ?
C7 C15 1.387(5) . ?
C7 C8 1.398(5) . ?
C7 N3 1.424(4) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9300 . ?
C9 C13 1.386(5) . ?
C9 N4 1.417(4) . ?
C10 C11 1.353(5) . ?
C10 N4 1.381(5) . ?
C10 H10 0.9300 . ?
C11 N5 1.367(5) . ?
C11 H11 0.9300 . ?
C12 N5 1.304(4) . ?
C12 N4 1.346(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.376(5) . ?
C13 H13 0.9300 . ?
C14 C15 1.386(5) . ?
C14 N6 1.429(4) . ?
C15 H15 0.9300 . ?
C16 N6 1.347(5) . ?
C16 C17 1.355(6) . ?
C16 H16 0.9300 . ?
C17 N7 1.368(5) . ?
C17 H17 0.9300 . ?
C18 N7 1.306(4) . ?
C18 N6 1.342(4) . ?
C18 H18 0.9300 . ?
Co1 O9 1.981(2) . ?
Co1 O6 2.000(2) . ?
Co1 O3 2.028(2) . ?
Co1 N5 2.080(3) 2_665 ?
Co1 N1 2.268(3) . ?
Co2 O4 1.940(2) . ?
Co2 O2 1.953(2) 2_556 ?
Co2 O1 1.969(2) 1_655 ?
Co2 N7 2.021(3) 1_546 ?
Co3 O7 1.933(2) 1_655 ?
Co3 O8 1.946(2) 2_566 ?
Co3 O5 1.952(2) . ?
Co3 N2 2.016(3) . ?
N5 Co1 2.080(3) 2_665 ?
N7 Co2 2.021(3) 1_564 ?
O1 P1 1.525(2) . ?
O1 Co2 1.969(2) 1_455 ?
O2 P1 1.527(2) . ?
O2 Co2 1.953(2) 2_556 ?
O3 P1 1.524(2) . ?
O4 P2 1.523(2) . ?
O5 P2 1.528(2) . ?
O6 P2 1.523(2) . ?
O7 P3 1.503(2) . ?
O7 Co3 1.933(2) 1_455 ?
O8 P3 1.525(2) . ?
O8 Co3 1.946(2) 2_566 ?
O9 P3 1.535(2) . ?

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
N1 C1 P1 110.3(2) . . ?
N1 C1 H1A 109.6 . . ?
P1 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
P1 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 P2 110.3(2) . . ?
N1 C2 H2A 109.6 . . ?
P2 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
P2 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N1 C3 P3 110.0(2) . . ?
N1 C3 H3A 109.7 . . ?
P3 C3 H3A 109.7 . . ?
N1 C3 H3B 109.7 . . ?
P3 C3 H3B 109.7 . . ?
H3A C3 H3B 108.2 . . ?
C5 C4 N2 110.2(3) . . ?
C5 C4 H4 124.9 . . ?
N2 C4 H4 124.9 . . ?
C4 C5 N3 106.2(3) . . ?
C4 C5 H5 126.9 . . ?
N3 C5 H5 126.9 . . ?
N2 C6 N3 110.7(3) . . ?
N2 C6 H6 124.6 . . ?
N3 C6 H6 124.6 . . ?
C15 C7 C8 122.3(3) . . ?
C15 C7 N3 119.4(3) . . ?
C8 C7 N3 118.3(3) . . ?
C9 C8 C7 117.6(3) . . ?
C9 C8 H8 121.2 . . ?
C7 C8 H8 121.2 . . ?
C13 C9 C8 120.8(3) . . ?
C13 C9 N4 118.6(3) . . ?
C8 C9 N4 120.5(3) . . ?
C11 C10 N4 105.9(3) . . ?
C11 C10 H10 127.0 . . ?
N4 C10 H10 127.0 . . ?
C10 C11 N5 110.5(4) . . ?
C10 C11 H11 124.7 . . ?
N5 C11 H11 124.7 . . ?
N5 C12 N4 113.1(3) . . ?
N5 C12 H12 123.4 . . ?
N4 C12 H12 123.4 . . ?
C14 C13 C9 120.0(3) . . ?
C14 C13 H13 120.0 . . ?
C9 C13 H13 120.0 . . ?
C13 C14 C15 121.2(3) . . ?
C13 C14 N6 118.6(3) . . ?
C15 C14 N6 120.2(3) . . ?
C14 C15 C7 118.1(3) . . ?
C14 C15 H15 121.0 . . ?
C7 C15 H15 121.0 . . ?
N6 C16 C17 106.7(4) . . ?
N6 C16 H16 126.7 . . ?
C17 C16 H16 126.7 . . ?
C16 C17 N7 109.5(4) . . ?
C16 C17 H17 125.2 . . ?
N7 C17 H17 125.2 . . ?
N7 C18 N6 112.3(3) . . ?
N7 C18 H18 123.9 . . ?
N6 C18 H18 123.9 . . ?
O9 Co1 O6 123.23(10) . . ?
O9 Co1 O3 117.33(11) . . ?
O6 Co1 O3 116.64(11) . . ?
O9 Co1 N5 98.03(10) . 2_665 ?
O6 Co1 N5 92.14(11) . 2_665 ?
O3 Co1 N5 96.57(11) . 2_665 ?
O9 Co1 N1 85.64(9) . . ?
O6 Co1 N1 84.07(9) . . ?
O3 Co1 N1 83.52(9) . . ?
N5 Co1 N1 175.78(10) 2_665 . ?
O4 Co2 O2 111.17(11) . 2_556 ?
O4 Co2 O1 117.65(10) . 1_655 ?
O2 Co2 O1 105.55(11) 2_556 1_655 ?
O4 Co2 N7 100.75(11) . 1_546 ?
O2 Co2 N7 112.97(12) 2_556 1_546 ?
O1 Co2 N7 108.95(12) 1_655 1_546 ?
O7 Co3 O8 116.11(10) 1_655 2_566 ?
O7 Co3 O5 109.92(10) 1_655 . ?
O8 Co3 O5 105.42(10) 2_566 . ?
O7 Co3 N2 98.19(11) 1_655 . ?
O8 Co3 N2 106.16(11) 2_566 . ?
O5 Co3 N2 121.57(11) . . ?
C1 N1 C3 111.6(2) . . ?
C1 N1 C2 110.9(2) . . ?
C3 N1 C2 111.6(2) . . ?
C1 N1 Co1 108.04(18) . . ?
C3 N1 Co1 107.02(17) . . ?
C2 N1 Co1 107.45(17) . . ?
C6 N2 C4 106.2(3) . . ?
C6 N2 Co3 122.8(2) . . ?
C4 N2 Co3 130.8(2) . . ?
C6 N3 C5 106.6(3) . . ?
C6 N3 C7 126.5(3) . . ?
C5 N3 C7 127.0(3) . . ?
C12 N4 C10 105.7(3) . . ?
C12 N4 C9 125.0(3) . . ?
C10 N4 C9 129.1(3) . . ?
C12 N5 C11 104.8(3) . . ?
C12 N5 Co1 116.2(2) . 2_665 ?
C11 N5 Co1 138.2(2) . 2_665 ?
C18 N6 C16 106.6(3) . . ?
C18 N6 C14 125.3(3) . . ?
C16 N6 C14 128.1(3) . . ?
C18 N7 C17 104.9(3) . . ?
C18 N7 Co2 129.5(3) . 1_564 ?
C17 N7 Co2 125.6(3) . 1_564 ?
P1 O1 Co2 135.02(15) . 1_455 ?
P1 O2 Co2 133.33(16) . 2_556 ?
P1 O3 Co1 120.47(13) . . ?
P2 O4 Co2 139.85(15) . . ?
P2 O5 Co3 129.81(15) . . ?
P2 O6 Co1 121.37(13) . . ?
P3 O7 Co3 149.25(16) . 1_455 ?
P3 O8 Co3 128.49(14) . 2_566 ?
P3 O9 Co1 119.28(13) . . ?
O3 P1 O1 111.40(14) . . ?
O3 P1 O2 112.13(15) . . ?
O1 P1 O2 111.96(14) . . ?
O3 P1 C1 104.49(14) . . ?
O1 P1 C1 110.47(15) . . ?
O2 P1 C1 105.98(15) . . ?
O6 P2 O4 112.56(14) . . ?
O6 P2 O5 112.01(14) . . ?
O4 P2 O5 110.77(14) . . ?
O6 P2 C2 104.60(14) . . ?
O4 P2 C2 110.12(14) . . ?
O5 P2 C2 106.43(14) . . ?
O7 P3 O8 112.44(14) . . ?
O7 P3 O9 111.29(14) . . ?
O8 P3 O9 111.02(13) . . ?
O7 P3 C3 108.73(14) . . ?
O8 P3 C3 108.43(15) . . ?
O9 P3 C3 104.57(14) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N2 C4 C5 N3 1.5(4) . . . . ?
C15 C7 C8 C9 0.6(6) . . . . ?
N3 C7 C8 C9 179.2(3) . . . . ?
C7 C8 C9 C13 0.3(6) . . . . ?
C7 C8 C9 N4 -178.7(3) . . . . ?
N4 C10 C11 N5 0.2(6) . . . . ?
C8 C9 C13 C14 -1.9(6) . . . . ?
N4 C9 C13 C14 177.2(4) . . . . ?
C9 C13 C14 C15 2.6(6) . . . . ?
C9 C13 C14 N6 -176.0(4) . . . . ?
C13 C14 C15 C7 -1.7(6) . . . . ?
N6 C14 C15 C7 176.9(4) . . . . ?
C8 C7 C15 C14 0.1(6) . . . . ?
N3 C7 C15 C14 -178.5(3) . . . . ?
N6 C16 C17 N7 -1.8(7) . . . . ?
P1 C1 N1 C3 81.3(3) . . . . ?
P1 C1 N1 C2 -153.7(2) . . . . ?
P1 C1 N1 Co1 -36.1(2) . . . . ?
P3 C3 N1 C1 -152.7(2) . . . . ?
P3 C3 N1 C2 82.6(3) . . . . ?
P3 C3 N1 Co1 -34.7(2) . . . . ?
P2 C2 N1 C1 82.0(3) . . . . ?
P2 C2 N1 C3 -152.9(2) . . . . ?
P2 C2 N1 Co1 -35.9(2) . . . . ?
O9 Co1 N1 C1 138.93(19) . . . . ?
O6 Co1 N1 C1 -96.98(19) . . . . ?
O3 Co1 N1 C1 20.76(19) . . . . ?
N5 Co1 N1 C1 -70.6(14) 2_665 . . . ?
O9 Co1 N1 C3 18.66(18) . . . . ?
O6 Co1 N1 C3 142.74(19) . . . . ?
O3 Co1 N1 C3 -99.52(19) . . . . ?
N5 Co1 N1 C3 169.1(13) 2_665 . . . ?
O9 Co1 N1 C2 -101.32(19) . . . . ?
O6 Co1 N1 C2 22.77(18) . . . . ?
O3 Co1 N1 C2 140.51(19) . . . . ?
N5 Co1 N1 C2 49.1(15) 2_665 . . . ?
N3 C6 N2 C4 -0.3(4) . . . . ?
N3 C6 N2 Co3 -175.5(2) . . . . ?
C5 C4 N2 C6 -0.8(4) . . . . ?
C5 C4 N2 Co3 173.9(3) . . . . ?
O7 Co3 N2 C6 8.2(3) 1_655 . . . ?
O8 Co3 N2 C6 128.5(3) 2_566 . . . ?
O5 Co3 N2 C6 -111.3(3) . . . . ?
O7 Co3 N2 C4 -165.7(3) 1_655 . . . ?
O8 Co3 N2 C4 -45.4(3) 2_566 . . . ?
O5 Co3 N2 C4 74.8(3) . . . . ?
N2 C6 N3 C5 1.2(4) . . . . ?
N2 C6 N3 C7 -179.4(3) . . . . ?
C4 C5 N3 C6 -1.6(4) . . . . ?
C4 C5 N3 C7 179.0(3) . . . . ?
C15 C7 N3 C6 -152.2(4) . . . . ?
C8 C7 N3 C6 29.2(6) . . . . ?
C15 C7 N3 C5 27.1(6) . . . . ?
C8 C7 N3 C5 -151.5(4) . . . . ?
N5 C12 N4 C10 -0.5(5) . . . . ?
N5 C12 N4 C9 -176.3(3) . . . . ?
C11 C10 N4 C12 0.2(5) . . . . ?
C11 C10 N4 C9 175.7(4) . . . . ?
C13 C9 N4 C12 8.1(6) . . . . ?
C8 C9 N4 C12 -172.9(4) . . . . ?
C13 C9 N4 C10 -166.7(4) . . . . ?
C8 C9 N4 C10 12.3(6) . . . . ?
N4 C12 N5 C11 0.6(5) . . . . ?
N4 C12 N5 Co1 172.0(3) . . . 2_665 ?
C10 C11 N5 C12 -0.5(5) . . . . ?
C10 C11 N5 Co1 -168.9(3) . . . 2_665 ?
N7 C18 N6 C16 -1.4(5) . . . . ?
N7 C18 N6 C14 177.8(3) . . . . ?
C17 C16 N6 C18 1.9(6) . . . . ?
C17 C16 N6 C14 -177.2(4) . . . . ?
C13 C14 N6 C18 32.2(6) . . . . ?
C15 C14 N6 C18 -146.4(4) . . . . ?
C13 C14 N6 C16 -148.7(5) . . . . ?
C15 C14 N6 C16 32.6(7) . . . . ?
N6 C18 N7 C17 0.3(5) . . . . ?
N6 C18 N7 Co2 -178.2(3) . . . 1_564 ?
C16 C17 N7 C18 1.0(6) . . . . ?
C16 C17 N7 Co2 179.5(4) . . . 1_564 ?
O9 Co1 O3 P1 -78.52(19) . . . . ?
O6 Co1 O3 P1 83.18(18) . . . . ?
N5 Co1 O3 P1 178.90(17) 2_665 . . . ?
N1 Co1 O3 P1 3.15(16) . . . . ?
O2 Co2 O4 P2 -114.0(2) 2_556 . . . ?
O1 Co2 O4 P2 7.8(3) 1_655 . . . ?
N7 Co2 O4 P2 126.0(2) 1_546 . . . ?
O7 Co3 O5 P2 -115.61(19) 1_655 . . . ?
O8 Co3 O5 P2 118.55(19) 2_566 . . . ?
N2 Co3 O5 P2 -2.0(2) . . . . ?
O9 Co1 O6 P2 79.94(18) . . . . ?
O3 Co1 O6 P2 -80.58(18) . . . . ?
N5 Co1 O6 P2 -179.02(17) 2_665 . . . ?
N1 Co1 O6 P2 -0.89(16) . . . . ?
O6 Co1 O9 P3 -73.65(18) . . . . ?
O3 Co1 O9 P3 86.74(17) . . . . ?
N5 Co1 O9 P3 -171.55(15) 2_665 . . . ?
N1 Co1 O9 P3 6.35(15) . . . . ?
Co1 O3 P1 O1 97.80(18) . . . . ?
Co1 O3 P1 O2 -135.83(16) . . . . ?
Co1 O3 P1 C1 -21.5(2) . . . . ?
Co2 O1 P1 O3 173.49(18) 1_455 . . . ?
Co2 O1 P1 O2 47.0(3) 1_455 . . . ?
Co2 O1 P1 C1 -70.8(2) 1_455 . . . ?
Co2 O2 P1 O3 -79.3(2) 2_556 . . . ?
Co2 O2 P1 O1 46.7(3) 2_556 . . . ?
Co2 O2 P1 C1 167.2(2) 2_556 . . . ?
N1 C1 P1 O3 38.1(2) . . . . ?
N1 C1 P1 O1 -81.8(2) . . . . ?
N1 C1 P1 O2 156.7(2) . . . . ?
Co1 O6 P2 O4 102.71(17) . . . . ?
Co1 O6 P2 O5 -131.70(16) . . . . ?
Co1 O6 P2 C2 -16.8(2) . . . . ?
Co2 O4 P2 O6 60.9(3) . . . . ?
Co2 O4 P2 O5 -65.3(3) . . . . ?
Co2 O4 P2 C2 177.2(2) . . . . ?
Co3 O5 P2 O6 23.0(2) . . . . ?
Co3 O5 P2 O4 149.60(17) . . . . ?
Co3 O5 P2 C2 -90.7(2) . . . . ?
N1 C2 P2 O6 35.3(2) . . . . ?
N1 C2 P2 O4 -85.9(2) . . . . ?
N1 C2 P2 O5 154.0(2) . . . . ?
Co3 O7 P3 O8 -102.3(3) 1_455 . . . ?
Co3 O7 P3 O9 132.4(3) 1_455 . . . ?
Co3 O7 P3 C3 17.7(4) 1_455 . . . ?
Co3 O8 P3 O7 33.3(2) 2_566 . . . ?
Co3 O8 P3 O9 158.69(15) 2_566 . . . ?
Co3 O8 P3 C3 -87.0(2) 2_566 . . . ?
Co1 O9 P3 O7 -141.89(15) . . . . ?
Co1 O9 P3 O8 92.05(17) . . . . ?
Co1 O9 P3 C3 -24.68(18) . . . . ?
N1 C3 P3 O7 158.4(2) . . . . ?
N1 C3 P3 O8 -79.0(2) . . . . ?
N1 C3 P3 O9 39.5(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.092
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.011 0.000 0.000 697 180 ' '
_platon_squeeze_details          
;
The PLATON SQUEEZE procedure was used to treat 
regions of diffuse solvent which could not be modeled 
properly in terms of atomic sites. Their contribution to 
the diffraction pattern was removed and modified F² was
written to a new HKL file. The number of located electrons, 
in one void per unit cell is 180.There are two formula units 
in one unit cell. On base of charge balance considerations, 
volume/count_electrons analysis, TG analyses and elemental analyses, 
this residual electron density was assigned to nine water molecules.  
So SQUEEZE removed these disordered units per unit cell. 
See refs. (a) O. V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake,
L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun.
2004, 642; (b) Y. Du, A. L. Thompson and D. O. Hare. Chem. Commun. 2008, 5987;
(c) Y. F. Bi, X. T. Wang, W. P. Liao, X. F. Wang, X. W. Wang, H. J. Zhang,
and S. Gao, J. Am. Chem. Soc. 2009, 131, 11650.
;
