# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2015

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

data_activated
_database_code_depnum_ccdc_archive 'CCDC 1419218'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2015-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H36.50 N3 Ni1.50 O12.25 P3'
_chemical_formula_weight         780.06

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.5126(12)
_cell_length_b                   18.5126(12)
_cell_length_c                   22.922(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7855.6(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.414
_cell_measurement_theta_max      27.559

_exptl_crystal_description       colum
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_F_000             3236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.904
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14573
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.414
_diffrn_reflns_theta_max         27.559
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4617
_reflns_number_gt                2231
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_max     0.958
_reflns_Friedel_fraction_full    0.980

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_vrf_PLAT430_activated           
;
PROBLEM: Short Inter D...A Contact  O2..  O4W..  2.01 Ang.
RESPONSE: The lattice water O4w could be disordered.
;
_vrf_PLAT043_activated           
;
PROBLEM: Calculated and Reported Mol. Weight Differ by .. 36.38
RESPONSE: The hydrogen atoms are not added to the water molecules.
;
_vrf_PLAT602_activated           
;
PROBLEM:  VERY LARGE Solvent Accessible VOID(S) in Structure.
RESPONSE: The lattice water molecules in the void are squeezed.
;
_vrf_PLAT306_activated           
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O4W 
RESPONSE: The hydrogen atoms are not added to the water molecules.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.0800P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 779 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.028(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         4617
_refine_ls_number_parameters     231
_refine_ls_number_restraints     21
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0585
_refine_ls_wR_factor_ref         0.1468
_refine_ls_wR_factor_gt          0.1313
_refine_ls_goodness_of_fit_ref   0.857
_refine_ls_restrained_S_all      0.862
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 1.0000 0.7500 0.0484(4) Uani 1 4 d S T P . .
Ni2 Ni 0.28579(6) 0.71421(6) 0.41853(6) 0.0784(5) Uani 1 2 d S T P . .
O1 O 0.3233(3) 0.6767(3) 0.4974(4) 0.109(3) Uani 1 2 d S TU P . .
O1W O 0.2796(4) 0.6083(3) 0.3893(3) 0.113(2) Uani 1 1 d . . . . .
O2 O 0.4234(5) 0.5766(5) 0.4929(7) 0.230(9) Uani 1 2 d S TU P . .
O2W O 0.2554(3) 0.7446(3) 0.3346(3) 0.075(2) Uani 1 2 d S T P . .
O3 O 0.3105(9) 0.5612(7) 0.4929(7) 0.142(6) Uani 0.5 1 d . U P . .
H3A H 0.3231 0.5222 0.5064 0.213 Uiso 0.5 1 calc R U P . .
O4W O 0.5000 0.5000 0.5000 0.0147(18) Uani 1 8 d S T P . .
O4 O 0.3950(2) 0.9595(2) 0.7488(2) 0.0569(11) Uani 1 1 d . . . . .
O5 O 0.3017(3) 0.8772(3) 0.7938(2) 0.0826(16) Uani 1 1 d . . . . .
O6 O 0.4185(3) 0.8276(3) 0.7609(3) 0.0909(18) Uani 1 1 d . . . . .
H6D H 0.4586 0.8463 0.7588 0.136 Uiso 1 1 calc R U . . .
N1 N 0.5000 1.0000 0.8443(3) 0.0496(17) Uani 1 2 d S T P . .
P1 P 0.37176(14) 0.62824(14) 0.5145(2) 0.1089(14) Uani 1 2 d S TU P . .
P2 P 0.35944(9) 0.88591(9) 0.74954(11) 0.0608(5) Uani 1 1 d . . . . .
C1 C 0.3245(4) 0.6755(4) 0.6266(6) 0.074(3) Uani 1 2 d S T P . .
C2 C 0.3469(5) 0.7453(5) 0.6399(4) 0.075(2) Uani 1 1 d . . . . .
C3 C 0.2977(4) 0.7940(4) 0.6639(3) 0.0557(17) Uani 1 1 d . . . . .
C4 C 0.2266(5) 0.7734(5) 0.6759(5) 0.069(3) Uani 1 2 d S T P . .
C5 C 0.3774(4) 0.6226(4) 0.5901(8) 0.102(5) Uani 1 2 d S T P . .
H5A H 0.4269 0.6323 0.6009 0.122 Uiso 0.5 1 d R U P . .
C6 C 0.4242(5) 0.7667(5) 0.6266(5) 0.107(3) Uani 1 1 d . . . . .
H6A H 0.4489 0.7269 0.6086 0.161 Uiso 1 1 calc R U . . .
H6B H 0.4484 0.7795 0.6622 0.161 Uiso 1 1 calc R U . . .
H6C H 0.4244 0.8073 0.6006 0.161 Uiso 1 1 calc R U . . .
C7 C 0.3229(4) 0.8706(4) 0.6772(3) 0.067(2) Uani 1 1 d . . . . .
H7A H 0.2824 0.9030 0.6717 0.080 Uiso 1 1 calc R U . . .
H7B H 0.3596 0.8837 0.6489 0.080 Uiso 1 1 calc R U . . .
C8 C 0.1721(4) 0.8279(4) 0.7006(6) 0.073(3) Uani 1 2 d S T P . .
H8A H 0.1261 0.8048 0.7055 0.110 Uiso 0.25 1 calc R U P . .
H8B H 0.1672 0.8677 0.6741 0.110 Uiso 0.25 1 calc R U P . .
H8C H 0.1889 0.8453 0.7376 0.110 Uiso 0.25 1 calc R U P . .
C9 C 0.1630(5) 0.6982(7) 0.5001(5) 0.120(4) Uani 1 1 d . . . . .
H9A H 0.2017 0.6903 0.5252 0.144 Uiso 1 1 calc R U . . .
C10 C 0.0949(6) 0.6981(9) 0.5248(5) 0.135(5) Uani 1 1 d . . . . .
H10A H 0.0882 0.6885 0.5643 0.162 Uiso 1 1 calc R U . . .
C11 C 0.0395(5) 0.7123(5) 0.4901(3) 0.077(2) Uani 1 1 d . . . . .
C12 C 0.0519(5) 0.7204(7) 0.4307(4) 0.111(3) Uani 1 1 d . . . . .
H12A H 0.0142 0.7256 0.4042 0.133 Uiso 1 1 calc R U . . .
C13 C 0.1231(6) 0.7202(7) 0.4132(4) 0.109(3) Uani 1 1 d . . . . .
H13A H 0.1321 0.7297 0.3740 0.131 Uiso 1 1 calc R U . . .
N2 N 0.1783(5) 0.7079(4) 0.4461(4) 0.086(2) Uani 1 1 d . . . . .
C14 C 0.4424(4) 0.9805(4) 0.8763(4) 0.068(2) Uani 1 1 d . . . . .
H14A H 0.4010 0.9661 0.8565 0.081 Uiso 1 1 calc R U . . .
C15 C 0.4404(4) 0.9806(4) 0.9344(3) 0.064(2) Uani 1 1 d . . . . .
H15A H 0.3978 0.9671 0.9530 0.077 Uiso 1 1 calc R U . . .
C16 C 0.5000 1.0000 0.9683(4) 0.053(2) Uani 1 2 d S T P . .


_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 O4 2.084(4) . ?
Ni1 O4 2.084(4) 2_675 ?
Ni1 O4 2.084(4) 12_656 ?
Ni1 O4 2.084(4) 11_466 ?
Ni1 N1 2.161(8) . ?
Ni1 N1 2.161(8) 11_466 ?
Ni2 O1 2.056(11) . ?
Ni2 O1W 2.076(6) . ?
Ni2 O1W 2.076(6) 7_665 ?
Ni2 O2W 2.082(8) . ?
Ni2 N2 2.091(8) . ?
Ni2 N2 2.091(8) 7_665 ?
O1 P1 1.329(10) . ?
O2 P1 1.440(14) . ?
O3 P1 1.753(12) . ?
O4 P2 1.513(4) . ?
O5 P2 1.483(6) . ?
O6 P2 1.558(6) . ?
N1 C14 1.344(9) . ?
N1 C14 1.344(9) 2_675 ?
P1 C5 1.738(17) . ?
P1 O3 1.753(12) 7_665 ?
P2 C7 1.813(8) . ?
C1 C2 1.391(10) 7_665 ?
C1 C2 1.391(10) . ?
C1 C5 1.616(18) . ?
C2 C3 1.395(11) . ?
C2 C6 1.517(12) . ?
C3 C4 1.397(9) . ?
C3 C7 1.524(10) . ?
C4 C3 1.397(9) 7_665 ?
C4 C8 1.537(16) . ?
C9 N2 1.282(13) . ?
C9 C10 1.383(13) . ?
C10 C11 1.324(13) . ?
C11 C12 1.388(11) . ?
C11 C11 1.533(16) 5_556 ?
C12 C13 1.377(12) . ?
C13 N2 1.292(11) . ?
C14 C15 1.333(11) . ?
C15 C16 1.397(9) . ?
C16 C15 1.397(9) 2_675 ?
C16 C16 1.452(18) 5_657 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O4 178.5(3) . 2_675 ?
O4 Ni1 O4 90.008(5) . 12_656 ?
O4 Ni1 O4 90.009(5) 2_675 12_656 ?
O4 Ni1 O4 90.010(5) . 11_466 ?
O4 Ni1 O4 90.009(5) 2_675 11_466 ?
O4 Ni1 O4 178.5(3) 12_656 11_466 ?
O4 Ni1 N1 90.73(15) . . ?
O4 Ni1 N1 90.73(15) 2_675 . ?
O4 Ni1 N1 89.27(15) 12_656 . ?
O4 Ni1 N1 89.27(15) 11_466 . ?
O4 Ni1 N1 89.27(15) . 11_466 ?
O4 Ni1 N1 89.27(15) 2_675 11_466 ?
O4 Ni1 N1 90.73(15) 12_656 11_466 ?
O4 Ni1 N1 90.73(15) 11_466 11_466 ?
N1 Ni1 N1 180.0 . 11_466 ?
O1 Ni2 O1W 89.1(3) . . ?
O1 Ni2 O1W 89.1(3) . 7_665 ?
O1W Ni2 O1W 90.0(4) . 7_665 ?
O1 Ni2 O2W 174.0(3) . . ?
O1W Ni2 O2W 86.7(2) . . ?
O1W Ni2 O2W 86.7(2) 7_665 . ?
O1 Ni2 N2 92.1(3) . . ?
O1W Ni2 N2 89.6(3) . . ?
O1W Ni2 N2 178.8(3) 7_665 . ?
O2W Ni2 N2 92.1(3) . . ?
O1 Ni2 N2 92.1(3) . 7_665 ?
O1W Ni2 N2 178.8(3) . 7_665 ?
O1W Ni2 N2 89.6(3) 7_665 7_665 ?
O2W Ni2 N2 92.1(3) . 7_665 ?
N2 Ni2 N2 90.8(4) . 7_665 ?
P1 O1 Ni2 135.7(6) . . ?
P2 O4 Ni1 136.9(2) . . ?
C14 N1 C14 113.8(9) . 2_675 ?
C14 N1 Ni1 123.1(5) . . ?
C14 N1 Ni1 123.1(5) 2_675 . ?
O1 P1 O2 142.6(8) . . ?
O1 P1 C5 112.1(6) . . ?
O2 P1 C5 105.3(7) . . ?
O1 P1 O3 87.6(6) . 7_665 ?
O2 P1 O3 82.1(6) . 7_665 ?
C5 P1 O3 106.1(6) . 7_665 ?
O1 P1 O3 87.6(6) . . ?
O2 P1 O3 82.1(6) . . ?
C5 P1 O3 106.1(6) . . ?
O3 P1 O3 146.8(12) 7_665 . ?
O5 P2 O4 114.8(3) . . ?
O5 P2 O6 108.4(3) . . ?
O4 P2 O6 108.6(3) . . ?
O5 P2 C7 109.9(3) . . ?
O4 P2 C7 107.1(3) . . ?
O6 P2 C7 107.8(4) . . ?
C2 C1 C2 120.3(12) 7_665 . ?
C2 C1 C5 119.7(6) 7_665 . ?
C2 C1 C5 119.7(6) . . ?
C1 C2 C3 119.6(8) . . ?
C1 C2 C6 118.7(9) . . ?
C3 C2 C6 121.7(7) . . ?
C2 C3 C4 121.0(8) . . ?
C2 C3 C7 118.7(7) . . ?
C4 C3 C7 120.2(8) . . ?
C3 C4 C3 118.4(11) 7_665 . ?
C3 C4 C8 120.8(6) 7_665 . ?
C3 C4 C8 120.8(6) . . ?
C1 C5 P1 116.3(8) . . ?
C3 C7 P2 116.4(5) . . ?
N2 C9 C10 126.7(10) . . ?
C11 C10 C9 117.4(9) . . ?
C10 C11 C12 118.9(8) . . ?
C10 C11 C11 124.1(9) . 5_556 ?
C12 C11 C11 116.7(10) . 5_556 ?
C13 C12 C11 116.4(9) . . ?
N2 C13 C12 125.9(9) . . ?
C9 N2 C13 114.5(8) . . ?
C9 N2 Ni2 120.7(8) . . ?
C13 N2 Ni2 124.5(6) . . ?
C15 C14 N1 124.6(8) . . ?
C14 C15 C16 122.3(7) . . ?
C15 C16 C15 112.4(9) . 2_675 ?
C15 C16 C16 123.8(4) . 5_657 ?
C15 C16 C16 123.8(4) 2_675 5_657 ?

_refine_diff_density_max         0.611
_refine_diff_density_min         -0.466
_refine_diff_density_rms         0.066

_shelxl_version_number           2013-2



####################################################################### 
# 
# 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_as-synthesized
_database_code_depnum_ccdc_archive 'CCDC 1419219'
_audit_update_record             
;
2015-08-14 deposited with the CCDC.
2015-12-08 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C27 H37 N3 Ni1.50 O12.50 P3'
_chemical_formula_weight         784.57

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   18.5564(16)
_cell_length_b                   18.5564(16)
_cell_length_c                   22.937(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7898(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      25

_exptl_crystal_description       column
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_F_000             3256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.900
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31588
_diffrn_reflns_av_unetI/netI     0.1005
_diffrn_reflns_av_R_equivalents  0.1509
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.359
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.969
_reflns_number_total             3641
_reflns_number_gt                2112
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.830
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.971

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_vrf_PLAT430_as-synthesized      
;
PROBLEM: Short Inter D...A Contact  O2..  O4W..  2.11 Ang.
RESPONSE: The lattice water molecules are disordered.
;
_vrf_PLAT602_as-synthesized      
;
PROBLEM:  VERY LARGE Solvent Accessible VOID(S) in Structure.
RESPONSE: The lattice water molecules in the void are squeezed.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 w=1/[σ²(Fo²)+(0.1185P)²]
 where P=(Fo²+2Fc²)/3
;
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 656 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.06(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3641
_refine_ls_number_parameters     235
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.1402
_refine_ls_R_factor_gt           0.0856
_refine_ls_wR_factor_ref         0.2226
_refine_ls_wR_factor_gt          0.1941
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.030
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.0000 0.2500 0.0572(9) Uani 1 4 d S T P . .
Ni2 Ni 0.71458(12) 0.28542(12) 0.58145(13) 0.0913(11) Uani 1 2 d S T P . .
O1 O 0.6775(7) 0.3225(7) 0.5056(10) 0.146(8) Uani 1 2 d S T P . .
O1W O 0.7205(7) 0.3929(6) 0.6109(6) 0.124(4) Uani 1 1 d . . . . .
O2 O 0.5798(9) 0.4202(9) 0.5113(13) 0.234(14) Uani 1 2 d S T P . .
O2W O 0.7456(5) 0.2544(5) 0.6643(6) 0.080(4) Uani 1 2 d S T P . .
O3 O 0.6928(14) 0.4376(11) 0.5101(13) 0.133(10) Uani 0.5 1 d . U P . .
H3A H 0.6818 0.4774 0.4973 0.200 Uiso 0.5 1 calc R U P . .
O3W O 0.5000 0.5000 0.591(2) 0.117(18) Uani 0.5 4 d S T P . .
O4W O 0.5000 0.5000 0.5000 0.018(3) Uani 1 8 d S T P . .
O4 O 0.6045(4) 0.0403(4) 0.2508(5) 0.064(2) Uani 1 1 d . . . . .
O5 O 0.6997(5) 0.1228(6) 0.2060(5) 0.092(3) Uani 1 1 d . . . . .
O6 O 0.5811(5) 0.1725(4) 0.2401(6) 0.108(4) Uani 1 1 d . . . . .
H6D H 0.5412 0.1537 0.2422 0.162 Uiso 1 1 calc R U . . .
N1 N 0.5000 0.0000 0.1555(7) 0.064(4) Uani 1 2 d S T P . .
P1 P 0.6283(3) 0.3717(3) 0.4856(4) 0.123(3) Uani 1 2 d S T P . .
P2 P 0.64090(16) 0.11381(16) 0.2503(2) 0.0713(11) Uani 1 1 d . . . . .
C1 C 0.6740(8) 0.3260(8) 0.3737(11) 0.080(6) Uani 1 2 d S T P . .
C2 C 0.6537(8) 0.2563(8) 0.3611(8) 0.086(5) Uani 1 1 d . . . . .
C3 C 0.7028(7) 0.2069(8) 0.3349(7) 0.073(4) Uani 1 1 d . . . . .
C4 C 0.7717(8) 0.2283(8) 0.3229(7) 0.067(5) Uani 1 2 d S T P . .
C5 C 0.6216(6) 0.3784(6) 0.4092(12) 0.091(7) Uani 1 2 d S TU P . .
H5A H 0.5721 0.3677 0.3984 0.110 Uiso 0.5 1 d R U P . .
C6 C 0.5766(8) 0.2342(10) 0.3737(10) 0.135(8) Uani 1 1 d . . . . .
H6A H 0.5515 0.2736 0.3917 0.202 Uiso 1 1 calc R U . . .
H6B H 0.5765 0.1934 0.3995 0.202 Uiso 1 1 calc R U . . .
H6C H 0.5530 0.2215 0.3379 0.202 Uiso 1 1 calc R U . . .
C7 C 0.6772(8) 0.1296(7) 0.3214(6) 0.075(4) Uani 1 1 d . . . . .
H7A H 0.6408 0.1166 0.3498 0.090 Uiso 1 1 calc R U . . .
H7B H 0.7177 0.0973 0.3269 0.090 Uiso 1 1 calc R U . . .
C8 C 0.8274(6) 0.1726(6) 0.3008(10) 0.068(5) Uani 1 2 d S T P . .
H8A H 0.8733 0.1957 0.2960 0.103 Uiso 0.25 1 calc R U P . .
H8B H 0.8117 0.1534 0.2640 0.103 Uiso 0.25 1 calc R U P . .
H8C H 0.8317 0.1342 0.3286 0.103 Uiso 0.25 1 calc R U P . .
C9 C 0.8362(10) 0.3017(14) 0.5015(9) 0.138(9) Uani 1 1 d . . . . .
H9A H 0.7980 0.3119 0.4766 0.165 Uiso 1 1 calc R U . . .
C10 C 0.9081(11) 0.2981(13) 0.4768(8) 0.117(7) Uani 1 1 d . U . . .
H10A H 0.9155 0.3052 0.4371 0.140 Uiso 1 1 calc R U . . .
C11 C 0.9625(8) 0.2846(9) 0.5121(6) 0.078(4) Uani 1 1 d . U . . .
C12 C 0.9468(10) 0.2796(15) 0.5705(7) 0.148(9) Uani 1 1 d . U . . .
H12A H 0.9846 0.2761 0.5969 0.177 Uiso 1 1 calc R U . . .
C13 C 0.8786(11) 0.2795(15) 0.5910(11) 0.145(9) Uani 1 1 d . . . . .
H13A H 0.8700 0.2710 0.6303 0.174 Uiso 1 1 calc R U . . .
N2 N 0.8224(8) 0.2919(8) 0.5540(6) 0.092(4) Uani 1 1 d . . . . .
C14 C 0.5581(8) 0.0174(8) 0.1250(7) 0.069(4) Uani 1 1 d . . . . .
H14A H 0.5997 0.0302 0.1451 0.083 Uiso 1 1 calc R U . . .
C15 C 0.5598(7) 0.0174(7) 0.0661(8) 0.074(4) Uani 1 1 d . . . . .
H15A H 0.6027 0.0296 0.0476 0.089 Uiso 1 1 calc R U . . .
C16 C 0.5000 0.0000 0.0315(7) 0.059(4) Uani 1 2 d S T P . .


_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 O4 2.078(7) 2_655 ?
Ni1 O4 2.078(7) 12_545 ?
Ni1 O4 2.078(7) 11 ?
Ni1 O4 2.078(7) . ?
Ni1 N1 2.167(16) . ?
Ni1 N1 2.167(16) 11 ?
Ni2 O1 1.99(2) . ?
Ni2 O2W 2.068(15) . ?
Ni2 N2 2.101(14) 7_665 ?
Ni2 N2 2.101(14) . ?
Ni2 O1W 2.109(11) . ?
Ni2 O1W 2.109(11) 7_665 ?
O1 P1 1.37(2) . ?
O2 P1 1.40(2) . ?
O3 P1 1.801(19) . ?
O3 H3A 0.8200 . ?
O4 P2 1.523(7) . ?
O5 P2 1.500(11) . ?
O6 P2 1.572(10) . ?
O6 H6D 0.8200 . ?
N1 C14 1.326(17) 2_655 ?
N1 C14 1.326(17) . ?
P1 C5 1.76(3) . ?
P1 O3 1.801(19) 7_665 ?
P2 C7 1.788(15) . ?
C1 C2 1.378(18) 7_665 ?
C1 C2 1.378(18) . ?
C1 C5 1.60(3) . ?
C2 C3 1.43(2) . ?
C2 C6 1.52(2) . ?
C3 C4 1.367(16) . ?
C3 C7 1.541(18) . ?
C4 C3 1.367(16) 7_665 ?
C4 C8 1.55(3) . ?
C5 H5A 0.9727 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 N2 1.24(2) . ?
C9 C10 1.45(2) . ?
C9 H9A 0.9300 . ?
C10 C11 1.32(2) . ?
C10 H10A 0.9300 . ?
C11 C12 1.373(19) . ?
C11 C11 1.50(3) 5_756 ?
C12 C13 1.35(2) . ?
C12 H12A 0.9300 . ?
C13 N2 1.36(2) . ?
C13 H13A 0.9300 . ?
C14 C15 1.35(2) . ?
C14 H14A 0.9300 . ?
C15 C16 1.402(18) . ?
C15 H15A 0.9300 . ?
C16 C15 1.402(18) 2_655 ?
C16 C16 1.44(3) 5_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ni1 O4 90.005(6) 2_655 12_545 ?
O4 Ni1 O4 90.005(6) 2_655 11 ?
O4 Ni1 O4 178.9(6) 12_545 11 ?
O4 Ni1 O4 178.9(6) 2_655 . ?
O4 Ni1 O4 90.007(6) 12_545 . ?
O4 Ni1 O4 90.003(6) 11 . ?
O4 Ni1 N1 90.5(3) 2_655 . ?
O4 Ni1 N1 89.5(3) 12_545 . ?
O4 Ni1 N1 89.5(3) 11 . ?
O4 Ni1 N1 90.5(3) . . ?
O4 Ni1 N1 89.5(3) 2_655 11 ?
O4 Ni1 N1 90.5(3) 12_545 11 ?
O4 Ni1 N1 90.5(3) 11 11 ?
O4 Ni1 N1 89.5(3) . 11 ?
N1 Ni1 N1 180.0 . 11 ?
O1 Ni2 O2W 174.0(5) . . ?
O1 Ni2 N2 92.7(6) . 7_665 ?
O2W Ni2 N2 91.6(6) . 7_665 ?
O1 Ni2 N2 92.7(6) . . ?
O2W Ni2 N2 91.6(6) . . ?
N2 Ni2 N2 91.1(7) 7_665 . ?
O1 Ni2 O1W 88.4(5) . . ?
O2W Ni2 O1W 87.4(5) . . ?
N2 Ni2 O1W 178.8(6) 7_665 . ?
N2 Ni2 O1W 89.6(5) . . ?
O1 Ni2 O1W 88.4(5) . 7_665 ?
O2W Ni2 O1W 87.4(5) . 7_665 ?
N2 Ni2 O1W 89.6(5) 7_665 7_665 ?
N2 Ni2 O1W 178.8(6) . 7_665 ?
O1W Ni2 O1W 89.8(7) . 7_665 ?
P1 O1 Ni2 138.7(11) . . ?
P1 O3 H3A 109.5 . . ?
P2 O4 Ni1 137.4(4) . . ?
P2 O6 H6D 109.5 . . ?
C14 N1 C14 116.2(17) 2_655 . ?
C14 N1 Ni1 121.9(9) 2_655 . ?
C14 N1 Ni1 121.9(9) . . ?
O1 P1 O2 135.6(17) . . ?
O1 P1 C5 115.2(10) . . ?
O2 P1 C5 109.2(15) . . ?
O1 P1 O3 84.5(10) . 7_665 ?
O2 P1 O3 82.0(9) . 7_665 ?
C5 P1 O3 108.0(10) . 7_665 ?
O1 P1 O3 84.5(10) . . ?
O2 P1 O3 82.0(9) . . ?
C5 P1 O3 108.0(10) . . ?
O3 P1 O3 143.7(19) 7_665 . ?
O5 P2 O4 115.3(6) . . ?
O5 P2 O6 109.7(6) . . ?
O4 P2 O6 108.0(4) . . ?
O5 P2 C7 108.9(6) . . ?
O4 P2 C7 107.9(6) . . ?
O6 P2 C7 106.7(7) . . ?
C2 C1 C2 118(2) 7_665 . ?
C2 C1 C5 120.7(11) 7_665 . ?
C2 C1 C5 120.7(11) . . ?
C1 C2 C3 121.1(14) . . ?
C1 C2 C6 118.2(16) . . ?
C3 C2 C6 120.6(14) . . ?
C4 C3 C2 119.7(14) . . ?
C4 C3 C7 121.2(14) . . ?
C2 C3 C7 119.1(11) . . ?
C3 C4 C3 120(2) 7_665 . ?
C3 C4 C8 119.8(10) 7_665 . ?
C3 C4 C8 119.8(10) . . ?
C1 C5 P1 114.9(13) . . ?
C1 C5 H5A 108.7 . . ?
P1 C5 H5A 107.9 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C3 C7 P2 116.9(10) . . ?
C3 C7 H7A 108.1 . . ?
P2 C7 H7A 108.1 . . ?
C3 C7 H7B 108.1 . . ?
P2 C7 H7B 108.1 . . ?
H7A C7 H7B 107.3 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 124.2(18) . . ?
N2 C9 H9A 117.9 . . ?
C10 C9 H9A 117.9 . . ?
C11 C10 C9 118.2(15) . . ?
C11 C10 H10A 120.9 . . ?
C9 C10 H10A 120.9 . . ?
C10 C11 C12 116.7(15) . . ?
C10 C11 C11 118.9(17) . 5_756 ?
C12 C11 C11 124.0(19) . 5_756 ?
C13 C12 C11 123(2) . . ?
C13 C12 H12A 118.7 . . ?
C11 C12 H12A 118.7 . . ?
C12 C13 N2 120(2) . . ?
C12 C13 H13A 120.0 . . ?
N2 C13 H13A 120.0 . . ?
C9 N2 C13 117.9(17) . . ?
C9 N2 Ni2 119.7(15) . . ?
C13 N2 Ni2 122.1(11) . . ?
N1 C14 C15 123.2(13) . . ?
N1 C14 H14A 118.4 . . ?
C15 C14 H14A 118.4 . . ?
C14 C15 C16 123.2(13) . . ?
C14 C15 H15A 118.4 . . ?
C16 C15 H15A 118.4 . . ?
C15 C16 C15 111.1(18) . 2_655 ?
C15 C16 C16 124.5(9) . 5_655 ?
C15 C16 C16 124.5(9) 2_655 5_655 ?

_refine_diff_density_max         0.725
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.071

_shelxl_version_number           2013-2



