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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
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# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_comp1

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C43.35 H56.40 F14 N12 Ni3 O14.85 P4'
_chemical_formula_weight         1549.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   17.3467(3)
_cell_length_b                   17.1048(3)
_cell_length_c                   24.5607(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.689(1)
_cell_angle_gamma                90.00
_cell_volume                     6942.9(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    44485
_cell_measurement_theta_min      6.51
_cell_measurement_theta_max      71.85

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            blue
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3157
_exptl_absorpt_coefficient_mu    2.725
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52382
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         6.97
_diffrn_reflns_theta_max         61.00
_reflns_number_total             10461
_reflns_number_gt                7720
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_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)+(0.1759P)²+3.7507P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10461
_refine_ls_number_parameters     789
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0796
_refine_ls_wR_factor_ref         0.2621
_refine_ls_wR_factor_gt          0.2380
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.006
_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 0.54964(5) 0.09555(5) 0.69056(4) 0.0594(3) Uani 1 1 d . . .
Ni2 Ni 0.61585(5) -0.06920(5) 0.85389(4) 0.0651(3) Uani 1 1 d . . .
Ni3 Ni 0.35791(6) -0.06686(5) 0.72902(5) 0.0733(3) Uani 1 1 d . . .
O1 O 0.3721(2) 0.1505(2) 0.67281(17) 0.0737(10) Uani 1 1 d . . .
N1 N 0.4315(2) 0.1317(3) 0.6467(2) 0.0696(12) Uani 1 1 d . . .
N2 N 0.5461(3) 0.0971(3) 0.6046(2) 0.0644(11) Uani 1 1 d . . .
C1 C 0.3418(4) 0.1967(5) 0.5615(3) 0.095(2) Uani 1 1 d . . .
H1A H 0.3090 0.2100 0.5864 0.114 Uiso 1 1 calc R . .
H1B H 0.3102 0.1634 0.5302 0.114 Uiso 1 1 calc R . .
H1C H 0.3574 0.2448 0.5458 0.114 Uiso 1 1 calc R . .
C2 C 0.4167(3) 0.1537(3) 0.5955(3) 0.0713(14) Uani 1 1 d . . .
C3 C 0.4795(3) 0.1290(3) 0.5695(3) 0.0718(14) Uani 1 1 d . . .
C4 C 0.4669(4) 0.1339(4) 0.5108(3) 0.0861(17) Uani 1 1 d . . .
H4 H 0.4186 0.1564 0.4864 0.103 Uiso 1 1 calc R . .
C5 C 0.5261(4) 0.1054(4) 0.4882(3) 0.0892(19) Uani 1 1 d . . .
H5 H 0.5199 0.1098 0.4486 0.107 Uiso 1 1 calc R . .
C6 C 0.5942(4) 0.0704(4) 0.5252(3) 0.0820(18) Uani 1 1 d . . .
H6 H 0.6352 0.0495 0.5111 0.098 Uiso 1 1 calc R . .
C7 C 0.6014(3) 0.0666(3) 0.5822(3) 0.0716(15) Uani 1 1 d . . .
H7 H 0.6474 0.0412 0.6070 0.086 Uiso 1 1 calc R . .
O11 O 0.7134(2) 0.0092(2) 0.73686(18) 0.0782(11) Uani 1 1 d . . .
N11 N 0.6734(2) 0.0805(2) 0.72458(19) 0.0621(11) Uani 1 1 d . . .
N12 N 0.5931(2) 0.2106(2) 0.70168(19) 0.0622(10) Uani 1 1 d . . .
C11 C 0.8097(3) 0.1395(4) 0.7525(3) 0.0873(18) Uani 1 1 d . . .
H11A H 0.8274 0.0852 0.7608 0.105 Uiso 1 1 calc R . .
H11B H 0.8299 0.1710 0.7873 0.105 Uiso 1 1 calc R . .
H11C H 0.8310 0.1603 0.7228 0.105 Uiso 1 1 calc R . .
C12 C 0.7198(3) 0.1425(4) 0.7323(2) 0.0680(14) Uani 1 1 d . . .
C13 C 0.6756(3) 0.2158(3) 0.7219(2) 0.0655(13) Uani 1 1 d . . .
C14 C 0.7128(4) 0.2872(4) 0.7331(3) 0.0836(17) Uani 1 1 d . . .
H14 H 0.7702 0.2904 0.7458 0.100 Uiso 1 1 calc R . .
C15 C 0.6662(4) 0.3558(4) 0.7261(3) 0.0929(19) Uani 1 1 d . . .
H15 H 0.6914 0.4055 0.7351 0.112 Uiso 1 1 calc R . .
C16 C 0.5832(4) 0.3497(4) 0.7058(3) 0.095(2) Uani 1 1 d . . .
H16 H 0.5500 0.3950 0.7002 0.114 Uiso 1 1 calc R . .
C17 C 0.5492(3) 0.2756(3) 0.6935(3) 0.0735(15) Uani 1 1 d . . .
H17 H 0.4920 0.2713 0.6787 0.088 Uiso 1 1 calc R . .
O21 O 0.6865(2) 0.0989(2) 0.85383(18) 0.0765(10) Uani 1 1 d . . .
N21 N 0.7020(3) 0.0195(3) 0.8647(2) 0.0673(11) Uani 1 1 d . . .
N22 N 0.7254(3) -0.1297(3) 0.8803(2) 0.0749(13) Uani 1 1 d . . .
C21 C 0.8433(4) 0.0603(5) 0.9032(4) 0.106(2) Uani 1 1 d . . .
H21A H 0.8219 0.1122 0.8899 0.127 Uiso 1 1 calc R . .
H21B H 0.8846 0.0458 0.8853 0.127 Uiso 1 1 calc R . .
H21C H 0.8675 0.0613 0.9449 0.127 Uiso 1 1 calc R . .
C22 C 0.7760(3) 0.0017(4) 0.8875(3) 0.0756(15) Uani 1 1 d . . .
C23 C 0.7911(4) -0.0817(4) 0.8982(3) 0.0863(18) Uani 1 1 d . . .
C24 C 0.8677(5) -0.1134(6) 0.9229(4) 0.112(2) Uani 1 1 d . . .
H24 H 0.9137 -0.0803 0.9352 0.134 Uiso 1 1 calc R . .
C25 C 0.8761(6) -0.1913(7) 0.9294(4) 0.133(3) Uani 1 1 d . . .
H25 H 0.9284 -0.2133 0.9458 0.160 Uiso 1 1 calc R . .
C26 C 0.8104(6) -0.2388(5) 0.9125(4) 0.116(3) Uani 1 1 d . . .
H26 H 0.8162 -0.2938 0.9176 0.139 Uiso 1 1 calc R . .
C27 C 0.7349(5) -0.2064(4) 0.8879(3) 0.0914(19) Uani 1 1 d . . .
H27 H 0.6889 -0.2395 0.8761 0.110 Uiso 1 1 calc R . .
O31 O 0.5149(3) -0.2215(2) 0.8150(2) 0.0856(11) Uani 1 1 d . . .
N31 N 0.5476(3) -0.1683(3) 0.8582(2) 0.0745(13) Uani 1 1 d . . .
N32 N 0.6163(3) -0.0692(2) 0.9389(2) 0.0658(11) Uani 1 1 d . . .
C31 C 0.5088(6) -0.2643(4) 0.9197(4) 0.110(2) Uani 1 1 d . . .
H31A H 0.4693 -0.2832 0.8846 0.132 Uiso 1 1 calc R . .
H31B H 0.4817 -0.2556 0.9489 0.132 Uiso 1 1 calc R . .
H31C H 0.5517 -0.3033 0.9335 0.132 Uiso 1 1 calc R . .
C32 C 0.5446(4) -0.1896(3) 0.9079(3) 0.0812(17) Uani 1 1 d . . .
C33 C 0.5785(3) -0.1314(3) 0.9539(3) 0.0747(15) Uani 1 1 d . . .
C34 C 0.5689(4) -0.1358(4) 1.0084(3) 0.0839(17) Uani 1 1 d . . .
H34 H 0.5436 -0.1800 1.0190 0.101 Uiso 1 1 calc R . .
C35 C 0.5961(4) -0.0763(4) 1.0462(3) 0.0867(18) Uani 1 1 d . . .
H35 H 0.5885 -0.0782 1.0829 0.104 Uiso 1 1 calc R . .
C36 C 0.6344(4) -0.0141(4) 1.0313(3) 0.0814(16) Uani 1 1 d . . .
H36 H 0.6535 0.0278 1.0573 0.098 Uiso 1 1 calc R . .
C37 C 0.6451(3) -0.0126(4) 0.9789(3) 0.0778(16) Uani 1 1 d . . .
H37 H 0.6741 0.0300 0.9696 0.093 Uiso 1 1 calc R . .
O41 O 0.3698(3) -0.0379(3) 0.60755(19) 0.0904(12) Uani 1 1 d . . .
N41 N 0.3251(3) -0.0279(3) 0.6450(2) 0.0803(14) Uani 1 1 d . . .
N42 N 0.2440(3) -0.0167(3) 0.7184(2) 0.0791(13) Uani 1 1 d . . .
C41 C 0.2173(5) 0.0183(7) 0.5622(4) 0.137(3) Uani 1 1 d . . .
H41A H 0.2567 0.0089 0.5416 0.164 Uiso 1 1 calc R . .
H41B H 0.2021 0.0737 0.5592 0.164 Uiso 1 1 calc R . .
H41C H 0.1691 -0.0138 0.5456 0.164 Uiso 1 1 calc R . .
C42 C 0.2534(4) -0.0025(4) 0.6226(3) 0.0935(19) Uani 1 1 d . . .
C43 C 0.2071(4) 0.0088(4) 0.6651(4) 0.0928(19) Uani 1 1 d . . .
C44 C 0.1318(4) 0.0450(5) 0.6495(4) 0.109(2) Uani 1 1 d . . .
H44 H 0.1076 0.0637 0.6117 0.131 Uiso 1 1 calc R . .
C45 C 0.0927(5) 0.0530(5) 0.6915(4) 0.112(3) Uani 1 1 d . . .
H45 H 0.0403 0.0757 0.6819 0.135 Uiso 1 1 calc R . .
C46 C 0.1288(4) 0.0288(4) 0.7446(4) 0.100(2) Uani 1 1 d . . .
H46 H 0.1038 0.0358 0.7737 0.120 Uiso 1 1 calc R . .
C47 C 0.2056(4) -0.0078(4) 0.7567(4) 0.0912(19) Uani 1 1 d . . .
H47 H 0.2306 -0.0268 0.7943 0.109 Uiso 1 1 calc R . .
O51 O 0.3928(3) -0.0731(3) 0.8606(2) 0.0891(13) Uani 1 1 d . . .
N51 N 0.3626(3) -0.1116(3) 0.8086(3) 0.0828(15) Uani 1 1 d . . .
N52 N 0.3031(3) -0.1763(3) 0.7098(3) 0.0920(16) Uani 1 1 d . . .
C51 C 0.2987(6) -0.2000(5) 0.8608(5) 0.134(3) Uani 1 1 d . . .
H51A H 0.3258 -0.1667 0.8935 0.161 Uiso 1 1 calc R . .
H51B H 0.3171 -0.2541 0.8692 0.161 Uiso 1 1 calc R . .
H51C H 0.2400 -0.1975 0.8539 0.161 Uiso 1 1 calc R . .
C52 C 0.3186(4) -0.1721(4) 0.8088(4) 0.095(2) Uani 1 1 d . . .
C53 C 0.2888(4) -0.2122(4) 0.7552(4) 0.097(2) Uani 1 1 d . . .
C54 C 0.2497(5) -0.2848(5) 0.7468(6) 0.129(4) Uani 1 1 d . . .
H54 H 0.2396 -0.3094 0.7787 0.154 Uiso 1 1 calc R . .
C55 C 0.2254(6) -0.3216(7) 0.6956(8) 0.153(5) Uani 1 1 d . . .
H55 H 0.1974 -0.3701 0.6906 0.184 Uiso 1 1 calc R . .
C56 C 0.2428(6) -0.2861(6) 0.6527(7) 0.165(5) Uani 1 1 d . . .
H56 H 0.2295 -0.3107 0.6163 0.198 Uiso 1 1 calc R . .
C57 C 0.2821(5) -0.2099(5) 0.6607(5) 0.123(3) Uani 1 1 d . . .
H57 H 0.2923 -0.1847 0.6291 0.148 Uiso 1 1 calc R . .
P61 P 0.48164(8) 0.06726(7) 0.79962(6) 0.0599(4) Uani 1 1 d . . .
O61 O 0.54413(19) 0.10041(19) 0.77375(15) 0.0618(9) Uani 1 1 d . . .
O62 O 0.5140(2) -0.0010(2) 0.83987(16) 0.0667(9) Uani 1 1 d . . .
O63 O 0.4028(2) 0.0445(2) 0.75316(16) 0.0664(9) Uani 1 1 d . . .
F61 F 0.4579(2) 0.1329(2) 0.83642(16) 0.0928(10) Uani 1 1 d . . .
P62 P 0.53837(9) -0.09197(8) 0.71593(7) 0.0680(4) Uani 1 1 d . . .
O71 O 0.5178(2) -0.0210(2) 0.67753(16) 0.0696(9) Uani 1 1 d . . .
O72 O 0.6111(2) -0.0768(2) 0.76881(16) 0.0661(9) Uani 1 1 d . . .
O73 O 0.4645(2) -0.1222(2) 0.73094(17) 0.0729(10) Uani 1 1 d . . .
F71 F 0.5640(3) -0.1592(2) 0.68101(19) 0.1045(12) Uani 1 1 d . . .
P1 P 0.37754(12) 0.44237(14) 0.58910(11) 0.1078(7) Uani 1 1 d . . .
F1 F 0.3001(3) 0.3962(3) 0.5521(2) 0.1426(18) Uani 1 1 d . . .
F2 F 0.3225(3) 0.4948(4) 0.6143(2) 0.1452(19) Uani 1 1 d . . .
F3 F 0.3675(5) 0.5036(4) 0.5390(3) 0.177(3) Uani 1 1 d . . .
F4 F 0.3865(3) 0.3801(4) 0.6393(3) 0.157(2) Uani 1 1 d . . .
F5 F 0.4323(3) 0.3879(4) 0.5648(3) 0.173(2) Uani 1 1 d . . .
F6 F 0.4547(3) 0.4879(3) 0.6271(3) 0.1450(18) Uani 1 1 d . . .
P11 P 0.85148(13) 0.03649(17) 0.60843(11) 0.1171(8) Uani 1 1 d . . .
F11 F 0.8979(4) 0.1057(6) 0.6471(3) 0.200(4) Uani 1 1 d . . .
F12 F 0.8010(5) 0.0938(5) 0.5621(5) 0.256(5) Uani 1 1 d . . .
F13 F 0.8026(6) -0.0297(5) 0.5681(3) 0.227(4) Uani 1 1 d . . .
F14 F 0.7873(3) 0.0259(8) 0.6401(3) 0.261(6) Uani 1 1 d . . .
F15 F 0.9009(6) -0.0137(8) 0.6542(5) 0.279(5) Uani 1 1 d . . .
F16 F 0.9161(4) 0.0433(4) 0.5763(3) 0.178(3) Uani 1 1 d . . .
O1W O 0.4550 0.7037 0.0481 0.089 Uiso 0.20 1 d P . .
O2W O 0.3619 0.7906 0.0377 0.086 Uiso 0.35 1 d P . .
O3W O 0.4650 0.7347 0.1202 0.090 Uiso 0.35 1 d P . .
O4W O 0.5523 0.7138 0.1583 0.092 Uiso 0.10 1 d P . .
O5W O 0.9780 0.7873 0.1462 0.112 Uiso 0.20 1 d P . .
O6W O 0.9563 0.8224 0.0994 0.105 Uiso 0.10 1 d P . .
O7W O 0.8362 0.7725 0.0539 0.080 Uiso 0.10 1 d P . .
O8W O 0.7017 0.6948 0.0186 0.067 Uiso 0.10 1 d P . .
O1M O 0.5580 0.6690 0.2033 0.088 Uiso 0.40 1 d P . .
C1M C 0.4968 0.7206 0.1629 0.121 Uiso 0.40 1 d P . .
O2M O 0.5621 0.6580 0.0582 0.118 Uiso 0.30 1 d P . .
C2M C 0.5100 0.6076 0.0354 0.058 Uiso 0.30 1 d P . .
O3M O 0.1849 0.6309 0.1292 0.084 Uiso 0.40 1 d PD . .
C3M C 0.2286 0.6965 0.1213 0.127 Uiso 0.40 1 d PD . .
O4M O 0.1630 0.6984 0.1180 0.068 Uiso 0.10 1 d PD . .
C4M C 0.1999 0.6382 0.1559 0.053 Uiso 0.10 1 d PD . .
O5M O 0.3804 0.7372 0.0814 0.084 Uiso 0.15 1 d P . .
C5M C 0.3729 0.7126 0.0240 0.039 Uiso 0.15 1 d P . .
H1O H 0.3837 0.1070 0.7036 0.050 Uiso 1 1 d . . .
H11O H 0.6790 -0.0322 0.7508 0.050 Uiso 1 1 d . . .
H21O H 0.6361 0.0991 0.8318 0.050 Uiso 1 1 d . . .
H31O H 0.5295 -0.2111 0.7869 0.050 Uiso 1 1 d . . .
H41O H 0.4224 -0.0364 0.6304 0.050 Uiso 1 1 d . . .
H51O H 0.4263 -0.0400 0.8432 0.050 Uiso 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
Ni1 O71 2.068(4) . ?
Ni1 N11 2.070(4) . ?
Ni1 O61 2.076(3) . ?
Ni1 N2 2.095(5) . ?
Ni1 N12 2.095(4) . ?
Ni1 N1 2.098(5) . ?
Ni2 O62 2.057(3) . ?
Ni2 O72 2.070(4) . ?
Ni2 N32 2.085(5) . ?
Ni2 N22 2.087(5) . ?
Ni2 N31 2.089(5) . ?
Ni2 N21 2.089(5) . ?
Ni3 O73 2.065(4) . ?
Ni3 O63 2.076(4) . ?
Ni3 N51 2.077(6) . ?
Ni3 N41 2.077(6) . ?
Ni3 N52 2.088(5) . ?
Ni3 N42 2.096(5) . ?
O1 N1 1.406(5) . ?
O1 H1O 1.0365 . ?
N1 C2 1.264(7) . ?
N2 C3 1.331(7) . ?
N2 C7 1.347(7) . ?
C1 C2 1.505(8) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.481(7) . ?
C3 C4 1.394(8) . ?
C4 C5 1.395(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.388(10) . ?
C5 H5 0.9500 . ?
C6 C7 1.368(9) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
O11 N11 1.390(5) . ?
O11 H11O 1.0482 . ?
N11 C12 1.311(7) . ?
N12 C17 1.328(7) . ?
N12 C13 1.368(7) . ?
C11 C12 1.486(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C13 1.452(8) . ?
C13 C14 1.369(8) . ?
C14 C15 1.406(9) . ?
C14 H14 0.9500 . ?
C15 C16 1.376(10) . ?
C15 H15 0.9500 . ?
C16 C17 1.393(8) . ?
C16 H16 0.9500 . ?
C17 H17 0.9500 . ?
O21 N21 1.394(6) . ?
O21 H21O 0.8768 . ?
N21 C22 1.272(7) . ?
N22 C27 1.327(8) . ?
N22 C23 1.365(8) . ?
C21 C22 1.498(9) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.459(9) . ?
C23 C24 1.393(9) . ?
C24 C25 1.345(13) . ?
C24 H24 0.9500 . ?
C25 C26 1.358(13) . ?
C25 H25 0.9500 . ?
C26 C27 1.381(11) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
O31 N31 1.382(6) . ?
O31 H31O 0.8233 . ?
N31 C32 1.290(8) . ?
N32 C33 1.358(7) . ?
N32 C37 1.362(8) . ?
C31 C32 1.488(9) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.485(9) . ?
C33 C34 1.403(8) . ?
C34 C35 1.361(9) . ?
C34 H34 0.9500 . ?
C35 C36 1.363(9) . ?
C35 H35 0.9500 . ?
C36 C37 1.355(8) . ?
C36 H36 0.9500 . ?
C37 H37 0.9500 . ?
O41 N41 1.381(6) . ?
O41 H41O 0.9150 . ?
N41 C42 1.273(9) . ?
N42 C47 1.316(8) . ?
N42 C43 1.344(9) . ?
C41 C42 1.467(11) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.511(10) . ?
C43 C44 1.390(10) . ?
C44 C45 1.401(11) . ?
C44 H44 0.9500 . ?
C45 C46 1.331(11) . ?
C45 H45 0.9500 . ?
C46 C47 1.420(9) . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
O51 N51 1.391(7) . ?
O51 H51O 0.9964 . ?
N51 C52 1.286(8) . ?
N52 C57 1.285(11) . ?
N52 C53 1.360(9) . ?
C51 C52 1.501(10) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.435(11) . ?
C53 C54 1.399(11) . ?
C54 C55 1.356(16) . ?
C54 H54 0.9500 . ?
C55 C56 1.328(17) . ?
C55 H55 0.9500 . ?
C56 C57 1.456(13) . ?
C56 H56 0.9500 . ?
C57 H57 0.9500 . ?
P61 O62 1.522(4) . ?
P61 O61 1.523(3) . ?
P61 O63 1.541(4) . ?
P61 F61 1.573(4) . ?
P62 O71 1.512(4) . ?
P62 O73 1.527(3) . ?
P62 O72 1.533(4) . ?
P62 F71 1.577(4) . ?
P1 F2 1.568(5) . ?
P1 F5 1.572(6) . ?
P1 F6 1.584(6) . ?
P1 F3 1.585(6) . ?
P1 F1 1.585(6) . ?
P1 F4 1.601(5) . ?
P11 F15 1.465(8) . ?
P11 F14 1.550(7) . ?
P11 F12 1.555(8) . ?
P11 F16 1.558(6) . ?
P11 F13 1.571(8) . ?
P11 F11 1.577(7) . ?
O1W C5M 1.3734 . ?
O1W O3W 1.8058 . ?
O1W O5M 1.8200 . ?
O2W O5M 1.3712 . ?
O2W C5M 1.4020 . ?
O3W C1M 1.0541 . ?
O3W O5M 1.4869 . ?
O3W O4W 1.5615 . ?
O4W C1M 1.0110 . ?
O4W O1M 1.3238 . ?
O5W O6W 1.2493 . ?
O1M C1M 1.5003 . ?
O2M C2M 1.2528 . ?
O3M C4M 0.6396 . ?
O3M O4M 1.2196 . ?
O3M C3M 1.4003 . ?
C3M O4M 1.1162 . ?
C3M C4M 1.4911 . ?
O4M C4M 1.4054 . ?
O5M C5M 1.4390 . ?

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
O71 Ni1 N11 97.93(16) . . ?
O71 Ni1 O61 95.79(14) . . ?
N11 Ni1 O61 87.71(15) . . ?
O71 Ni1 N2 86.10(16) . . ?
N11 Ni1 N2 96.74(17) . . ?
O61 Ni1 N2 174.90(15) . . ?
O71 Ni1 N12 173.95(14) . . ?
N11 Ni1 N12 77.08(17) . . ?
O61 Ni1 N12 87.50(15) . . ?
N2 Ni1 N12 91.05(17) . . ?
O71 Ni1 N1 91.80(16) . . ?
N11 Ni1 N1 167.34(18) . . ?
O61 Ni1 N1 99.39(16) . . ?
N2 Ni1 N1 75.78(17) . . ?
N12 Ni1 N1 92.67(17) . . ?
O62 Ni2 O72 95.60(14) . . ?
O62 Ni2 N32 84.80(16) . . ?
O72 Ni2 N32 175.89(16) . . ?
O62 Ni2 N22 171.17(18) . . ?
O72 Ni2 N22 92.04(16) . . ?
N32 Ni2 N22 87.89(17) . . ?
O62 Ni2 N31 89.88(16) . . ?
O72 Ni2 N31 98.66(17) . . ?
N32 Ni2 N31 77.24(19) . . ?
N22 Ni2 N31 93.3(2) . . ?
O62 Ni2 N21 98.86(16) . . ?
O72 Ni2 N21 88.96(16) . . ?
N32 Ni2 N21 95.02(18) . . ?
N22 Ni2 N21 76.84(19) . . ?
N31 Ni2 N21 167.8(2) . . ?
O73 Ni3 O63 99.12(14) . . ?
O73 Ni3 N51 91.78(17) . . ?
O63 Ni3 N51 99.5(2) . . ?
O73 Ni3 N41 98.21(18) . . ?
O63 Ni3 N41 87.45(17) . . ?
N51 Ni3 N41 166.8(2) . . ?
O73 Ni3 N52 86.41(18) . . ?
O63 Ni3 N52 173.4(2) . . ?
N51 Ni3 N52 76.6(3) . . ?
N41 Ni3 N52 95.4(2) . . ?
O73 Ni3 N42 173.71(19) . . ?
O63 Ni3 N42 85.28(16) . . ?
N51 Ni3 N42 91.9(2) . . ?
N41 Ni3 N42 77.4(2) . . ?
N52 Ni3 N42 89.5(2) . . ?
N1 O1 H1O 99.2 . . ?
C2 N1 O1 115.5(4) . . ?
C2 N1 Ni1 118.1(3) . . ?
O1 N1 Ni1 124.8(4) . . ?
C3 N2 C7 118.7(5) . . ?
C3 N2 Ni1 114.3(3) . . ?
C7 N2 Ni1 126.9(4) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 113.0(5) . . ?
N1 C2 C1 125.3(5) . . ?
C3 C2 C1 121.6(5) . . ?
N2 C3 C4 121.7(5) . . ?
N2 C3 C2 116.5(5) . . ?
C4 C3 C2 121.6(6) . . ?
C3 C4 C5 119.2(6) . . ?
C3 C4 H4 120.4 . . ?
C5 C4 H4 120.4 . . ?
C6 C5 C4 118.3(6) . . ?
C6 C5 H5 120.9 . . ?
C4 C5 H5 120.9 . . ?
C7 C6 C5 119.0(6) . . ?
C7 C6 H6 120.5 . . ?
C5 C6 H6 120.5 . . ?
N2 C7 C6 123.0(6) . . ?
N2 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
N11 O11 H11O 111.5 . . ?
C12 N11 O11 115.7(4) . . ?
C12 N11 Ni1 118.3(4) . . ?
O11 N11 Ni1 125.8(3) . . ?
C17 N12 C13 119.3(5) . . ?
C17 N12 Ni1 126.8(4) . . ?
C13 N12 Ni1 113.9(3) . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N11 C12 C13 113.9(4) . . ?
N11 C12 C11 123.8(5) . . ?
C13 C12 C11 122.2(5) . . ?
N12 C13 C14 120.6(5) . . ?
N12 C13 C12 116.5(5) . . ?
C14 C13 C12 122.9(5) . . ?
C13 C14 C15 120.1(5) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C16 C15 C14 118.7(6) . . ?
C16 C15 H15 120.7 . . ?
C14 C15 H15 120.7 . . ?
C15 C16 C17 118.4(6) . . ?
C15 C16 H16 120.8 . . ?
C17 C16 H16 120.8 . . ?
N12 C17 C16 122.9(6) . . ?
N12 C17 H17 118.6 . . ?
C16 C17 H17 118.6 . . ?
N21 O21 H21O 102.8 . . ?
C22 N21 O21 115.4(5) . . ?
C22 N21 Ni2 118.0(4) . . ?
O21 N21 Ni2 126.4(3) . . ?
C27 N22 C23 119.6(6) . . ?
C27 N22 Ni2 126.6(5) . . ?
C23 N22 Ni2 113.2(4) . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C22 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N21 C22 C23 114.5(5) . . ?
N21 C22 C21 123.8(6) . . ?
C23 C22 C21 121.7(6) . . ?
N22 C23 C24 119.9(7) . . ?
N22 C23 C22 116.4(5) . . ?
C24 C23 C22 123.6(7) . . ?
C25 C24 C23 119.5(9) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.3(8) . . ?
C24 C25 H25 119.8 . . ?
C26 C25 H25 119.8 . . ?
C25 C26 C27 119.4(8) . . ?
C25 C26 H26 120.3 . . ?
C27 C26 H26 120.3 . . ?
N22 C27 C26 121.3(8) . . ?
N22 C27 H27 119.4 . . ?
C26 C27 H27 119.4 . . ?
N31 O31 H31O 110.0 . . ?
C32 N31 O31 114.6(5) . . ?
C32 N31 Ni2 117.6(4) . . ?
O31 N31 Ni2 127.0(3) . . ?
C33 N32 C37 117.6(5) . . ?
C33 N32 Ni2 114.5(4) . . ?
C37 N32 Ni2 127.7(4) . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N31 C32 C33 114.2(5) . . ?
N31 C32 C31 124.5(6) . . ?
C33 C32 C31 121.3(6) . . ?
N32 C33 C34 120.5(6) . . ?
N32 C33 C32 115.6(5) . . ?
C34 C33 C32 123.8(6) . . ?
C35 C34 C33 119.6(6) . . ?
C35 C34 H34 120.2 . . ?
C33 C34 H34 120.2 . . ?
C34 C35 C36 119.8(6) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C37 C36 C35 119.3(7) . . ?
C37 C36 H36 120.4 . . ?
C35 C36 H36 120.4 . . ?
C36 C37 N32 123.0(6) . . ?
C36 C37 H37 118.5 . . ?
N32 C37 H37 118.5 . . ?
N41 O41 H41O 104.2 . . ?
C42 N41 O41 115.2(6) . . ?
C42 N41 Ni3 118.4(5) . . ?
O41 N41 Ni3 125.6(4) . . ?
C47 N42 C43 117.7(6) . . ?
C47 N42 Ni3 128.4(5) . . ?
C43 N42 Ni3 114.0(4) . . ?
C42 C41 H41A 109.5 . . ?
C42 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C42 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
N41 C42 C41 125.5(7) . . ?
N41 C42 C43 113.6(7) . . ?
C41 C42 C43 120.9(7) . . ?
N42 C43 C44 122.8(7) . . ?
N42 C43 C42 115.8(6) . . ?
C44 C43 C42 121.3(8) . . ?
C43 C44 C45 117.7(8) . . ?
C43 C44 H44 121.1 . . ?
C45 C44 H44 121.1 . . ?
C46 C45 C44 120.1(7) . . ?
C46 C45 H45 119.9 . . ?
C44 C45 H45 119.9 . . ?
C45 C46 C47 118.4(8) . . ?
C45 C46 H46 120.8 . . ?
C47 C46 H46 120.8 . . ?
N42 C47 C46 123.2(8) . . ?
N42 C47 H47 118.4 . . ?
C46 C47 H47 118.4 . . ?
N51 O51 H51O 88.9 . . ?
C52 N51 O51 115.8(6) . . ?
C52 N51 Ni3 116.5(6) . . ?
O51 N51 Ni3 125.9(3) . . ?
C57 N52 C53 119.8(7) . . ?
C57 N52 Ni3 126.4(6) . . ?
C53 N52 Ni3 113.8(5) . . ?
C52 C51 H51A 109.5 . . ?
C52 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C52 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N51 C52 C53 115.5(6) . . ?
N51 C52 C51 123.3(8) . . ?
C53 C52 C51 121.1(7) . . ?
N52 C53 C54 118.8(9) . . ?
N52 C53 C52 115.5(6) . . ?
C54 C53 C52 125.6(9) . . ?
C55 C54 C53 123.2(10) . . ?
C55 C54 H54 118.4 . . ?
C53 C54 H54 118.4 . . ?
C56 C55 C54 116.3(10) . . ?
C56 C55 H55 121.9 . . ?
C54 C55 H55 121.9 . . ?
C55 C56 C57 120.8(12) . . ?
C55 C56 H56 119.6 . . ?
C57 C56 H56 119.6 . . ?
N52 C57 C56 121.0(11) . . ?
N52 C57 H57 119.5 . . ?
C56 C57 H57 119.5 . . ?
O62 P61 O61 112.81(19) . . ?
O62 P61 O63 110.9(2) . . ?
O61 P61 O63 111.6(2) . . ?
O62 P61 F61 106.5(2) . . ?
O61 P61 F61 108.5(2) . . ?
O63 P61 F61 106.1(2) . . ?
P61 O61 Ni1 130.3(2) . . ?
P61 O62 Ni2 132.23(19) . . ?
P61 O63 Ni3 127.9(2) . . ?
O71 P62 O73 111.4(2) . . ?
O71 P62 O72 111.7(2) . . ?
O73 P62 O72 112.8(2) . . ?
O71 P62 F71 107.3(2) . . ?
O73 P62 F71 106.3(2) . . ?
O72 P62 F71 106.8(2) . . ?
P62 O71 Ni1 132.5(2) . . ?
P62 O72 Ni2 129.5(2) . . ?
P62 O73 Ni3 130.6(2) . . ?
F2 P1 F5 178.4(4) . . ?
F2 P1 F6 89.6(4) . . ?
F5 P1 F6 90.9(4) . . ?
F2 P1 F3 89.6(4) . . ?
F5 P1 F3 91.9(4) . . ?
F6 P1 F3 90.4(4) . . ?
F2 P1 F1 90.0(3) . . ?
F5 P1 F1 89.5(3) . . ?
F6 P1 F1 179.0(3) . . ?
F3 P1 F1 90.5(4) . . ?
F2 P1 F4 90.2(4) . . ?
F5 P1 F4 88.2(4) . . ?
F6 P1 F4 90.4(3) . . ?
F3 P1 F4 179.2(4) . . ?
F1 P1 F4 88.7(3) . . ?
F15 P11 F14 83.6(6) . . ?
F15 P11 F12 176.7(7) . . ?
F14 P11 F12 96.3(6) . . ?
F15 P11 F16 95.1(5) . . ?
F14 P11 F16 177.6(6) . . ?
F12 P11 F16 85.1(6) . . ?
F15 P11 F13 98.0(7) . . ?
F14 P11 F13 84.3(5) . . ?
F12 P11 F13 85.2(5) . . ?
F16 P11 F13 93.9(4) . . ?
F15 P11 F11 84.5(6) . . ?
F14 P11 F11 95.7(4) . . ?
F12 P11 F11 92.2(5) . . ?
F16 P11 F11 86.2(4) . . ?
F13 P11 F11 177.4(6) . . ?
C5M O1W O3W 99.7 . . ?
C5M O1W O5M 51.3 . . ?
O3W O1W O5M 48.4 . . ?
O5M O2W C5M 62.5 . . ?
C1M O3W O5M 139.5 . . ?
C1M O3W O4W 39.8 . . ?
O5M O3W O4W 168.3 . . ?
C1M O3W O1W 140.7 . . ?
O5M O3W O1W 66.3 . . ?
O4W O3W O1W 107.9 . . ?
C1M O4W O1M 78.7 . . ?
C1M O4W O3W 41.9 . . ?
O1M O4W O3W 116.4 . . ?
O4W O1M C1M 41.4 . . ?
O4W C1M O3W 98.2 . . ?
O4W C1M O1M 59.9 . . ?
O3W C1M O1M 147.5 . . ?
C4M O3M O4M 92.9 . . ?
C4M O3M C3M 85.3 . . ?
O4M O3M C3M 49.8 . . ?
O4M C3M O3M 56.6 . . ?
O4M C3M C4M 63.3 . . ?
O3M C3M C4M 25.3 . . ?
C3M O4M O3M 73.5 . . ?
C3M O4M C4M 71.5 . . ?
O3M O4M C4M 27.0 . . ?
O3M C4M O4M 60.1 . . ?
O3M C4M C3M 69.4 . . ?
O4M C4M C3M 45.2 . . ?
O2W O5M C5M 59.8 . . ?
O2W O5M O3W 118.2 . . ?
C5M O5M O3W 113.4 . . ?
O2W O5M O1W 83.5 . . ?
C5M O5M O1W 48.1 . . ?
O3W O5M O1W 65.3 . . ?
O1W C5M O2W 101.6 . . ?
O1W C5M O5M 80.6 . . ?
O2W C5M O5M 57.7 . . ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        61.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.095

# start Validation Reply Form
_vrf_PLAT222_comp1               
;
PROBLEM: Large Non-Solvent    H    Uiso(max)/Uiso(min) ..       10.0 Ratio 
RESPONSE: The crystals showed poor diffraction ability and data were collected
only to establish the structure of the complex. Full data to 2theta=143 deg were
collected but only those to 2theta=122 deg were used for the refinement because
of the large number of unorbserved data at higher theta values. The hydrogen atoms
were introduced at calculated positions as riding on bonded atoms with U depending
on the U(eq) of the parent atom. Therefore, large thermal motion for the carbon
atoms results in large thermal coefficients for the hydrogen atoms.

;
# end Validation Reply Form
_database_code_depnum_ccdc_archive 'CCDC 1015273'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
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#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_comp2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H24 F6 N7 Ni O6 P'
_chemical_formula_weight         674.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   13.4305(2)
_cell_length_b                   13.7894(2)
_cell_length_c                   15.9761(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 112.968(1)
_cell_angle_gamma                90.00
_cell_volume                     2724.19(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    183(2)
_cell_measurement_reflns_used    28629
_cell_measurement_theta_min      6.52
_cell_measurement_theta_max      71.83

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.52
_exptl_crystal_size_min          0.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    2.433
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.768
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      183(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27818
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_sigmaI/netI    0.0132
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         6.52
_diffrn_reflns_theta_max         64.99
_reflns_number_total             4606
_reflns_number_gt                4368
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_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)+(0.0667P)²+4.3761P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4606
_refine_ls_number_parameters     464
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0493
_refine_ls_wR_factor_ref         0.1315
_refine_ls_wR_factor_gt          0.1296
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_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
Ni Ni 0.25064(3) 0.19945(3) 0.32852(3) 0.02373(16) Uani 1 1 d . . .
O1 O 0.2873(2) 0.28247(18) 0.16232(14) 0.0377(5) Uani 1 1 d . . .
N1 N 0.32868(19) 0.26988(17) 0.25567(15) 0.0283(5) Uani 1 1 d . . .
N2 N 0.38117(18) 0.26688(17) 0.43006(15) 0.0266(5) Uani 1 1 d . . .
C1 C 0.4472(3) 0.4050(3) 0.2550(2) 0.0557(10) Uani 1 1 d . . .
H1A H 0.5239 0.3917 0.2698 0.084 Uiso 1 1 calc R . .
H1B H 0.4396 0.4695 0.2775 0.084 Uiso 1 1 calc R . .
H1C H 0.4074 0.4027 0.1890 0.084 Uiso 1 1 calc R . .
C2 C 0.4028(2) 0.3306(2) 0.2989(2) 0.0331(6) Uani 1 1 d . . .
C3 C 0.4425(2) 0.3220(2) 0.3991(2) 0.0311(6) Uani 1 1 d . . .
C4 C 0.5354(3) 0.3676(3) 0.4573(2) 0.0424(8) Uani 1 1 d . . .
C5 C 0.5671(3) 0.3552(3) 0.5499(2) 0.0451(8) Uani 1 1 d . . .
C6 C 0.5060(3) 0.2987(2) 0.5819(2) 0.0381(7) Uani 1 1 d . . .
C7 C 0.4133(2) 0.2554(2) 0.52023(19) 0.0305(6) Uani 1 1 d . . .
O11 O 0.40997(19) 0.03653(18) 0.32458(16) 0.0413(6) Uani 1 1 d . . .
N11 N 0.33371(19) 0.06820(17) 0.35731(15) 0.0293(5) Uani 1 1 d . . .
N12 N 0.19343(18) 0.13342(17) 0.41733(15) 0.0270(5) Uani 1 1 d . . .
C11 C 0.3841(3) -0.0788(3) 0.4520(3) 0.0454(8) Uani 1 1 d . . .
C12 C 0.3244(2) 0.0143(2) 0.41910(18) 0.0302(6) Uani 1 1 d . . .
C13 C 0.2451(2) 0.0498(2) 0.45474(18) 0.0281(6) Uani 1 1 d . . .
C14 C 0.2217(3) 0.0010(2) 0.5206(2) 0.0365(7) Uani 1 1 d . . .
C15 C 0.1417(3) 0.0373(3) 0.5465(2) 0.0415(8) Uani 1 1 d . . .
C16 C 0.0873(3) 0.1200(3) 0.5063(2) 0.0399(7) Uani 1 1 d . . .
C17 C 0.1163(2) 0.1668(2) 0.4420(2) 0.0320(6) Uani 1 1 d . . .
O21 O 0.1587(2) 0.40898(16) 0.33048(16) 0.0446(6) Uani 1 1 d . . .
N21 N 0.14247(19) 0.31598(18) 0.29529(16) 0.0296(5) Uani 1 1 d . . .
N22 N 0.12187(19) 0.14703(18) 0.21701(15) 0.0296(5) Uani 1 1 d . . .
C21` C -0.0266(3) 0.3858(3) 0.1876(2) 0.0471(9) Uani 1 1 d . . .
C22 C 0.0542(2) 0.3059(2) 0.22502(19) 0.0332(7) Uani 1 1 d . . .
C23 C 0.0376(2) 0.2089(2) 0.18353(19) 0.0335(7) Uani 1 1 d . . .
C24 C -0.0587(3) 0.1817(3) 0.1140(2) 0.0496(9) Uani 1 1 d . . .
C25 C -0.0683(3) 0.0902(3) 0.0787(3) 0.0577(11) Uani 1 1 d . . .
C26 C 0.0171(3) 0.0267(3) 0.1123(2) 0.0494(9) Uani 1 1 d . . .
C27 C 0.1114(3) 0.0574(2) 0.1819(2) 0.0356(7) Uani 1 1 d . . .
N31 N 0.2856(2) 0.41935(18) 0.56321(16) 0.0333(6) Uani 1 1 d . . .
O31 O 0.29895(18) 0.45807(16) 0.49770(14) 0.0402(5) Uani 1 1 d . . .
O32 O 0.20675(18) 0.36338(17) 0.54866(15) 0.0431(5) Uani 1 1 d . . .
O33 O 0.3520(2) 0.43455(19) 0.64192(15) 0.0509(6) Uani 1 1 d . . .
P P -0.22281(9) 0.25138(8) 0.32825(7) 0.0576(3) Uani 1 1 d . . .
F1 F -0.1890(7) 0.1551(4) 0.3016(4) 0.227(4) Uani 1 1 d . . .
F2 F -0.2568(3) 0.2882(4) 0.2289(2) 0.153(2) Uani 1 1 d . . .
F3 F -0.1078(3) 0.2989(3) 0.3513(3) 0.1187(13) Uani 1 1 d . . .
F4 F -0.1832(4) 0.2118(2) 0.42714(19) 0.1280(16) Uani 1 1 d . . .
F5 F -0.3347(4) 0.2075(5) 0.3057(3) 0.207(3) Uani 1 1 d . . .
F6 F -0.2496(4) 0.3518(3) 0.3621(4) 0.1500(17) Uani 1 1 d . . .
H1O H 0.258(4) 0.233(4) 0.139(3) 0.067(14) Uiso 1 1 d . . .
H11O H 0.396(3) 0.063(3) 0.280(3) 0.051(13) Uiso 1 1 d . . .
H21O H 0.198(5) 0.404(4) 0.383(4) 0.096(19) Uiso 1 1 d . . .
H4 H 0.574(3) 0.402(3) 0.435(3) 0.048(11) Uiso 1 1 d . . .
H5 H 0.629(3) 0.379(3) 0.591(3) 0.058(12) Uiso 1 1 d . . .
H6 H 0.525(3) 0.285(2) 0.643(3) 0.037(9) Uiso 1 1 d . . .
H7 H 0.371(3) 0.214(2) 0.540(2) 0.026(8) Uiso 1 1 d . . .
H14 H 0.258(3) -0.050(3) 0.548(2) 0.035(9) Uiso 1 1 d . . .
H15 H 0.123(3) 0.010(3) 0.589(3) 0.049(10) Uiso 1 1 d . . .
H16 H 0.030(3) 0.145(3) 0.521(2) 0.043(9) Uiso 1 1 d . . .
H17 H 0.079(3) 0.224(2) 0.418(2) 0.030(8) Uiso 1 1 d . . .
H11A H 0.332(4) -0.126(4) 0.438(3) 0.072(14) Uiso 1 1 d . . .
H11B H 0.425(4) -0.071(3) 0.514(3) 0.066(13) Uiso 1 1 d . . .
H11C H 0.432(4) -0.091(3) 0.424(3) 0.067(13) Uiso 1 1 d . . .
H24 H -0.115(3) 0.227(3) 0.093(3) 0.054(11) Uiso 1 1 d . . .
H25 H -0.137(4) 0.072(3) 0.031(3) 0.075(14) Uiso 1 1 d . . .
H26 H 0.014(3) -0.042(3) 0.089(3) 0.062(12) Uiso 1 1 d . . .
H27 H 0.165(3) 0.019(3) 0.202(2) 0.032(9) Uiso 1 1 d . . .
H21A H -0.055(4) 0.385(4) 0.128(4) 0.088(16) Uiso 1 1 d . . .
H21B H -0.084(4) 0.378(3) 0.206(3) 0.067(13) Uiso 1 1 d . . .
H21C H 0.011(3) 0.451(3) 0.205(3) 0.059(12) Uiso 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
Ni N22 2.069(2) . ?
Ni N12 2.070(2) . ?
Ni N11 2.081(2) . ?
Ni N1 2.085(2) . ?
Ni N2 2.086(2) . ?
Ni N21 2.091(2) . ?
O1 N1 1.384(3) . ?
O1 H1O 0.80(5) . ?
N1 C2 1.278(4) . ?
N2 C7 1.342(4) . ?
N2 C3 1.349(4) . ?
C1 C2 1.492(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.482(4) . ?
C3 C4 1.382(4) . ?
C4 C5 1.381(5) . ?
C4 H4 0.87(4) . ?
C5 C6 1.368(5) . ?
C5 H5 0.90(4) . ?
C6 C7 1.385(4) . ?
C6 H6 0.93(4) . ?
C7 H7 0.94(3) . ?
O11 N11 1.390(3) . ?
O11 H11O 0.75(4) . ?
N11 C12 1.280(4) . ?
N12 C17 1.326(4) . ?
N12 C13 1.359(4) . ?
C11 C12 1.496(4) . ?
C11 H11A 0.92(5) . ?
C11 H11B 0.93(5) . ?
C11 H11C 0.94(5) . ?
C12 C13 1.474(4) . ?
C13 C14 1.384(4) . ?
C14 C15 1.387(5) . ?
C14 H14 0.87(4) . ?
C15 C16 1.371(5) . ?
C15 H15 0.89(4) . ?
C16 C17 1.390(4) . ?
C16 H16 0.95(4) . ?
C17 H17 0.94(3) . ?
O21 N21 1.383(3) . ?
O21 H21O 0.80(6) . ?
N21 C22 1.283(4) . ?
N22 C27 1.342(4) . ?
N22 C23 1.350(4) . ?
C21` C22 1.498(4) . ?
C21` H21A 0.88(6) . ?
C21` H21B 0.93(5) . ?
C21` H21C 1.01(5) . ?
C22 C23 1.470(5) . ?
C23 C24 1.387(5) . ?
C24 C25 1.368(6) . ?
C24 H24 0.94(4) . ?
C25 C26 1.374(6) . ?
C25 H25 0.98(5) . ?
C26 C27 1.386(5) . ?
C26 H26 1.01(4) . ?
C27 H27 0.85(3) . ?
N31 O33 1.243(3) . ?
N31 O31 1.249(3) . ?
N31 O32 1.257(3) . ?
P F1 1.517(5) . ?
P F5 1.528(4) . ?
P F2 1.556(3) . ?
P F4 1.556(3) . ?
P F6 1.578(4) . ?
P F3 1.583(3) . ?

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
N22 Ni N12 91.57(9) . . ?
N22 Ni N11 94.72(10) . . ?
N12 Ni N11 77.07(9) . . ?
N22 Ni N1 96.63(9) . . ?
N12 Ni N1 171.67(9) . . ?
N11 Ni N1 100.69(9) . . ?
N22 Ni N2 172.63(9) . . ?
N12 Ni N2 95.00(9) . . ?
N11 Ni N2 90.02(9) . . ?
N1 Ni N2 76.91(9) . . ?
N22 Ni N21 77.61(10) . . ?
N12 Ni N21 96.03(9) . . ?
N11 Ni N21 169.66(10) . . ?
N1 Ni N21 87.20(9) . . ?
N2 Ni N21 98.32(9) . . ?
N1 O1 H1O 108(3) . . ?
C2 N1 O1 113.6(2) . . ?
C2 N1 Ni 117.34(19) . . ?
O1 N1 Ni 125.56(18) . . ?
C7 N2 C3 118.2(3) . . ?
C7 N2 Ni 127.1(2) . . ?
C3 N2 Ni 114.49(18) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 114.1(3) . . ?
N1 C2 C1 124.6(3) . . ?
C3 C2 C1 121.4(3) . . ?
N2 C3 C4 122.0(3) . . ?
N2 C3 C2 115.3(2) . . ?
C4 C3 C2 122.7(3) . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4 121(3) . . ?
C3 C4 H4 120(3) . . ?
C6 C5 C4 119.5(3) . . ?
C6 C5 H5 117(3) . . ?
C4 C5 H5 123(3) . . ?
C5 C6 C7 118.9(3) . . ?
C5 C6 H6 123(2) . . ?
C7 C6 H6 118(2) . . ?
N2 C7 C6 122.4(3) . . ?
N2 C7 H7 116.6(19) . . ?
C6 C7 H7 120.9(19) . . ?
N11 O11 H11O 105(3) . . ?
C12 N11 O11 114.5(2) . . ?
C12 N11 Ni 118.1(2) . . ?
O11 N11 Ni 126.90(18) . . ?
C17 N12 C13 119.2(2) . . ?
C17 N12 Ni 126.4(2) . . ?
C13 N12 Ni 114.38(18) . . ?
C12 C11 H11A 106(3) . . ?
C12 C11 H11B 107(3) . . ?
H11A C11 H11B 114(4) . . ?
C12 C11 H11C 111(3) . . ?
H11A C11 H11C 112(4) . . ?
H11B C11 H11C 108(4) . . ?
N11 C12 C13 114.1(2) . . ?
N11 C12 C11 124.7(3) . . ?
C13 C12 C11 121.2(3) . . ?
N12 C13 C14 121.2(3) . . ?
N12 C13 C12 115.7(2) . . ?
C14 C13 C12 123.0(3) . . ?
C13 C14 C15 118.9(3) . . ?
C13 C14 H14 121(2) . . ?
C15 C14 H14 120(2) . . ?
C16 C15 C14 119.6(3) . . ?
C16 C15 H15 117(2) . . ?
C14 C15 H15 124(2) . . ?
C15 C16 C17 118.7(3) . . ?
C15 C16 H16 121(2) . . ?
C17 C16 H16 120(2) . . ?
N12 C17 C16 122.3(3) . . ?
N12 C17 H17 122(2) . . ?
C16 C17 H17 116(2) . . ?
N21 O21 H21O 106(4) . . ?
C22 N21 O21 113.7(2) . . ?
C22 N21 Ni 116.9(2) . . ?
O21 N21 Ni 128.73(18) . . ?
C27 N22 C23 118.8(3) . . ?
C27 N22 Ni 126.7(2) . . ?
C23 N22 Ni 114.2(2) . . ?
C22 C21` H21A 112(3) . . ?
C22 C21` H21B 111(3) . . ?
H21A C21` H21B 106(4) . . ?
C22 C21` H21C 110(2) . . ?
H21A C21` H21C 105(4) . . ?
H21B C21` H21C 113(4) . . ?
N21 C22 C23 114.8(3) . . ?
N21 C22 C21` 123.2(3) . . ?
C23 C22 C21` 122.0(3) . . ?
N22 C23 C24 121.4(3) . . ?
N22 C23 C22 116.1(3) . . ?
C24 C23 C22 122.5(3) . . ?
C25 C24 C23 119.3(4) . . ?
C25 C24 H24 122(2) . . ?
C23 C24 H24 119(3) . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 H25 118(3) . . ?
C26 C25 H25 122(3) . . ?
C25 C26 C27 118.7(4) . . ?
C25 C26 H26 123(2) . . ?
C27 C26 H26 118(2) . . ?
N22 C27 C26 122.0(3) . . ?
N22 C27 H27 119(2) . . ?
C26 C27 H27 119(2) . . ?
O33 N31 O31 119.7(3) . . ?
O33 N31 O32 120.7(3) . . ?
O31 N31 O32 119.6(2) . . ?
F1 P F5 87.8(4) . . ?
F1 P F2 90.0(3) . . ?
F5 P F2 91.1(2) . . ?
F1 P F4 87.5(3) . . ?
F5 P F4 90.9(2) . . ?
F2 P F4 176.8(3) . . ?
F1 P F6 175.7(4) . . ?
F5 P F6 95.4(4) . . ?
F2 P F6 92.7(3) . . ?
F4 P F6 89.6(3) . . ?
F1 P F3 93.2(4) . . ?
F5 P F3 178.9(3) . . ?
F2 P F3 88.5(2) . . ?
F4 P F3 89.6(2) . . ?
F6 P F3 83.6(3) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        64.99
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.067
_database_code_depnum_ccdc_archive 'CCDC 1015274'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_comp3

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 F2 N8 Ni2 O12 P2'
_chemical_formula_weight         894.01

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

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

_cell_length_a                   10.3339(1)
_cell_length_b                   12.9700(1)
_cell_length_c                   13.7335(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.312(1)
_cell_angle_gamma                90.00
_cell_volume                     1783.58(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    160(2)
_cell_measurement_reflns_used    23287
_cell_measurement_theta_min      6.65
_cell_measurement_theta_max      72.03

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            'light blue'
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.665
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             920
_exptl_absorpt_coefficient_mu    2.899
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.805
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      160(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            25502
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0252
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         6.65
_diffrn_reflns_theta_max         64.99
_reflns_number_total             2914
_reflns_number_gt                2690
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_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)+(0.0472P)²+1.5911P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2914
_refine_ls_number_parameters     293
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0350
_refine_ls_wR_factor_ref         0.0901
_refine_ls_wR_factor_gt          0.0880
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.045
_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
Ni Ni 0.44671(4) 0.07873(3) 0.31888(3) 0.01991(14) Uani 1 1 d . . .
O1 O 0.16089(19) 0.11510(15) 0.34837(15) 0.0335(4) Uani 1 1 d . . .
N1 N 0.2401(2) 0.06910(14) 0.29344(15) 0.0246(5) Uani 1 1 d . . .
N2 N 0.3927(2) -0.00622(14) 0.18574(14) 0.0247(5) Uani 1 1 d . . .
C1 C 0.0264(3) 0.0138(2) 0.1827(2) 0.0405(7) Uani 1 1 d . . .
H1A H 0.0004 -0.0570 0.1617 0.061 Uiso 1 1 calc R . .
H1B H -0.0077 0.0609 0.1265 0.061 Uiso 1 1 calc R . .
H1C H -0.0110 0.0326 0.2392 0.061 Uiso 1 1 calc R . .
C2 C 0.1753(3) 0.02118(18) 0.21437(18) 0.0278(6) Uani 1 1 d . . .
C3 C 0.2611(3) -0.02775(17) 0.15563(17) 0.0267(6) Uani 1 1 d . . .
C4 C 0.2109(3) -0.0934(2) 0.0754(2) 0.0373(7) Uani 1 1 d . . .
C5 C 0.2982(3) -0.1367(2) 0.0255(2) 0.0434(8) Uani 1 1 d . . .
C6 C 0.4320(3) -0.1141(2) 0.0554(2) 0.0376(7) Uani 1 1 d . . .
C7 C 0.4760(3) -0.04865(19) 0.13702(19) 0.0309(6) Uani 1 1 d . . .
O2 O 0.75707(17) 0.04308(14) 0.37311(14) 0.0304(4) Uani 1 1 d . . .
N3 N 0.6480(2) 0.09745(14) 0.31907(14) 0.0214(4) Uani 1 1 d . . .
N4 N 0.4431(2) 0.21277(14) 0.23310(14) 0.0212(4) Uani 1 1 d . . .
C8 C 0.8177(3) 0.2139(2) 0.2834(2) 0.0386(7) Uani 1 1 d . . .
H8A H 0.8785 0.1790 0.3398 0.058 Uiso 1 1 calc R . .
H8B H 0.8228 0.2886 0.2946 0.058 Uiso 1 1 calc R . .
H8C H 0.8432 0.1977 0.2210 0.058 Uiso 1 1 calc R . .
C9 C 0.6787(2) 0.17814(17) 0.27547(17) 0.0235(5) Uani 1 1 d . . .
C10 C 0.5632(2) 0.23749(17) 0.21694(17) 0.0222(5) Uani 1 1 d . . .
C11 C 0.5762(3) 0.31361(18) 0.1492(2) 0.0294(6) Uani 1 1 d . . .
C12 C 0.4625(3) 0.3651(2) 0.0962(2) 0.0334(6) Uani 1 1 d . . .
C13 C 0.3412(3) 0.34227(19) 0.1149(2) 0.0311(6) Uani 1 1 d . . .
C14 C 0.3356(3) 0.26550(18) 0.18400(19) 0.0263(6) Uani 1 1 d . . .
F F 0.48310(16) 0.23696(10) 0.60861(10) 0.0357(4) Uani 1 1 d . . .
P P 0.45350(6) 0.13401(4) 0.54433(4) 0.02192(17) Uani 1 1 d . . .
O3 O 0.48378(17) 0.16568(11) 0.44685(11) 0.0243(4) Uani 1 1 d . . .
O4 O 0.45556(17) -0.05618(12) 0.39470(12) 0.0253(4) Uani 1 1 d . . .
O5 O 0.30599(17) 0.11397(13) 0.53413(13) 0.0296(4) Uani 1 1 d . . .
O1W O 0.6568(3) 0.33300(19) 0.45295(19) 0.0666(7) Uani 1 1 d D . .
H1WA H 0.597(4) 0.276(3) 0.453(3) 0.112(17) Uiso 1 1 d D . .
H1WB H 0.714(4) 0.329(4) 0.517(2) 0.139 Uiso 1 1 d D . .
H1O H 0.204(4) 0.113(3) 0.405(3) 0.054(11) Uiso 1 1 d . . .
H2O H 0.731(3) -0.006(3) 0.405(3) 0.051(10) Uiso 1 1 d . . .
H4 H 0.118(3) -0.114(2) 0.060(2) 0.044(9) Uiso 1 1 d . . .
H5 H 0.267(3) -0.180(2) -0.025(2) 0.048(9) Uiso 1 1 d . . .
H6 H 0.498(3) -0.138(2) 0.025(2) 0.033(8) Uiso 1 1 d . . .
H7 H 0.573(3) -0.032(2) 0.1607(19) 0.026(7) Uiso 1 1 d . . .
H11 H 0.660(3) 0.331(2) 0.141(2) 0.028(7) Uiso 1 1 d . . .
H12 H 0.468(3) 0.419(2) 0.048(2) 0.036(8) Uiso 1 1 d . . .
H13 H 0.262(3) 0.376(2) 0.084(2) 0.032(7) Uiso 1 1 d . . .
H14 H 0.255(3) 0.249(2) 0.197(2) 0.029(7) Uiso 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
Ni O4 2.0266(16) . ?
Ni O3 2.0431(16) . ?
Ni N1 2.080(2) . ?
Ni N2 2.0892(19) . ?
Ni N3 2.094(2) . ?
Ni N4 2.0951(19) . ?
O1 N1 1.379(3) . ?
O1 H1O 0.80(4) . ?
N1 C2 1.286(3) . ?
N2 C7 1.333(3) . ?
N2 C3 1.349(3) . ?
C1 C2 1.495(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.481(4) . ?
C3 C4 1.388(3) . ?
C4 C5 1.379(5) . ?
C4 H4 0.96(3) . ?
C5 C6 1.373(4) . ?
C5 H5 0.89(3) . ?
C6 C7 1.390(4) . ?
C6 H6 0.94(3) . ?
C7 H7 1.00(3) . ?
O2 N3 1.380(2) . ?
O2 H2O 0.85(3) . ?
N3 C9 1.284(3) . ?
N4 C14 1.336(3) . ?
N4 C10 1.353(3) . ?
C8 C9 1.487(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.479(3) . ?
C10 C11 1.385(3) . ?
C11 C12 1.390(4) . ?
C11 H11 0.93(3) . ?
C12 C13 1.372(4) . ?
C12 H12 0.97(3) . ?
C13 C14 1.386(4) . ?
C13 H13 0.93(3) . ?
C14 H14 0.92(3) . ?
F P 1.5882(14) . ?
P O4 1.4881(16) 3_656 ?
P O3 1.5053(17) . ?
P O5 1.5184(18) . ?
O4 P 1.4881(16) 3_656 ?
O1W H1WA 0.969(19) . ?
O1W H1WB 0.938(19) . ?

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 Ni O3 93.41(6) . . ?
O4 Ni N1 87.05(7) . . ?
O3 Ni N1 98.28(7) . . ?
O4 Ni N2 87.86(7) . . ?
O3 Ni N2 175.35(8) . . ?
N1 Ni N2 77.30(8) . . ?
O4 Ni N3 100.42(7) . . ?
O3 Ni N3 87.70(7) . . ?
N1 Ni N3 170.18(7) . . ?
N2 Ni N3 96.47(8) . . ?
O4 Ni N4 176.00(7) . . ?
O3 Ni N4 89.95(6) . . ?
N1 Ni N4 94.61(7) . . ?
N2 Ni N4 88.95(7) . . ?
N3 Ni N4 77.54(7) . . ?
N1 O1 H1O 105(3) . . ?
C2 N1 O1 114.6(2) . . ?
C2 N1 Ni 117.99(18) . . ?
O1 N1 Ni 127.28(15) . . ?
C7 N2 C3 119.2(2) . . ?
C7 N2 Ni 126.23(17) . . ?
C3 N2 Ni 114.11(17) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 114.2(2) . . ?
N1 C2 C1 124.1(3) . . ?
C3 C2 C1 121.7(2) . . ?
N2 C3 C4 121.4(3) . . ?
N2 C3 C2 116.0(2) . . ?
C4 C3 C2 122.6(2) . . ?
C5 C4 C3 118.8(3) . . ?
C5 C4 H4 121.1(18) . . ?
C3 C4 H4 119.7(18) . . ?
C6 C5 C4 119.9(3) . . ?
C6 C5 H5 121(2) . . ?
C4 C5 H5 119(2) . . ?
C5 C6 C7 118.4(3) . . ?
C5 C6 H6 125.9(17) . . ?
C7 C6 H6 115.7(18) . . ?
N2 C7 C6 122.3(3) . . ?
N2 C7 H7 118.0(15) . . ?
C6 C7 H7 119.8(15) . . ?
N3 O2 H2O 110(2) . . ?
C9 N3 O2 113.9(2) . . ?
C9 N3 Ni 116.97(16) . . ?
O2 N3 Ni 128.34(15) . . ?
C14 N4 C10 118.6(2) . . ?
C14 N4 Ni 127.27(17) . . ?
C10 N4 Ni 113.53(15) . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N3 C9 C10 114.8(2) . . ?
N3 C9 C8 124.4(2) . . ?
C10 C9 C8 120.8(2) . . ?
N4 C10 C11 121.6(2) . . ?
N4 C10 C9 115.9(2) . . ?
C11 C10 C9 122.5(2) . . ?
C10 C11 C12 119.0(3) . . ?
C10 C11 H11 120.1(16) . . ?
C12 C11 H11 120.8(16) . . ?
C13 C12 C11 119.4(2) . . ?
C13 C12 H12 119.3(17) . . ?
C11 C12 H12 121.3(17) . . ?
C12 C13 C14 118.5(2) . . ?
C12 C13 H13 123.9(17) . . ?
C14 C13 H13 117.5(17) . . ?
N4 C14 C13 122.8(3) . . ?
N4 C14 H14 117.8(17) . . ?
C13 C14 H14 119.4(17) . . ?
O4 P O3 116.39(10) 3_656 . ?
O4 P O5 114.57(9) 3_656 . ?
O3 P O5 112.91(10) . . ?
O4 P F 104.45(9) 3_656 . ?
O3 P F 102.18(8) . . ?
O5 P F 104.25(9) . . ?
P O3 Ni 125.34(9) . . ?
P O4 Ni 144.77(11) 3_656 . ?
H1WA O1W H1WB 103(3) . . ?

_diffrn_measured_fraction_theta_max 0.960
_diffrn_reflns_theta_full        64.99
_diffrn_measured_fraction_theta_full 0.960
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.061
_database_code_depnum_ccdc_archive 'CCDC 1015275'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_comp4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C15.20 H19.10 F2 N4.60 Ni O7.65 P2'
_chemical_formula_weight         547.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c

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

_cell_length_a                   11.9266(6)
_cell_length_b                   18.0040(11)
_cell_length_c                   13.3621(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.294(1)
_cell_angle_gamma                90.00
_cell_volume                     2673.3(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7966
_cell_measurement_theta_min      6.51
_cell_measurement_theta_max      72.01

_exptl_crystal_description       parallelepiped
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1119
_exptl_absorpt_coefficient_mu    2.696
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.116
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC, 2005'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       'θ scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            10864
_diffrn_reflns_av_R_equivalents  0.0891
_diffrn_reflns_av_sigmaI/netI    0.1086
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         6.70
_diffrn_reflns_theta_max         52.00
_reflns_number_total             2728
_reflns_number_gt                1356
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear, Rigaku MSC, 2005'
_computing_cell_refinement       'CrystalClear, Rigaku MSC, 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC, 2005'
_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)+(0.2000P)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    refall
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0007(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2728
_refine_ls_number_parameters     294
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1761
_refine_ls_R_factor_gt           0.1065
_refine_ls_wR_factor_ref         0.3231
_refine_ls_wR_factor_gt          0.2618
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003

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
Ni Ni 0.81988(13) 0.05058(7) 0.68412(13) 0.0868(10) Uani 1 1 d . . .
N1 N 0.7434(8) -0.0415(4) 0.5916(7) 0.083(3) Uani 1 1 d . . .
N2 N 0.6580(7) 0.0404(4) 0.7060(8) 0.090(3) Uani 1 1 d . . .
O1 O 0.6197(7) 0.0802(4) 0.7773(7) 0.115(2) Uani 1 1 d . . .
C1 C 0.4817(10) -0.0342(6) 0.6891(10) 0.123(4) Uani 1 1 d . . .
H1A H 0.4814 -0.0073 0.7510 0.173 Uiso 1 1 calc R . .
H1B H 0.4822 -0.0866 0.7028 0.173 Uiso 1 1 calc R . .
H1C H 0.4112 -0.0218 0.6283 0.173 Uiso 1 1 calc R . .
C2 C 0.5907(9) -0.0142(6) 0.6662(9) 0.087(3) Uani 1 1 d . . .
C3 C 0.6346(10) -0.0620(5) 0.5926(10) 0.084(3) Uani 1 1 d . . .
C4 C 0.5681(10) -0.1162(6) 0.5273(11) 0.107(4) Uani 1 1 d . . .
H4 H 0.4917 -0.1275 0.5264 0.139 Uiso 1 1 calc R . .
C5 C 0.6158(18) -0.1545(7) 0.4615(13) 0.140(5) Uani 1 1 d . . .
H5 H 0.5747 -0.1948 0.4214 0.182 Uiso 1 1 calc R . .
C6 C 0.7203(14) -0.1334(6) 0.4562(11) 0.130(5) Uani 1 1 d . . .
H6 H 0.7497 -0.1548 0.4073 0.169 Uiso 1 1 calc R . .
C7 C 0.7832(9) -0.0787(6) 0.5258(10) 0.092(3) Uani 1 1 d . . .
H7 H 0.8595 -0.0669 0.5267 0.119 Uiso 1 1 calc R . .
N11 N 0.9143(8) -0.0185(4) 0.8143(8) 0.093(3) Uani 1 1 d . . .
N12 N 0.9856(7) 0.0388(4) 0.6695(8) 0.079(2) Uani 1 1 d . . .
O11 O 1.0221(6) 0.0725(4) 0.5910(7) 0.106(2) Uani 1 1 d . . .
C11 C 1.1778(10) -0.0218(6) 0.7272(10) 0.116(4) Uani 1 1 d . . .
H11A H 1.1686 -0.0358 0.6553 0.162 Uiso 1 1 calc R . .
H11B H 1.2131 -0.0622 0.7752 0.162 Uiso 1 1 calc R . .
H11C H 1.2291 0.0210 0.7483 0.162 Uiso 1 1 calc R . .
C12 C 1.0656(10) -0.0050(6) 0.7311(12) 0.090(4) Uani 1 1 d . . .
C13 C 1.0261(11) -0.0378(5) 0.8101(10) 0.092(4) Uani 1 1 d . . .
C14 C 1.0976(11) -0.0862(7) 0.8843(13) 0.115(4) Uani 1 1 d . . .
H14 H 1.1728 -0.0987 0.8833 0.150 Uiso 1 1 calc R . .
C15 C 1.0580(14) -0.1175(7) 0.9630(11) 0.115(4) Uani 1 1 d . . .
H15 H 1.1068 -0.1508 1.0132 0.150 Uiso 1 1 calc R . .
C16 C 0.9472(15) -0.0986(6) 0.9649(10) 0.118(5) Uani 1 1 d . . .
H16 H 0.9199 -0.1190 1.0157 0.153 Uiso 1 1 calc R . .
C17 C 0.8779(12) -0.0490(8) 0.8905(14) 0.119(5) Uani 1 1 d . . .
H17 H 0.8032 -0.0357 0.8920 0.155 Uiso 1 1 calc R . .
O21 O 0.8823(6) 0.1462(3) 0.7717(6) 0.107(2) Uani 1 1 d . . .
O22 O 0.7041(7) 0.2175(4) 0.7720(7) 0.124(3) Uani 1 1 d . . .
O23 O 0.7897(8) 0.2440(4) 0.6303(9) 0.145(3) Uani 1 1 d . . .
O24 O 0.7385(5) 0.1141(3) 0.5516(5) 0.091(2) Uani 1 1 d . . .
O25 O 0.8901(6) 0.1896(3) 0.5021(7) 0.115(3) Uani 1 1 d . . .
F1 F 0.6710(6) 0.2290(4) 0.4383(7) 0.175(3) Uani 1 1 d . . .
F2 F 0.8987(7) 0.2824(3) 0.8162(8) 0.176(3) Uani 1 1 d . . .
P1 P 0.7740(3) 0.18767(16) 0.5252(3) 0.1105(14) Uani 1 1 d . . .
P2 P 0.8197(3) 0.21748(15) 0.7541(3) 0.1055(14) Uani 1 1 d . . .
C1S C 0.7468(17) -0.2691(10) 0.2579(14) 0.102(6) Uiso 0.60 1 d P . .
C2S C 0.8516(17) -0.2463(10) 0.2325(15) 0.117(6) Uiso 0.60 1 d P . .
N1S N 0.6751(17) -0.2867(10) 0.2798(15) 0.145(7) Uiso 0.60 1 d P . .
O1W O 0.513(2) 0.3583(14) 0.5089(18) 0.146(8) Uiso 0.35 1 d P . .
O2W O 0.373(3) 0.4152(16) 0.484(2) 0.146(9) Uiso 0.30 1 d P . .
H1O H 0.6474 0.1266 0.7929 0.050 Uiso 1 1 d . . .
H11O H 0.9557 0.1089 0.5393 0.050 Uiso 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
Ni O24 2.034(6) . ?
Ni O21 2.063(6) . ?
Ni N2 2.064(9) . ?
Ni N12 2.066(8) . ?
Ni N1 2.071(8) . ?
Ni N11 2.102(9) . ?
N1 C7 1.323(11) . ?
N1 C3 1.354(12) . ?
N2 C2 1.258(11) . ?
N2 O1 1.396(10) . ?
O1 H1O 0.8940 . ?
C1 C2 1.483(14) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.534(14) . ?
C3 C4 1.357(14) . ?
C4 C5 1.391(15) . ?
C4 H4 0.9300 . ?
C5 C6 1.328(17) . ?
C5 H5 0.9300 . ?
C6 C7 1.375(14) . ?
C6 H6 0.9300 . ?
C7 H7 0.9300 . ?
N11 C17 1.359(15) . ?
N11 C13 1.398(14) . ?
N12 C12 1.281(12) . ?
N12 O11 1.410(9) . ?
O11 H11O 1.0662 . ?
C11 C12 1.391(13) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.430(15) . ?
C13 C14 1.362(15) . ?
C14 C15 1.417(15) . ?
C14 H14 0.9300 . ?
C15 C16 1.373(15) . ?
C15 H15 0.9300 . ?
C16 C17 1.368(16) . ?
C16 H16 0.9300 . ?
C17 H17 0.9300 . ?
O21 P2 1.460(6) . ?
O22 P2 1.482(7) . ?
O23 P2 1.632(10) . ?
O23 P1 1.686(9) . ?
O24 P1 1.473(6) . ?
O25 P1 1.525(7) . ?
F1 P1 1.541(7) . ?
F2 P2 1.542(7) . ?
C1S N1S 1.05(2) . ?
C1S C2S 1.47(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
O24 Ni O21 89.1(2) . . ?
O24 Ni N2 89.9(3) . . ?
O21 Ni N2 99.1(3) . . ?
O24 Ni N12 98.4(3) . . ?
O21 Ni N12 88.8(3) . . ?
N2 Ni N12 168.7(3) . . ?
O24 Ni N1 87.9(3) . . ?
O21 Ni N1 175.3(3) . . ?
N2 Ni N1 77.4(4) . . ?
N12 Ni N1 95.2(3) . . ?
O24 Ni N11 174.9(4) . . ?
O21 Ni N11 92.9(3) . . ?
N2 Ni N11 94.5(4) . . ?
N12 Ni N11 76.9(4) . . ?
N1 Ni N11 90.4(3) . . ?
C7 N1 C3 116.5(9) . . ?
C7 N1 Ni 127.9(7) . . ?
C3 N1 Ni 115.3(8) . . ?
C2 N2 O1 112.0(9) . . ?
C2 N2 Ni 119.7(8) . . ?
O1 N2 Ni 127.3(7) . . ?
N2 O1 H1O 117.0 . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C2 C1 125.1(11) . . ?
N2 C2 C3 113.3(10) . . ?
C1 C2 C3 121.6(10) . . ?
N1 C3 C4 121.8(12) . . ?
N1 C3 C2 113.9(10) . . ?
C4 C3 C2 124.0(11) . . ?
C3 C4 C5 119.0(12) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C6 C5 C4 119.9(13) . . ?
C6 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C5 C6 C7 117.5(13) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 H6 121.3 . . ?
N1 C7 C6 124.9(10) . . ?
N1 C7 H7 117.6 . . ?
C6 C7 H7 117.6 . . ?
C17 N11 C13 119.9(10) . . ?
C17 N11 Ni 129.6(10) . . ?
C13 N11 Ni 110.3(9) . . ?
C12 N12 O11 112.6(9) . . ?
C12 N12 Ni 121.1(8) . . ?
O11 N12 Ni 126.2(7) . . ?
N12 O11 H11O 112.9 . . ?
C12 C11 H11A 109.5 . . ?
C12 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C12 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N12 C12 C11 127.7(13) . . ?
N12 C12 C13 111.1(10) . . ?
C11 C12 C13 121.2(12) . . ?
C14 C13 N11 119.0(12) . . ?
C14 C13 C12 120.9(13) . . ?
N11 C13 C12 120.1(9) . . ?
C13 C14 C15 120.3(12) . . ?
C13 C14 H14 119.8 . . ?
C15 C14 H14 119.8 . . ?
C16 C15 C14 119.8(13) . . ?
C16 C15 H15 120.1 . . ?
C14 C15 H15 120.1 . . ?
C17 C16 C15 118.7(13) . . ?
C17 C16 H16 120.6 . . ?
C15 C16 H16 120.7 . . ?
N11 C17 C16 122.3(12) . . ?
N11 C17 H17 118.8 . . ?
C16 C17 H17 118.8 . . ?
P2 O21 Ni 125.7(4) . . ?
P2 O23 P1 125.8(5) . . ?
P1 O24 Ni 128.8(4) . . ?
O24 P1 O25 115.5(4) . . ?
O24 P1 F1 113.3(4) . . ?
O25 P1 F1 111.7(4) . . ?
O24 P1 O23 107.3(4) . . ?
O25 P1 O23 108.7(4) . . ?
F1 P1 O23 98.8(5) . . ?
O21 P2 O22 115.1(4) . . ?
O21 P2 F2 113.8(4) . . ?
O22 P2 F2 109.6(4) . . ?
O21 P2 O23 109.3(5) . . ?
O22 P2 O23 106.9(5) . . ?
F2 P2 O23 100.9(5) . . ?
N1S C1S C2S 177(2) . . ?

_diffrn_measured_fraction_theta_max 0.911
_diffrn_reflns_theta_full        52.00
_diffrn_measured_fraction_theta_full 0.911
_refine_diff_density_max         0.682
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.097

# start Validation Reply Form
_vrf_THETM01_comp4               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystals showed very poor diffraction ability. Repeating
efforts to improve the quality of the crystals proved unsuccessful. 
Therefore we collected data to 2theta=143 deg from the 'best' crystal
we could find in order to establish the gross structure of the compound.
The data to 2theta=104 deg were used in the refinement. Even at that
low 2theta angle only half of the collected reflections are observed.
;
_vrf_PLAT023_comp4               
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      52.00 Degree
RESPONSE: Please see our answer above.
;
_vrf_PLAT029_comp4               
;
PROBLEM: _diffrn_measured_fraction_theta_full Low .......      0.911 Note  
RESPONSE: Please see our answer above.
;
# end Validation Reply Form 

#===END
_database_code_depnum_ccdc_archive 'CCDC 1015276'
