# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               'Dalton Trans.'

# 1. SUBMISSION DETAILS
_journal_coden_cambridge         0222
#===============================================================================
_audit_creation_date             2011-05-12
_publ_contact_author_name        'Audrey Auffrant'
_publ_contact_author_address     
;Laboratoire DCPH
Ecole Polytechnique
Route de Saclay
F91128 Palaiseau
France
;
_publ_contact_author_email       audrey.auffrant@polytechnique.edu
_publ_contact_author_phone       330169334410
_publ_contact_author_fax         330169334440

_publ_contact_letter             
;
Please consider this CIF submission for publication as a new structure
paper in DALTON TRANSACTIONS. The figures, chemical
structure diagram (scheme), Transfert of Copyright Agreement form and
structure factors will be sent on receipt of your acknowledgement letter
;
#===============================================================================

# 2. PROCESSING SUMMARY (IUCr Office Use Only)

#===============================================================================

# 3. TITLE AND AUTHOR LIST

_publ_section_title              
;
Pd(II) and Ni(II) Complexes Featuring a "Phosphasalen" ligand:
Synthesis and DFT study
;

_publ_author_address             
;
Laboratoire Heteroelements et Coordination,
Ecole Polytechnique, CNRS
F-91128 Palaiseau Cedex
France

;

#===============================================================================
# 4. TEXT

_publ_section_abstract           
; ?
;

_publ_section_comment            
;
;
_publ_section_exptl_prep         
;All structures were solved using SIR97 (Altomare et al.) and refined with
SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990).
;

_publ_section_references         
;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A.
(1993) J. Appl. Cryst. 26, 343-350.

Sheldrick, G.M. SHELXL97. Program for crystal structure
refinement. University of G\\"ottingen, Germany, 1997.

Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201.

Spek, A.L. (1990). Acta Cryst. A46, C-34.

Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7
;

_publ_section_figure_captions    
; ?
;

_publ_section_acknowledgements   
; ?
;
loop_
_publ_author_name
'T.-P.-A. Cao'
'S. Labouille'
E.Payet
A.Auffrant
Y.Jean
'X.F.Le Goff'
;
P.Le Floch
;

#===============================================================================
# If more than one structure is reported, sections 5-10 should be filled in
# per structure. For each data set, replace the ? in the data_? line below
# by a unique identifier.

#===============================================================================

#compound 6
data_pa236
_database_code_depnum_ccdc_archive 'CCDC 804616'
#TrackingRef '- 2011_cao_dalton.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H32 N2 O2 P2 Pd, 4(C H2 Cl2)'
_chemical_formula_sum            'C42 H40 Cl8 N2 O2 P2 Pd'
_chemical_formula_weight         1056.70

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'
Cl Cl 0.1484 0.1585 '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'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   'Pna21 '

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

_cell_length_a                   23.441(1)
_cell_length_b                   10.218(1)
_cell_length_c                   19.401(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4646.9(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    7363
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      30.034

_exptl_crystal_description       Block
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7738
_exptl_absorpt_correction_T_max  0.8608
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44198
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0412
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         30.02
_reflns_number_total             12183
_reflns_number_gt                10068
_reflns_threshold_expression     >2sigma(I)

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

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

Crystal were found to be twinned; twin fraction 0.62/0.38
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+1.4946P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.38(2)
_refine_ls_number_reflns         12183
_refine_ls_number_parameters     515
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1165
_refine_ls_wR_factor_gt          0.1104
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_restrained_S_all      1.092
_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
Pd1 Pd -0.622128(9) -0.18491(2) -0.399426(18) 0.02560(7) Uani 1 1 d . . .
P1 P -0.74263(3) -0.30002(8) -0.41082(5) 0.0269(2) Uani 1 1 d . . .
P2 P -0.50123(3) -0.29650(8) -0.38933(5) 0.0263(2) Uani 1 1 d . . .
O1 O -0.67763(10) -0.0390(2) -0.42248(13) 0.0331(6) Uani 1 1 d . . .
O2 O -0.56668(10) -0.0367(2) -0.37795(14) 0.0340(6) Uani 1 1 d . . .
N1 N -0.67556(12) -0.3343(3) -0.41988(17) 0.0309(7) Uani 1 1 d . . .
N2 N -0.56790(11) -0.3319(3) -0.37656(17) 0.0281(6) Uani 1 1 d . . .
C1 C -0.65388(13) -0.4557(3) -0.3873(3) 0.0382(10) Uani 1 1 d . . .
H1A H -0.6730 -0.5336 -0.4069 0.046 Uiso 1 1 calc R . .
H1B H -0.6605 -0.4540 -0.3369 0.046 Uiso 1 1 calc R . .
C2 C -0.59039(13) -0.4579(3) -0.4033(3) 0.0348(7) Uani 1 1 d . . .
H2A H -0.5716 -0.5327 -0.3800 0.042 Uiso 1 1 calc R . .
H2B H -0.5839 -0.4651 -0.4535 0.042 Uiso 1 1 calc R . .
C3 C -0.75794(14) -0.1649(4) -0.4654(2) 0.0285(7) Uani 1 1 d . . .
C4 C -0.72226(14) -0.0521(4) -0.46287(19) 0.0305(7) Uani 1 1 d . . .
C5 C -0.73813(15) 0.0544(4) -0.5056(2) 0.0342(8) Uani 1 1 d . . .
H5 H -0.7161 0.1324 -0.5045 0.041 Uiso 1 1 calc R . .
C6 C -0.78488(16) 0.0473(4) -0.5487(2) 0.0361(8) Uani 1 1 d . . .
H6 H -0.7946 0.1209 -0.5762 0.043 Uiso 1 1 calc R . .
C7 C -0.81793(16) -0.0652(4) -0.5526(2) 0.0359(9) Uani 1 1 d . . .
H7 H -0.8491 -0.0698 -0.5839 0.043 Uiso 1 1 calc R . .
C8 C -0.80503(15) -0.1705(4) -0.5107(2) 0.0330(8) Uani 1 1 d . . .
H8 H -0.8280 -0.2471 -0.5123 0.040 Uiso 1 1 calc R . .
C9 C -0.78415(14) -0.4375(4) -0.4392(2) 0.0301(7) Uani 1 1 d . . .
C10 C -0.76754(16) -0.5006(4) -0.5012(2) 0.0384(9) Uani 1 1 d . . .
H10 H -0.7344 -0.4723 -0.5251 0.046 Uiso 1 1 calc R . .
C11 C -0.79924(19) -0.6025(5) -0.5267(3) 0.0475(10) Uani 1 1 d . . .
H11 H -0.7877 -0.6451 -0.5680 0.057 Uiso 1 1 calc R . .
C12 C -0.84823(18) -0.6438(4) -0.4924(2) 0.0442(10) Uani 1 1 d . . .
H12 H -0.8701 -0.7141 -0.5104 0.053 Uiso 1 1 calc R . .
C13 C -0.86505(16) -0.5825(4) -0.4323(2) 0.0393(9) Uani 1 1 d . . .
H13 H -0.8985 -0.6112 -0.4092 0.047 Uiso 1 1 calc R . .
C14 C -0.83370(12) -0.4799(3) -0.4054(2) 0.0325(7) Uani 1 1 d . . .
H14 H -0.8457 -0.4382 -0.3641 0.039 Uiso 1 1 calc R . .
C15 C -0.76476(13) -0.2638(4) -0.3230(2) 0.0286(8) Uani 1 1 d . . .
C16 C -0.76420(16) -0.3631(4) -0.2732(2) 0.0363(8) Uani 1 1 d . . .
H16 H -0.7530 -0.4494 -0.2853 0.044 Uiso 1 1 calc R . .
C17 C -0.78001(17) -0.3347(5) -0.2065(2) 0.0463(11) Uani 1 1 d . . .
H17 H -0.7803 -0.4024 -0.1729 0.056 Uiso 1 1 calc R . .
C18 C -0.79532(18) -0.2097(6) -0.1878(2) 0.0513(13) Uani 1 1 d . . .
H18 H -0.8056 -0.1910 -0.1415 0.062 Uiso 1 1 calc R . .
C19 C -0.79567(19) -0.1100(5) -0.2375(2) 0.0454(10) Uani 1 1 d . . .
H19 H -0.8063 -0.0235 -0.2250 0.054 Uiso 1 1 calc R . .
C20 C -0.78050(16) -0.1378(4) -0.3045(2) 0.0369(9) Uani 1 1 d . . .
H20 H -0.7808 -0.0703 -0.3382 0.044 Uiso 1 1 calc R . .
C21 C -0.48576(14) -0.1586(4) -0.3368(2) 0.0287(7) Uani 1 1 d . . .
C22 C -0.52169(14) -0.0479(3) -0.33807(19) 0.0279(7) Uani 1 1 d . . .
C23 C -0.50700(15) 0.0580(4) -0.2944(2) 0.0355(8) Uani 1 1 d . . .
H23 H -0.5299 0.1347 -0.2949 0.043 Uiso 1 1 calc R . .
C24 C -0.46052(15) 0.0528(4) -0.2514(2) 0.0362(8) Uani 1 1 d . . .
H24 H -0.4518 0.1257 -0.2229 0.043 Uiso 1 1 calc R . .
C25 C -0.42571(16) -0.0591(4) -0.2491(2) 0.0364(8) Uani 1 1 d . . .
H25 H -0.3939 -0.0626 -0.2189 0.044 Uiso 1 1 calc R . .
C26 C -0.43841(15) -0.1638(4) -0.2914(2) 0.0317(8) Uani 1 1 d . . .
H26 H -0.4152 -0.2400 -0.2901 0.038 Uiso 1 1 calc R . .
C27 C -0.45811(13) -0.4330(3) -0.36161(19) 0.0279(7) Uani 1 1 d . . .
C28 C -0.41069(11) -0.4757(3) -0.3982(2) 0.0305(6) Uani 1 1 d . . .
H28 H -0.3997 -0.4327 -0.4396 0.037 Uiso 1 1 calc R . .
C29 C -0.37969(14) -0.5810(4) -0.3742(2) 0.0371(9) Uani 1 1 d . . .
H29 H -0.3476 -0.6110 -0.3995 0.045 Uiso 1 1 calc R . .
C30 C -0.39487(17) -0.6435(4) -0.3136(2) 0.0418(9) Uani 1 1 d . . .
H30 H -0.3736 -0.7167 -0.2978 0.050 Uiso 1 1 calc R . .
C31 C -0.44144(17) -0.5985(4) -0.2759(2) 0.0392(9) Uani 1 1 d . . .
H31 H -0.4515 -0.6392 -0.2336 0.047 Uiso 1 1 calc R . .
C32 C -0.47287(15) -0.4945(4) -0.3005(2) 0.0356(8) Uani 1 1 d . . .
H32 H -0.5050 -0.4646 -0.2752 0.043 Uiso 1 1 calc R . .
C33 C -0.48170(14) -0.2599(4) -0.4766(2) 0.0332(9) Uani 1 1 d . . .
C34 C -0.48285(15) -0.3577(5) -0.5279(2) 0.0372(9) Uani 1 1 d . . .
H34 H -0.4927 -0.4451 -0.5163 0.045 Uiso 1 1 calc R . .
C35 C -0.46953(18) -0.3250(5) -0.5954(2) 0.0462(11) Uani 1 1 d . . .
H35 H -0.4702 -0.3910 -0.6299 0.055 Uiso 1 1 calc R . .
C36 C -0.45541(19) -0.1986(5) -0.6134(2) 0.0482(11) Uani 1 1 d . . .
H36 H -0.4459 -0.1781 -0.6597 0.058 Uiso 1 1 calc R . .
C37 C -0.4552(2) -0.1021(6) -0.5636(3) 0.0583(13) Uani 1 1 d . . .
H37 H -0.4456 -0.0147 -0.5758 0.070 Uiso 1 1 calc R . .
C38 C -0.46869(19) -0.1317(4) -0.4963(2) 0.0413(9) Uani 1 1 d . . .
H38 H -0.4692 -0.0640 -0.4628 0.050 Uiso 1 1 calc R . .
Cl1 Cl -0.63419(7) -0.10244(19) -0.19540(9) 0.0864(5) Uani 1 1 d . . .
Cl2 Cl -0.58511(13) -0.3470(2) -0.15316(14) 0.1422(12) Uani 1 1 d . . .
C39 C -0.5812(3) -0.2199(6) -0.2076(3) 0.0767(17) Uani 1 1 d . . .
H39A H -0.5837 -0.2532 -0.2554 0.092 Uiso 1 1 calc R . .
H39B H -0.5434 -0.1776 -0.2022 0.092 Uiso 1 1 calc R . .
Cl3 Cl -0.63974(8) 0.28228(16) -0.25945(10) 0.0889(6) Uani 1 1 d . . .
Cl4 Cl -0.74085(5) 0.24213(14) -0.34253(9) 0.0632(4) Uani 1 1 d . . .
C40 C -0.6821(2) 0.1665(5) -0.3008(3) 0.0603(14) Uani 1 1 d . . .
H40A H -0.6964 0.1024 -0.2666 0.072 Uiso 1 1 calc R . .
H40B H -0.6590 0.1187 -0.3352 0.072 Uiso 1 1 calc R . .
Cl5 Cl -0.82363(10) 0.3021(2) -0.15136(11) 0.1086(7) Uani 1 1 d . . .
Cl6 Cl -0.87751(5) 0.06709(18) -0.10031(7) 0.0702(4) Uani 1 1 d . . .
C41 C -0.8676(2) 0.2360(7) -0.0862(3) 0.0702(16) Uani 1 1 d . . .
H41A H -0.8496 0.2500 -0.0406 0.084 Uiso 1 1 calc R . .
H41B H -0.9050 0.2810 -0.0864 0.084 Uiso 1 1 calc R . .
Cl7 Cl -0.91589(11) -0.3328(3) -0.07259(12) 0.1442(11) Uani 1 1 d . . .
Cl8 Cl -0.99253(5) -0.25153(14) 0.03698(9) 0.0660(4) Uani 1 1 d . . .
C42 C -0.9247(3) -0.3125(6) 0.0129(3) 0.0709(16) Uani 1 1 d . . .
H42A H -0.8951 -0.2515 0.0299 0.085 Uiso 1 1 calc R . .
H42B H -0.9187 -0.3978 0.0360 0.085 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pd1 0.02251(9) 0.02461(11) 0.02968(12) 0.00074(15) 0.00134(10) 0.00072(8)
P1 0.0216(3) 0.0277(4) 0.0314(6) 0.0007(4) 0.0017(3) 0.0004(3)
P2 0.0220(3) 0.0277(4) 0.0293(6) 0.0011(4) 0.0011(3) 0.0016(3)
O1 0.0274(11) 0.0276(13) 0.0443(16) -0.0008(11) -0.0038(10) 0.0048(9)
O2 0.0301(11) 0.0281(13) 0.0437(16) 0.0002(11) -0.0076(10) -0.0010(9)
N1 0.0205(11) 0.0281(15) 0.044(2) -0.0008(13) -0.0022(11) -0.0015(10)
N2 0.0234(12) 0.0245(14) 0.0363(17) -0.0003(12) 0.0036(10) 0.0019(10)
C1 0.0243(13) 0.0284(17) 0.062(3) 0.002(2) 0.0000(17) -0.0003(11)
C2 0.0305(14) 0.0250(15) 0.049(2) 0.001(2) 0.0003(19) 0.0018(11)
C3 0.0258(15) 0.0298(19) 0.030(2) 0.0011(15) 0.0035(13) 0.0017(13)
C4 0.0289(16) 0.0325(19) 0.0299(19) -0.0009(16) 0.0011(13) 0.0027(13)
C5 0.0324(17) 0.032(2) 0.038(2) 0.0047(17) 0.0014(14) -0.0013(14)
C6 0.0372(18) 0.041(2) 0.030(2) 0.0074(17) 0.0027(15) 0.0051(16)
C7 0.0330(18) 0.044(2) 0.030(2) 0.0053(18) 0.0000(15) 0.0032(16)
C8 0.0234(15) 0.035(2) 0.040(2) -0.0032(17) 0.0012(14) -0.0022(13)
C9 0.0261(15) 0.0313(19) 0.0329(19) 0.0040(16) 0.0000(14) -0.0016(13)
C10 0.0353(19) 0.037(2) 0.043(2) -0.0050(19) 0.0071(16) -0.0046(16)
C11 0.049(2) 0.043(2) 0.050(3) -0.004(2) 0.009(2) -0.0028(19)
C12 0.043(2) 0.039(2) 0.051(3) -0.003(2) -0.0054(18) -0.0098(17)
C13 0.0278(16) 0.041(2) 0.049(2) 0.0054(19) -0.0038(15) -0.0041(15)
C14 0.0240(13) 0.0368(17) 0.037(2) 0.001(2) 0.0023(17) -0.0008(11)
C15 0.0228(15) 0.0346(19) 0.028(2) 0.0023(16) -0.0026(13) 0.0004(13)
C16 0.0340(18) 0.042(2) 0.032(2) 0.0038(18) -0.0036(15) -0.0019(16)
C17 0.041(2) 0.060(3) 0.038(2) 0.009(2) -0.0044(18) -0.0113(19)
C18 0.037(2) 0.086(4) 0.031(2) -0.009(2) 0.0020(17) -0.009(2)
C19 0.045(2) 0.055(3) 0.037(2) -0.007(2) 0.0032(18) 0.002(2)
C20 0.0339(19) 0.042(2) 0.035(2) -0.0026(19) 0.0014(16) 0.0005(17)
C21 0.0249(15) 0.0342(19) 0.0271(19) 0.0024(15) 0.0021(13) -0.0032(13)
C22 0.0276(15) 0.0280(17) 0.0281(18) 0.0029(15) 0.0028(13) -0.0037(13)
C23 0.0340(17) 0.0275(19) 0.045(2) -0.0053(18) 0.0010(16) 0.0000(14)
C24 0.0296(16) 0.038(2) 0.041(2) -0.0107(18) -0.0034(16) -0.0004(14)
C25 0.0306(17) 0.039(2) 0.040(2) -0.0023(19) -0.0016(16) -0.0023(15)
C26 0.0311(17) 0.037(2) 0.0267(19) 0.0020(16) 0.0015(14) 0.0024(14)
C27 0.0244(14) 0.0269(17) 0.0324(19) -0.0011(15) -0.0014(13) 0.0012(12)
C28 0.0246(12) 0.0338(16) 0.0331(17) -0.004(2) 0.0014(18) 0.0007(11)
C29 0.0268(16) 0.043(2) 0.041(2) -0.0019(17) -0.0019(14) 0.0049(14)
C30 0.0368(19) 0.039(2) 0.049(3) -0.002(2) -0.0072(17) 0.0075(16)
C31 0.044(2) 0.039(2) 0.035(2) 0.0043(18) 0.0010(16) 0.0098(17)
C32 0.0339(17) 0.036(2) 0.036(2) -0.0054(18) 0.0055(15) 0.0068(15)
C33 0.0248(15) 0.038(2) 0.037(2) 0.0008(18) 0.0020(15) 0.0042(14)
C34 0.0316(18) 0.045(2) 0.035(2) -0.0057(19) -0.0037(15) 0.0040(15)
C35 0.042(2) 0.069(3) 0.028(2) -0.011(2) -0.0056(16) 0.018(2)
C36 0.050(2) 0.063(3) 0.031(2) 0.006(2) 0.0033(18) 0.014(2)
C37 0.067(3) 0.060(3) 0.048(3) 0.018(3) 0.008(2) 0.006(3)
C38 0.047(2) 0.041(2) 0.035(2) 0.004(2) 0.0074(18) 0.0038(18)
Cl1 0.0818(9) 0.1039(13) 0.0736(10) 0.0110(9) 0.0117(8) 0.0382(9)
Cl2 0.197(3) 0.1018(15) 0.1284(19) 0.0634(14) 0.0991(19) 0.0680(16)
C39 0.095(4) 0.070(4) 0.065(4) 0.010(3) 0.024(3) 0.023(3)
Cl3 0.0984(11) 0.0642(8) 0.1042(13) -0.0194(9) -0.0607(10) 0.0208(8)
Cl4 0.0488(6) 0.0536(8) 0.0872(11) 0.0058(7) -0.0190(6) -0.0092(5)
C40 0.068(3) 0.047(3) 0.066(4) -0.002(2) -0.023(3) 0.000(2)
Cl5 0.1236(15) 0.1292(18) 0.0732(12) -0.0044(11) -0.0138(11) -0.0406(13)
Cl6 0.0593(7) 0.1035(12) 0.0476(7) -0.0106(7) 0.0011(5) 0.0163(7)
C41 0.077(4) 0.094(5) 0.040(3) -0.005(3) -0.003(2) 0.018(3)
Cl7 0.1129(16) 0.240(3) 0.0792(13) 0.0276(16) 0.0383(12) 0.0321(19)
Cl8 0.0538(7) 0.0621(9) 0.0820(11) -0.0053(7) 0.0101(6) -0.0058(6)
C42 0.064(3) 0.076(4) 0.073(4) 0.021(3) 0.004(3) 0.014(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 N1 2.014(3) . ?
Pd1 N2 2.017(3) . ?
Pd1 O1 2.029(2) . ?
Pd1 O2 2.039(2) . ?
P1 N1 1.620(3) . ?
P1 C3 1.777(4) . ?
P1 C9 1.795(4) . ?
P1 C15 1.819(4) . ?
P2 N2 1.623(3) . ?
P2 C21 1.777(4) . ?
P2 C33 1.793(4) . ?
P2 C27 1.804(3) . ?
O1 C4 1.314(4) . ?
O2 C22 1.313(4) . ?
N1 C1 1.482(5) . ?
N2 C2 1.484(4) . ?
C1 C2 1.520(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C8 1.412(5) . ?
C3 C4 1.425(5) . ?
C4 C5 1.417(5) . ?
C5 C6 1.381(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.388(6) . ?
C6 H6 0.9500 . ?
C7 C8 1.383(6) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C9 C14 1.402(5) . ?
C9 C10 1.420(6) . ?
C10 C11 1.371(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.393(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.382(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.383(5) . ?
C13 H13 0.9500 . ?
C14 H14 0.9500 . ?
C15 C20 1.387(6) . ?
C15 C16 1.402(6) . ?
C16 C17 1.377(6) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.403(7) . ?
C18 H18 0.9500 . ?
C19 C20 1.377(6) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.411(5) . ?
C21 C26 1.417(5) . ?
C22 C23 1.417(5) . ?
C23 C24 1.373(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.406(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.381(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.386(5) . ?
C27 C28 1.390(5) . ?
C28 C29 1.380(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.384(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.392(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.378(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.399(6) . ?
C33 C34 1.410(6) . ?
C34 C35 1.387(6) . ?
C34 H34 0.9500 . ?
C35 C36 1.378(7) . ?
C35 H35 0.9500 . ?
C36 C37 1.380(7) . ?
C36 H36 0.9500 . ?
C37 C38 1.377(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
Cl1 C39 1.744(6) . ?
Cl2 C39 1.677(6) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
Cl3 C40 1.741(5) . ?
Cl4 C40 1.774(5) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
Cl5 C41 1.765(6) . ?
Cl6 C41 1.763(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
Cl7 C42 1.684(7) . ?
Cl8 C42 1.770(6) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Pd1 N2 82.58(10) . . ?
N1 Pd1 O1 96.59(11) . . ?
N2 Pd1 O1 179.15(11) . . ?
N1 Pd1 O2 178.69(11) . . ?
N2 Pd1 O2 96.12(11) . . ?
O1 Pd1 O2 84.71(9) . . ?
N1 P1 C3 107.41(16) . . ?
N1 P1 C9 108.89(16) . . ?
C3 P1 C9 108.41(17) . . ?
N1 P1 C15 114.98(16) . . ?
C3 P1 C15 110.04(18) . . ?
C9 P1 C15 106.95(17) . . ?
N2 P2 C21 106.61(16) . . ?
N2 P2 C33 115.88(17) . . ?
C21 P2 C33 108.94(19) . . ?
N2 P2 C27 108.75(15) . . ?
C21 P2 C27 109.12(17) . . ?
C33 P2 C27 107.42(17) . . ?
C4 O1 Pd1 124.6(2) . . ?
C22 O2 Pd1 124.6(2) . . ?
C1 N1 P1 117.9(2) . . ?
C1 N1 Pd1 109.7(2) . . ?
P1 N1 Pd1 114.71(16) . . ?
C2 N2 P2 118.8(2) . . ?
C2 N2 Pd1 110.2(2) . . ?
P2 N2 Pd1 114.02(16) . . ?
N1 C1 C2 105.1(3) . . ?
N1 C1 H1A 110.7 . . ?
C2 C1 H1A 110.7 . . ?
N1 C1 H1B 110.7 . . ?
C2 C1 H1B 110.7 . . ?
H1A C1 H1B 108.8 . . ?
N2 C2 C1 105.3(3) . . ?
N2 C2 H2A 110.7 . . ?
C1 C2 H2A 110.7 . . ?
N2 C2 H2B 110.7 . . ?
C1 C2 H2B 110.7 . . ?
H2A C2 H2B 108.8 . . ?
C8 C3 C4 120.9(3) . . ?
C8 C3 P1 119.8(3) . . ?
C4 C3 P1 119.3(3) . . ?
O1 C4 C5 118.7(3) . . ?
O1 C4 C3 124.8(3) . . ?
C5 C4 C3 116.5(3) . . ?
C6 C5 C4 121.5(4) . . ?
C6 C5 H5 119.3 . . ?
C4 C5 H5 119.3 . . ?
C5 C6 C7 121.3(4) . . ?
C5 C6 H6 119.3 . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 119.3(4) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.3 . . ?
C7 C8 C3 120.4(4) . . ?
C7 C8 H8 119.8 . . ?
C3 C8 H8 119.8 . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 P1 123.2(3) . . ?
C10 C9 P1 117.8(3) . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C10 C11 C12 120.3(4) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C13 C12 C11 120.1(4) . . ?
C13 C12 H12 119.9 . . ?
C11 C12 H12 119.9 . . ?
C12 C13 C14 120.7(4) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C13 C14 C9 119.9(4) . . ?
C13 C14 H14 120.1 . . ?
C9 C14 H14 120.1 . . ?
C20 C15 C16 119.7(4) . . ?
C20 C15 P1 120.5(3) . . ?
C16 C15 P1 119.8(3) . . ?
C17 C16 C15 119.6(4) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C18 C17 C16 120.9(4) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 119.7(4) . . ?
C17 C18 H18 120.2 . . ?
C19 C18 H18 120.2 . . ?
C20 C19 C18 119.8(5) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C15 120.3(4) . . ?
C19 C20 H20 119.8 . . ?
C15 C20 H20 119.8 . . ?
C22 C21 C26 120.6(3) . . ?
C22 C21 P2 120.3(3) . . ?
C26 C21 P2 119.1(3) . . ?
O2 C22 C21 124.0(3) . . ?
O2 C22 C23 118.8(3) . . ?
C21 C22 C23 117.2(3) . . ?
C24 C23 C22 121.8(3) . . ?
C24 C23 H23 119.1 . . ?
C22 C23 H23 119.1 . . ?
C23 C24 C25 120.7(4) . . ?
C23 C24 H24 119.6 . . ?
C25 C24 H24 119.6 . . ?
C26 C25 C24 119.1(3) . . ?
C26 C25 H25 120.5 . . ?
C24 C25 H25 120.5 . . ?
C25 C26 C21 120.6(4) . . ?
C25 C26 H26 119.7 . . ?
C21 C26 H26 119.7 . . ?
C32 C27 C28 119.6(3) . . ?
C32 C27 P2 117.8(3) . . ?
C28 C27 P2 122.6(3) . . ?
C29 C28 C27 119.6(4) . . ?
C29 C28 H28 120.2 . . ?
C27 C28 H28 120.2 . . ?
C28 C29 C30 120.7(4) . . ?
C28 C29 H29 119.6 . . ?
C30 C29 H29 119.6 . . ?
C29 C30 C31 119.7(4) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.1 . . ?
C32 C31 C30 119.5(4) . . ?
C32 C31 H31 120.3 . . ?
C30 C31 H31 120.3 . . ?
C31 C32 C27 120.8(3) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
C38 C33 C34 118.3(4) . . ?
C38 C33 P2 120.6(3) . . ?
C34 C33 P2 120.9(3) . . ?
C35 C34 C33 119.4(4) . . ?
C35 C34 H34 120.3 . . ?
C33 C34 H34 120.3 . . ?
C36 C35 C34 121.2(4) . . ?
C36 C35 H35 119.4 . . ?
C34 C35 H35 119.4 . . ?
C35 C36 C37 119.6(4) . . ?
C35 C36 H36 120.2 . . ?
C37 C36 H36 120.2 . . ?
C38 C37 C36 120.3(5) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C33 121.0(4) . . ?
C37 C38 H38 119.5 . . ?
C33 C38 H38 119.5 . . ?
Cl2 C39 Cl1 114.1(3) . . ?
Cl2 C39 H39A 108.7 . . ?
Cl1 C39 H39A 108.7 . . ?
Cl2 C39 H39B 108.7 . . ?
Cl1 C39 H39B 108.7 . . ?
H39A C39 H39B 107.6 . . ?
Cl3 C40 Cl4 110.9(3) . . ?
Cl3 C40 H40A 109.5 . . ?
Cl4 C40 H40A 109.5 . . ?
Cl3 C40 H40B 109.5 . . ?
Cl4 C40 H40B 109.5 . . ?
H40A C40 H40B 108.0 . . ?
Cl6 C41 Cl5 109.9(3) . . ?
Cl6 C41 H41A 109.7 . . ?
Cl5 C41 H41A 109.7 . . ?
Cl6 C41 H41B 109.7 . . ?
Cl5 C41 H41B 109.7 . . ?
H41A C41 H41B 108.2 . . ?
Cl7 C42 Cl8 114.5(4) . . ?
Cl7 C42 H42A 108.6 . . ?
Cl8 C42 H42A 108.6 . . ?
Cl7 C42 H42B 108.6 . . ?
Cl8 C42 H42B 108.6 . . ?
H42A C42 H42B 107.6 . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        30.02
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.874
_refine_diff_density_rms         0.082
#===END

#compound 7
data_pa185
_database_code_depnum_ccdc_archive 'CCDC 804617'
#TrackingRef '- 2011_cao_dalton.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C38 H32 N2 Ni O2 P2, C H2 Cl2'
_chemical_formula_sum            'C39 H34 Cl2 N2 Ni O2 P2'
_chemical_formula_weight         754.23

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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'Pc '

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

_cell_length_a                   14.095(1)
_cell_length_b                   9.040(1)
_cell_length_c                   16.233(1)
_cell_angle_alpha                90.00
_cell_angle_beta                 122.384(4)
_cell_angle_gamma                90.00
_cell_volume                     1746.7(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150.0(1)
_cell_measurement_reflns_used    779
_cell_measurement_theta_min      0.998
_cell_measurement_theta_max      26.022

_exptl_crystal_description       Needle
_exptl_crystal_colour            Purple
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             780
_exptl_absorpt_coefficient_mu    0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7753
_exptl_absorpt_correction_T_max  0.9672
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      150.0(1)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9847
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0494
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.38
_diffrn_reflns_theta_max         26.00
_reflns_number_total             5021
_reflns_number_gt                4499
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0739P)^2^+0.7114P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.022(16)
_refine_ls_number_reflns         5021
_refine_ls_number_parameters     433
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0449
_refine_ls_wR_factor_ref         0.1219
_refine_ls_wR_factor_gt          0.1166
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.09132(4) -0.93834(6) -0.26683(4) 0.03169(17) Uani 1 1 d . . .
P1 P -0.12531(10) -1.02124(13) -0.28075(9) 0.0307(3) Uani 1 1 d . . .
P2 P 0.25456(10) -1.15729(13) -0.26051(9) 0.0324(3) Uani 1 1 d . . .
O1 O -0.0137(3) -0.7837(4) -0.3246(3) 0.0403(8) Uani 1 1 d . . .
O2 O 0.1695(4) -0.8318(4) -0.3102(4) 0.0570(12) Uani 1 1 d . . .
N1 N 0.0083(3) -1.0482(4) -0.2259(3) 0.0328(9) Uani 1 1 d . . .
N2 N 0.2024(4) -1.0855(5) -0.2019(3) 0.0357(10) Uani 1 1 d . . .
C1 C 0.0576(4) -1.1954(5) -0.1867(4) 0.0380(12) Uani 1 1 d . . .
H1A H 0.0304 -1.2687 -0.2400 0.046 Uiso 1 1 calc R . .
H1B H 0.0378 -1.2299 -0.1399 0.046 Uiso 1 1 calc R . .
C2 C 0.1824(4) -1.1742(6) -0.1365(4) 0.0409(12) Uani 1 1 d . . .
H2A H 0.2121 -1.1221 -0.0736 0.049 Uiso 1 1 calc R . .
H2B H 0.2205 -1.2712 -0.1233 0.049 Uiso 1 1 calc R . .
C3 C -0.1491(4) -0.8282(5) -0.2830(3) 0.0293(10) Uani 1 1 d . . .
C4 C -0.0872(4) -0.7338(5) -0.3065(4) 0.0328(11) Uani 1 1 d . . .
C5 C -0.1112(5) -0.5799(5) -0.3131(4) 0.0431(13) Uani 1 1 d . . .
H5 H -0.0731 -0.5130 -0.3308 0.052 Uiso 1 1 calc R . .
C6 C -0.1890(5) -0.5272(6) -0.2941(4) 0.0421(13) Uani 1 1 d . . .
H6 H -0.2038 -0.4240 -0.2991 0.051 Uiso 1 1 calc R . .
C7 C -0.2465(5) -0.6201(6) -0.2679(4) 0.0416(12) Uani 1 1 d . . .
H7 H -0.2984 -0.5801 -0.2536 0.050 Uiso 1 1 calc R . .
C8 C -0.2286(4) -0.7705(5) -0.2627(4) 0.0364(11) Uani 1 1 d . . .
H8 H -0.2687 -0.8350 -0.2457 0.044 Uiso 1 1 calc R . .
C9 C -0.1810(4) -1.1099(5) -0.2156(4) 0.0351(11) Uani 1 1 d . . .
C10 C -0.1172(5) -1.1027(6) -0.1137(4) 0.0447(13) Uani 1 1 d . . .
H10 H -0.0476 -1.0512 -0.0812 0.054 Uiso 1 1 calc R . .
C11 C -0.1551(6) -1.1702(6) -0.0605(5) 0.0539(16) Uani 1 1 d . . .
H11 H -0.1109 -1.1668 0.0087 0.065 Uiso 1 1 calc R . .
C12 C -0.2569(6) -1.2427(7) -0.1075(6) 0.0622(19) Uani 1 1 d . . .
H12 H -0.2829 -1.2887 -0.0706 0.075 Uiso 1 1 calc R . .
C13 C -0.3219(5) -1.2487(6) -0.2089(5) 0.0515(15) Uani 1 1 d . . .
H13 H -0.3921 -1.2988 -0.2411 0.062 Uiso 1 1 calc R . .
C14 C -0.2843(4) -1.1819(5) -0.2621(4) 0.0381(12) Uani 1 1 d . . .
H14 H -0.3291 -1.1849 -0.3314 0.046 Uiso 1 1 calc R . .
C15 C -0.2065(4) -1.0853(5) -0.4053(4) 0.0312(11) Uani 1 1 d . . .
C16 C -0.3147(4) -1.0288(6) -0.4707(4) 0.0435(13) Uani 1 1 d . . .
H16 H -0.3456 -0.9570 -0.4489 0.052 Uiso 1 1 calc R . .
C17 C -0.3762(5) -1.0764(7) -0.5661(4) 0.0478(14) Uani 1 1 d . . .
H17 H -0.4493 -1.0378 -0.6094 0.057 Uiso 1 1 calc R . .
C18 C -0.3326(4) -1.1789(6) -0.5990(4) 0.0427(13) Uani 1 1 d . . .
H18 H -0.3757 -1.2115 -0.6648 0.051 Uiso 1 1 calc R . .
C19 C -0.2264(5) -1.2351(6) -0.5368(4) 0.0472(14) Uani 1 1 d . . .
H19 H -0.1964 -1.3063 -0.5599 0.057 Uiso 1 1 calc R . .
C20 C -0.1631(5) -1.1876(6) -0.4405(4) 0.0402(12) Uani 1 1 d . . .
H20 H -0.0894 -1.2255 -0.3983 0.048 Uiso 1 1 calc R . .
C21 C 0.3011(4) -1.0114(5) -0.3031(4) 0.0322(11) Uani 1 1 d . . .
C22 C 0.2528(5) -0.8692(5) -0.3209(4) 0.0392(12) Uani 1 1 d . . .
C23 C 0.2962(5) -0.7592(5) -0.3534(4) 0.0426(13) Uani 1 1 d . . .
H23 H 0.2652 -0.6625 -0.3656 0.051 Uiso 1 1 calc R . .
C24 C 0.3827(5) -0.7877(6) -0.3681(4) 0.0431(13) Uani 1 1 d . . .
H24 H 0.4104 -0.7109 -0.3897 0.052 Uiso 1 1 calc R . .
C25 C 0.4290(5) -0.9283(6) -0.3514(4) 0.0463(13) Uani 1 1 d . . .
H25 H 0.4875 -0.9487 -0.3623 0.056 Uiso 1 1 calc R . .
C26 C 0.3894(5) -1.0369(6) -0.3191(4) 0.0428(13) Uani 1 1 d . . .
H26 H 0.4220 -1.1327 -0.3069 0.051 Uiso 1 1 calc R . .
C27 C 0.3722(4) -1.2758(5) -0.1808(4) 0.0343(11) Uani 1 1 d . . .
C28 C 0.4385(4) -1.2397(5) -0.0824(4) 0.0403(12) Uani 1 1 d . . .
H28 H 0.4211 -1.1537 -0.0594 0.048 Uiso 1 1 calc R . .
C29 C 0.5300(4) -1.3269(6) -0.0167(4) 0.0487(14) Uani 1 1 d . . .
H29 H 0.5737 -1.3030 0.0508 0.058 Uiso 1 1 calc R . .
C30 C 0.5556(5) -1.4517(6) -0.0535(5) 0.0514(16) Uani 1 1 d . . .
H30 H 0.6181 -1.5121 -0.0106 0.062 Uiso 1 1 calc R . .
C31 C 0.4914(5) -1.4857(6) -0.1497(5) 0.0494(14) Uani 1 1 d . . .
H31 H 0.5088 -1.5714 -0.1730 0.059 Uiso 1 1 calc R . .
C32 C 0.4011(5) -1.3983(6) -0.2149(4) 0.0410(12) Uani 1 1 d . . .
H32 H 0.3592 -1.4218 -0.2824 0.049 Uiso 1 1 calc R . .
C33 C 0.1596(4) -1.2746(5) -0.3642(4) 0.0329(11) Uani 1 1 d . . .
C34 C 0.1132(5) -1.2268(6) -0.4581(4) 0.0448(13) Uani 1 1 d . . .
H34 H 0.1318 -1.1318 -0.4703 0.054 Uiso 1 1 calc R . .
C35 C 0.0399(5) -1.3157(7) -0.5347(4) 0.0512(14) Uani 1 1 d . . .
H35 H 0.0082 -1.2810 -0.5995 0.061 Uiso 1 1 calc R . .
C36 C 0.0115(5) -1.4539(6) -0.5194(4) 0.0489(15) Uani 1 1 d . . .
H36 H -0.0392 -1.5144 -0.5731 0.059 Uiso 1 1 calc R . .
C37 C 0.0576(4) -1.5040(6) -0.4246(4) 0.0431(13) Uani 1 1 d . . .
H37 H 0.0388 -1.5993 -0.4130 0.052 Uiso 1 1 calc R . .
C38 C 0.1309(4) -1.4151(6) -0.3473(4) 0.0392(12) Uani 1 1 d . . .
H38 H 0.1621 -1.4490 -0.2823 0.047 Uiso 1 1 calc R . .
Cl1 Cl 0.2951(3) -0.5630(3) -0.0217(3) 0.1377(14) Uani 1 1 d . . .
Cl2 Cl 0.4293(2) -0.7980(3) -0.0276(3) 0.1210(10) Uani 1 1 d . . .
C39 C 0.3019(10) -0.7267(11) -0.0729(9) 0.126(4) Uani 1 1 d . . .
H39A H 0.2554 -0.8009 -0.0654 0.151 Uiso 1 1 calc R . .
H39B H 0.2675 -0.7104 -0.1436 0.151 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ni1 0.0341(3) 0.0288(3) 0.0346(3) 0.0033(3) 0.0200(3) 0.0030(3)
P1 0.0319(7) 0.0291(6) 0.0333(7) 0.0010(6) 0.0189(6) 0.0018(5)
P2 0.0307(6) 0.0313(6) 0.0343(7) 0.0041(6) 0.0168(5) 0.0039(5)
O1 0.045(2) 0.0336(18) 0.047(2) 0.0094(17) 0.0284(18) 0.0055(15)
O2 0.063(3) 0.037(2) 0.100(4) 0.020(2) 0.064(3) 0.0115(18)
N1 0.030(2) 0.028(2) 0.039(2) 0.0072(18) 0.0177(19) 0.0038(16)
N2 0.041(2) 0.039(2) 0.037(2) 0.0037(19) 0.028(2) 0.0019(18)
C1 0.044(3) 0.028(2) 0.043(3) 0.009(2) 0.024(3) 0.006(2)
C2 0.040(3) 0.048(3) 0.036(3) 0.012(2) 0.021(2) 0.012(2)
C3 0.037(3) 0.026(2) 0.024(2) -0.003(2) 0.015(2) -0.0013(18)
C4 0.038(3) 0.029(2) 0.034(3) 0.002(2) 0.021(2) 0.003(2)
C5 0.047(3) 0.032(3) 0.051(3) -0.002(2) 0.026(3) -0.003(2)
C6 0.053(3) 0.027(2) 0.041(3) 0.003(2) 0.022(3) 0.007(2)
C7 0.043(3) 0.041(3) 0.042(3) -0.001(3) 0.023(2) 0.012(2)
C8 0.039(3) 0.035(3) 0.032(3) 0.002(2) 0.017(2) 0.011(2)
C9 0.037(3) 0.027(2) 0.046(3) 0.007(2) 0.026(3) 0.007(2)
C10 0.051(3) 0.043(3) 0.046(3) 0.006(3) 0.031(3) 0.009(2)
C11 0.080(5) 0.045(3) 0.057(4) 0.013(3) 0.050(4) 0.018(3)
C12 0.084(5) 0.041(3) 0.101(6) 0.016(3) 0.075(5) 0.013(3)
C13 0.054(4) 0.041(3) 0.078(5) 0.009(3) 0.048(4) 0.008(3)
C14 0.037(3) 0.035(3) 0.049(3) 0.001(2) 0.027(3) 0.004(2)
C15 0.039(3) 0.026(2) 0.036(3) -0.003(2) 0.025(2) -0.0037(19)
C16 0.035(3) 0.047(3) 0.045(3) -0.002(3) 0.019(3) 0.005(2)
C17 0.036(3) 0.058(4) 0.043(3) -0.010(3) 0.017(3) -0.006(2)
C18 0.042(3) 0.044(3) 0.042(3) -0.006(2) 0.023(3) -0.013(2)
C19 0.057(4) 0.043(3) 0.047(3) -0.010(3) 0.032(3) -0.004(3)
C20 0.042(3) 0.039(3) 0.042(3) 0.002(2) 0.024(3) 0.007(2)
C21 0.034(3) 0.027(2) 0.034(3) -0.002(2) 0.018(2) -0.0026(19)
C22 0.044(3) 0.033(3) 0.045(3) -0.002(2) 0.027(3) -0.002(2)
C23 0.051(3) 0.030(3) 0.055(4) 0.004(2) 0.035(3) -0.001(2)
C24 0.052(3) 0.041(3) 0.044(3) 0.000(2) 0.030(3) -0.005(2)
C25 0.046(3) 0.057(3) 0.047(3) 0.007(3) 0.032(3) 0.001(3)
C26 0.043(3) 0.042(3) 0.048(3) 0.006(3) 0.028(3) 0.008(2)
C27 0.032(3) 0.033(3) 0.037(3) -0.003(2) 0.018(2) -0.001(2)
C28 0.035(3) 0.033(3) 0.045(3) 0.008(2) 0.016(2) 0.001(2)
C29 0.032(3) 0.052(3) 0.046(3) 0.007(3) 0.010(3) -0.003(2)
C30 0.030(3) 0.041(3) 0.061(4) 0.018(3) 0.010(3) 0.005(2)
C31 0.039(3) 0.038(3) 0.063(4) 0.006(3) 0.022(3) 0.005(2)
C32 0.037(3) 0.037(3) 0.042(3) 0.003(2) 0.016(2) 0.007(2)
C33 0.030(3) 0.034(3) 0.036(3) 0.003(2) 0.019(2) 0.0055(19)
C34 0.045(3) 0.039(3) 0.038(3) 0.006(2) 0.014(3) 0.003(2)
C35 0.050(4) 0.053(3) 0.035(3) 0.002(3) 0.012(3) -0.004(3)
C36 0.046(4) 0.044(3) 0.041(3) -0.007(3) 0.013(3) 0.000(2)
C37 0.037(3) 0.033(3) 0.046(3) -0.001(3) 0.014(3) -0.003(2)
C38 0.033(3) 0.042(3) 0.036(3) 0.000(2) 0.014(2) -0.004(2)
Cl1 0.177(3) 0.0628(13) 0.250(4) -0.0231(18) 0.165(3) -0.0148(14)
Cl2 0.0939(18) 0.0923(16) 0.176(3) 0.0397(18) 0.0716(19) 0.0160(13)
C39 0.125(8) 0.086(6) 0.109(8) -0.033(6) 0.023(7) 0.000(6)

_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 O2 1.863(4) . ?
Ni1 O1 1.881(3) . ?
Ni1 N2 1.888(4) . ?
Ni1 N1 1.905(4) . ?
P1 N1 1.613(4) . ?
P1 C3 1.774(5) . ?
P1 C15 1.804(5) . ?
P1 C9 1.807(5) . ?
P2 N2 1.617(4) . ?
P2 C21 1.771(5) . ?
P2 C27 1.809(5) . ?
P2 C33 1.827(5) . ?
O1 C4 1.301(6) . ?
O2 C22 1.319(6) . ?
N1 C1 1.478(6) . ?
N2 C2 1.474(6) . ?
C1 C2 1.502(7) . ?
C3 C4 1.410(7) . ?
C3 C8 1.425(7) . ?
C4 C5 1.421(7) . ?
C5 C6 1.373(8) . ?
C6 C7 1.382(8) . ?
C7 C8 1.378(7) . ?
C9 C14 1.391(7) . ?
C9 C10 1.398(8) . ?
C10 C11 1.378(8) . ?
C11 C12 1.378(9) . ?
C12 C13 1.391(10) . ?
C13 C14 1.373(8) . ?
C15 C20 1.389(7) . ?
C15 C16 1.407(7) . ?
C16 C17 1.377(8) . ?
C17 C18 1.368(8) . ?
C18 C19 1.378(8) . ?
C19 C20 1.390(8) . ?
C21 C22 1.410(7) . ?
C21 C26 1.419(7) . ?
C22 C23 1.409(7) . ?
C23 C24 1.387(8) . ?
C24 C25 1.387(8) . ?
C25 C26 1.366(8) . ?
C27 C28 1.390(7) . ?
C27 C32 1.392(7) . ?
C28 C29 1.397(7) . ?
C29 C30 1.410(9) . ?
C30 C31 1.356(9) . ?
C31 C32 1.386(8) . ?
C33 C34 1.367(7) . ?
C33 C38 1.404(7) . ?
C34 C35 1.372(8) . ?
C35 C36 1.375(8) . ?
C36 C37 1.387(8) . ?
C37 C38 1.378(7) . ?
Cl1 C39 1.724(10) . ?
Cl2 C39 1.664(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ni1 O1 83.92(16) . . ?
O2 Ni1 N2 95.36(17) . . ?
O1 Ni1 N2 176.33(19) . . ?
O2 Ni1 N1 178.5(2) . . ?
O1 Ni1 N1 95.44(15) . . ?
N2 Ni1 N1 85.36(17) . . ?
N1 P1 C3 108.2(2) . . ?
N1 P1 C15 115.0(2) . . ?
C3 P1 C15 107.1(2) . . ?
N1 P1 C9 110.8(2) . . ?
C3 P1 C9 108.2(2) . . ?
C15 P1 C9 107.4(2) . . ?
N2 P2 C21 108.1(2) . . ?
N2 P2 C27 110.4(2) . . ?
C21 P2 C27 109.3(2) . . ?
N2 P2 C33 115.8(2) . . ?
C21 P2 C33 108.3(2) . . ?
C27 P2 C33 104.7(2) . . ?
C4 O1 Ni1 130.9(3) . . ?
C22 O2 Ni1 131.7(3) . . ?
C1 N1 P1 121.0(3) . . ?
C1 N1 Ni1 112.6(3) . . ?
P1 N1 Ni1 118.8(2) . . ?
C2 N2 P2 121.9(3) . . ?
C2 N2 Ni1 111.3(3) . . ?
P2 N2 Ni1 117.2(2) . . ?
N1 C1 C2 105.3(4) . . ?
N2 C2 C1 107.4(4) . . ?
C4 C3 C8 121.2(4) . . ?
C4 C3 P1 117.6(3) . . ?
C8 C3 P1 121.2(4) . . ?
O1 C4 C3 122.3(4) . . ?
O1 C4 C5 120.5(4) . . ?
C3 C4 C5 117.1(4) . . ?
C6 C5 C4 120.5(5) . . ?
C5 C6 C7 121.9(5) . . ?
C8 C7 C6 120.1(5) . . ?
C7 C8 C3 119.2(5) . . ?
C14 C9 C10 119.1(5) . . ?
C14 C9 P1 123.1(4) . . ?
C10 C9 P1 117.7(4) . . ?
C11 C10 C9 120.1(6) . . ?
C12 C11 C10 120.1(6) . . ?
C11 C12 C13 120.3(6) . . ?
C14 C13 C12 119.7(6) . . ?
C13 C14 C9 120.6(6) . . ?
C20 C15 C16 118.0(5) . . ?
C20 C15 P1 121.3(4) . . ?
C16 C15 P1 120.6(4) . . ?
C17 C16 C15 120.7(5) . . ?
C18 C17 C16 120.4(5) . . ?
C17 C18 C19 120.2(5) . . ?
C18 C19 C20 120.1(5) . . ?
C15 C20 C19 120.6(5) . . ?
C22 C21 C26 119.1(5) . . ?
C22 C21 P2 121.3(4) . . ?
C26 C21 P2 119.6(4) . . ?
O2 C22 C23 117.6(4) . . ?
O2 C22 C21 125.0(5) . . ?
C23 C22 C21 117.4(5) . . ?
C24 C23 C22 122.1(5) . . ?
C25 C24 C23 120.1(5) . . ?
C26 C25 C24 119.2(5) . . ?
C25 C26 C21 122.1(5) . . ?
C28 C27 C32 118.9(5) . . ?
C28 C27 P2 118.5(4) . . ?
C32 C27 P2 122.6(4) . . ?
C27 C28 C29 121.5(5) . . ?
C28 C29 C30 118.0(5) . . ?
C31 C30 C29 120.3(5) . . ?
C30 C31 C32 121.5(6) . . ?
C31 C32 C27 119.7(5) . . ?
C34 C33 C38 119.2(5) . . ?
C34 C33 P2 121.4(4) . . ?
C38 C33 P2 119.4(4) . . ?
C33 C34 C35 120.2(5) . . ?
C34 C35 C36 121.3(5) . . ?
C35 C36 C37 119.2(5) . . ?
C38 C37 C36 119.8(5) . . ?
C37 C38 C33 120.2(5) . . ?
Cl2 C39 Cl1 116.4(6) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.909
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.069
#===END