# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © the Partner Organisations 2016

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

data_p205-1
_database_code_depnum_ccdc_archive 'CCDC 1446704'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            {Na}{(PNP)Ni(CO)}
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H96 N2 Na2 Ni2 O4 P4'
_chemical_formula_sum            'C62 H96 N2 Na2 Ni2 O4 P4'
_chemical_formula_weight         1220.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0360 0.0240 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3580 1.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I4(1)/acd

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+1/4, x+3/4, z+1/4'
'y+1/4, -x+1/4, z+3/4'
'-x+1/2, y, -z'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+3/4, x+5/4, z+3/4'
'y+3/4, -x+3/4, z+5/4'
'-x+1, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-1/4, -x-3/4, -z-1/4'
'-y-1/4, x-1/4, -z-3/4'
'x-1/2, -y, z'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y+1/4, -x-1/4, -z+1/4'
'-y+1/4, x+1/4, -z-1/4'
'x, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   24.031(3)
_cell_length_b                   24.031(3)
_cell_length_c                   45.282(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     26149(7)
_cell_formula_units_Z            16
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    114821
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      28.00

_exptl_crystal_description       platy
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             10432
_exptl_absorpt_coefficient_mu    0.703
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.8494
_exptl_absorpt_correction_T_max  0.8721
_exptl_absorpt_process_details   'HKL3000 Scalepack'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.70000
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'PLSII 2D bending magnet'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            114821
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0090
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_theta_min         2.78
_diffrn_reflns_theta_max         28.00
_reflns_number_total             8146
_reflns_number_gt                7982
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_cell_refinement       HKL3000
_computing_data_reduction        HKL3000
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'

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

_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)+(0.0499P)²+34.7351P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8146
_refine_ls_number_parameters     346
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0874
_refine_ls_wR_factor_gt          0.0871
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.004
_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 0.763720(6) 0.645595(6) 0.113598(3) 0.01147(6) Uani 1 1 d . . .
O1 O 0.80538(4) 0.53463(4) 0.12283(3) 0.0281(2) Uani 1 1 d . . .
O2 O 0.83457(5) 0.41774(5) 0.07850(3) 0.0351(3) Uani 1 1 d . . .
P1 P 0.794530(13) 0.700848(13) 0.148359(7) 0.01394(7) Uani 1 1 d . . .
P2 P 0.750754(12) 0.665609(12) 0.067150(7) 0.01174(7) Uani 1 1 d . . .
C1 C 0.78317(5) 0.57812(5) 0.11979(3) 0.0165(2) Uani 1 1 d . . .
C2 C 0.72894(5) 0.70753(5) 0.16880(3) 0.0150(2) Uani 1 1 d . . .
C3 C 0.72320(6) 0.71505(6) 0.19920(3) 0.0193(2) Uani 1 1 d . . .
H3 H 0.7557 0.7195 0.2109 0.023 Uiso 1 1 calc R . .
C4 C 0.67104(6) 0.71616(6) 0.21288(3) 0.0204(3) Uani 1 1 d . . .
C5 C 0.62423(5) 0.71091(5) 0.19505(3) 0.0181(2) Uani 1 1 d . . .
H5 H 0.5884 0.7123 0.2038 0.022 Uiso 1 1 calc R . .
C6 C 0.62855(5) 0.70375(5) 0.16464(3) 0.0158(2) Uani 1 1 d . . .
H6 H 0.5958 0.7007 0.1530 0.019 Uiso 1 1 calc R . .
C7 C 0.68093(5) 0.70107(5) 0.15091(3) 0.0134(2) Uani 1 1 d . . .
C8 C 0.66571(7) 0.72030(8) 0.24603(3) 0.0327(3) Uani 1 1 d . . .
H8A H 0.6584 0.7590 0.2516 0.049 Uiso 1 1 calc R . .
H8B H 0.7004 0.7078 0.2553 0.049 Uiso 1 1 calc R . .
H8C H 0.6349 0.6968 0.2527 0.049 Uiso 1 1 calc R . .
C9 C 0.68461(5) 0.70261(5) 0.06901(3) 0.0135(2) Uani 1 1 d . . .
C10 C 0.65629(5) 0.72342(5) 0.04435(3) 0.0155(2) Uani 1 1 d . . .
H10 H 0.6698 0.7145 0.0252 0.019 Uiso 1 1 calc R . .
C11 C 0.60893(5) 0.75672(5) 0.04680(3) 0.0168(2) Uani 1 1 d . . .
C12 C 0.59175(5) 0.77046(5) 0.07544(3) 0.0186(2) Uani 1 1 d . . .
H12 H 0.5608 0.7946 0.0779 0.022 Uiso 1 1 calc R . .
C13 C 0.61823(5) 0.75003(5) 0.10032(3) 0.0173(2) Uani 1 1 d . . .
H13 H 0.6058 0.7614 0.1193 0.021 Uiso 1 1 calc R . .
C14 C 0.66368(5) 0.71245(5) 0.09807(3) 0.0134(2) Uani 1 1 d . . .
C15 C 0.57826(6) 0.77747(6) 0.01994(3) 0.0236(3) Uani 1 1 d . . .
H15A H 0.6049 0.7932 0.0059 0.035 Uiso 1 1 calc R . .
H15B H 0.5515 0.8062 0.0258 0.035 Uiso 1 1 calc R . .
H15C H 0.5584 0.7465 0.0106 0.035 Uiso 1 1 calc R . .
C16 C 0.83333(7) 0.62205(7) 0.18914(3) 0.0284(3) Uani 1 1 d . . .
H16A H 0.7964 0.6230 0.1983 0.043 Uiso 1 1 calc R . .
H16B H 0.8613 0.6123 0.2040 0.043 Uiso 1 1 calc R . .
H16C H 0.8337 0.5942 0.1733 0.043 Uiso 1 1 calc R . .
C17 C 0.84680(5) 0.67933(6) 0.17626(3) 0.0208(2) Uani 1 1 d . . .
H17 H 0.8469 0.7072 0.1926 0.025 Uiso 1 1 calc R . .
C18 C 0.90447(6) 0.67890(8) 0.16177(4) 0.0339(3) Uani 1 1 d . . .
H18A H 0.9125 0.7158 0.1536 0.051 Uiso 1 1 calc R . .
H18B H 0.9051 0.6513 0.1458 0.051 Uiso 1 1 calc R . .
H18C H 0.9326 0.6693 0.1766 0.051 Uiso 1 1 calc R . .
C19 C 0.82938(7) 0.80963(6) 0.16768(4) 0.0297(3) Uani 1 1 d . . .
H19A H 0.8591 0.7911 0.1788 0.045 Uiso 1 1 calc R . .
H19B H 0.7966 0.8140 0.1803 0.045 Uiso 1 1 calc R . .
H19C H 0.8423 0.8463 0.1612 0.045 Uiso 1 1 calc R . .
C20 C 0.81410(6) 0.77451(5) 0.14076(3) 0.0202(3) Uani 1 1 d . . .
H20 H 0.8477 0.7735 0.1278 0.024 Uiso 1 1 calc R . .
C21 C 0.76782(6) 0.80233(6) 0.12295(3) 0.0237(3) Uani 1 1 d . . .
H21A H 0.7587 0.7792 0.1058 0.036 Uiso 1 1 calc R . .
H21B H 0.7804 0.8390 0.1162 0.036 Uiso 1 1 calc R . .
H21C H 0.7347 0.8067 0.1354 0.036 Uiso 1 1 calc R . .
C22 C 0.68844(6) 0.56933(6) 0.05461(3) 0.0228(3) Uani 1 1 d . . .
H22A H 0.6554 0.5922 0.0584 0.034 Uiso 1 1 calc R . .
H22B H 0.7009 0.5522 0.0731 0.034 Uiso 1 1 calc R . .
H22C H 0.6792 0.5402 0.0403 0.034 Uiso 1 1 calc R . .
C23 C 0.73483(5) 0.60584(5) 0.04223(3) 0.0160(2) Uani 1 1 d . . .
H23 H 0.7218 0.6213 0.0229 0.019 Uiso 1 1 calc R . .
C24 C 0.78668(6) 0.57058(6) 0.03622(3) 0.0233(3) Uani 1 1 d . . .
H24A H 0.8163 0.5943 0.0283 0.035 Uiso 1 1 calc R . .
H24B H 0.7777 0.5414 0.0219 0.035 Uiso 1 1 calc R . .
H24C H 0.7993 0.5534 0.0547 0.035 Uiso 1 1 calc R . .
C25 C 0.78736(6) 0.76919(6) 0.04143(3) 0.0247(3) Uani 1 1 d . . .
H25A H 0.7486 0.7767 0.0359 0.037 Uiso 1 1 calc R . .
H25B H 0.8123 0.7867 0.0270 0.037 Uiso 1 1 calc R . .
H25C H 0.7947 0.7845 0.0611 0.037 Uiso 1 1 calc R . .
C26 C 0.79736(5) 0.70662(5) 0.04178(3) 0.0167(2) Uani 1 1 d . . .
H26 H 0.7917 0.6924 0.0213 0.020 Uiso 1 1 calc R . .
C27 C 0.85797(6) 0.69522(7) 0.05045(4) 0.0325(4) Uani 1 1 d . . .
H27A H 0.8646 0.6550 0.0507 0.049 Uiso 1 1 calc R . .
H27B H 0.8652 0.7106 0.0701 0.049 Uiso 1 1 calc R . .
H27C H 0.8829 0.7128 0.0361 0.049 Uiso 1 1 calc R . .
C28 C 0.79948(9) 0.38271(11) 0.06107(5) 0.0544(6) Uani 1 1 d . . .
H28A H 0.7599 0.3877 0.0665 0.065 Uiso 1 1 calc R . .
H28B H 0.8097 0.3431 0.0635 0.065 Uiso 1 1 calc R . .
C29 C 0.81037(11) 0.40241(10) 0.02912(5) 0.0546(6) Uani 1 1 d . . .
H29A H 0.8098 0.3705 0.0153 0.066 Uiso 1 1 calc R . .
H29B H 0.7819 0.4298 0.0229 0.066 Uiso 1 1 calc R . .
C30 C 0.86782(9) 0.42909(9) 0.02996(4) 0.0465(4) Uani 1 1 d . . .
H30A H 0.8944 0.4082 0.0175 0.056 Uiso 1 1 calc R . .
H30B H 0.8663 0.4682 0.0231 0.056 Uiso 1 1 calc R . .
C31 C 0.88386(9) 0.42605(10) 0.06158(4) 0.0480(5) Uani 1 1 d . . .
H31A H 0.9101 0.3948 0.0648 0.058 Uiso 1 1 calc R . .
H31B H 0.9024 0.4610 0.0677 0.058 Uiso 1 1 calc R . .
N1 N 0.68982(4) 0.68608(4) 0.12121(2) 0.01333(19) Uani 1 1 d . . .
Na1 Na 0.80920(2) 0.44080(2) 0.1250 0.02158(16) Uani 1 2 d S . .
Na2 Na 0.66243(2) 0.58757(2) 0.1250 0.01866(15) Uani 1 2 d S . .


_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 C1 1.7106(13) . ?
Ni1 N1 2.0541(10) . ?
Ni1 P2 2.1799(5) . ?
Ni1 P1 2.1883(4) . ?
Ni1 Na2 2.8523(5) . ?
O1 C1 1.1816(16) . ?
O1 Na1 2.2587(12) . ?
O2 C31 1.425(2) . ?
O2 C28 1.429(2) . ?
O2 Na1 2.2609(13) . ?
P1 C2 1.8350(13) . ?
P1 C17 1.8550(14) . ?
P1 C20 1.8635(14) . ?
P2 C9 1.8232(12) . ?
P2 C23 1.8662(13) . ?
P2 C26 1.8828(13) . ?
C2 C3 1.3950(17) . ?
C2 C7 1.4182(17) . ?
C3 C4 1.3985(18) . ?
C4 C5 1.3904(19) . ?
C4 C8 1.5097(19) . ?
C5 C6 1.3915(18) . ?
C6 C7 1.4053(16) . ?
C7 N1 1.4085(15) . ?
C9 C10 1.4000(17) . ?
C9 C14 1.4282(16) . ?
C10 C11 1.3956(16) . ?
C11 C12 1.4002(18) . ?
C11 C15 1.5075(18) . ?
C12 C13 1.3840(18) . ?
C13 C14 1.4207(16) . ?
C14 N1 1.3764(16) . ?
C16 C17 1.530(2) . ?
C17 C18 1.533(2) . ?
C19 C20 1.5274(19) . ?
C20 C21 1.528(2) . ?
C22 C23 1.5252(19) . ?
C23 C24 1.5312(17) . ?
C25 C26 1.5229(18) . ?
C26 C27 1.5330(19) . ?
C28 C29 1.545(4) . ?
C29 C30 1.523(3) . ?
C30 C31 1.485(3) . ?
N1 Na2 2.4631(11) . ?
Na1 O1 2.2587(12) 8_665 ?
Na1 O2 2.2609(13) 8_665 ?
Na2 N1 2.4631(11) 8_665 ?
Na2 Ni1 2.8523(5) 8_665 ?
Na2 C1 2.9199(14) 8_665 ?
Na2 C7 3.0022(12) 8_665 ?

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
C1 Ni1 N1 131.12(5) . . ?
C1 Ni1 P2 113.98(4) . . ?
N1 Ni1 P2 86.21(3) . . ?
C1 Ni1 P1 111.39(4) . . ?
N1 Ni1 P1 83.36(3) . . ?
P2 Ni1 P1 127.481(16) . . ?
C1 Ni1 Na2 74.94(4) . . ?
N1 Ni1 Na2 57.55(3) . . ?
P2 Ni1 Na2 99.239(11) . . ?
P1 Ni1 Na2 117.073(14) . . ?
C1 O1 Na1 155.01(10) . . ?
C31 O2 C28 106.02(14) . . ?
C31 O2 Na1 133.69(11) . . ?
C28 O2 Na1 119.97(12) . . ?
C2 P1 C17 105.22(6) . . ?
C2 P1 C20 103.11(6) . . ?
C17 P1 C20 102.69(6) . . ?
C2 P1 Ni1 97.20(4) . . ?
C17 P1 Ni1 123.35(5) . . ?
C20 P1 Ni1 121.93(5) . . ?
C9 P2 C23 102.98(5) . . ?
C9 P2 C26 106.95(5) . . ?
C23 P2 C26 98.97(6) . . ?
C9 P2 Ni1 100.81(4) . . ?
C23 P2 Ni1 116.29(4) . . ?
C26 P2 Ni1 128.25(4) . . ?
O1 C1 Ni1 168.80(11) . . ?
C3 C2 C7 119.83(11) . . ?
C3 C2 P1 126.44(10) . . ?
C7 C2 P1 113.64(9) . . ?
C2 C3 C4 121.88(12) . . ?
C5 C4 C3 117.78(12) . . ?
C5 C4 C8 120.98(12) . . ?
C3 C4 C8 121.18(13) . . ?
C4 C5 C6 121.70(12) . . ?
C5 C6 C7 120.69(12) . . ?
C6 C7 N1 124.74(11) . . ?
C6 C7 C2 118.09(11) . . ?
N1 C7 C2 116.75(10) . . ?
C10 C9 C14 120.29(11) . . ?
C10 C9 P2 124.13(9) . . ?
C14 C9 P2 115.49(9) . . ?
C11 C10 C9 122.53(11) . . ?
C10 C11 C12 116.71(11) . . ?
C10 C11 C15 121.62(12) . . ?
C12 C11 C15 121.67(11) . . ?
C13 C12 C11 122.31(11) . . ?
C12 C13 C14 121.37(11) . . ?
N1 C14 C13 126.07(11) . . ?
N1 C14 C9 117.68(10) . . ?
C13 C14 C9 116.23(11) . . ?
C16 C17 C18 110.39(13) . . ?
C16 C17 P1 111.55(9) . . ?
C18 C17 P1 108.82(10) . . ?
C19 C20 C21 110.76(12) . . ?
C19 C20 P1 115.99(10) . . ?
C21 C20 P1 109.24(9) . . ?
C22 C23 C24 109.99(11) . . ?
C22 C23 P2 111.74(9) . . ?
C24 C23 P2 111.49(9) . . ?
C25 C26 C27 109.21(12) . . ?
C25 C26 P2 115.43(9) . . ?
C27 C26 P2 108.38(9) . . ?
O2 C28 C29 103.70(18) . . ?
C30 C29 C28 105.04(16) . . ?
C31 C30 C29 103.80(17) . . ?
O2 C31 C30 108.06(17) . . ?
C14 N1 C7 122.70(10) . . ?
C14 N1 Ni1 119.00(8) . . ?
C7 N1 Ni1 114.36(8) . . ?
C14 N1 Na2 111.93(7) . . ?
C7 N1 Na2 97.97(7) . . ?
Ni1 N1 Na2 77.73(4) . . ?
O1 Na1 O1 85.46(6) . 8_665 ?
O1 Na1 O2 108.64(5) . 8_665 ?
O1 Na1 O2 102.43(5) 8_665 8_665 ?
O1 Na1 O2 102.43(5) . . ?
O1 Na1 O2 108.64(5) 8_665 . ?
O2 Na1 O2 137.30(8) 8_665 . ?
N1 Na2 N1 121.23(5) . 8_665 ?
N1 Na2 Ni1 44.73(2) . . ?
N1 Na2 Ni1 164.46(4) 8_665 . ?
N1 Na2 Ni1 164.46(4) . 8_665 ?
N1 Na2 Ni1 44.73(2) 8_665 8_665 ?
Ni1 Na2 Ni1 150.13(3) . 8_665 ?
N1 Na2 C1 160.04(4) . 8_665 ?
N1 Na2 C1 78.67(3) 8_665 8_665 ?
Ni1 Na2 C1 115.72(3) . 8_665 ?
Ni1 Na2 C1 34.45(2) 8_665 8_665 ?
N1 Na2 C7 110.97(4) . 8_665 ?
N1 Na2 C7 27.68(3) 8_665 8_665 ?
Ni1 Na2 C7 140.98(3) . 8_665 ?
Ni1 Na2 C7 60.02(2) 8_665 8_665 ?
C1 Na2 C7 87.42(3) 8_665 8_665 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.647
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.057
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_n0374a-2
_database_code_depnum_ccdc_archive 'CCDC 1446705'
_audit_update_record             
;
2016-03-13 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            {(PNCOONaP)Ni(CO)2}4
_chemical_melting_point          ?
_chemical_formula_moiety         'C116 H160 N4 Na4 Ni4 O16 P8'
_chemical_formula_sum            'C116 H160 N4 Na4 Ni4 O16 P8'
_chemical_formula_weight         2441.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I-4

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

_cell_length_a                   21.043(2)
_cell_length_b                   21.043(2)
_cell_length_c                   15.6470(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     6928.5(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    27973
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      24.99

_exptl_crystal_description       platy
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2576
_exptl_absorpt_coefficient_mu    0.694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8511
_exptl_absorpt_correction_T_max  0.9338
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27973
_diffrn_reflns_av_R_equivalents  0.1137
_diffrn_reflns_av_sigmaI/netI    0.1002
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.74
_diffrn_reflns_theta_max         24.99
_reflns_number_total             6039
_reflns_number_gt                4355
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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)+(0.0855P)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    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   0.51(2)
_refine_ls_number_reflns         6039
_refine_ls_number_parameters     341
_refine_ls_number_restraints     116
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0670
_refine_ls_wR_factor_ref         0.1607
_refine_ls_wR_factor_gt          0.1477
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.000 504 133 ' '
2 0.134 0.581 0.158 16 0 ' '
3 0.866 0.419 0.158 16 0 ' '
4 0.000 0.000 0.500 504 133 ' '
5 0.081 0.366 0.342 17 0 ' '
6 0.919 0.634 0.342 16 0 ' '
7 0.366 0.919 0.658 16 0 ' '
8 0.634 0.081 0.658 16 0 ' '
9 0.419 0.134 0.842 16 0 ' '
10 0.581 0.866 0.842 17 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
'The unit cell contains 6 diethyl ether molecules which have been treated as a diffuse contribution to the overall scattering without specific atom positions by SQUEEZE/PLATON.'

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 0.74441(4) 0.13400(4) 0.11444(5) 0.0291(2) Uani 1 1 d U . .
P1 P 0.69295(7) 0.20578(8) 0.03650(11) 0.0286(4) Uani 1 1 d U . .
C5 C 0.6060(3) 0.1985(3) 0.0226(5) 0.0360(16) Uani 1 1 d U . .
C8 C 0.4740(3) 0.1952(4) 0.0118(6) 0.058(2) Uani 1 1 d U . .
H8 H 0.4289 0.1931 0.0096 0.069 Uiso 1 1 calc R . .
C4 C 0.5736(3) 0.1424(3) 0.0298(4) 0.0325(14) Uani 1 1 d U . .
C6 C 0.5707(4) 0.2528(4) 0.0087(6) 0.064(3) Uani 1 1 d U . .
H6 H 0.5928 0.2917 0.0008 0.076 Uiso 1 1 calc R . .
C7 C 0.5036(4) 0.2536(5) 0.0055(11) 0.110(3) Uani 1 1 d U . .
C9 C 0.5077(3) 0.1411(4) 0.0210(5) 0.0418(17) Uani 1 1 d U . .
H9 H 0.4861 0.1014 0.0214 0.050 Uiso 1 1 calc R . .
C10 C 0.4670(5) 0.3128(5) 0.0003(10) 0.110(3) Uani 1 1 d U . .
H10A H 0.4581 0.3227 -0.0598 0.165 Uiso 1 1 calc R . .
H10B H 0.4916 0.3476 0.0257 0.165 Uiso 1 1 calc R . .
H10C H 0.4269 0.3078 0.0314 0.165 Uiso 1 1 calc R . .
N1 N 0.6040(2) 0.0815(2) 0.0444(4) 0.0334(12) Uani 1 1 d U . .
C2 C 0.8225(3) 0.1608(3) 0.1287(4) 0.0335(15) Uani 1 1 d U . .
O2 O 0.8741(2) 0.1777(3) 0.1404(4) 0.0643(18) Uani 1 1 d U . .
C21 C 0.7227(3) 0.2216(3) -0.0740(5) 0.0409(16) Uani 1 1 d U . .
H21 H 0.7702 0.2227 -0.0713 0.049 Uiso 1 1 calc R . .
C23 C 0.7005(5) 0.2850(4) -0.1150(6) 0.069(2) Uani 1 1 d U . .
H23A H 0.7189 0.2890 -0.1723 0.104 Uiso 1 1 calc R . .
H23B H 0.7145 0.3207 -0.0795 0.104 Uiso 1 1 calc R . .
H23C H 0.6540 0.2853 -0.1192 0.104 Uiso 1 1 calc R . .
C18 C 0.7000(3) 0.2859(3) 0.0876(5) 0.0413(17) Uani 1 1 d U . .
H18 H 0.6769 0.3172 0.0509 0.050 Uiso 1 1 calc R . .
C20 C 0.7694(4) 0.3066(3) 0.0931(6) 0.053(2) Uani 1 1 d U . .
H20A H 0.7716 0.3506 0.1137 0.080 Uiso 1 1 calc R . .
H20B H 0.7889 0.3039 0.0364 0.080 Uiso 1 1 calc R . .
H20C H 0.7922 0.2787 0.1328 0.080 Uiso 1 1 calc R . .
C19 C 0.6702(5) 0.2872(4) 0.1760(5) 0.063(2) Uani 1 1 d U . .
H19A H 0.6962 0.2620 0.2154 0.094 Uiso 1 1 calc R . .
H19B H 0.6273 0.2692 0.1732 0.094 Uiso 1 1 calc R . .
H19C H 0.6679 0.3312 0.1963 0.094 Uiso 1 1 calc R . .
C22 C 0.7049(4) 0.1701(4) -0.1327(5) 0.062(2) Uani 1 1 d U . .
H22A H 0.6585 0.1657 -0.1337 0.093 Uiso 1 1 calc R . .
H22B H 0.7240 0.1302 -0.1131 0.093 Uiso 1 1 calc R . .
H22C H 0.7203 0.1800 -0.1903 0.093 Uiso 1 1 calc R . .
C3 C 0.5798(3) 0.0444(4) 0.1101(7) 0.058(2) Uani 1 1 d U . .
O3 O 0.5557(3) 0.0730(3) 0.1719(4) 0.0673(17) Uani 1 1 d U . .
O4 O 0.5875(3) -0.0156(3) 0.1027(6) 0.094(2) Uani 1 1 d U . .
C1 C 0.7028(3) 0.1234(3) 0.2109(5) 0.0364(15) Uani 1 1 d U . .
O1 O 0.6782(3) 0.1154(3) 0.2744(3) 0.0526(14) Uani 1 1 d U . .
C16 C 0.5880(4) 0.0403(4) -0.0984(6) 0.061(2) Uani 1 1 d U . .
H16 H 0.5458 0.0562 -0.0951 0.074 Uiso 1 1 calc R . .
C12 C 0.6886(3) 0.0236(3) -0.0320(5) 0.0437(17) Uani 1 1 d U . .
C11 C 0.6277(5) 0.0473(5) -0.0295(7) 0.0731(19) Uani 1 1 d U . .
C13 C 0.7065(5) -0.0095(4) -0.1053(7) 0.078(3) Uani 1 1 d U . .
H13 H 0.7476 -0.0280 -0.1068 0.094 Uiso 1 1 calc R . .
C14 C 0.6674(6) -0.0170(5) -0.1767(7) 0.095(4) Uani 1 1 d U . .
C15 C 0.6079(5) 0.0106(5) -0.1723(8) 0.096(4) Uani 1 1 d U . .
H15 H 0.5805 0.0092 -0.2206 0.115 Uiso 1 1 calc R . .
P2 P 0.74785(8) 0.03925(8) 0.05253(13) 0.0361(5) Uani 1 1 d U . .
C17 C 0.6951(5) -0.0470(5) -0.2586(6) 0.0731(19) Uani 1 1 d U . .
H17A H 0.7269 -0.0184 -0.2832 0.110 Uiso 1 1 calc R . .
H17B H 0.6609 -0.0541 -0.3000 0.110 Uiso 1 1 calc R . .
H17C H 0.7151 -0.0878 -0.2444 0.110 Uiso 1 1 calc R . .
C26 C 0.8407(5) 0.0648(5) -0.0712(6) 0.076(3) Uani 1 1 d U . .
H26A H 0.8432 0.1078 -0.0473 0.113 Uiso 1 1 calc R . .
H26B H 0.8075 0.0634 -0.1151 0.113 Uiso 1 1 calc R . .
H26C H 0.8816 0.0534 -0.0968 0.113 Uiso 1 1 calc R . .
C24 C 0.8249(3) 0.0185(3) -0.0014(6) 0.052(2) Uani 1 1 d U . .
H24 H 0.8204 -0.0246 -0.0275 0.063 Uiso 1 1 calc R . .
C25 C 0.8781(4) 0.0159(4) 0.0649(7) 0.074(3) Uani 1 1 d U . .
H25A H 0.9193 0.0145 0.0358 0.111 Uiso 1 1 calc R . .
H25B H 0.8730 -0.0222 0.1002 0.111 Uiso 1 1 calc R . .
H25C H 0.8760 0.0538 0.1013 0.111 Uiso 1 1 calc R . .
C29 C 0.7387(4) -0.0925(4) 0.0910(7) 0.073(3) Uani 1 1 d U . .
H29A H 0.7826 -0.1004 0.0733 0.110 Uiso 1 1 calc R . .
H29B H 0.7105 -0.0962 0.0414 0.110 Uiso 1 1 calc R . .
H29C H 0.7262 -0.1238 0.1343 0.110 Uiso 1 1 calc R . .
C27 C 0.7335(4) -0.0268(3) 0.1280(6) 0.054(2) Uani 1 1 d U . .
H27 H 0.6878 -0.0224 0.1449 0.065 Uiso 1 1 calc R . .
C28 C 0.7704(5) -0.0213(5) 0.2115(7) 0.082(3) Uani 1 1 d U . .
H28A H 0.7424 -0.0320 0.2595 0.123 Uiso 1 1 calc R . .
H28B H 0.7860 0.0222 0.2182 0.123 Uiso 1 1 calc R . .
H28C H 0.8065 -0.0508 0.2105 0.123 Uiso 1 1 calc R . .
Na1 Na 0.54902(12) -0.08509(12) 0.19414(17) 0.0358(6) Uani 1 1 d U . .


_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 C2 1.752(7) . ?
Ni1 C1 1.760(8) . ?
Ni1 P2 2.2179(19) . ?
Ni1 P1 2.2229(18) . ?
Ni1 N1 3.339(5) . ?
P1 C5 1.848(6) . ?
P1 C21 1.870(7) . ?
P1 C18 1.872(7) . ?
C5 C4 1.369(9) . ?
C5 C6 1.379(10) . ?
C8 C9 1.349(10) . ?
C8 C7 1.382(13) . ?
C4 C9 1.396(9) . ?
C4 N1 1.450(9) . ?
C6 C7 1.414(12) . ?
C7 C10 1.467(13) . ?
N1 C3 1.387(10) . ?
N1 C11 1.450(11) . ?
C2 O2 1.155(8) . ?
C21 C22 1.470(10) . ?
C21 C23 1.551(11) . ?
C18 C19 1.519(10) . ?
C18 C20 1.527(10) . ?
C3 O3 1.248(12) . ?
C3 O4 1.279(11) . ?
C3 Na1 3.067(11) 8_545 ?
C3 Na1 3.094(9) . ?
O3 Na1 2.244(6) 8_545 ?
O3 Na1 2.244(6) 2_655 ?
O4 Na1 2.200(6) . ?
C1 O1 1.132(8) . ?
O1 Na1 2.455(6) 8_545 ?
C16 C11 1.372(12) . ?
C16 C15 1.380(13) . ?
C12 C11 1.376(11) . ?
C12 C13 1.394(12) . ?
C12 P2 1.847(7) . ?
C13 C14 1.397(14) . ?
C14 C15 1.382(14) . ?
C14 C17 1.542(14) . ?
P2 C27 1.849(8) . ?
P2 C24 1.879(7) . ?
C26 C24 1.500(12) . ?
C24 C25 1.527(12) . ?
C29 C27 1.503(11) . ?
C27 C28 1.525(13) . ?
Na1 O3 2.243(6) 7 ?
Na1 O3 2.244(6) 2_655 ?
Na1 O1 2.455(6) 7 ?
Na1 C3 3.067(11) 7 ?
Na1 Na1 3.405(4) 8_545 ?
Na1 Na1 3.405(4) 7 ?
Na1 Na1 4.133(5) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 Ni1 C1 113.5(3) . . ?
C2 Ni1 P2 108.4(2) . . ?
C1 Ni1 P2 106.1(2) . . ?
C2 Ni1 P1 107.9(2) . . ?
C1 Ni1 P1 108.3(2) . . ?
P2 Ni1 P1 112.78(7) . . ?
C2 Ni1 N1 168.1(2) . . ?
C1 Ni1 N1 78.4(2) . . ?
P2 Ni1 N1 65.68(11) . . ?
P1 Ni1 N1 67.28(10) . . ?
C5 P1 C21 103.7(3) . . ?
C5 P1 C18 101.7(3) . . ?
C21 P1 C18 102.0(3) . . ?
C5 P1 Ni1 119.4(2) . . ?
C21 P1 Ni1 117.8(2) . . ?
C18 P1 Ni1 109.8(2) . . ?
C4 C5 C6 117.4(6) . . ?
C4 C5 P1 123.6(5) . . ?
C6 C5 P1 118.9(5) . . ?
C9 C8 C7 121.4(7) . . ?
C5 C4 C9 120.2(6) . . ?
C5 C4 N1 123.8(5) . . ?
C9 C4 N1 115.9(6) . . ?
C5 C6 C7 123.7(8) . . ?
C8 C7 C6 115.9(8) . . ?
C8 C7 C10 121.5(9) . . ?
C6 C7 C10 122.5(9) . . ?
C8 C9 C4 121.2(7) . . ?
C3 N1 C4 116.9(6) . . ?
C3 N1 C11 115.9(8) . . ?
C4 N1 C11 117.7(6) . . ?
C3 N1 Ni1 105.6(4) . . ?
C4 N1 Ni1 98.6(3) . . ?
C11 N1 Ni1 97.0(4) . . ?
O2 C2 Ni1 178.0(7) . . ?
C22 C21 C23 107.4(7) . . ?
C22 C21 P1 111.1(5) . . ?
C23 C21 P1 115.8(6) . . ?
C19 C18 C20 109.8(7) . . ?
C19 C18 P1 111.9(5) . . ?
C20 C18 P1 110.9(5) . . ?
O3 C3 O4 126.8(9) . . ?
O3 C3 N1 116.9(8) . . ?
O4 C3 N1 116.3(9) . . ?
O3 C3 Na1 39.2(4) . 8_545 ?
O4 C3 Na1 96.7(6) . 8_545 ?
N1 C3 Na1 135.1(6) . 8_545 ?
O3 C3 Na1 90.6(5) . . ?
O4 C3 Na1 36.4(4) . . ?
N1 C3 Na1 152.5(7) . . ?
Na1 C3 Na1 67.1(2) 8_545 . ?
C3 O3 Na1 120.2(6) . 8_545 ?
C3 O3 Na1 125.0(5) . 2_655 ?
Na1 O3 Na1 98.7(2) 8_545 2_655 ?
C3 O4 Na1 123.4(7) . . ?
O1 C1 Ni1 177.1(7) . . ?
C1 O1 Na1 128.7(5) . 8_545 ?
C11 C16 C15 121.5(8) . . ?
C11 C12 C13 117.2(8) . . ?
C11 C12 P2 122.9(6) . . ?
C13 C12 P2 119.7(6) . . ?
C16 C11 C12 120.4(9) . . ?
C16 C11 N1 118.1(8) . . ?
C12 C11 N1 121.5(8) . . ?
C12 C13 C14 123.8(8) . . ?
C15 C14 C13 116.5(9) . . ?
C15 C14 C17 123.8(9) . . ?
C13 C14 C17 119.2(9) . . ?
C16 C15 C14 120.5(9) . . ?
C12 P2 C27 102.3(4) . . ?
C12 P2 C24 102.7(4) . . ?
C27 P2 C24 104.7(4) . . ?
C12 P2 Ni1 116.8(2) . . ?
C27 P2 Ni1 113.0(3) . . ?
C24 P2 Ni1 115.7(2) . . ?
C26 C24 C25 110.8(7) . . ?
C26 C24 P2 111.6(6) . . ?
C25 C24 P2 109.6(6) . . ?
C29 C27 C28 111.2(7) . . ?
C29 C27 P2 115.7(7) . . ?
C28 C27 P2 114.0(6) . . ?
O4 Na1 O3 110.0(3) . 7 ?
O4 Na1 O3 100.7(3) . 2_655 ?
O3 Na1 O3 109.6(3) 7 2_655 ?
O4 Na1 O1 116.8(2) . 7 ?
O3 Na1 O1 84.5(2) 7 7 ?
O3 Na1 O1 132.8(3) 2_655 7 ?
O4 Na1 C3 129.6(3) . 7 ?
O3 Na1 C3 20.6(2) 7 7 ?
O3 Na1 C3 96.9(2) 2_655 7 ?
O1 Na1 C3 81.18(19) 7 7 ?
O4 Na1 C3 20.2(3) . . ?
O3 Na1 C3 96.1(3) 7 . ?
O3 Na1 C3 92.3(2) 2_655 . ?
O1 Na1 C3 132.0(2) 7 . ?
C3 Na1 C3 113.5(3) 7 . ?
O4 Na1 Na1 72.6(3) . 8_545 ?
O3 Na1 Na1 40.65(16) 7 8_545 ?
O3 Na1 Na1 101.81(17) 2_655 8_545 ?
O1 Na1 Na1 115.56(18) 7 8_545 ?
C3 Na1 Na1 57.60(16) 7 8_545 ?
C3 Na1 Na1 56.1(2) . 8_545 ?
O4 Na1 Na1 119.38(19) . 7 ?
O3 Na1 Na1 69.2(2) 7 7 ?
O3 Na1 Na1 40.63(15) 2_655 7 ?
O1 Na1 Na1 123.10(18) 7 7 ?
C3 Na1 Na1 56.83(18) 7 7 ?
C3 Na1 Na1 101.26(18) . 7 ?
Na1 Na1 Na1 74.72(8) 8_545 7 ?
O4 Na1 Na1 66.91(19) . 2_655 ?
O3 Na1 Na1 82.71(15) 7 2_655 ?
O3 Na1 Na1 54.00(18) 2_655 2_655 ?
O1 Na1 Na1 167.19(15) 7 2_655 ?
C3 Na1 Na1 87.28(14) 7 2_655 ?
C3 Na1 Na1 48.81(17) . 2_655 ?
Na1 Na1 Na1 52.64(4) 8_545 2_655 ?
Na1 Na1 Na1 52.64(4) 7 2_655 ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.094
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_n0375a-1
_database_code_depnum_ccdc_archive 'CCDC 1446706'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            (PNP)Ni(CO)
_chemical_melting_point          ?
_chemical_formula_moiety         'C27 H40 N Ni O P2'
_chemical_formula_sum            'C27 H40 N Ni O P2'
_chemical_formula_weight         515.25

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P21/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                   15.7516(15)
_cell_length_b                   9.8103(9)
_cell_length_c                   18.1748(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.239(3)
_cell_angle_gamma                90.00
_cell_volume                     2796.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    32589
_cell_measurement_theta_min      2.65
_cell_measurement_theta_max      25.57

_exptl_crystal_description       platy
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1100
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8522
_exptl_absorpt_correction_T_max  0.9219
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32589
_diffrn_reflns_av_R_equivalents  0.0787
_diffrn_reflns_av_sigmaI/netI    0.0474
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.65
_diffrn_reflns_theta_max         25.57
_reflns_number_total             5233
_reflns_number_gt                4056
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5233
_refine_ls_number_parameters     299
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0586
_refine_ls_wR_factor_ref         0.1892
_refine_ls_wR_factor_gt          0.1740
_refine_ls_goodness_of_fit_ref   1.331
_refine_ls_restrained_S_all      1.331
_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 0.22708(4) 0.17257(5) 0.18565(3) 0.0280(2) Uani 1 1 d . . .
P1 P 0.31302(6) 0.04153(10) 0.25840(6) 0.0185(3) Uani 1 1 d . . .
P2 P 0.20023(6) 0.35895(10) 0.11787(6) 0.0186(3) Uani 1 1 d . . .
N1 N 0.2360(2) 0.3020(3) 0.26827(19) 0.0203(7) Uani 1 1 d . . .
C9 C 0.1843(2) 0.4192(4) 0.2610(2) 0.0167(8) Uani 1 1 d . . .
C11 C 0.1016(2) 0.5723(4) 0.1764(2) 0.0227(9) Uani 1 1 d . . .
H11 H 0.0857 0.6011 0.1272 0.027 Uiso 1 1 calc R . .
C10 C 0.1581(2) 0.4639(4) 0.1883(2) 0.0190(8) Uani 1 1 d . . .
C4 C 0.4049(2) 0.1375(4) 0.3909(2) 0.0207(9) Uani 1 1 d . . .
H4 H 0.4324 0.0512 0.3945 0.025 Uiso 1 1 calc R . .
C13 C 0.0938(2) 0.5946(4) 0.3052(2) 0.0227(9) Uani 1 1 d . . .
H13 H 0.0720 0.6388 0.3460 0.027 Uiso 1 1 calc R . .
C2 C 0.2983(2) 0.2868(4) 0.3264(2) 0.0176(8) Uani 1 1 d . . .
C14 C 0.1503(2) 0.4873(4) 0.3186(2) 0.0206(9) Uani 1 1 d . . .
H14 H 0.1661 0.4597 0.3680 0.025 Uiso 1 1 calc R . .
C12 C 0.0678(3) 0.6399(4) 0.2342(2) 0.0245(9) Uani 1 1 d . . .
C3 C 0.3419(2) 0.1596(4) 0.3334(2) 0.0179(8) Uani 1 1 d . . .
C6 C 0.3897(3) 0.3633(4) 0.4343(2) 0.0249(9) Uani 1 1 d . . .
H6 H 0.4062 0.4345 0.4680 0.030 Uiso 1 1 calc R . .
C7 C 0.3267(3) 0.3881(4) 0.3772(2) 0.0249(9) Uani 1 1 d . . .
H7 H 0.3022 0.4765 0.3724 0.030 Uiso 1 1 calc R . .
C22 C 0.2927(3) 0.4575(5) 0.0893(2) 0.0287(10) Uani 1 1 d . . .
H22 H 0.3177 0.4052 0.0493 0.034 Uiso 1 1 calc R . .
C5 C 0.4291(2) 0.2361(4) 0.4432(2) 0.0229(9) Uani 1 1 d . . .
C19 C 0.4152(3) -0.0260(4) 0.2303(2) 0.0264(10) Uani 1 1 d . . .
H19 H 0.4488 -0.0645 0.2749 0.032 Uiso 1 1 calc R . .
C25 C 0.1216(3) 0.3638(5) 0.0361(2) 0.0253(9) Uani 1 1 d . . .
H25 H 0.1149 0.4605 0.0191 0.030 Uiso 1 1 calc R . .
C8 C 0.4977(3) 0.2108(5) 0.5056(3) 0.0319(11) Uani 1 1 d . . .
H8A H 0.4712 0.1998 0.5520 0.048 Uiso 1 1 calc R . .
H8B H 0.5370 0.2884 0.5098 0.048 Uiso 1 1 calc R . .
H8C H 0.5292 0.1277 0.4955 0.048 Uiso 1 1 calc R . .
C24 C 0.3605(3) 0.4675(5) 0.1549(3) 0.0368(12) Uani 1 1 d . . .
H24A H 0.4090 0.5206 0.1406 0.055 Uiso 1 1 calc R . .
H24B H 0.3797 0.3757 0.1699 0.055 Uiso 1 1 calc R . .
H24C H 0.3362 0.5125 0.1963 0.055 Uiso 1 1 calc R . .
C15 C 0.0043(3) 0.7539(5) 0.2208(3) 0.0340(11) Uani 1 1 d . . .
H15A H 0.0106 0.7953 0.1725 0.051 Uiso 1 1 calc R . .
H15B H 0.0146 0.8230 0.2595 0.051 Uiso 1 1 calc R . .
H15C H -0.0536 0.7177 0.2215 0.051 Uiso 1 1 calc R . .
C16 C 0.2590(3) -0.1046(4) 0.2975(2) 0.0246(9) Uani 1 1 d . . .
H16 H 0.2388 -0.1656 0.2554 0.029 Uiso 1 1 calc R . .
C27 C 0.0345(3) 0.3107(5) 0.0542(3) 0.0370(12) Uani 1 1 d . . .
H27A H -0.0040 0.3056 0.0087 0.056 Uiso 1 1 calc R . .
H27B H 0.0105 0.3728 0.0891 0.056 Uiso 1 1 calc R . .
H27C H 0.0411 0.2198 0.0763 0.056 Uiso 1 1 calc R . .
C18 C 0.3149(3) -0.1908(5) 0.3529(3) 0.0390(12) Uani 1 1 d . . .
H18A H 0.3348 -0.1347 0.3956 0.059 Uiso 1 1 calc R . .
H18B H 0.3641 -0.2254 0.3293 0.059 Uiso 1 1 calc R . .
H18C H 0.2816 -0.2677 0.3693 0.059 Uiso 1 1 calc R . .
C23 C 0.2673(3) 0.5982(5) 0.0588(3) 0.0397(12) Uani 1 1 d . . .
H23A H 0.2421 0.6513 0.0969 0.060 Uiso 1 1 calc R . .
H23B H 0.2257 0.5880 0.0157 0.060 Uiso 1 1 calc R . .
H23C H 0.3180 0.6454 0.0441 0.060 Uiso 1 1 calc R . .
C17 C 0.1802(3) -0.0537(5) 0.3319(3) 0.0349(11) Uani 1 1 d . . .
H17A H 0.1501 -0.1312 0.3515 0.052 Uiso 1 1 calc R . .
H17B H 0.1423 -0.0070 0.2943 0.052 Uiso 1 1 calc R . .
H17C H 0.1974 0.0099 0.3721 0.052 Uiso 1 1 calc R . .
C26 C 0.1553(3) 0.2800(5) -0.0258(2) 0.0388(12) Uani 1 1 d . . .
H26A H 0.1546 0.1831 -0.0128 0.058 Uiso 1 1 calc R . .
H26B H 0.2138 0.3081 -0.0324 0.058 Uiso 1 1 calc R . .
H26C H 0.1191 0.2951 -0.0718 0.058 Uiso 1 1 calc R . .
C20 C 0.3988(3) -0.1385(5) 0.1736(3) 0.0431(13) Uani 1 1 d . . .
H20A H 0.3698 -0.1005 0.1282 0.065 Uiso 1 1 calc R . .
H20B H 0.3627 -0.2087 0.1932 0.065 Uiso 1 1 calc R . .
H20C H 0.4531 -0.1790 0.1628 0.065 Uiso 1 1 calc R . .
C21 C 0.4662(3) 0.0896(5) 0.1995(3) 0.0406(12) Uani 1 1 d . . .
H21A H 0.5220 0.0551 0.1882 0.061 Uiso 1 1 calc R . .
H21B H 0.4742 0.1628 0.2361 0.061 Uiso 1 1 calc R . .
H21C H 0.4353 0.1250 0.1543 0.061 Uiso 1 1 calc R . .
C1 C 0.1678(5) 0.0399(6) 0.1337(4) 0.0627(18) Uani 1 1 d . . .
O1 O 0.1410(4) -0.0476(5) 0.0996(3) 0.0858(16) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C1 1.815(7) . ?
Ni1 N1 1.962(3) . ?
Ni1 P1 2.2151(11) . ?
Ni1 P2 2.2236(12) . ?
P1 C3 1.815(4) . ?
P1 C16 1.842(4) . ?
P1 C19 1.854(4) . ?
P2 C10 1.815(4) . ?
P2 C25 1.846(4) . ?
P2 C22 1.861(4) . ?
N1 C2 1.384(5) . ?
N1 C9 1.408(5) . ?
C9 C14 1.389(5) . ?
C9 C10 1.416(5) . ?
C11 C12 1.389(6) . ?
C11 C10 1.391(5) . ?
C4 C5 1.385(6) . ?
C4 C3 1.391(5) . ?
C13 C14 1.385(6) . ?
C13 C12 1.391(6) . ?
C2 C7 1.401(6) . ?
C2 C3 1.425(5) . ?
C12 C15 1.505(6) . ?
C6 C7 1.390(6) . ?
C6 C5 1.398(6) . ?
C22 C23 1.527(6) . ?
C22 C24 1.529(6) . ?
C5 C8 1.514(6) . ?
C19 C20 1.516(6) . ?
C19 C21 1.526(6) . ?
C25 C26 1.526(6) . ?
C25 C27 1.531(6) . ?
C16 C17 1.525(6) . ?
C16 C18 1.531(6) . ?
C1 O1 1.119(7) . ?

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
C1 Ni1 N1 149.3(3) . . ?
C1 Ni1 P1 98.72(19) . . ?
N1 Ni1 P1 85.50(10) . . ?
C1 Ni1 P2 103.80(18) . . ?
N1 Ni1 P2 83.61(10) . . ?
P1 Ni1 P2 152.00(5) . . ?
C3 P1 C16 107.43(19) . . ?
C3 P1 C19 105.66(19) . . ?
C16 P1 C19 105.73(19) . . ?
C3 P1 Ni1 100.13(13) . . ?
C16 P1 Ni1 113.79(13) . . ?
C19 P1 Ni1 122.78(15) . . ?
C10 P2 C25 106.95(19) . . ?
C10 P2 C22 104.36(19) . . ?
C25 P2 C22 104.3(2) . . ?
C10 P2 Ni1 97.98(13) . . ?
C25 P2 Ni1 123.15(15) . . ?
C22 P2 Ni1 117.86(15) . . ?
C2 N1 C9 121.6(3) . . ?
C2 N1 Ni1 120.8(3) . . ?
C9 N1 Ni1 117.1(3) . . ?
C14 C9 N1 125.5(4) . . ?
C14 C9 C10 117.0(4) . . ?
N1 C9 C10 117.2(3) . . ?
C12 C11 C10 122.1(4) . . ?
C11 C10 C9 120.6(4) . . ?
C11 C10 P2 126.5(3) . . ?
C9 C10 P2 112.8(3) . . ?
C5 C4 C3 122.7(4) . . ?
C14 C13 C12 122.4(4) . . ?
N1 C2 C7 126.0(4) . . ?
N1 C2 C3 117.7(3) . . ?
C7 C2 C3 116.1(4) . . ?
C13 C14 C9 121.3(4) . . ?
C11 C12 C13 116.6(4) . . ?
C11 C12 C15 121.8(4) . . ?
C13 C12 C15 121.6(4) . . ?
C4 C3 C2 120.6(4) . . ?
C4 C3 P1 125.3(3) . . ?
C2 C3 P1 114.0(3) . . ?
C7 C6 C5 121.5(4) . . ?
C6 C7 C2 122.1(4) . . ?
C23 C22 C24 111.5(4) . . ?
C23 C22 P2 112.7(3) . . ?
C24 C22 P2 108.9(3) . . ?
C4 C5 C6 116.9(4) . . ?
C4 C5 C8 122.2(4) . . ?
C6 C5 C8 120.8(4) . . ?
C20 C19 C21 110.7(4) . . ?
C20 C19 P1 110.4(3) . . ?
C21 C19 P1 109.6(3) . . ?
C26 C25 C27 110.7(4) . . ?
C26 C25 P2 109.0(3) . . ?
C27 C25 P2 111.5(3) . . ?
C17 C16 C18 110.6(4) . . ?
C17 C16 P1 109.0(3) . . ?
C18 C16 P1 115.2(3) . . ?
O1 C1 Ni1 171.3(7) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.57
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         1.706
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.112
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_0063a-2
_database_code_depnum_ccdc_archive 'CCDC 1446707'
_audit_update_record             
;
2016-01-12 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            {(PNP)NiCOONa}2(THF)
_chemical_melting_point          ?
_chemical_formula_moiety         'C35 H56 N Na Ni O4 P2'
_chemical_formula_sum            'C35 H56 N Na Ni O4 P2'
_chemical_formula_weight         698.45

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

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

_cell_length_a                   10.9465(3)
_cell_length_b                   12.3880(3)
_cell_length_c                   14.3038(4)
_cell_angle_alpha                101.8930(10)
_cell_angle_beta                 96.7630(10)
_cell_angle_gamma                96.9260(10)
_cell_volume                     1863.77(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    34833
_cell_measurement_theta_min      0.8970
_cell_measurement_theta_max      0.9140

_exptl_crystal_description       platy
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             748
_exptl_absorpt_coefficient_mu    0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8970
_exptl_absorpt_correction_T_max  0.9140
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34833
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         35.82
_reflns_number_total             16891
_reflns_number_gt                13256
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 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)+(0.0522P)²+0.2475P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         16891
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.1028
_refine_ls_wR_factor_gt          0.0906
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.991850(11) 0.785217(12) 0.705696(9) 0.01474(4) Uani 1 1 d . . .
P1 P 0.80285(2) 0.80331(2) 0.726066(19) 0.01489(5) Uani 1 1 d . . .
P2 P 1.18350(2) 0.76154(2) 0.708612(19) 0.01541(5) Uani 1 1 d . . .
Na1 Na 0.98310(5) 1.11242(4) 0.58231(3) 0.02119(9) Uani 1 1 d . . .
N1 N 0.99645(8) 0.71840(8) 0.81876(7) 0.01777(16) Uani 1 1 d . . .
O2 O 1.00352(9) 0.93877(8) 0.59124(6) 0.02496(17) Uani 1 1 d . . .
O1 O 0.97057(9) 0.75942(8) 0.51370(6) 0.02453(17) Uani 1 1 d . . .
C2 C 0.88541(9) 0.66754(9) 0.83820(7) 0.01651(17) Uani 1 1 d . . .
C15 C 1.11005(9) 0.72348(9) 0.87490(7) 0.01655(17) Uani 1 1 d . . .
C3 C 0.77416(9) 0.69977(9) 0.79733(7) 0.01628(17) Uani 1 1 d . . .
O3 O 1.10787(10) 1.19883(9) 0.72455(7) 0.0321(2) Uani 1 1 d . . .
C9 C 0.78807(10) 0.93887(9) 0.80505(8) 0.01916(18) Uani 1 1 d . . .
H9A H 0.8109 0.9985 0.7699 0.023 Uiso 1 1 calc R . .
C16 C 1.21829(9) 0.74497(9) 0.83190(7) 0.01726(18) Uani 1 1 d . . .
C22 C 1.19935(10) 0.62909(10) 0.62698(8) 0.0207(2) Uani 1 1 d . . .
H22A H 1.1868 0.6406 0.5596 0.025 Uiso 1 1 calc R . .
C4 C 0.65791(10) 0.64942(9) 0.80953(8) 0.01919(18) Uani 1 1 d . . .
H4A H 0.5852 0.6732 0.7823 0.023 Uiso 1 1 calc R . .
O4 O 0.81781(9) 1.20376(8) 0.65160(8) 0.0325(2) Uani 1 1 d . . .
C5 C 0.64550(11) 0.56508(10) 0.86061(8) 0.02084(19) Uani 1 1 d . . .
C7 C 0.87201(11) 0.58170(10) 0.88899(8) 0.01989(19) Uani 1 1 d . . .
H7A H 0.9439 0.5569 0.9163 0.024 Uiso 1 1 calc R . .
C20 C 1.12855(11) 0.71950(10) 0.97358(8) 0.02055(19) Uani 1 1 d . . .
H20A H 1.0588 0.7040 1.0049 0.025 Uiso 1 1 calc R . .
C1 C 0.98760(10) 0.83503(9) 0.58981(8) 0.01810(18) Uani 1 1 d . . .
C17 C 1.33666(10) 0.76141(10) 0.88542(8) 0.0206(2) Uani 1 1 d . . .
H17A H 1.4074 0.7745 0.8544 0.025 Uiso 1 1 calc R . .
C12 C 0.66970(10) 0.77381(10) 0.62809(8) 0.01986(19) Uani 1 1 d . . .
H12A H 0.5912 0.7721 0.6575 0.024 Uiso 1 1 calc R . .
C18 C 1.35419(11) 0.75922(10) 0.98336(8) 0.0226(2) Uani 1 1 d . . .
C6 C 0.75447(11) 0.53285(9) 0.89963(8) 0.0214(2) Uani 1 1 d . . .
H6A H 0.7484 0.4756 0.9347 0.026 Uiso 1 1 calc R . .
C25 C 1.31291(10) 0.86512(10) 0.69568(8) 0.02032(19) Uani 1 1 d . . .
H25A H 1.3927 0.8418 0.7202 0.024 Uiso 1 1 calc R . .
C19 C 1.24801(11) 0.73807(10) 1.02530(8) 0.0226(2) Uani 1 1 d . . .
H19A H 1.2573 0.7362 1.0918 0.027 Uiso 1 1 calc R . .
C23 C 1.09515(12) 0.53785(11) 0.63383(10) 0.0290(2) Uani 1 1 d . . .
H23A H 1.1035 0.4676 0.5905 0.043 Uiso 1 1 calc R . .
H23B H 1.0143 0.5596 0.6150 0.043 Uiso 1 1 calc R . .
H23C H 1.1010 0.5280 0.7004 0.043 Uiso 1 1 calc R . .
C35 C 1.07134(12) 1.16756(12) 0.80984(9) 0.0273(2) Uani 1 1 d . . .
H35A H 1.0631 1.0857 0.8025 0.033 Uiso 1 1 calc R . .
H35B H 0.9907 1.1919 0.8224 0.033 Uiso 1 1 calc R . .
C8 C 0.51898(12) 0.50677(11) 0.86857(10) 0.0278(2) Uani 1 1 d . . .
H8A H 0.5290 0.4504 0.9068 0.042 Uiso 1 1 calc R . .
H8B H 0.4752 0.4705 0.8038 0.042 Uiso 1 1 calc R . .
H8C H 0.4707 0.5615 0.9002 0.042 Uiso 1 1 calc R . .
C14 C 0.67410(12) 0.86491(12) 0.56958(10) 0.0290(3) Uani 1 1 d . . .
H14A H 0.6025 0.8474 0.5181 0.044 Uiso 1 1 calc R . .
H14B H 0.7512 0.8683 0.5410 0.044 Uiso 1 1 calc R . .
H14C H 0.6714 0.9372 0.6123 0.044 Uiso 1 1 calc R . .
C13 C 0.66922(12) 0.65925(11) 0.56203(9) 0.0282(2) Uani 1 1 d . . .
H13A H 0.5984 0.6440 0.5101 0.042 Uiso 1 1 calc R . .
H13B H 0.6622 0.6016 0.5997 0.042 Uiso 1 1 calc R . .
H13C H 0.7468 0.6589 0.5341 0.042 Uiso 1 1 calc R . .
C11 C 0.88206(12) 0.96102(11) 0.89766(9) 0.0262(2) Uani 1 1 d . . .
H11A H 0.8742 1.0326 0.9392 0.039 Uiso 1 1 calc R . .
H11B H 0.9665 0.9635 0.8811 0.039 Uiso 1 1 calc R . .
H11C H 0.8656 0.9012 0.9319 0.039 Uiso 1 1 calc R . .
C34 C 1.17387(12) 1.22609(12) 0.89148(9) 0.0289(3) Uani 1 1 d . . .
H34A H 1.1417 1.2430 0.9539 0.035 Uiso 1 1 calc R . .
H34B H 1.2420 1.1810 0.8973 0.035 Uiso 1 1 calc R . .
C28 C 0.69129(14) 1.18481(12) 0.66775(10) 0.0302(3) Uani 1 1 d . . .
H28A H 0.6856 1.1492 0.7233 0.036 Uiso 1 1 calc R . .
H28B H 0.6396 1.1349 0.6100 0.036 Uiso 1 1 calc R . .
C21 C 1.48308(12) 0.78315(13) 1.04101(10) 0.0311(3) Uani 1 1 d . . .
H21A H 1.4773 0.7778 1.1078 0.047 Uiso 1 1 calc R . .
H21B H 1.5217 0.8585 1.0402 0.047 Uiso 1 1 calc R . .
H21C H 1.5337 0.7287 1.0124 0.047 Uiso 1 1 calc R . .
C24 C 1.32708(12) 0.59285(13) 0.64362(11) 0.0346(3) Uani 1 1 d . . .
H24A H 1.3287 0.5224 0.5980 0.052 Uiso 1 1 calc R . .
H24B H 1.3436 0.5826 0.7098 0.052 Uiso 1 1 calc R . .
H24C H 1.3910 0.6503 0.6337 0.052 Uiso 1 1 calc R . .
C26 C 1.30342(13) 0.97896(11) 0.75807(10) 0.0300(3) Uani 1 1 d . . .
H26A H 1.3721 1.0340 0.7512 0.045 Uiso 1 1 calc R . .
H26B H 1.3081 0.9740 0.8259 0.045 Uiso 1 1 calc R . .
H26C H 1.2240 1.0020 0.7372 0.045 Uiso 1 1 calc R . .
C30 C 0.74173(16) 1.37360(12) 0.65280(10) 0.0345(3) Uani 1 1 d . . .
H30A H 0.7190 1.3719 0.5834 0.041 Uiso 1 1 calc R . .
H30B H 0.7513 1.4515 0.6904 0.041 Uiso 1 1 calc R . .
C27 C 1.31594(13) 0.87224(13) 0.59069(10) 0.0316(3) Uani 1 1 d . . .
H27A H 1.3859 0.9280 0.5873 0.047 Uiso 1 1 calc R . .
H27B H 1.2379 0.8939 0.5649 0.047 Uiso 1 1 calc R . .
H27C H 1.3260 0.7993 0.5525 0.047 Uiso 1 1 calc R . .
C29 C 0.64590(15) 1.29727(13) 0.68827(12) 0.0356(3) Uani 1 1 d . . .
H29A H 0.6439 1.3239 0.7582 0.043 Uiso 1 1 calc R . .
H29B H 0.5617 1.2931 0.6525 0.043 Uiso 1 1 calc R . .
C10 C 0.65703(12) 0.94862(12) 0.82947(11) 0.0312(3) Uani 1 1 d . . .
H10A H 0.6568 1.0221 0.8711 0.047 Uiso 1 1 calc R . .
H10B H 0.6312 0.8904 0.8632 0.047 Uiso 1 1 calc R . .
H10C H 0.5991 0.9397 0.7698 0.047 Uiso 1 1 calc R . .
C32 C 1.21021(15) 1.28852(13) 0.75146(11) 0.0362(3) Uani 1 1 d . . .
H32A H 1.1958 1.3481 0.7165 0.043 Uiso 1 1 calc R . .
H32B H 1.2887 1.2613 0.7365 0.043 Uiso 1 1 calc R . .
C33 C 1.21627(15) 1.33165(13) 0.85916(11) 0.0369(3) Uani 1 1 d . . .
H33A H 1.1596 1.3875 0.8735 0.044 Uiso 1 1 calc R . .
H33B H 1.3020 1.3650 0.8901 0.044 Uiso 1 1 calc R . .
C31 C 0.85824(15) 1.32245(12) 0.67061(13) 0.0379(3) Uani 1 1 d . . .
H31A H 0.9176 1.3402 0.6268 0.045 Uiso 1 1 calc R . .
H31B H 0.8993 1.3508 0.7382 0.045 Uiso 1 1 calc R . .


_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 C1 1.8818(11) . ?
Ni1 N1 1.9611(9) . ?
Ni1 P2 2.1499(3) . ?
Ni1 P1 2.1546(3) . ?
P1 C3 1.8166(11) . ?
P1 C12 1.8443(10) . ?
P1 C9 1.8572(12) . ?
P2 C16 1.8185(11) . ?
P2 C25 1.8462(11) . ?
P2 C22 1.8473(12) . ?
Na1 O2 2.2173(10) . ?
Na1 O3 2.2905(10) . ?
Na1 O1 2.3521(10) 2_776 ?
Na1 O4 2.4475(11) . ?
Na1 O2 2.4587(10) 2_776 ?
Na1 C1 2.7173(12) 2_776 ?
Na1 Na1 3.3451(10) 2_776 ?
N1 C2 1.3852(14) . ?
N1 C15 1.3857(13) . ?
O2 C1 1.2714(14) . ?
O2 Na1 2.4586(10) 2_776 ?
O1 C1 1.2597(14) . ?
O1 Na1 2.3520(10) 2_776 ?
C2 C7 1.4092(15) . ?
C2 C3 1.4248(14) . ?
C15 C20 1.4142(15) . ?
C15 C16 1.4199(15) . ?
C3 C4 1.3944(15) . ?
O3 C32 1.4351(17) . ?
O3 C35 1.4390(16) . ?
C9 C10 1.5286(16) . ?
C9 C11 1.5329(16) . ?
C16 C17 1.3945(14) . ?
C22 C24 1.5265(17) . ?
C22 C23 1.5326(17) . ?
C4 C5 1.3956(16) . ?
O4 C28 1.4304(18) . ?
O4 C31 1.4428(18) . ?
C5 C6 1.3942(17) . ?
C5 C8 1.5108(16) . ?
C7 C6 1.3933(16) . ?
C20 C19 1.3927(15) . ?
C1 Na1 2.7173(12) 2_776 ?
C17 C18 1.3977(16) . ?
C12 C13 1.5334(17) . ?
C12 C14 1.5370(17) . ?
C18 C19 1.3912(18) . ?
C18 C21 1.5109(15) . ?
C25 C27 1.5264(17) . ?
C25 C26 1.5278(18) . ?
C35 C34 1.5149(17) . ?
C34 C33 1.514(2) . ?
C28 C29 1.519(2) . ?
C30 C31 1.509(2) . ?
C30 C29 1.528(2) . ?
C32 C33 1.514(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
C1 Ni1 N1 174.30(5) . . ?
C1 Ni1 P2 92.85(3) . . ?
N1 Ni1 P2 85.48(3) . . ?
C1 Ni1 P1 96.46(3) . . ?
N1 Ni1 P1 85.37(3) . . ?
P2 Ni1 P1 170.606(12) . . ?
C3 P1 C12 105.79(5) . . ?
C3 P1 C9 105.58(5) . . ?
C12 P1 C9 105.85(5) . . ?
C3 P1 Ni1 99.36(3) . . ?
C12 P1 Ni1 124.82(4) . . ?
C9 P1 Ni1 113.44(3) . . ?
C16 P2 C25 104.39(5) . . ?
C16 P2 C22 107.55(5) . . ?
C25 P2 C22 106.10(5) . . ?
C16 P2 Ni1 99.85(3) . . ?
C25 P2 Ni1 125.94(4) . . ?
C22 P2 Ni1 111.40(4) . . ?
O2 Na1 O3 96.93(4) . . ?
O2 Na1 O1 140.27(4) . 2_776 ?
O3 Na1 O1 100.61(4) . 2_776 ?
O2 Na1 O4 121.07(4) . . ?
O3 Na1 O4 86.06(4) . . ?
O1 Na1 O4 95.59(4) 2_776 . ?
O2 Na1 O2 88.80(3) . 2_776 ?
O3 Na1 O2 139.25(4) . 2_776 ?
O1 Na1 O2 55.30(3) 2_776 2_776 ?
O4 Na1 O2 124.85(4) . 2_776 ?
O2 Na1 C1 115.84(4) . 2_776 ?
O3 Na1 C1 123.48(4) . 2_776 ?
O1 Na1 C1 27.59(3) 2_776 2_776 ?
O4 Na1 C1 110.29(4) . 2_776 ?
O2 Na1 C1 27.87(3) 2_776 2_776 ?
O2 Na1 Na1 47.29(3) . 2_776 ?
O3 Na1 Na1 129.55(4) . 2_776 ?
O1 Na1 Na1 95.24(3) 2_776 2_776 ?
O4 Na1 Na1 139.65(4) . 2_776 ?
O2 Na1 Na1 41.51(2) 2_776 2_776 ?
C1 Na1 Na1 68.85(3) 2_776 2_776 ?
C2 N1 C15 123.14(9) . . ?
C2 N1 Ni1 118.11(7) . . ?
C15 N1 Ni1 118.75(7) . . ?
C1 O2 Na1 166.41(8) . . ?
C1 O2 Na1 87.45(7) . 2_776 ?
Na1 O2 Na1 91.20(3) . 2_776 ?
C1 O1 Na1 92.56(7) . 2_776 ?
N1 C2 C7 125.99(9) . . ?
N1 C2 C3 116.79(9) . . ?
C7 C2 C3 117.07(10) . . ?
N1 C15 C20 126.01(10) . . ?
N1 C15 C16 116.88(9) . . ?
C20 C15 C16 116.84(9) . . ?
C4 C3 C2 120.76(10) . . ?
C4 C3 P1 126.13(8) . . ?
C2 C3 P1 113.03(8) . . ?
C32 O3 C35 109.64(10) . . ?
C32 O3 Na1 134.25(9) . . ?
C35 O3 Na1 115.71(7) . . ?
C10 C9 C11 110.45(11) . . ?
C10 C9 P1 114.36(8) . . ?
C11 C9 P1 109.58(8) . . ?
C17 C16 C15 120.97(10) . . ?
C17 C16 P2 125.68(9) . . ?
C15 C16 P2 113.08(7) . . ?
C24 C22 C23 111.43(11) . . ?
C24 C22 P2 114.01(8) . . ?
C23 C22 P2 109.45(8) . . ?
C3 C4 C5 121.80(10) . . ?
C28 O4 C31 108.70(11) . . ?
C28 O4 Na1 143.44(8) . . ?
C31 O4 Na1 107.05(9) . . ?
C6 C5 C4 117.32(10) . . ?
C6 C5 C8 121.34(11) . . ?
C4 C5 C8 121.26(11) . . ?
C6 C7 C2 120.75(10) . . ?
C19 C20 C15 120.70(11) . . ?
O1 C1 O2 123.97(10) . . ?
O1 C1 Ni1 115.48(8) . . ?
O2 C1 Ni1 120.54(8) . . ?
O1 C1 Na1 59.85(6) . 2_776 ?
O2 C1 Na1 64.68(6) . 2_776 ?
Ni1 C1 Na1 169.77(6) . 2_776 ?
C16 C17 C18 121.88(11) . . ?
C13 C12 C14 110.42(11) . . ?
C13 C12 P1 109.77(8) . . ?
C14 C12 P1 111.05(8) . . ?
C19 C18 C17 117.04(10) . . ?
C19 C18 C21 122.06(11) . . ?
C17 C18 C21 120.87(12) . . ?
C7 C6 C5 122.29(10) . . ?
C27 C25 C26 110.73(11) . . ?
C27 C25 P2 112.30(8) . . ?
C26 C25 P2 109.45(8) . . ?
C18 C19 C20 122.55(10) . . ?
O3 C35 C34 105.62(10) . . ?
C33 C34 C35 101.65(11) . . ?
O4 C28 C29 107.60(12) . . ?
C31 C30 C29 101.83(12) . . ?
C28 C29 C30 103.71(12) . . ?
O3 C32 C33 105.45(12) . . ?
C32 C33 C34 101.78(12) . . ?
O4 C31 C30 105.62(12) . . ?

_diffrn_measured_fraction_theta_max 0.968
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.073
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_n0423a-2
_database_code_depnum_ccdc_archive 'CCDC 1453323'
_audit_update_record             
;
2016-02-15 deposited with the CCDC.
2016-03-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            {(PNP)Ni}2(CO3)
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H80 N2 Ni2 O3 P4'
_chemical_formula_sum            'C53 H80 N2 Ni2 O3 P4'
_chemical_formula_weight         1034.49

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   Cc

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

_cell_length_a                   12.8027(9)
_cell_length_b                   24.6644(18)
_cell_length_c                   17.9274(13)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.769(2)
_cell_angle_gamma                90.00
_cell_volume                     5447.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    21218
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      28.35

_exptl_crystal_description       platy
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2208
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7383
_exptl_absorpt_correction_T_max  0.9274
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21218
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.62
_diffrn_reflns_theta_max         28.35
_reflns_number_total             10634
_reflns_number_gt                8843
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_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)+(0.0227P)²+83.9632P] where P=(Fo²+2Fc²)/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   0.00(2)
_refine_ls_number_reflns         10634
_refine_ls_number_parameters     592
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.1087
_refine_ls_R_factor_gt           0.0824
_refine_ls_wR_factor_ref         0.2084
_refine_ls_wR_factor_gt          0.1897
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_restrained_S_all      1.183
_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
Ni1 Ni 0.64759(9) 0.51147(4) 0.65989(6) 0.0285(2) Uani 1 1 d . . .
P1 P 0.6963(2) 0.59309(9) 0.70694(14) 0.0306(5) Uani 1 1 d . . .
P2 P 0.63461(19) 0.42666(9) 0.62229(12) 0.0265(4) Uani 1 1 d . . .
N1 N 0.7576(7) 0.4861(3) 0.7449(4) 0.0314(17) Uani 1 1 d . . .
C2 C 0.8446(8) 0.5204(4) 0.7826(5) 0.035(2) Uani 1 1 d . . .
C3 C 0.8266(7) 0.5764(4) 0.7737(5) 0.0301(18) Uani 1 1 d . . .
C4 C 0.9091(8) 0.6122(4) 0.8104(5) 0.034(2) Uani 1 1 d . . .
H4A H 0.8958 0.6501 0.8055 0.041 Uiso 1 1 calc R . .
C5 C 1.0093(8) 0.5941(4) 0.8536(5) 0.036(2) Uani 1 1 d . . .
C6 C 1.0258(8) 0.5390(4) 0.8570(5) 0.036(2) Uani 1 1 d . . .
H6A H 1.0954 0.5259 0.8846 0.043 Uiso 1 1 calc R . .
C7 C 0.9474(8) 0.5016(4) 0.8227(5) 0.036(2) Uani 1 1 d . . .
H7A H 0.9630 0.4638 0.8262 0.043 Uiso 1 1 calc R . .
C8 C 1.0957(9) 0.6330(5) 0.8954(6) 0.046(3) Uani 1 1 d . . .
H8A H 1.0982 0.6338 0.9505 0.069 Uiso 1 1 calc R . .
H8B H 1.0792 0.6693 0.8733 0.069 Uiso 1 1 calc R . .
H8C H 1.1662 0.6212 0.8896 0.069 Uiso 1 1 calc R . .
C9 C 0.7527(7) 0.4327(3) 0.7678(4) 0.0263(17) Uani 1 1 d . . .
C10 C 0.6976(7) 0.3939(3) 0.7133(5) 0.0257(16) Uani 1 1 d . . .
C11 C 0.6868(7) 0.3409(3) 0.7337(5) 0.0289(18) Uani 1 1 d . . .
H11A H 0.6502 0.3159 0.6951 0.035 Uiso 1 1 calc R . .
C12 C 0.7282(7) 0.3229(3) 0.8099(5) 0.0296(18) Uani 1 1 d . . .
C13 C 0.7804(7) 0.3610(3) 0.8650(5) 0.0283(18) Uani 1 1 d . . .
H13A H 0.8083 0.3497 0.9173 0.034 Uiso 1 1 calc R . .
C14 C 0.7930(8) 0.4142(4) 0.8464(5) 0.0325(19) Uani 1 1 d . . .
H14A H 0.8285 0.4389 0.8858 0.039 Uiso 1 1 calc R . .
C15 C 0.7199(9) 0.2643(4) 0.8314(6) 0.039(2) Uani 1 1 d . . .
H15A H 0.7540 0.2595 0.8869 0.058 Uiso 1 1 calc R . .
H15B H 0.7569 0.2415 0.8017 0.058 Uiso 1 1 calc R . .
H15C H 0.6433 0.2538 0.8194 0.058 Uiso 1 1 calc R . .
C16 C 0.6688(11) 0.6765(6) 0.8083(8) 0.078(5) Uani 1 1 d . . .
H16A H 0.6209 0.6923 0.8369 0.117 Uiso 1 1 calc R . .
H16B H 0.6830 0.7034 0.7720 0.117 Uiso 1 1 calc R . .
H16C H 0.7375 0.6657 0.8449 0.117 Uiso 1 1 calc R . .
C17 C 0.6143(9) 0.6270(5) 0.7636(7) 0.051(3) Uani 1 1 d . . .
H17A H 0.5469 0.6402 0.7253 0.061 Uiso 1 1 calc R . .
C18 C 0.5789(13) 0.5854(7) 0.8127(8) 0.081(5) Uani 1 1 d . . .
H18A H 0.5351 0.6030 0.8429 0.122 Uiso 1 1 calc R . .
H18B H 0.6429 0.5687 0.8479 0.122 Uiso 1 1 calc R . .
H18C H 0.5355 0.5575 0.7793 0.122 Uiso 1 1 calc R . .
C19 C 0.7817(13) 0.6137(6) 0.5878(8) 0.076(5) Uani 1 1 d . . .
H19A H 0.8012 0.6399 0.5527 0.114 Uiso 1 1 calc R . .
H19B H 0.7294 0.5876 0.5575 0.114 Uiso 1 1 calc R . .
H19C H 0.8470 0.5945 0.6170 0.114 Uiso 1 1 calc R . .
C20 C 0.7320(9) 0.6429(4) 0.6428(6) 0.045(3) Uani 1 1 d . . .
H20A H 0.7888 0.6673 0.6754 0.054 Uiso 1 1 calc R . .
C21 C 0.6369(15) 0.6786(8) 0.5990(11) 0.120(8) Uani 1 1 d . . .
H21A H 0.6622 0.7042 0.5658 0.180 Uiso 1 1 calc R . .
H21B H 0.6083 0.6988 0.6362 0.180 Uiso 1 1 calc R . .
H21C H 0.5795 0.6557 0.5669 0.180 Uiso 1 1 calc R . .
C22 C 0.7188(9) 0.3484(4) 0.5399(6) 0.044(2) Uani 1 1 d . . .
H22A H 0.7608 0.3418 0.5025 0.066 Uiso 1 1 calc R . .
H22B H 0.6454 0.3337 0.5195 0.066 Uiso 1 1 calc R . .
H22C H 0.7544 0.3305 0.5890 0.066 Uiso 1 1 calc R . .
C23 C 0.7123(8) 0.4093(4) 0.5532(6) 0.038(2) Uani 1 1 d . . .
H23A H 0.6735 0.4258 0.5023 0.046 Uiso 1 1 calc R . .
C24 C 0.8237(9) 0.4356(5) 0.5787(8) 0.053(3) Uani 1 1 d . . .
H24A H 0.8650 0.4265 0.5417 0.080 Uiso 1 1 calc R . .
H24B H 0.8625 0.4222 0.6302 0.080 Uiso 1 1 calc R . .
H24C H 0.8155 0.4750 0.5806 0.080 Uiso 1 1 calc R . .
C25 C 0.4316(9) 0.4092(4) 0.6409(6) 0.040(2) Uani 1 1 d . . .
H25A H 0.3603 0.3920 0.6217 0.060 Uiso 1 1 calc R . .
H25B H 0.4227 0.4486 0.6424 0.060 Uiso 1 1 calc R . .
H25C H 0.4669 0.3958 0.6932 0.060 Uiso 1 1 calc R . .
C26 C 0.5026(7) 0.3951(4) 0.5864(5) 0.0266(17) Uani 1 1 d . . .
H26A H 0.5129 0.3549 0.5869 0.032 Uiso 1 1 calc R . .
C27 C 0.4447(9) 0.4127(4) 0.5022(5) 0.042(2) Uani 1 1 d . . .
H27A H 0.3739 0.3947 0.4852 0.063 Uiso 1 1 calc R . .
H27B H 0.4892 0.4024 0.4678 0.063 Uiso 1 1 calc R . .
H27C H 0.4343 0.4521 0.5004 0.063 Uiso 1 1 calc R . .
C28 C 0.1199(7) 0.6618(3) 0.3560(5) 0.0268(17) Uani 1 1 d . A .
Ni2 Ni 0.26566(10) 0.61243(5) 0.48703(6) 0.0353(3) Uani 1 1 d . . .
P3 P 0.32658(18) 0.62994(9) 0.38733(12) 0.0281(5) Uani 1 1 d . A .
P4 P 0.1949(3) 0.61183(10) 0.58619(14) 0.0403(7) Uani 1 1 d . A .
N2 N 0.1459(6) 0.6559(3) 0.4372(4) 0.0285(15) Uani 1 1 d . A .
C29 C 0.2019(7) 0.6504(3) 0.3193(4) 0.0259(17) Uani 1 1 d . . .
C30 C 0.1840(8) 0.6537(4) 0.2396(5) 0.033(2) Uani 1 1 d . A .
H30A H 0.2422 0.6470 0.2174 0.039 Uiso 1 1 calc R . .
C31 C 0.0826(8) 0.6666(4) 0.1921(5) 0.034(2) Uani 1 1 d . . .
C32 C 0.0004(9) 0.6752(4) 0.2267(6) 0.041(2) Uani 1 1 d . A .
H32A H -0.0703 0.6830 0.1947 0.050 Uiso 1 1 calc R . .
C33 C 0.0159(7) 0.6730(4) 0.3053(5) 0.0313(19) Uani 1 1 d . . .
H33A H -0.0437 0.6791 0.3262 0.038 Uiso 1 1 calc R A .
C34 C 0.0604(10) 0.6687(5) 0.1050(5) 0.051(3) Uani 1 1 d . A .
H34A H 0.1282 0.6628 0.0908 0.077 Uiso 1 1 calc R . .
H34B H 0.0306 0.7043 0.0862 0.077 Uiso 1 1 calc R . .
H34C H 0.0081 0.6404 0.0816 0.077 Uiso 1 1 calc R . .
C35 C 0.0859(7) 0.6831(4) 0.4788(5) 0.0307(19) Uani 1 1 d . . .
C36 C 0.0955(8) 0.6643(4) 0.5554(5) 0.034(2) Uani 1 1 d . A .
C37 C 0.0346(9) 0.6892(4) 0.6007(6) 0.042(2) Uani 1 1 d . . .
H37A H 0.0391 0.6750 0.6507 0.050 Uiso 1 1 calc R A .
C38 C -0.0311(8) 0.7333(4) 0.5749(6) 0.041(2) Uani 1 1 d . A .
C39 C -0.0358(8) 0.7525(4) 0.5005(6) 0.041(2) Uani 1 1 d . . .
H39A H -0.0806 0.7829 0.4811 0.049 Uiso 1 1 calc R A .
C40 C 0.0216(8) 0.7292(4) 0.4545(6) 0.0335(19) Uani 1 1 d . A .
H40A H 0.0178 0.7446 0.4053 0.040 Uiso 1 1 calc R . .
C41 C -0.0957(11) 0.7593(5) 0.6250(8) 0.061(4) Uani 1 1 d . . .
H41A H -0.0946 0.7356 0.6690 0.092 Uiso 1 1 calc R A .
H41B H -0.1709 0.7648 0.5942 0.092 Uiso 1 1 calc R . .
H41C H -0.0634 0.7944 0.6441 0.092 Uiso 1 1 calc R . .
C42 C 0.4360(10) 0.7094(5) 0.3254(6) 0.050(3) Uani 1 1 d . A .
H42A H 0.4862 0.7402 0.3362 0.075 Uiso 1 1 calc R . .
H42B H 0.3661 0.7211 0.2913 0.075 Uiso 1 1 calc R . .
H42C H 0.4663 0.6806 0.2999 0.075 Uiso 1 1 calc R . .
C43 C 0.4197(8) 0.6880(4) 0.4013(6) 0.037(2) Uani 1 1 d . . .
H43A H 0.4919 0.6757 0.4343 0.044 Uiso 1 1 calc R A .
C44 C 0.3788(10) 0.7323(4) 0.4451(6) 0.047(3) Uani 1 1 d . A .
H44A H 0.4279 0.7635 0.4524 0.070 Uiso 1 1 calc R . .
H44B H 0.3761 0.7185 0.4958 0.070 Uiso 1 1 calc R . .
H44C H 0.3059 0.7436 0.4154 0.070 Uiso 1 1 calc R . .
C45 C 0.5060(9) 0.5661(5) 0.3778(7) 0.051(3) Uani 1 1 d . A .
H45A H 0.5313 0.5369 0.3500 0.077 Uiso 1 1 calc R . .
H45B H 0.5170 0.5555 0.4321 0.077 Uiso 1 1 calc R . .
H45C H 0.5470 0.5992 0.3753 0.077 Uiso 1 1 calc R . .
C46 C 0.3839(8) 0.5764(4) 0.3402(5) 0.037(2) Uani 1 1 d . . .
H46A H 0.3765 0.5885 0.2857 0.045 Uiso 1 1 calc R A .
C47 C 0.3177(9) 0.5253(4) 0.3355(7) 0.045(2) Uani 1 1 d . A .
H47A H 0.3484 0.4968 0.3098 0.068 Uiso 1 1 calc R . .
H47B H 0.2426 0.5325 0.3058 0.068 Uiso 1 1 calc R . .
H47C H 0.3190 0.5135 0.3880 0.068 Uiso 1 1 calc R . .
C48 C 0.3274(10) 0.6900(5) 0.6729(6) 0.055(3) Uani 1 1 d . A .
H48A H 0.3771 0.7006 0.7226 0.082 Uiso 1 1 calc R . .
H48B H 0.2655 0.7149 0.6598 0.082 Uiso 1 1 calc R . .
H48C H 0.3656 0.6915 0.6324 0.082 Uiso 1 1 calc R . .
C49 C 0.2867(10) 0.6321(5) 0.6788(5) 0.047(3) Uani 1 1 d . . .
H49A H 0.3518 0.6080 0.6870 0.056 Uiso 1 1 calc R A .
C50 C 0.2460(13) 0.6255(5) 0.7504(6) 0.068(4) Uani 1 1 d . A .
H50A H 0.3021 0.6377 0.7962 0.102 Uiso 1 1 calc R . .
H50B H 0.2295 0.5872 0.7566 0.102 Uiso 1 1 calc R . .
H50C H 0.1803 0.6472 0.7446 0.102 Uiso 1 1 calc R . .
C51 C 0.1815(13) 0.5039(6) 0.6198(9) 0.077(4) Uani 1 1 d . A .
H51A H 0.1379 0.4730 0.6282 0.116 Uiso 1 1 calc R . .
H51B H 0.2410 0.5101 0.6666 0.116 Uiso 1 1 calc R . .
H51C H 0.2115 0.4960 0.5761 0.116 Uiso 1 1 calc R . .
C52 C 0.1147(14) 0.5513(5) 0.6028(7) 0.067(4) Uani 1 1 d . . .
H52A H 0.0846 0.5590 0.6477 0.080 Uiso 1 1 calc R A .
C53 C 0.0160(16) 0.5429(7) 0.5269(9) 0.089(5) Uani 1 1 d . A .
H53A H -0.0264 0.5111 0.5337 0.134 Uiso 1 1 calc R . .
H53B H 0.0445 0.5373 0.4820 0.134 Uiso 1 1 calc R . .
H53C H -0.0305 0.5751 0.5184 0.134 Uiso 1 1 calc R . .
C1 C 0.4551(9) 0.5587(5) 0.5726(6) 0.042(2) Uani 1 1 d D . .
O1 O 0.5369(8) 0.5308(4) 0.5760(4) 0.073(3) Uani 1 1 d D A .
O2A O 0.3571(11) 0.5539(5) 0.5261(7) 0.036(2) Uani 0.532(10) 1 d PD A 1
O3A O 0.4752(12) 0.6105(6) 0.5951(9) 0.053(4) Uani 0.532(10) 1 d PD A 1
O2B O 0.4043(13) 0.5801(6) 0.5190(9) 0.036(2) Uani 0.468(10) 1 d PD A 2
O3B O 0.4298(11) 0.5470(5) 0.6394(7) 0.031(3) Uani 0.468(10) 1 d PD A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O1 1.828(7) . ?
Ni1 N1 1.879(7) . ?
Ni1 P2 2.190(2) . ?
Ni1 P1 2.206(2) . ?
P1 C3 1.817(10) . ?
P1 C20 1.824(10) . ?
P1 C17 1.846(11) . ?
P2 C10 1.803(8) . ?
P2 C26 1.812(9) . ?
P2 C23 1.838(9) . ?
N1 C9 1.384(11) . ?
N1 C2 1.416(12) . ?
C2 C7 1.396(13) . ?
C2 C3 1.403(13) . ?
C3 C4 1.397(12) . ?
C4 C5 1.380(14) . ?
C5 C6 1.376(14) . ?
C5 C8 1.501(13) . ?
C6 C7 1.379(13) . ?
C9 C10 1.413(11) . ?
C9 C14 1.438(11) . ?
C10 C11 1.375(12) . ?
C11 C12 1.396(12) . ?
C12 C13 1.395(12) . ?
C12 C15 1.507(12) . ?
C13 C14 1.375(12) . ?
C16 C17 1.523(16) . ?
C17 C18 1.499(18) . ?
C19 C20 1.496(18) . ?
C20 C21 1.535(18) . ?
C22 C23 1.526(14) . ?
C23 C24 1.520(15) . ?
C25 C26 1.544(12) . ?
C26 C27 1.552(12) . ?
C28 N2 1.410(11) . ?
C28 C29 1.410(11) . ?
C28 C33 1.420(12) . ?
Ni2 O2A 1.871(12) . ?
Ni2 N2 1.886(7) . ?
Ni2 O2B 1.887(15) . ?
Ni2 P3 2.179(2) . ?
Ni2 P4 2.203(2) . ?
P3 C29 1.797(9) . ?
P3 C46 1.827(9) . ?
P3 C43 1.837(10) . ?
P4 C36 1.795(10) . ?
P4 C49 1.824(11) . ?
P4 C52 1.882(12) . ?
N2 C35 1.381(11) . ?
C29 C30 1.386(11) . ?
C30 C31 1.383(13) . ?
C31 C32 1.376(14) . ?
C31 C34 1.510(12) . ?
C32 C33 1.368(13) . ?
C35 C40 1.403(13) . ?
C35 C36 1.421(13) . ?
C36 C37 1.410(12) . ?
C37 C38 1.376(15) . ?
C38 C39 1.402(15) . ?
C38 C41 1.519(13) . ?
C39 C40 1.370(13) . ?
C42 C43 1.526(13) . ?
C43 C44 1.520(13) . ?
C45 C46 1.545(14) . ?
C46 C47 1.509(14) . ?
C48 C49 1.534(17) . ?
C49 C50 1.520(13) . ?
C51 C52 1.433(19) . ?
C52 C53 1.60(2) . ?
C1 O2B 1.134(18) . ?
C1 O1 1.240(13) . ?
C1 O2A 1.309(17) . ?
C1 O3A 1.343(17) . ?
C1 O3B 1.355(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ni1 N1 175.6(4) . . ?
O1 Ni1 P2 91.1(3) . . ?
N1 Ni1 P2 84.8(2) . . ?
O1 Ni1 P1 98.8(3) . . ?
N1 Ni1 P1 85.6(2) . . ?
P2 Ni1 P1 168.27(11) . . ?
C3 P1 C20 103.0(5) . . ?
C3 P1 C17 107.3(5) . . ?
C20 P1 C17 108.6(6) . . ?
C3 P1 Ni1 99.1(3) . . ?
C20 P1 Ni1 117.8(4) . . ?
C17 P1 Ni1 118.6(4) . . ?
C10 P2 C26 105.9(4) . . ?
C10 P2 C23 108.3(5) . . ?
C26 P2 C23 106.5(4) . . ?
C10 P2 Ni1 99.9(3) . . ?
C26 P2 Ni1 120.3(3) . . ?
C23 P2 Ni1 114.9(3) . . ?
C9 N1 C2 121.3(8) . . ?
C9 N1 Ni1 118.3(6) . . ?
C2 N1 Ni1 120.4(6) . . ?
C7 C2 C3 119.2(9) . . ?
C7 C2 N1 123.8(9) . . ?
C3 C2 N1 116.8(9) . . ?
C4 C3 C2 119.3(9) . . ?
C4 C3 P1 127.4(7) . . ?
C2 C3 P1 113.0(7) . . ?
C5 C4 C3 121.9(9) . . ?
C6 C5 C4 117.0(9) . . ?
C6 C5 C8 121.7(10) . . ?
C4 C5 C8 121.3(9) . . ?
C5 C6 C7 123.9(9) . . ?
C6 C7 C2 118.5(9) . . ?
N1 C9 C10 119.6(7) . . ?
N1 C9 C14 124.0(7) . . ?
C10 C9 C14 116.2(8) . . ?
C11 C10 C9 121.9(8) . . ?
C11 C10 P2 128.0(7) . . ?
C9 C10 P2 109.7(6) . . ?
C10 C11 C12 121.6(8) . . ?
C13 C12 C11 117.5(8) . . ?
C13 C12 C15 121.2(8) . . ?
C11 C12 C15 121.3(8) . . ?
C14 C13 C12 122.4(8) . . ?
C13 C14 C9 120.5(8) . . ?
C18 C17 C16 114.0(11) . . ?
C18 C17 P1 108.8(9) . . ?
C16 C17 P1 113.9(8) . . ?
C19 C20 C21 111.0(12) . . ?
C19 C20 P1 108.4(8) . . ?
C21 C20 P1 114.2(10) . . ?
C24 C23 C22 112.4(9) . . ?
C24 C23 P2 109.5(7) . . ?
C22 C23 P2 113.4(7) . . ?
C25 C26 C27 110.2(8) . . ?
C25 C26 P2 109.3(6) . . ?
C27 C26 P2 112.3(6) . . ?
N2 C28 C29 117.7(8) . . ?
N2 C28 C33 126.7(7) . . ?
C29 C28 C33 115.3(8) . . ?
O2A Ni2 N2 164.2(5) . . ?
O2A Ni2 O2B 28.3(5) . . ?
N2 Ni2 O2B 163.9(5) . . ?
O2A Ni2 P3 97.7(4) . . ?
N2 Ni2 P3 85.7(2) . . ?
O2B Ni2 P3 79.4(5) . . ?
O2A Ni2 P4 92.6(4) . . ?
N2 Ni2 P4 85.8(2) . . ?
O2B Ni2 P4 108.1(5) . . ?
P3 Ni2 P4 168.62(11) . . ?
C29 P3 C46 106.5(4) . . ?
C29 P3 C43 107.3(4) . . ?
C46 P3 C43 107.4(5) . . ?
C29 P3 Ni2 99.3(3) . . ?
C46 P3 Ni2 121.0(3) . . ?
C43 P3 Ni2 114.0(3) . . ?
C36 P4 C49 108.1(5) . . ?
C36 P4 C52 104.4(6) . . ?
C49 P4 C52 108.5(6) . . ?
C36 P4 Ni2 99.2(3) . . ?
C49 P4 Ni2 115.4(4) . . ?
C52 P4 Ni2 119.7(4) . . ?
C35 N2 C28 119.9(7) . . ?
C35 N2 Ni2 121.3(6) . . ?
C28 N2 Ni2 118.8(5) . . ?
C30 C29 C28 122.2(8) . . ?
C30 C29 P3 125.7(7) . . ?
C28 C29 P3 112.1(6) . . ?
C31 C30 C29 120.9(8) . . ?
C32 C31 C30 117.6(8) . . ?
C32 C31 C34 120.6(9) . . ?
C30 C31 C34 121.7(9) . . ?
C33 C32 C31 122.9(9) . . ?
C32 C33 C28 121.0(8) . . ?
N2 C35 C40 126.2(8) . . ?
N2 C35 C36 116.7(8) . . ?
C40 C35 C36 116.9(8) . . ?
C37 C36 C35 119.9(9) . . ?
C37 C36 P4 126.4(8) . . ?
C35 C36 P4 113.5(6) . . ?
C38 C37 C36 122.3(9) . . ?
C37 C38 C39 116.8(9) . . ?
C37 C38 C41 121.1(10) . . ?
C39 C38 C41 122.1(10) . . ?
C40 C39 C38 122.7(10) . . ?
C39 C40 C35 121.3(9) . . ?
C44 C43 C42 111.3(8) . . ?
C44 C43 P3 109.2(7) . . ?
C42 C43 P3 112.9(7) . . ?
C47 C46 C45 111.9(9) . . ?
C47 C46 P3 109.8(7) . . ?
C45 C46 P3 113.7(7) . . ?
C50 C49 C48 111.1(9) . . ?
C50 C49 P4 117.1(10) . . ?
C48 C49 P4 109.8(7) . . ?
C51 C52 C53 111.3(12) . . ?
C51 C52 P4 111.1(11) . . ?
C53 C52 P4 107.9(9) . . ?
O2B C1 O1 125.7(11) . . ?
O2B C1 O2A 43.4(9) . . ?
O1 C1 O2A 129.2(10) . . ?
O2B C1 O3A 80.1(12) . . ?
O1 C1 O3A 115.0(11) . . ?
O2A C1 O3A 110.4(12) . . ?
O2B C1 O3B 128.9(13) . . ?
O1 C1 O3B 103.9(11) . . ?
O2A C1 O3B 97.2(10) . . ?
O3A C1 O3B 90.5(11) . . ?
C1 O1 Ni1 129.8(7) . . ?
C1 O2A Ni2 124.3(10) . . ?
C1 O2B Ni2 136.9(12) . . ?

_diffrn_measured_fraction_theta_max 0.980
_diffrn_reflns_theta_full        28.35
_diffrn_measured_fraction_theta_full 0.980
_refine_diff_density_max         1.510
_refine_diff_density_min         -1.932
_refine_diff_density_rms         0.142
