# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_8
_database_code_depnum_ccdc_archive 'CCDC 1420817'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;
_audit_creation_date             2014-02-27
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '3dem_145_0m in P-1'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   9.9478(3)
_cell_length_b                   12.3725(4)
_cell_length_c                   28.7138(9)
_cell_angle_alpha                87.7587(16)
_cell_angle_beta                 82.8945(17)
_cell_angle_gamma                71.3079(16)
_cell_volume                     3321.95(18)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1 '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C38 H32 Cl1 N2 Ni1 P3 
# Dc =      1.41 Fooo =   1456.00 Mu =      8.40 M =   1407.54
# Found Formula = C38 H32 Cl1 N2 Ni1 P3 
# Dc =      1.41 FOOO =   1456.00 Mu =      8.40 M =   1407.54

_chemical_formula_sum            'C38 H32 Cl1 N2 Ni1 P3'
_chemical_formula_moiety         'C38 H32 Cl1 N2 Ni1 P3'
_chemical_compound_source        ?
_chemical_formula_weight         703.77


_cell_measurement_reflns_used    9920
_cell_measurement_theta_min      2
_cell_measurement_theta_max      28
_cell_measurement_temperature    120

_exptl_crystal_description       prism
_exptl_crystal_colour            purple
_exptl_crystal_size_min          0.110
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_max          0.270

_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1456
_exptl_absorpt_coefficient_mu    0.840

# Sheldrick geometric approximatio 0.83 0.91 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.91
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      120
_diffrn_reflns_number            16068
_reflns_number_total             16068
_diffrn_reflns_av_R_equivalents  0.049
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 16068 
# Theoretical number of reflections is about 32234 


_diffrn_reflns_theta_min         1.429
_diffrn_reflns_theta_max         28.047
_diffrn_measured_fraction_theta_max 0.997

_diffrn_reflns_theta_full        28.047
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       37
_reflns_limit_h_min              -13
_reflns_limit_h_max              13
_reflns_limit_k_min              -16
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              37

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.55
_refine_diff_density_max         1.29


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         16068
_refine_ls_number_restraints     0
_refine_ls_number_parameters     811
_oxford_refine_ls_R_factor_ref   0.0530
_refine_ls_wR_factor_ref         0.0993
_refine_ls_goodness_of_fit_ref   0.9885
_refine_ls_shift/su_max          0.0039871
_refine_ls_shift/su_mean         0.0007784


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        16068
_refine_ls_R_factor_all          0.0530
_refine_ls_wR_factor_all         0.0993

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                12260
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_gt          0.0905

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 1.94P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.67043(3) 0.55700(2) 0.863125(9) 0.0136 1.0000 Uani . . . . . .
Ni101 Ni 0.27579(3) 0.46531(2) 0.652778(9) 0.0126 1.0000 Uani . . . . . .
Cl1 Cl 0.88867(6) 0.55491(5) 0.87617(2) 0.0229 1.0000 Uani . . . . . .
Cl101 Cl 0.50263(5) 0.46463(5) 0.64742(2) 0.0202 1.0000 Uani . . . . . .
P1 P 0.57583(6) 0.74431(5) 0.858759(19) 0.0145 1.0000 Uani . . . . . .
P2 P 0.54198(6) 0.55788(5) 0.810648(19) 0.0146 1.0000 Uani . . . . . .
P3 P 0.65057(6) 0.39340(4) 0.886714(19) 0.0132 1.0000 Uani . . . . . .
P101 P 0.26916(5) 0.29253(4) 0.662202(19) 0.0127 1.0000 Uani . . . . . .
P102 P 0.08966(6) 0.52001(4) 0.699249(19) 0.0134 1.0000 Uani . . . . . .
P103 P 0.18006(6) 0.62551(5) 0.615232(19) 0.0135 1.0000 Uani . . . . . .
N1 N 0.36244(19) 0.63284(16) 0.82005(6) 0.0180 1.0000 Uani . . . . . .
N2 N 0.50225(19) 0.43531(15) 0.80342(6) 0.0167 1.0000 Uani . . . . . .
N101 N 0.03531(18) 0.41978(15) 0.73193(6) 0.0163 1.0000 Uani . . . . . .
N102 N -0.07317(18) 0.56815(15) 0.67789(6) 0.0150 1.0000 Uani . . . . . .
C1 C 0.6440(2) 0.79617(17) 0.80339(8) 0.0162 1.0000 Uani . . . . . .
C2 C 0.5554(2) 0.84156(19) 0.76898(8) 0.0212 1.0000 Uani . . . . . .
C3 C 0.6112(3) 0.8678(2) 0.72476(9) 0.0258 1.0000 Uani . . . . . .
C4 C 0.7563(3) 0.85122(19) 0.71530(9) 0.0247 1.0000 Uani . . . . . .
C5 C 0.8453(3) 0.80779(19) 0.74967(9) 0.0245 1.0000 Uani . . . . . .
C6 C 0.7906(2) 0.77932(19) 0.79351(9) 0.0216 1.0000 Uani . . . . . .
C7 C 0.6186(2) 0.82415(18) 0.90351(8) 0.0177 1.0000 Uani . . . . . .
C8 C 0.6422(3) 0.9285(2) 0.89466(9) 0.0240 1.0000 Uani . . . . . .
C9 C 0.6728(3) 0.9855(2) 0.93064(9) 0.0286 1.0000 Uani . . . . . .
C10 C 0.6793(3) 0.9393(2) 0.97529(9) 0.0303 1.0000 Uani . . . . . .
C11 C 0.6566(3) 0.8353(2) 0.98402(9) 0.0283 1.0000 Uani . . . . . .
C12 C 0.6273(2) 0.7776(2) 0.94852(8) 0.0219 1.0000 Uani . . . . . .
C13 C 0.3818(2) 0.79941(18) 0.86046(7) 0.0161 1.0000 Uani . . . . . .
C14 C 0.3079(2) 0.90501(19) 0.88215(8) 0.0202 1.0000 Uani . . . . . .
C15 C 0.1606(2) 0.94842(19) 0.88797(8) 0.0228 1.0000 Uani . . . . . .
C16 C 0.0827(2) 0.8858(2) 0.87234(9) 0.0252 1.0000 Uani . . . . . .
C17 C 0.1499(2) 0.7823(2) 0.85055(8) 0.0242 1.0000 Uani . . . . . .
C18 C 0.3008(2) 0.73646(19) 0.84329(8) 0.0182 1.0000 Uani . . . . . .
C19 C 0.2697(2) 0.5666(2) 0.80882(9) 0.0237 1.0000 Uani . . . . . .
C20 C 0.3679(2) 0.4596(2) 0.78340(8) 0.0223 1.0000 Uani . . . . . .
C21 C 0.6060(2) 0.32764(18) 0.80056(8) 0.0168 1.0000 Uani . . . . . .
C22 C 0.6240(3) 0.2536(2) 0.76323(8) 0.0215 1.0000 Uani . . . . . .
C23 C 0.7254(3) 0.1456(2) 0.76299(9) 0.0266 1.0000 Uani . . . . . .
C24 C 0.8105(3) 0.1114(2) 0.79905(9) 0.0255 1.0000 Uani . . . . . .
C25 C 0.7923(2) 0.18501(18) 0.83655(8) 0.0199 1.0000 Uani . . . . . .
C26 C 0.6890(2) 0.29240(18) 0.83835(7) 0.0153 1.0000 Uani . . . . . .
C27 C 0.7552(2) 0.31044(17) 0.93149(7) 0.0146 1.0000 Uani . . . . . .
C28 C 0.9008(2) 0.29757(19) 0.92899(8) 0.0184 1.0000 Uani . . . . . .
C29 C 0.9825(2) 0.2325(2) 0.96222(8) 0.0226 1.0000 Uani . . . . . .
C30 C 0.9198(3) 0.1816(2) 0.99873(8) 0.0231 1.0000 Uani . . . . . .
C31 C 0.7753(3) 0.1961(2) 1.00199(8) 0.0237 1.0000 Uani . . . . . .
C32 C 0.6935(2) 0.25904(19) 0.96846(8) 0.0193 1.0000 Uani . . . . . .
C33 C 0.4673(2) 0.40737(18) 0.91046(7) 0.0154 1.0000 Uani . . . . . .
C34 C 0.3908(2) 0.3407(2) 0.89632(8) 0.0217 1.0000 Uani . . . . . .
C35 C 0.2474(3) 0.3643(2) 0.91318(8) 0.0255 1.0000 Uani . . . . . .
C36 C 0.1801(3) 0.4506(2) 0.94512(9) 0.0272 1.0000 Uani . . . . . .
C37 C 0.2558(3) 0.5156(2) 0.96029(10) 0.0320 1.0000 Uani . . . . . .
C38 C 0.3985(2) 0.4950(2) 0.94238(9) 0.0264 1.0000 Uani . . . . . .
C101 C 0.1113(2) 0.28200(17) 0.63911(8) 0.0150 1.0000 Uani . . . . . .
C102 C 0.0075(2) 0.24402(18) 0.66535(8) 0.0177 1.0000 Uani . . . . . .
C103 C -0.1182(2) 0.25280(19) 0.64765(8) 0.0206 1.0000 Uani . . . . . .
C104 C -0.1426(2) 0.2971(2) 0.60350(8) 0.0230 1.0000 Uani . . . . . .
C105 C -0.0391(3) 0.3334(2) 0.57638(8) 0.0246 1.0000 Uani . . . . . .
C106 C 0.0862(2) 0.3269(2) 0.59450(8) 0.0215 1.0000 Uani . . . . . .
C107 C 0.4140(2) 0.17031(18) 0.63690(7) 0.0156 1.0000 Uani . . . . . .
C108 C 0.3879(3) 0.0759(2) 0.62003(10) 0.0281 1.0000 Uani . . . . . .
C109 C 0.5007(3) -0.0171(2) 0.60228(11) 0.0358 1.0000 Uani . . . . . .
C110 C 0.6401(3) -0.0164(2) 0.60086(10) 0.0297 1.0000 Uani . . . . . .
C111 C 0.6667(2) 0.0765(2) 0.61715(9) 0.0241 1.0000 Uani . . . . . .
C112 C 0.5545(2) 0.17036(18) 0.63511(8) 0.0188 1.0000 Uani . . . . . .
C113 C 0.2449(2) 0.25297(18) 0.72379(7) 0.0147 1.0000 Uani . . . . . .
C114 C 0.3354(2) 0.15725(19) 0.74382(8) 0.0197 1.0000 Uani . . . . . .
C115 C 0.3081(3) 0.1294(2) 0.79046(8) 0.0243 1.0000 Uani . . . . . .
C116 C 0.1875(3) 0.1975(2) 0.81768(8) 0.0237 1.0000 Uani . . . . . .
C117 C 0.0977(2) 0.29516(19) 0.79919(8) 0.0196 1.0000 Uani . . . . . .
C118 C 0.1259(2) 0.32457(17) 0.75246(7) 0.0154 1.0000 Uani . . . . . .
C119 C -0.1171(2) 0.4657(2) 0.74861(8) 0.0207 1.0000 Uani . . . . . .
C120 C -0.1842(2) 0.53030(19) 0.70673(8) 0.0198 1.0000 Uani . . . . . .
C121 C -0.1029(2) 0.61724(17) 0.63439(7) 0.0149 1.0000 Uani . . . . . .
C122 C -0.2407(2) 0.63548(19) 0.62087(8) 0.0200 1.0000 Uani . . . . . .
C123 C -0.2738(2) 0.6763(2) 0.57709(9) 0.0229 1.0000 Uani . . . . . .
C124 C -0.1756(2) 0.7062(2) 0.54541(9) 0.0246 1.0000 Uani . . . . . .
C125 C -0.0413(2) 0.69276(19) 0.55830(8) 0.0206 1.0000 Uani . . . . . .
C126 C -0.0007(2) 0.64798(17) 0.60202(7) 0.0152 1.0000 Uani . . . . . .
C127 C 0.2762(2) 0.64596(19) 0.55911(8) 0.0179 1.0000 Uani . . . . . .
C128 C 0.2916(2) 0.5696(2) 0.52254(8) 0.0220 1.0000 Uani . . . . . .
C129 C 0.3645(3) 0.5807(2) 0.47946(8) 0.0256 1.0000 Uani . . . . . .
C130 C 0.4244(3) 0.6675(2) 0.47215(9) 0.0294 1.0000 Uani . . . . . .
C131 C 0.4114(3) 0.7432(2) 0.50782(9) 0.0301 1.0000 Uani . . . . . .
C132 C 0.3363(2) 0.7329(2) 0.55126(9) 0.0248 1.0000 Uani . . . . . .
C133 C 0.1651(2) 0.75110(18) 0.64946(8) 0.0172 1.0000 Uani . . . . . .
C134 C 0.2495(3) 0.7400(2) 0.68568(9) 0.0241 1.0000 Uani . . . . . .
C135 C 0.2360(3) 0.8342(2) 0.71279(10) 0.0332 1.0000 Uani . . . . . .
C136 C 0.1420(3) 0.9393(2) 0.70385(10) 0.0343 1.0000 Uani . . . . . .
C137 C 0.0587(3) 0.9512(2) 0.66772(10) 0.0325 1.0000 Uani . . . . . .
C138 C 0.0694(3) 0.8577(2) 0.64071(9) 0.0240 1.0000 Uani . . . . . .
H21 H 0.4566 0.8555 0.7756 0.0252 1.0000 Uiso R . . . . .
H31 H 0.5524 0.8947 0.7007 0.0309 1.0000 Uiso R . . . . .
H41 H 0.7955 0.8692 0.6857 0.0300 1.0000 Uiso R . . . . .
H51 H 0.9426 0.7967 0.7438 0.0293 1.0000 Uiso R . . . . .
H61 H 0.8494 0.7493 0.8161 0.0262 1.0000 Uiso R . . . . .
H81 H 0.6374 0.9602 0.8645 0.0283 1.0000 Uiso R . . . . .
H91 H 0.6872 1.0550 0.9252 0.0338 1.0000 Uiso R . . . . .
H101 H 0.7001 0.9779 0.9999 0.0354 1.0000 Uiso R . . . . .
H111 H 0.6577 0.8038 1.0141 0.0341 1.0000 Uiso R . . . . .
H121 H 0.6151 0.7075 0.9546 0.0255 1.0000 Uiso R . . . . .
H141 H 0.3598 0.9475 0.8931 0.0235 1.0000 Uiso R . . . . .
H151 H 0.1157 1.0188 0.9024 0.0261 1.0000 Uiso R . . . . .
H161 H -0.0178 0.9129 0.8770 0.0304 1.0000 Uiso R . . . . .
H171 H 0.0962 0.7398 0.8405 0.0288 1.0000 Uiso R . . . . .
H191 H 0.2210 0.5480 0.8374 0.0285 1.0000 Uiso R . . . . .
H192 H 0.2003 0.6106 0.7890 0.0282 1.0000 Uiso R . . . . .
H201 H 0.3303 0.3961 0.7906 0.0271 1.0000 Uiso R . . . . .
H202 H 0.3831 0.4693 0.7500 0.0266 1.0000 Uiso R . . . . .
H221 H 0.5687 0.2767 0.7387 0.0260 1.0000 Uiso R . . . . .
H231 H 0.7350 0.0957 0.7387 0.0317 1.0000 Uiso R . . . . .
H241 H 0.8808 0.0402 0.7978 0.0300 1.0000 Uiso R . . . . .
H251 H 0.8479 0.1624 0.8612 0.0235 1.0000 Uiso R . . . . .
H281 H 0.9425 0.3348 0.9061 0.0220 1.0000 Uiso R . . . . .
H291 H 1.0825 0.2228 0.9598 0.0267 1.0000 Uiso R . . . . .
H301 H 0.9758 0.1393 1.0211 0.0275 1.0000 Uiso R . . . . .
H311 H 0.7304 0.1633 1.0270 0.0301 1.0000 Uiso R . . . . .
H321 H 0.5977 0.2660 0.9700 0.0230 1.0000 Uiso R . . . . .
H341 H 0.4358 0.2801 0.8758 0.0259 1.0000 Uiso R . . . . .
H351 H 0.1968 0.3206 0.9021 0.0305 1.0000 Uiso R . . . . .
H361 H 0.0828 0.4647 0.9561 0.0332 1.0000 Uiso R . . . . .
H371 H 0.2128 0.5736 0.9826 0.0396 1.0000 Uiso R . . . . .
H381 H 0.4489 0.5413 0.9518 0.0322 1.0000 Uiso R . . . . .
H1021 H 0.0218 0.2129 0.6953 0.0213 1.0000 Uiso R . . . . .
H1031 H -0.1885 0.2288 0.6661 0.0250 1.0000 Uiso R . . . . .
H1041 H -0.2283 0.3019 0.5924 0.0289 1.0000 Uiso R . . . . .
H1051 H -0.0529 0.3645 0.5463 0.0293 1.0000 Uiso R . . . . .
H1061 H 0.1559 0.3536 0.5765 0.0265 1.0000 Uiso R . . . . .
H1081 H 0.2923 0.0761 0.6205 0.0344 1.0000 Uiso R . . . . .
H1091 H 0.4831 -0.0821 0.5917 0.0431 1.0000 Uiso R . . . . .
H1101 H 0.7171 -0.0802 0.5887 0.0364 1.0000 Uiso R . . . . .
H1111 H 0.7613 0.0762 0.6165 0.0296 1.0000 Uiso R . . . . .
H1121 H 0.5728 0.2350 0.6451 0.0228 1.0000 Uiso R . . . . .
H1141 H 0.4150 0.1092 0.7245 0.0233 1.0000 Uiso R . . . . .
H1151 H 0.3717 0.0661 0.8039 0.0294 1.0000 Uiso R . . . . .
H1161 H 0.1644 0.1765 0.8491 0.0291 1.0000 Uiso R . . . . .
H1171 H 0.0186 0.3433 0.8181 0.0227 1.0000 Uiso R . . . . .
H1191 H -0.1315 0.5150 0.7758 0.0244 1.0000 Uiso R . . . . .
H1192 H -0.1530 0.4031 0.7571 0.0250 1.0000 Uiso R . . . . .
H1201 H -0.2650 0.5963 0.7175 0.0237 1.0000 Uiso R . . . . .
H1202 H -0.2143 0.4801 0.6882 0.0235 1.0000 Uiso R . . . . .
H1221 H -0.3106 0.6170 0.6427 0.0240 1.0000 Uiso R . . . . .
H1231 H -0.3659 0.6843 0.5700 0.0277 1.0000 Uiso R . . . . .
H1241 H -0.1988 0.7351 0.5160 0.0288 1.0000 Uiso R . . . . .
H1251 H 0.0230 0.7128 0.5371 0.0247 1.0000 Uiso R . . . . .
H1281 H 0.2508 0.5098 0.5275 0.0252 1.0000 Uiso R . . . . .
H1291 H 0.3754 0.5277 0.4558 0.0310 1.0000 Uiso R . . . . .
H1301 H 0.4720 0.6767 0.4423 0.0347 1.0000 Uiso R . . . . .
H1311 H 0.4514 0.8023 0.5036 0.0354 1.0000 Uiso R . . . . .
H1321 H 0.3272 0.7845 0.5744 0.0299 1.0000 Uiso R . . . . .
H1341 H 0.3132 0.6688 0.6925 0.0288 1.0000 Uiso R . . . . .
H1351 H 0.2924 0.8268 0.7371 0.0399 1.0000 Uiso R . . . . .
H1361 H 0.1354 1.0014 0.7216 0.0409 1.0000 Uiso R . . . . .
H1371 H -0.0059 1.0240 0.6616 0.0400 1.0000 Uiso R . . . . .
H1381 H 0.0114 0.8686 0.6172 0.0292 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.088593(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . Cl1 . 2.2403(6) yes
Ni1 . P1 . 2.2093(6) yes
Ni1 . P2 . 2.0903(6) yes
Ni1 . P3 . 2.1704(6) yes
Ni101 . Cl101 . 2.2401(6) yes
Ni101 . P101 . 2.1652(6) yes
Ni101 . P102 . 2.0792(6) yes
Ni101 . P103 . 2.2079(6) yes
P1 . C1 . 1.825(2) yes
P1 . C7 . 1.820(2) yes
P1 . C13 . 1.825(2) yes
P2 . N1 . 1.7209(18) yes
P2 . N2 . 1.7112(18) yes
P3 . C26 . 1.826(2) yes
P3 . C27 . 1.826(2) yes
P3 . C33 . 1.822(2) yes
P101 . C101 . 1.822(2) yes
P101 . C107 . 1.822(2) yes
P101 . C113 . 1.824(2) yes
P102 . N101 . 1.7098(18) yes
P102 . N102 . 1.7186(18) yes
P103 . C126 . 1.816(2) yes
P103 . C127 . 1.821(2) yes
P103 . C133 . 1.827(2) yes
N1 . C18 . 1.388(3) yes
N1 . C19 . 1.485(3) yes
N2 . C20 . 1.458(3) yes
N2 . C21 . 1.397(3) yes
N101 . C118 . 1.394(3) yes
N101 . C119 . 1.463(3) yes
N102 . C120 . 1.483(3) yes
N102 . C121 . 1.390(3) yes
C1 . C2 . 1.387(3) yes
C1 . C6 . 1.399(3) yes
C2 . C3 . 1.391(3) yes
C2 . H21 . 0.938 no
C3 . C4 . 1.385(3) yes
C3 . H31 . 0.943 no
C4 . C5 . 1.384(4) yes
C4 . H41 . 0.940 no
C5 . C6 . 1.387(3) yes
C5 . H51 . 0.928 no
C6 . H61 . 0.916 no
C7 . C8 . 1.393(3) yes
C7 . C12 . 1.395(3) yes
C8 . C9 . 1.389(3) yes
C8 . H81 . 0.936 no
C9 . C10 . 1.383(4) yes
C9 . H91 . 0.921 no
C10 . C11 . 1.385(4) yes
C10 . H101 . 0.946 no
C11 . C12 . 1.377(3) yes
C11 . H111 . 0.933 no
C12 . H121 . 0.921 no
C13 . C14 . 1.404(3) yes
C13 . C18 . 1.424(3) yes
C14 . C15 . 1.380(3) yes
C14 . H141 . 0.933 no
C15 . C16 . 1.378(4) yes
C15 . H151 . 0.929 no
C16 . C17 . 1.375(3) yes
C16 . H161 . 0.941 no
C17 . C18 . 1.416(3) yes
C17 . H171 . 0.936 no
C19 . C20 . 1.520(3) yes
C19 . H191 . 0.958 no
C19 . H192 . 0.962 no
C20 . H201 . 0.978 no
C20 . H202 . 0.962 no
C21 . C22 . 1.395(3) yes
C21 . C26 . 1.416(3) yes
C22 . C23 . 1.391(3) yes
C22 . H221 . 0.927 no
C23 . C24 . 1.386(4) yes
C23 . H231 . 0.925 no
C24 . C25 . 1.395(3) yes
C24 . H241 . 0.931 no
C25 . C26 . 1.393(3) yes
C25 . H251 . 0.932 no
C27 . C28 . 1.398(3) yes
C27 . C32 . 1.395(3) yes
C28 . C29 . 1.390(3) yes
C28 . H281 . 0.921 no
C29 . C30 . 1.387(3) yes
C29 . H291 . 0.957 no
C30 . C31 . 1.382(3) yes
C30 . H301 . 0.935 no
C31 . C32 . 1.388(3) yes
C31 . H311 . 0.945 no
C32 . H321 . 0.924 no
C33 . C34 . 1.389(3) yes
C33 . C38 . 1.390(3) yes
C34 . C35 . 1.388(3) yes
C34 . H341 . 0.929 no
C35 . C36 . 1.377(4) yes
C35 . H351 . 0.935 no
C36 . C37 . 1.378(4) yes
C36 . H361 . 0.942 no
C37 . C38 . 1.394(3) yes
C37 . H371 . 0.939 no
C38 . H381 . 0.939 no
C101 . C102 . 1.395(3) yes
C101 . C106 . 1.395(3) yes
C102 . C103 . 1.378(3) yes
C102 . H1021 . 0.937 no
C103 . C104 . 1.380(3) yes
C103 . H1031 . 0.942 no
C104 . C105 . 1.392(3) yes
C104 . H1041 . 0.930 no
C105 . C106 . 1.387(3) yes
C105 . H1051 . 0.939 no
C106 . H1061 . 0.950 no
C107 . C108 . 1.392(3) yes
C107 . C112 . 1.392(3) yes
C108 . C109 . 1.386(3) yes
C108 . H1081 . 0.948 no
C109 . C110 . 1.385(4) yes
C109 . H1091 . 0.944 no
C110 . C111 . 1.371(3) yes
C110 . H1101 . 0.948 no
C111 . C112 . 1.391(3) yes
C111 . H1111 . 0.937 no
C112 . H1121 . 0.937 no
C113 . C114 . 1.391(3) yes
C113 . C118 . 1.417(3) yes
C114 . C115 . 1.386(3) yes
C114 . H1141 . 0.951 no
C115 . C116 . 1.390(3) yes
C115 . H1151 . 0.938 no
C116 . C117 . 1.384(3) yes
C116 . H1161 . 0.952 no
C117 . C118 . 1.395(3) yes
C117 . H1171 . 0.942 no
C119 . C120 . 1.521(3) yes
C119 . H1191 . 0.977 no
C119 . H1192 . 0.964 no
C120 . H1201 . 0.972 no
C120 . H1202 . 0.971 no
C121 . C122 . 1.416(3) yes
C121 . C126 . 1.424(3) yes
C122 . C123 . 1.375(3) yes
C122 . H1221 . 0.954 no
C123 . C124 . 1.380(3) yes
C123 . H1231 . 0.937 no
C124 . C125 . 1.387(3) yes
C124 . H1241 . 0.931 no
C125 . C126 . 1.405(3) yes
C125 . H1251 . 0.914 no
C127 . C128 . 1.402(3) yes
C127 . C132 . 1.387(3) yes
C128 . C129 . 1.379(3) yes
C128 . H1281 . 0.950 no
C129 . C130 . 1.384(4) yes
C129 . H1291 . 0.935 no
C130 . C131 . 1.381(4) yes
C130 . H1301 . 0.948 no
C131 . C132 . 1.396(3) yes
C131 . H1311 . 0.936 no
C132 . H1321 . 0.916 no
C133 . C134 . 1.392(3) yes
C133 . C138 . 1.392(3) yes
C134 . C135 . 1.388(3) yes
C134 . H1341 . 0.935 no
C135 . C136 . 1.373(4) yes
C135 . H1351 . 0.932 no
C136 . C137 . 1.381(4) yes
C136 . H1361 . 0.919 no
C137 . C138 . 1.386(3) yes
C137 . H1371 . 0.949 no
C138 . H1381 . 0.920 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Ni1 . P1 . 96.65(2) yes
Cl1 . Ni1 . P2 . 143.88(3) yes
P1 . Ni1 . P2 . 83.50(2) yes
Cl1 . Ni1 . P3 . 106.57(2) yes
P1 . Ni1 . P3 . 149.48(2) yes
P2 . Ni1 . P3 . 88.90(2) yes
Cl101 . Ni101 . P101 . 109.62(2) yes
Cl101 . Ni101 . P102 . 138.56(2) yes
P101 . Ni101 . P102 . 88.56(2) yes
Cl101 . Ni101 . P103 . 99.99(2) yes
P101 . Ni101 . P103 . 142.01(2) yes
P102 . Ni101 . P103 . 84.40(2) yes
Ni1 . P1 . C1 . 110.10(7) yes
Ni1 . P1 . C7 . 115.03(7) yes
C1 . P1 . C7 . 104.36(10) yes
Ni1 . P1 . C13 . 116.14(7) yes
C1 . P1 . C13 . 104.87(10) yes
C7 . P1 . C13 . 105.22(10) yes
Ni1 . P2 . N1 . 118.84(7) yes
Ni1 . P2 . N2 . 116.87(7) yes
N1 . P2 . N2 . 89.94(9) yes
Ni1 . P3 . C26 . 112.04(7) yes
Ni1 . P3 . C27 . 121.31(7) yes
C26 . P3 . C27 . 103.40(10) yes
Ni1 . P3 . C33 . 111.13(7) yes
C26 . P3 . C33 . 104.02(10) yes
C27 . P3 . C33 . 103.26(9) yes
Ni101 . P101 . C101 . 109.06(7) yes
Ni101 . P101 . C107 . 121.89(7) yes
C101 . P101 . C107 . 104.25(10) yes
Ni101 . P101 . C113 . 112.96(7) yes
C101 . P101 . C113 . 103.83(10) yes
C107 . P101 . C113 . 103.13(10) yes
Ni101 . P102 . N101 . 118.36(6) yes
Ni101 . P102 . N102 . 119.64(7) yes
N101 . P102 . N102 . 89.87(9) yes
Ni101 . P103 . C126 . 114.92(7) yes
Ni101 . P103 . C127 . 116.35(7) yes
C126 . P103 . C127 . 104.12(10) yes
Ni101 . P103 . C133 . 111.96(7) yes
C126 . P103 . C133 . 104.06(10) yes
C127 . P103 . C133 . 104.11(10) yes
P2 . N1 . C18 . 126.41(15) yes
P2 . N1 . C19 . 113.43(15) yes
C18 . N1 . C19 . 119.25(18) yes
P2 . N2 . C20 . 111.09(14) yes
P2 . N2 . C21 . 122.65(14) yes
C20 . N2 . C21 . 122.43(18) yes
P102 . N101 . C118 . 124.96(14) yes
P102 . N101 . C119 . 110.05(14) yes
C118 . N101 . C119 . 122.07(17) yes
P102 . N102 . C120 . 112.69(14) yes
P102 . N102 . C121 . 127.80(14) yes
C120 . N102 . C121 . 118.34(17) yes
P1 . C1 . C2 . 121.06(16) yes
P1 . C1 . C6 . 119.45(17) yes
C2 . C1 . C6 . 119.2(2) yes
C1 . C2 . C3 . 120.7(2) yes
C1 . C2 . H21 . 119.8 no
C3 . C2 . H21 . 119.5 no
C2 . C3 . C4 . 119.7(2) yes
C2 . C3 . H31 . 121.1 no
C4 . C3 . H31 . 119.1 no
C3 . C4 . C5 . 119.9(2) yes
C3 . C4 . H41 . 120.7 no
C5 . C4 . H41 . 119.3 no
C4 . C5 . C6 . 120.5(2) yes
C4 . C5 . H51 . 120.8 no
C6 . C5 . H51 . 118.7 no
C1 . C6 . C5 . 119.8(2) yes
C1 . C6 . H61 . 119.4 no
C5 . C6 . H61 . 120.7 no
P1 . C7 . C8 . 122.93(18) yes
P1 . C7 . C12 . 117.70(17) yes
C8 . C7 . C12 . 119.4(2) yes
C7 . C8 . C9 . 119.9(2) yes
C7 . C8 . H81 . 120.0 no
C9 . C8 . H81 . 120.1 no
C8 . C9 . C10 . 120.3(2) yes
C8 . C9 . H91 . 120.4 no
C10 . C9 . H91 . 119.2 no
C9 . C10 . C11 . 119.8(2) yes
C9 . C10 . H101 . 120.5 no
C11 . C10 . H101 . 119.7 no
C10 . C11 . C12 . 120.4(2) yes
C10 . C11 . H111 . 121.2 no
C12 . C11 . H111 . 118.4 no
C7 . C12 . C11 . 120.3(2) yes
C7 . C12 . H121 . 120.2 no
C11 . C12 . H121 . 119.5 no
P1 . C13 . C14 . 118.88(17) yes
P1 . C13 . C18 . 122.69(16) yes
C14 . C13 . C18 . 118.31(19) yes
C13 . C14 . C15 . 122.3(2) yes
C13 . C14 . H141 . 119.0 no
C15 . C14 . H141 . 118.6 no
C14 . C15 . C16 . 119.1(2) yes
C14 . C15 . H151 . 119.7 no
C16 . C15 . H151 . 121.2 no
C15 . C16 . C17 . 120.9(2) yes
C15 . C16 . H161 . 120.2 no
C17 . C16 . H161 . 118.9 no
C16 . C17 . C18 . 121.4(2) yes
C16 . C17 . H171 . 120.3 no
C18 . C17 . H171 . 118.4 no
C13 . C18 . C17 . 118.0(2) yes
C13 . C18 . N1 . 123.32(19) yes
C17 . C18 . N1 . 118.7(2) yes
N1 . C19 . C20 . 106.41(18) yes
N1 . C19 . H191 . 109.2 no
C20 . C19 . H191 . 111.2 no
N1 . C19 . H192 . 110.4 no
C20 . C19 . H192 . 110.4 no
H191 . C19 . H192 . 109.2 no
C19 . C20 . N2 . 104.38(18) yes
C19 . C20 . H201 . 110.0 no
N2 . C20 . H201 . 108.8 no
C19 . C20 . H202 . 113.3 no
N2 . C20 . H202 . 110.2 no
H201 . C20 . H202 . 110.0 no
N2 . C21 . C22 . 122.1(2) yes
N2 . C21 . C26 . 117.78(19) yes
C22 . C21 . C26 . 120.1(2) yes
C21 . C22 . C23 . 119.7(2) yes
C21 . C22 . H221 . 119.8 no
C23 . C22 . H221 . 120.5 no
C22 . C23 . C24 . 120.8(2) yes
C22 . C23 . H231 . 119.6 no
C24 . C23 . H231 . 119.6 no
C23 . C24 . C25 . 119.6(2) yes
C23 . C24 . H241 . 119.9 no
C25 . C24 . H241 . 120.4 no
C24 . C25 . C26 . 120.8(2) yes
C24 . C25 . H251 . 120.4 no
C26 . C25 . H251 . 118.8 no
P3 . C26 . C21 . 116.42(16) yes
P3 . C26 . C25 . 124.65(17) yes
C21 . C26 . C25 . 118.9(2) yes
P3 . C27 . C28 . 119.72(16) yes
P3 . C27 . C32 . 121.54(16) yes
C28 . C27 . C32 . 118.74(19) yes
C27 . C28 . C29 . 120.3(2) yes
C27 . C28 . H281 . 120.2 no
C29 . C28 . H281 . 119.4 no
C28 . C29 . C30 . 120.3(2) yes
C28 . C29 . H291 . 119.6 no
C30 . C29 . H291 . 120.1 no
C29 . C30 . C31 . 119.6(2) yes
C29 . C30 . H301 . 119.3 no
C31 . C30 . H301 . 121.1 no
C30 . C31 . C32 . 120.4(2) yes
C30 . C31 . H311 . 120.8 no
C32 . C31 . H311 . 118.8 no
C27 . C32 . C31 . 120.5(2) yes
C27 . C32 . H321 . 119.2 no
C31 . C32 . H321 . 120.3 no
P3 . C33 . C34 . 123.89(17) yes
P3 . C33 . C38 . 117.25(17) yes
C34 . C33 . C38 . 118.7(2) yes
C33 . C34 . C35 . 119.9(2) yes
C33 . C34 . H341 . 120.0 no
C35 . C34 . H341 . 120.2 no
C34 . C35 . C36 . 121.1(2) yes
C34 . C35 . H351 . 118.5 no
C36 . C35 . H351 . 120.4 no
C35 . C36 . C37 . 119.6(2) yes
C35 . C36 . H361 . 119.5 no
C37 . C36 . H361 . 121.0 no
C36 . C37 . C38 . 119.7(2) yes
C36 . C37 . H371 . 121.1 no
C38 . C37 . H371 . 119.2 no
C37 . C38 . C33 . 120.9(2) yes
C37 . C38 . H381 . 119.7 no
C33 . C38 . H381 . 119.4 no
P101 . C101 . C102 . 123.69(17) yes
P101 . C101 . C106 . 117.18(16) yes
C102 . C101 . C106 . 118.7(2) yes
C101 . C102 . C103 . 120.3(2) yes
C101 . C102 . H1021 . 120.5 no
C103 . C102 . H1021 . 119.2 no
C102 . C103 . C104 . 120.8(2) yes
C102 . C103 . H1031 . 119.4 no
C104 . C103 . H1031 . 119.8 no
C103 . C104 . C105 . 119.7(2) yes
C103 . C104 . H1041 . 119.0 no
C105 . C104 . H1041 . 121.2 no
C104 . C105 . C106 . 119.6(2) yes
C104 . C105 . H1051 . 121.7 no
C106 . C105 . H1051 . 118.7 no
C101 . C106 . C105 . 120.8(2) yes
C101 . C106 . H1061 . 119.3 no
C105 . C106 . H1061 . 119.9 no
P101 . C107 . C108 . 121.62(16) yes
P101 . C107 . C112 . 119.29(16) yes
C108 . C107 . C112 . 119.1(2) yes
C107 . C108 . C109 . 120.2(2) yes
C107 . C108 . H1081 . 119.4 no
C109 . C108 . H1081 . 120.4 no
C108 . C109 . C110 . 120.3(2) yes
C108 . C109 . H1091 . 120.1 no
C110 . C109 . H1091 . 119.6 no
C109 . C110 . C111 . 119.9(2) yes
C109 . C110 . H1101 . 120.1 no
C111 . C110 . H1101 . 120.0 no
C110 . C111 . C112 . 120.4(2) yes
C110 . C111 . H1111 . 119.6 no
C112 . C111 . H1111 . 120.0 no
C107 . C112 . C111 . 120.1(2) yes
C107 . C112 . H1121 . 119.6 no
C111 . C112 . H1121 . 120.2 no
P101 . C113 . C114 . 123.96(17) yes
P101 . C113 . C118 . 117.33(15) yes
C114 . C113 . C118 . 118.71(19) yes
C113 . C114 . C115 . 121.2(2) yes
C113 . C114 . H1141 . 118.7 no
C115 . C114 . H1141 . 120.1 no
C114 . C115 . C116 . 119.5(2) yes
C114 . C115 . H1151 . 120.4 no
C116 . C115 . H1151 . 120.0 no
C115 . C116 . C117 . 120.7(2) yes
C115 . C116 . H1161 . 120.3 no
C117 . C116 . H1161 . 119.0 no
C116 . C117 . C118 . 120.0(2) yes
C116 . C117 . H1171 . 120.6 no
C118 . C117 . H1171 . 119.4 no
C113 . C118 . C117 . 119.81(19) yes
C113 . C118 . N101 . 118.23(18) yes
C117 . C118 . N101 . 121.85(19) yes
N101 . C119 . C120 . 104.46(17) yes
N101 . C119 . H1191 . 110.0 no
C120 . C119 . H1191 . 112.6 no
N101 . C119 . H1192 . 108.8 no
C120 . C119 . H1192 . 110.9 no
H1191 . C119 . H1192 . 110.0 no
C119 . C120 . N102 . 107.29(17) yes
C119 . C120 . H1201 . 109.9 no
N102 . C120 . H1201 . 109.8 no
C119 . C120 . H1202 . 109.9 no
N102 . C120 . H1202 . 109.3 no
H1201 . C120 . H1202 . 110.6 no
N102 . C121 . C122 . 118.68(19) yes
N102 . C121 . C126 . 123.36(18) yes
C122 . C121 . C126 . 117.95(19) yes
C121 . C122 . C123 . 121.5(2) yes
C121 . C122 . H1221 . 118.4 no
C123 . C122 . H1221 . 120.0 no
C122 . C123 . C124 . 121.0(2) yes
C122 . C123 . H1231 . 117.4 no
C124 . C123 . H1231 . 121.6 no
C123 . C124 . C125 . 118.7(2) yes
C123 . C124 . H1241 . 120.9 no
C125 . C124 . H1241 . 120.5 no
C124 . C125 . C126 . 122.5(2) yes
C124 . C125 . H1251 . 118.1 no
C126 . C125 . H1251 . 119.4 no
P103 . C126 . C121 . 121.61(16) yes
P103 . C126 . C125 . 120.06(16) yes
C121 . C126 . C125 . 118.29(19) yes
P103 . C127 . C128 . 118.46(17) yes
P103 . C127 . C132 . 122.82(18) yes
C128 . C127 . C132 . 118.7(2) yes
C127 . C128 . C129 . 120.8(2) yes
C127 . C128 . H1281 . 119.4 no
C129 . C128 . H1281 . 119.8 no
C128 . C129 . C130 . 119.9(2) yes
C128 . C129 . H1291 . 119.4 no
C130 . C129 . H1291 . 120.7 no
C129 . C130 . C131 . 120.2(2) yes
C129 . C130 . H1301 . 120.0 no
C131 . C130 . H1301 . 119.7 no
C130 . C131 . C132 . 119.9(2) yes
C130 . C131 . H1311 . 121.4 no
C132 . C131 . H1311 . 118.6 no
C131 . C132 . C127 . 120.4(2) yes
C131 . C132 . H1321 . 119.0 no
C127 . C132 . H1321 . 120.6 no
P103 . C133 . C134 . 119.42(17) yes
P103 . C133 . C138 . 121.58(17) yes
C134 . C133 . C138 . 119.0(2) yes
C133 . C134 . C135 . 119.9(2) yes
C133 . C134 . H1341 . 120.4 no
C135 . C134 . H1341 . 119.7 no
C134 . C135 . C136 . 120.9(2) yes
C134 . C135 . H1351 . 120.0 no
C136 . C135 . H1351 . 119.1 no
C135 . C136 . C137 . 119.5(2) yes
C135 . C136 . H1361 . 120.1 no
C137 . C136 . H1361 . 120.4 no
C136 . C137 . C138 . 120.3(2) yes
C136 . C137 . H1371 . 119.3 no
C138 . C137 . H1371 . 120.4 no
C133 . C138 . C137 . 120.3(2) yes
C133 . C138 . H1381 . 121.7 no
C137 . C138 . H1381 . 117.9 no


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 27/02/14 at 16:09:54
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   ( 102,X'S) H   (1021,X'S) 
RIDE C   ( 103,X'S) H   (1031,X'S) 
RIDE C   ( 104,X'S) H   (1041,X'S) 
RIDE C   ( 105,X'S) H   (1051,X'S) 
RIDE C   ( 106,X'S) H   (1061,X'S) 
RIDE C   ( 108,X'S) H   (1081,X'S) 
RIDE C   ( 109,X'S) H   (1091,X'S) 
RIDE C   ( 110,X'S) H   (1101,X'S) 
RIDE C   ( 111,X'S) H   (1111,X'S) 
RIDE C   ( 112,X'S) H   (1121,X'S) 
RIDE C   ( 114,X'S) H   (1141,X'S) 
RIDE C   ( 115,X'S) H   (1151,X'S) 
RIDE C   ( 116,X'S) H   (1161,X'S) 
RIDE C   ( 117,X'S) H   (1171,X'S) 
RIDE C   ( 119,X'S) H   (1191,X'S) H   (1192,X'S) 
RIDE C   ( 120,X'S) H   (1201,X'S) H   (1202,X'S) 
RIDE C   ( 122,X'S) H   (1221,X'S) 
RIDE C   ( 123,X'S) H   (1231,X'S) 
RIDE C   ( 124,X'S) H   (1241,X'S) 
RIDE C   ( 125,X'S) H   (1251,X'S) 
RIDE C   ( 128,X'S) H   (1281,X'S) 
RIDE C   ( 129,X'S) H   (1291,X'S) 
RIDE C   ( 130,X'S) H   (1301,X'S) 
RIDE C   ( 131,X'S) H   (1311,X'S) 
RIDE C   ( 132,X'S) H   (1321,X'S) 
RIDE C   ( 134,X'S) H   (1341,X'S) 
RIDE C   ( 135,X'S) H   (1351,X'S) 
RIDE C   ( 136,X'S) H   (1361,X'S) 
RIDE C   ( 137,X'S) H   (1371,X'S) 
RIDE C   ( 138,X'S) H   (1381,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 27/02/14 at 16:09:54
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.034 1.000 0.500 155 35 ' '
_platon_squeeze_details          
;
During the structure solution, electron density difference 
maps revealed that there was considerable disordered 
associated with a DCM solvent molecule, which could not 
be successfully modeled.  From history, the remaining 
solvate was likely DCM in a volume of 155.7 Å3 per unit 
cell (4.7%).  It appeared that the cavity area contained 
about one DCM molecule, located near an inversion center 
at (0, 0, 1/2), as shown in the bc projection below. 
Modeling with or without restraints was unsuccessful, 
as was step by step acquisition of peaks using successive 
electron density difference maps.  Thus, the structure 
factors were modified using the PLATON SQUEEZE, technique, 
in order to produce a "solvate-free" structure factor set.  
PLATON reported a total electron density of 34 e- per unit 
cell, likely representing one DCM molecule, consistent 
with our earlier observations.  Use of the SQUEEZE 
technique resulted in a decrease of ca. 2.7 % in R.  
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: CH2Cl2, pentane'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_9
_database_code_depnum_ccdc_archive 'CCDC 1420818'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;
_audit_creation_date             2013-10-15
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '3dem_59_0m in I4(1)/a'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   31.6465(7)
_cell_length_b                   31.6465(7)
_cell_length_c                   30.3830(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     30428.6(12)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a '
_symmetry_space_group_name_Hall  '-I 4ad '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z+1/2
-x+1/2,-y+1/2,-z+1/2
-y+3/4,x+1/4,z+1/4
y+3/4,-x+1/4,-z+1/4
-y+5/4,x+3/4,z+3/4
y+5/4,-x+3/4,-z+3/4
-x+1/2,-y,z+1/2
x+1/2,y,-z+1/2
-x+1,-y+1/2,z+1
x+1,y+1/2,-z+1
y+3/4,-x+3/4,z+3/4
-y+3/4,x+3/4,-z+3/4
y+5/4,-x+5/4,z+5/4
-y+5/4,x+5/4,-z+5/4

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            16

# Given Formula = C86 H80 Cl2 N4 Ni3 O1 P6 
# Dc =      1.41 Fooo =  13440.00 Mu =      9.82 M =   1618.49
# Found Formula = C86 H80 Cl2 N4 Ni3 O1 P6 
# Dc =      1.41 FOOO =  13440.00 Mu =      9.82 M =   1618.48

_chemical_formula_sum            'C86 H80 Cl2 N4 Ni3 O1 P6'
_chemical_formula_moiety         'C86 H80 Cl2 N4 Ni3 O1 P6'
_chemical_compound_source        ?
_chemical_formula_weight         1618.48


_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      2
_cell_measurement_theta_max      25
_cell_measurement_temperature    120

_exptl_crystal_description       'prism fragment'
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.180
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_max          0.240

_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             13440
_exptl_absorpt_coefficient_mu    0.982

# Sheldrick geometric approximatio 0.83 0.84 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.84
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      120
_diffrn_reflns_number            15039
_reflns_number_total             15039
_diffrn_reflns_av_R_equivalents  0.085
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 15039 
# Theoretical number of reflections is about 30068 


_diffrn_reflns_theta_min         1.287
_diffrn_reflns_theta_max         26.050
_diffrn_measured_fraction_theta_max 0.999

_diffrn_reflns_theta_full        26.050
_diffrn_measured_fraction_theta_full 0.999


_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       37
_reflns_limit_h_min              -27
_reflns_limit_h_max              27
_reflns_limit_k_min              0
_reflns_limit_k_max              39
_reflns_limit_l_min              0
_reflns_limit_l_max              37

_oxford_diffrn_Wilson_B_factor   0.96
_oxford_diffrn_Wilson_scale      2569.56

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -1.10
_refine_diff_density_max         1.28


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         15039
_refine_ls_number_restraints     1
_refine_ls_number_parameters     919
_oxford_refine_ls_R_factor_ref   0.0657
_refine_ls_wR_factor_ref         0.0959
_refine_ls_goodness_of_fit_ref   1.0109
_refine_ls_shift/su_max          0.0057343
_refine_ls_shift/su_mean         0.0002166


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        15039
_refine_ls_R_factor_all          0.0657
_refine_ls_wR_factor_all         0.0959

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                10952
_refine_ls_R_factor_gt           0.0409
_refine_ls_wR_factor_gt          0.0873

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.04P)² +94.79P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.647948(12) 0.555229(12) 0.262455(13) 0.0127 1.0000 Uani . . . . . .
Ni2 Ni 0.561615(11) 0.568869(11) 0.258451(12) 0.0108 1.0000 Uani . . . . . .
Ni3 Ni 0.609129(12) 0.527487(12) 0.326810(13) 0.0128 1.0000 Uani . . . . . .
Cl1 Cl 0.65570(2) 0.48276(2) 0.29403(2) 0.0153 1.0000 Uani . . . . . .
Cl2 Cl 0.66675(2) 0.58114(2) 0.32961(2) 0.0161 1.0000 Uani . . . . . .
P1 P 0.69522(2) 0.57334(2) 0.21584(3) 0.0125 1.0000 Uani . . . . . .
P2 P 0.60487(2) 0.53720(2) 0.21457(3) 0.0114 1.0000 Uani . . . . . .
P3 P 0.51194(2) 0.52613(2) 0.23776(3) 0.0121 1.0000 Uani . . . . . .
P4 P 0.55571(2) 0.63848(2) 0.25587(3) 0.0128 1.0000 Uani . . . . . .
P5 P 0.55857(2) 0.56965(2) 0.32875(3) 0.0120 1.0000 Uani . . . . . .
P6 P 0.58606(2) 0.49434(2) 0.38257(3) 0.0127 1.0000 Uani . . . . . .
O1 O 0.52726(19) 0.31092(16) 0.52572(17) 0.1240 1.0000 Uani . . . . . .
N1 N 0.62036(8) 0.54177(8) 0.16060(8) 0.0139 1.0000 Uani . . . . . .
N2 N 0.59170(8) 0.48566(7) 0.20417(8) 0.0132 1.0000 Uani . . . . . .
N3 N 0.56071(8) 0.61852(8) 0.35292(9) 0.0172 1.0000 Uani . . . . . .
N4 N 0.51780(8) 0.55698(8) 0.36352(8) 0.0151 1.0000 Uani . . . . . .
C1 C 0.73499(9) 0.61232(9) 0.23245(10) 0.0150 1.0000 Uani . . . . . .
C2 C 0.77618(10) 0.61204(10) 0.21612(11) 0.0212 1.0000 Uani . . . . . .
C3 C 0.80402(10) 0.64412(11) 0.22694(12) 0.0256 1.0000 Uani . . . . . .
C4 C 0.79142(11) 0.67668(10) 0.25406(11) 0.0232 1.0000 Uani . . . . . .
C5 C 0.75084(11) 0.67720(10) 0.27035(11) 0.0212 1.0000 Uani . . . . . .
C6 C 0.72272(10) 0.64521(10) 0.25969(10) 0.0181 1.0000 Uani . . . . . .
C7 C 0.72770(9) 0.52934(9) 0.19572(11) 0.0174 1.0000 Uani . . . . . .
C8 C 0.73190(11) 0.51938(10) 0.15141(12) 0.0255 1.0000 Uani . . . . . .
C9 C 0.75782(12) 0.48629(12) 0.13813(14) 0.0366 1.0000 Uani . . . . . .
C10 C 0.78035(12) 0.46393(11) 0.16845(16) 0.0379 1.0000 Uani . . . . . .
C11 C 0.77576(11) 0.47286(11) 0.21311(15) 0.0350 1.0000 Uani . . . . . .
C12 C 0.74921(10) 0.50530(10) 0.22663(13) 0.0244 1.0000 Uani . . . . . .
C13 C 0.67675(9) 0.59539(9) 0.16356(10) 0.0139 1.0000 Uani . . . . . .
C14 C 0.69849(10) 0.62740(10) 0.14178(11) 0.0172 1.0000 Uani . . . . . .
C15 C 0.68999(10) 0.63793(10) 0.09847(11) 0.0212 1.0000 Uani . . . . . .
C16 C 0.65935(10) 0.61579(10) 0.07593(11) 0.0217 1.0000 Uani . . . . . .
C17 C 0.63566(10) 0.58526(10) 0.09734(10) 0.0174 1.0000 Uani . . . . . .
C18 C 0.64373(9) 0.57493(9) 0.14129(10) 0.0143 1.0000 Uani . . . . . .
C19 C 0.61220(10) 0.50405(10) 0.13350(10) 0.0182 1.0000 Uani . . . . . .
C20 C 0.61444(10) 0.46836(10) 0.16602(10) 0.0182 1.0000 Uani . . . . . .
C21 C 0.56756(9) 0.45860(9) 0.23090(10) 0.0135 1.0000 Uani . . . . . .
C22 C 0.58034(10) 0.41667(10) 0.23683(11) 0.0177 1.0000 Uani . . . . . .
C23 C 0.55629(10) 0.38927(10) 0.26200(11) 0.0221 1.0000 Uani . . . . . .
C24 C 0.52012(11) 0.40298(10) 0.28236(11) 0.0228 1.0000 Uani . . . . . .
C25 C 0.50673(10) 0.44431(10) 0.27620(11) 0.0188 1.0000 Uani . . . . . .
C26 C 0.52891(9) 0.47216(9) 0.24957(10) 0.0137 1.0000 Uani . . . . . .
C27 C 0.50227(9) 0.52343(10) 0.17811(10) 0.0142 1.0000 Uani . . . . . .
C28 C 0.48714(9) 0.48721(10) 0.15719(11) 0.0172 1.0000 Uani . . . . . .
C29 C 0.47751(10) 0.48813(11) 0.11257(11) 0.0225 1.0000 Uani . . . . . .
C30 C 0.48279(10) 0.52471(11) 0.08853(11) 0.0244 1.0000 Uani . . . . . .
C31 C 0.49851(10) 0.56039(11) 0.10839(11) 0.0220 1.0000 Uani . . . . . .
C32 C 0.50816(9) 0.55988(10) 0.15307(10) 0.0164 1.0000 Uani . . . . . .
C33 C 0.45722(9) 0.52868(10) 0.25822(10) 0.0153 1.0000 Uani . . . . . .
C34 C 0.42657(10) 0.49857(10) 0.24760(11) 0.0210 1.0000 Uani . . . . . .
C35 C 0.38563(10) 0.50263(11) 0.26288(12) 0.0263 1.0000 Uani . . . . . .
C36 C 0.37441(10) 0.53708(11) 0.28849(12) 0.0256 1.0000 Uani . . . . . .
C37 C 0.40379(10) 0.56769(11) 0.29816(11) 0.0228 1.0000 Uani . . . . . .
C38 C 0.44516(10) 0.56321(10) 0.28356(10) 0.0173 1.0000 Uani . . . . . .
C39 C 0.56400(9) 0.67265(9) 0.20798(10) 0.0143 1.0000 Uani . . . . . .
C40 C 0.55257(10) 0.71540(10) 0.20987(11) 0.0203 1.0000 Uani . . . . . .
C41 C 0.55946(10) 0.74171(10) 0.17417(11) 0.0221 1.0000 Uani . . . . . .
C42 C 0.57786(10) 0.72585(10) 0.13639(11) 0.0201 1.0000 Uani . . . . . .
C43 C 0.58929(10) 0.68365(11) 0.13419(11) 0.0216 1.0000 Uani . . . . . .
C44 C 0.58217(9) 0.65743(10) 0.16986(11) 0.0172 1.0000 Uani . . . . . .
C45 C 0.50361(10) 0.66028(9) 0.27159(10) 0.0151 1.0000 Uani . . . . . .
C46 C 0.49619(11) 0.68552(10) 0.30804(11) 0.0220 1.0000 Uani . . . . . .
C47 C 0.45596(11) 0.70202(11) 0.31600(13) 0.0287 1.0000 Uani . . . . . .
C48 C 0.42345(11) 0.69392(11) 0.28734(13) 0.0286 1.0000 Uani . . . . . .
C49 C 0.43043(10) 0.66942(10) 0.25043(12) 0.0247 1.0000 Uani . . . . . .
C50 C 0.47035(10) 0.65257(9) 0.24270(11) 0.0180 1.0000 Uani . . . . . .
C51 C 0.59116(10) 0.66328(9) 0.29595(10) 0.0158 1.0000 Uani . . . . . .
C52 C 0.62080(10) 0.69414(10) 0.28461(11) 0.0198 1.0000 Uani . . . . . .
C53 C 0.64538(11) 0.71402(10) 0.31594(12) 0.0244 1.0000 Uani . . . . . .
C54 C 0.64013(11) 0.70385(10) 0.35973(12) 0.0250 1.0000 Uani . . . . . .
C55 C 0.61214(10) 0.67237(10) 0.37203(11) 0.0213 1.0000 Uani . . . . . .
C56 C 0.58847(10) 0.65093(9) 0.34034(10) 0.0159 1.0000 Uani . . . . . .
C57 C 0.53879(11) 0.62095(10) 0.39542(11) 0.0226 1.0000 Uani . . . . . .
C58 C 0.50090(11) 0.59250(10) 0.38872(11) 0.0226 1.0000 Uani . . . . . .
C59 C 0.50179(10) 0.51597(10) 0.37080(10) 0.0149 1.0000 Uani . . . . . .
C60 C 0.45834(10) 0.50890(11) 0.37198(10) 0.0194 1.0000 Uani . . . . . .
C61 C 0.44239(10) 0.46898(11) 0.37929(11) 0.0219 1.0000 Uani . . . . . .
C62 C 0.46978(10) 0.43567(11) 0.38647(11) 0.0209 1.0000 Uani . . . . . .
C63 C 0.51300(10) 0.44258(10) 0.38723(10) 0.0178 1.0000 Uani . . . . . .
C64 C 0.52973(9) 0.48256(10) 0.37976(10) 0.0141 1.0000 Uani . . . . . .
C65 C 0.59098(10) 0.52237(10) 0.43469(10) 0.0161 1.0000 Uani . . . . . .
C66 C 0.62991(10) 0.54085(10) 0.44369(11) 0.0200 1.0000 Uani . . . . . .
C67 C 0.63810(12) 0.55814(11) 0.48468(12) 0.0288 1.0000 Uani . . . . . .
C68 C 0.60657(13) 0.55800(12) 0.51648(13) 0.0362 1.0000 Uani . . . . . .
C69 C 0.56755(13) 0.54123(13) 0.50725(12) 0.0353 1.0000 Uani . . . . . .
C70 C 0.55980(11) 0.52290(11) 0.46683(11) 0.0245 1.0000 Uani . . . . . .
C71 C 0.60647(9) 0.44227(10) 0.39744(11) 0.0159 1.0000 Uani . . . . . .
C72 C 0.61408(10) 0.43020(11) 0.44083(11) 0.0234 1.0000 Uani . . . . . .
C73 C 0.62651(12) 0.38921(12) 0.45047(13) 0.0338 1.0000 Uani . . . . . .
C74 C 0.63010(13) 0.35992(12) 0.41721(13) 0.0401 1.0000 Uani . . . . . .
C75 C 0.62210(12) 0.37142(11) 0.37414(13) 0.0336 1.0000 Uani . . . . . .
C76 C 0.61104(10) 0.41260(10) 0.36392(11) 0.0208 1.0000 Uani . . . . . .
C77 C 0.6522(3) 0.4444(2) 0.5705(2) 0.0942 1.0000 Uani . . . . . .
C78 C 0.6863(2) 0.4209(2) 0.5859(2) 0.0936 1.0000 Uani . . . . . .
C79 C 0.6815(2) 0.3783(2) 0.59585(19) 0.0827 1.0000 Uani . . . . . .
C80 C 0.64485(19) 0.3592(2) 0.59081(19) 0.0790 1.0000 Uani . . . . . .
C81 C 0.6109(2) 0.3810(3) 0.5757(2) 0.0903 1.0000 Uani . . . . . .
C82 C 0.6145(2) 0.4228(3) 0.56579(18) 0.0847 1.0000 Uani . . . . . .
C83 C 0.5662(4) 0.2589(3) 0.5610(2) 0.1818 1.0000 Uani . . . . . .
C84 C 0.5591(3) 0.2808(3) 0.5202(3) 0.1525 1.0000 Uani . . . . . .
C85 C 0.5205(3) 0.3293(3) 0.4830(3) 0.1754 1.0000 Uani D . . . . .
C86 C 0.4889(3) 0.3600(3) 0.4888(2) 0.1539 1.0000 Uani D . . . . .
H21 H 0.7852 0.5893 0.2009 0.0254 1.0000 Uiso R . . . . .
H31 H 0.8309 0.6433 0.2174 0.0311 1.0000 Uiso R . . . . .
H41 H 0.8095 0.6980 0.2616 0.0279 1.0000 Uiso R . . . . .
H51 H 0.7416 0.6990 0.2868 0.0257 1.0000 Uiso R . . . . .
H61 H 0.6955 0.6447 0.2707 0.0217 1.0000 Uiso R . . . . .
H81 H 0.7166 0.5352 0.1306 0.0314 1.0000 Uiso R . . . . .
H91 H 0.7599 0.4800 0.1066 0.0447 1.0000 Uiso R . . . . .
H101 H 0.8002 0.4425 0.1653 0.0457 1.0000 Uiso R . . . . .
H111 H 0.7908 0.4574 0.2346 0.0409 1.0000 Uiso R . . . . .
H121 H 0.7460 0.5108 0.2560 0.0283 1.0000 Uiso R . . . . .
H141 H 0.7189 0.6432 0.1571 0.0210 1.0000 Uiso R . . . . .
H151 H 0.7035 0.6613 0.0841 0.0256 1.0000 Uiso R . . . . .
H161 H 0.6546 0.6209 0.0458 0.0256 1.0000 Uiso R . . . . .
H171 H 0.6151 0.5717 0.0796 0.0208 1.0000 Uiso R . . . . .
H191 H 0.5833 0.5062 0.1210 0.0218 1.0000 Uiso R . . . . .
H192 H 0.6324 0.5015 0.1080 0.0223 1.0000 Uiso R . . . . .
H201 H 0.6428 0.4633 0.1786 0.0221 1.0000 Uiso R . . . . .
H202 H 0.6005 0.4420 0.1590 0.0225 1.0000 Uiso R . . . . .
H221 H 0.6059 0.4084 0.2249 0.0204 1.0000 Uiso R . . . . .
H231 H 0.5669 0.3636 0.2643 0.0263 1.0000 Uiso R . . . . .
H241 H 0.5048 0.3859 0.3030 0.0274 1.0000 Uiso R . . . . .
H251 H 0.4823 0.4538 0.2904 0.0230 1.0000 Uiso R . . . . .
H281 H 0.4835 0.4629 0.1738 0.0208 1.0000 Uiso R . . . . .
H291 H 0.4670 0.4637 0.0990 0.0272 1.0000 Uiso R . . . . .
H301 H 0.4757 0.5252 0.0581 0.0290 1.0000 Uiso R . . . . .
H311 H 0.5018 0.5856 0.0930 0.0263 1.0000 Uiso R . . . . .
H321 H 0.5172 0.5843 0.1672 0.0194 1.0000 Uiso R . . . . .
H341 H 0.4333 0.4756 0.2306 0.0245 1.0000 Uiso R . . . . .
H351 H 0.3643 0.4815 0.2576 0.0315 1.0000 Uiso R . . . . .
H361 H 0.3465 0.5381 0.2966 0.0306 1.0000 Uiso R . . . . .
H371 H 0.3955 0.5908 0.3151 0.0269 1.0000 Uiso R . . . . .
H381 H 0.4647 0.5830 0.2918 0.0218 1.0000 Uiso R . . . . .
H401 H 0.5401 0.7262 0.2323 0.0241 1.0000 Uiso R . . . . .
H411 H 0.5499 0.7698 0.1738 0.0265 1.0000 Uiso R . . . . .
H421 H 0.5815 0.7432 0.1114 0.0238 1.0000 Uiso R . . . . .
H431 H 0.6019 0.6745 0.1078 0.0258 1.0000 Uiso R . . . . .
H441 H 0.5889 0.6292 0.1693 0.0210 1.0000 Uiso R . . . . .
H461 H 0.5179 0.6908 0.3315 0.0273 1.0000 Uiso R . . . . .
H471 H 0.4510 0.7174 0.3454 0.0344 1.0000 Uiso R . . . . .
H481 H 0.3957 0.7045 0.2937 0.0354 1.0000 Uiso R . . . . .
H491 H 0.4080 0.6637 0.2285 0.0300 1.0000 Uiso R . . . . .
H501 H 0.4748 0.6359 0.2146 0.0218 1.0000 Uiso R . . . . .
H521 H 0.6250 0.7007 0.2544 0.0237 1.0000 Uiso R . . . . .
H531 H 0.6658 0.7340 0.3067 0.0293 1.0000 Uiso R . . . . .
H541 H 0.6532 0.7193 0.3825 0.0302 1.0000 Uiso R . . . . .
H551 H 0.6069 0.6662 0.4021 0.0259 1.0000 Uiso R . . . . .
H571 H 0.5294 0.6503 0.4008 0.0261 1.0000 Uiso R . . . . .
H572 H 0.5563 0.6128 0.4173 0.0265 1.0000 Uiso R . . . . .
H581 H 0.4896 0.5837 0.4144 0.0266 1.0000 Uiso R . . . . .
H582 H 0.4798 0.6088 0.3739 0.0262 1.0000 Uiso R . . . . .
H601 H 0.4408 0.5318 0.3683 0.0225 1.0000 Uiso R . . . . .
H611 H 0.4146 0.4643 0.3802 0.0265 1.0000 Uiso R . . . . .
H621 H 0.4611 0.4077 0.3919 0.0249 1.0000 Uiso R . . . . .
H631 H 0.5306 0.4190 0.3934 0.0204 1.0000 Uiso R . . . . .
H661 H 0.6506 0.5415 0.4245 0.0245 1.0000 Uiso R . . . . .
H671 H 0.6651 0.5689 0.4936 0.0344 1.0000 Uiso R . . . . .
H681 H 0.6130 0.5686 0.5430 0.0431 1.0000 Uiso R . . . . .
H691 H 0.5474 0.5421 0.5306 0.0422 1.0000 Uiso R . . . . .
H701 H 0.5339 0.5095 0.4597 0.0293 1.0000 Uiso R . . . . .
H721 H 0.6124 0.4494 0.4641 0.0279 1.0000 Uiso R . . . . .
H731 H 0.6352 0.3835 0.4786 0.0406 1.0000 Uiso R . . . . .
H741 H 0.6372 0.3327 0.4236 0.0481 1.0000 Uiso R . . . . .
H751 H 0.6223 0.3496 0.3521 0.0409 1.0000 Uiso R . . . . .
H761 H 0.6062 0.4201 0.3333 0.0251 1.0000 Uiso R . . . . .
H771 H 0.6545 0.4738 0.5596 0.1136 1.0000 Uiso R . . . . .
H781 H 0.7126 0.4339 0.5859 0.1134 1.0000 Uiso R . . . . .
H791 H 0.7041 0.3615 0.6063 0.0993 1.0000 Uiso R . . . . .
H801 H 0.6396 0.3294 0.5981 0.0948 1.0000 Uiso R . . . . .
H811 H 0.5837 0.3658 0.5757 0.1070 1.0000 Uiso R . . . . .
H821 H 0.5912 0.4380 0.5551 0.1013 1.0000 Uiso R . . . . .
H831 H 0.5879 0.2384 0.5568 0.2163 1.0000 Uiso R . . . . .
H832 H 0.5748 0.2785 0.5828 0.2163 1.0000 Uiso R . . . . .
H833 H 0.5410 0.2452 0.5701 0.2163 1.0000 Uiso R . . . . .
H861 H 0.4832 0.3715 0.4605 0.1960 1.0000 Uiso R . . . . .
H862 H 0.5006 0.3812 0.5071 0.1960 1.0000 Uiso R . . . . .
H863 H 0.4633 0.3499 0.5014 0.1960 1.0000 Uiso R . . . . .
H851 H 0.5457 0.3392 0.4694 0.2217 1.0000 Uiso R . . . . .
H852 H 0.5079 0.3082 0.4650 0.2217 1.0000 Uiso R . . . . .
H841 H 0.5844 0.2942 0.5109 0.1881 1.0000 Uiso R . . . . .
H842 H 0.5502 0.2612 0.4984 0.1881 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.0194054(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . Ni2 . 2.7687(5) yes
Ni1 . Ni3 . 2.4705(5) yes
Ni1 . Cl1 . 2.4981(8) yes
Ni1 . Cl2 . 2.2781(8) yes
Ni1 . P1 . 2.1383(9) yes
Ni1 . P2 . 2.0740(9) yes
Ni2 . Ni3 . 2.8792(5) yes
Ni2 . P2 . 2.1577(8) yes
Ni2 . P3 . 2.1670(8) yes
Ni2 . P4 . 2.2122(8) yes
Ni2 . P5 . 2.1383(9) yes
Ni3 . Cl1 . 2.2732(8) yes
Ni3 . Cl2 . 2.4930(8) yes
Ni3 . P5 . 2.0843(8) yes
Ni3 . P6 . 2.1222(9) yes
P1 . C1 . 1.833(3) yes
P1 . C7 . 1.836(3) yes
P1 . C13 . 1.831(3) yes
P2 . N1 . 1.717(3) yes
P2 . N2 . 1.713(2) yes
P3 . C26 . 1.826(3) yes
P3 . C27 . 1.840(3) yes
P3 . C33 . 1.842(3) yes
P4 . C39 . 1.832(3) yes
P4 . C45 . 1.850(3) yes
P4 . C51 . 1.832(3) yes
P5 . N3 . 1.714(3) yes
P5 . N4 . 1.715(3) yes
P6 . C64 . 1.823(3) yes
P6 . C65 . 1.822(3) yes
P6 . C71 . 1.827(3) yes
O1 . C84 . 1.395(8) yes
O1 . C85 . 1.439(9) yes
N1 . C18 . 1.412(4) yes
N1 . C19 . 1.473(4) yes
N2 . C20 . 1.470(4) yes
N2 . C21 . 1.406(4) yes
N3 . C56 . 1.404(4) yes
N3 . C57 . 1.468(4) yes
N4 . C58 . 1.461(4) yes
N4 . C59 . 1.411(4) yes
C1 . C2 . 1.395(4) yes
C1 . C6 . 1.385(4) yes
C2 . C3 . 1.384(4) yes
C2 . H21 . 0.901 no
C3 . C4 . 1.378(5) yes
C3 . H31 . 0.900 no
C4 . C5 . 1.376(5) yes
C4 . H41 . 0.914 no
C5 . C6 . 1.386(4) yes
C5 . H51 . 0.899 no
C6 . H61 . 0.923 no
C7 . C8 . 1.389(5) yes
C7 . C12 . 1.387(5) yes
C8 . C9 . 1.390(5) yes
C8 . H81 . 0.941 no
C9 . C10 . 1.363(6) yes
C9 . H91 . 0.981 no
C10 . C11 . 1.394(6) yes
C10 . H101 . 0.930 no
C11 . C12 . 1.389(5) yes
C11 . H111 . 0.945 no
C12 . H121 . 0.916 no
C13 . C14 . 1.392(4) yes
C13 . C18 . 1.403(4) yes
C14 . C15 . 1.384(4) yes
C14 . H141 . 0.941 no
C15 . C16 . 1.379(5) yes
C15 . H151 . 0.960 no
C16 . C17 . 1.385(4) yes
C16 . H161 . 0.941 no
C17 . C18 . 1.398(4) yes
C17 . H171 . 0.949 no
C19 . C20 . 1.502(4) yes
C19 . H191 . 0.994 no
C19 . H192 . 1.006 no
C20 . H201 . 0.988 no
C20 . H202 . 0.968 no
C21 . C22 . 1.399(4) yes
C21 . C26 . 1.415(4) yes
C22 . C23 . 1.384(4) yes
C22 . H221 . 0.923 no
C23 . C24 . 1.371(5) yes
C23 . H231 . 0.884 no
C24 . C25 . 1.387(4) yes
C24 . H241 . 0.959 no
C25 . C26 . 1.387(4) yes
C25 . H251 . 0.934 no
C27 . C28 . 1.395(4) yes
C27 . C32 . 1.394(4) yes
C28 . C29 . 1.390(5) yes
C28 . H281 . 0.927 no
C29 . C30 . 1.379(5) yes
C29 . H291 . 0.937 no
C30 . C31 . 1.374(5) yes
C30 . H301 . 0.953 no
C31 . C32 . 1.392(4) yes
C31 . H311 . 0.930 no
C32 . H321 . 0.929 no
C33 . C34 . 1.397(4) yes
C33 . C38 . 1.390(4) yes
C34 . C35 . 1.382(4) yes
C34 . H341 . 0.917 no
C35 . C36 . 1.386(5) yes
C35 . H351 . 0.962 no
C36 . C37 . 1.374(5) yes
C36 . H361 . 0.917 no
C37 . C38 . 1.390(4) yes
C37 . H371 . 0.933 no
C38 . H381 . 0.916 no
C39 . C40 . 1.402(4) yes
C39 . C44 . 1.380(4) yes
C40 . C41 . 1.385(4) yes
C40 . H401 . 0.857 no
C41 . C42 . 1.382(5) yes
C41 . H411 . 0.938 no
C42 . C43 . 1.385(5) yes
C42 . H421 . 0.943 no
C43 . C44 . 1.383(4) yes
C43 . H431 . 0.939 no
C44 . H441 . 0.918 no
C45 . C46 . 1.386(4) yes
C45 . C50 . 1.392(4) yes
C46 . C47 . 1.397(5) yes
C46 . H461 . 1.003 no
C47 . C48 . 1.372(5) yes
C47 . H471 . 1.028 no
C48 . C49 . 1.381(5) yes
C48 . H481 . 0.960 no
C49 . C50 . 1.391(4) yes
C49 . H491 . 0.990 no
C50 . H501 . 1.014 no
C51 . C52 . 1.397(4) yes
C51 . C56 . 1.407(4) yes
C52 . C53 . 1.381(4) yes
C52 . H521 . 0.951 no
C53 . C54 . 1.379(5) yes
C53 . H531 . 0.947 no
C54 . C55 . 1.385(5) yes
C54 . H541 . 0.944 no
C55 . C56 . 1.396(4) yes
C55 . H551 . 0.949 no
C57 . C58 . 1.513(5) yes
C57 . H571 . 0.989 no
C57 . H572 . 0.903 no
C58 . H581 . 0.904 no
C58 . H582 . 0.956 no
C59 . C60 . 1.394(4) yes
C59 . C64 . 1.405(4) yes
C60 . C61 . 1.378(5) yes
C60 . H601 . 0.919 no
C61 . C62 . 1.382(5) yes
C61 . H611 . 0.893 no
C62 . C63 . 1.385(4) yes
C62 . H621 . 0.941 no
C63 . C64 . 1.390(4) yes
C63 . H631 . 0.949 no
C65 . C66 . 1.391(4) yes
C65 . C70 . 1.388(4) yes
C66 . C67 . 1.385(5) yes
C66 . H661 . 0.876 no
C67 . C68 . 1.389(5) yes
C67 . H671 . 0.959 no
C68 . C69 . 1.373(5) yes
C68 . H681 . 0.897 no
C69 . C70 . 1.380(5) yes
C69 . H691 . 0.953 no
C70 . H701 . 0.948 no
C71 . C72 . 1.394(4) yes
C71 . C76 . 1.393(5) yes
C72 . C73 . 1.387(5) yes
C72 . H721 . 0.933 no
C73 . C74 . 1.376(5) yes
C73 . H731 . 0.915 no
C74 . C75 . 1.382(5) yes
C74 . H741 . 0.912 no
C75 . C76 . 1.385(5) yes
C75 . H751 . 0.963 no
C76 . H761 . 0.973 no
C77 . C78 . 1.392(9) yes
C77 . C82 . 1.380(9) yes
C77 . H771 . 0.993 no
C78 . C79 . 1.389(9) yes
C78 . H781 . 0.930 no
C79 . C80 . 1.318(8) yes
C79 . H791 . 0.944 no
C80 . C81 . 1.359(8) yes
C80 . H801 . 0.983 no
C81 . C82 . 1.361(9) yes
C81 . H811 . 0.984 no
C82 . H821 . 0.939 no
C83 . C84 . 1.439(9) yes
C83 . H831 . 0.950 no
C83 . H832 . 0.950 no
C83 . H833 . 0.950 no
C84 . H841 . 0.950 no
C84 . H842 . 0.950 no
C85 . C86 . 1.405(7) yes
C85 . H851 . 0.950 no
C85 . H852 . 0.950 no
C86 . H861 . 0.950 no
C86 . H862 . 0.950 no
C86 . H863 . 0.950 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Ni2 . Ni1 . Ni3 . 66.389(15) yes
Ni2 . Ni1 . Cl1 . 104.89(2) yes
Ni3 . Ni1 . Cl1 . 54.45(2) yes
Ni2 . Ni1 . Cl2 . 103.94(2) yes
Ni3 . Ni1 . Cl2 . 63.18(2) yes
Cl1 . Ni1 . Cl2 . 87.75(3) yes
Ni2 . Ni1 . P1 . 128.28(3) yes
Ni3 . Ni1 . P1 . 165.33(3) yes
Cl1 . Ni1 . P1 . 115.58(3) yes
Cl2 . Ni1 . P1 . 108.31(3) yes
Ni2 . Ni1 . P2 . 50.46(2) yes
Ni3 . Ni1 . P2 . 97.51(3) yes
Cl1 . Ni1 . P2 . 94.67(3) yes
Cl2 . Ni1 . P2 . 154.04(3) yes
P1 . Ni1 . P2 . 93.95(3) yes
Ni1 . Ni2 . Ni3 . 51.833(13) yes
Ni1 . Ni2 . P2 . 47.84(2) yes
Ni3 . Ni2 . P2 . 84.45(2) yes
Ni1 . Ni2 . P3 . 129.15(3) yes
Ni3 . Ni2 . P3 . 107.71(3) yes
P2 . Ni2 . P3 . 89.48(3) yes
Ni1 . Ni2 . P4 . 103.89(3) yes
Ni3 . Ni2 . P4 . 121.51(3) yes
P2 . Ni2 . P4 . 119.61(3) yes
P3 . Ni2 . P4 . 123.37(3) yes
Ni1 . Ni2 . P5 . 90.14(3) yes
Ni3 . Ni2 . P5 . 46.23(2) yes
P2 . Ni2 . P5 . 130.64(3) yes
P3 . Ni2 . P5 . 105.32(3) yes
P4 . Ni2 . P5 . 91.15(3) yes
Ni2 . Ni3 . Ni1 . 61.778(14) yes
Ni2 . Ni3 . Cl1 . 107.80(2) yes
Ni1 . Ni3 . Cl1 . 63.39(2) yes
Ni2 . Ni3 . Cl2 . 95.56(2) yes
Ni1 . Ni3 . Cl2 . 54.64(2) yes
Cl1 . Ni3 . Cl2 . 87.99(3) yes
Ni2 . Ni3 . P5 . 47.80(2) yes
Ni1 . Ni3 . P5 . 100.18(3) yes
Cl1 . Ni3 . P5 . 155.33(3) yes
Cl2 . Ni3 . P5 . 97.16(3) yes
Ni2 . Ni3 . P6 . 128.39(3) yes
Ni1 . Ni3 . P6 . 168.12(3) yes
Cl1 . Ni3 . P6 . 105.37(3) yes
Cl2 . Ni3 . P6 . 124.13(3) yes
P5 . Ni3 . P6 . 91.70(3) yes
Ni1 . Cl1 . Ni3 . 62.16(2) yes
Ni3 . Cl2 . Ni1 . 62.18(2) yes
Ni1 . P1 . C1 . 118.58(10) yes
Ni1 . P1 . C7 . 114.14(10) yes
C1 . P1 . C7 . 102.57(14) yes
Ni1 . P1 . C13 . 116.97(10) yes
C1 . P1 . C13 . 101.63(14) yes
C7 . P1 . C13 . 100.31(14) yes
Ni2 . P2 . Ni1 . 81.70(3) yes
Ni2 . P2 . N1 . 137.05(9) yes
Ni1 . P2 . N1 . 117.32(9) yes
Ni2 . P2 . N2 . 113.70(9) yes
Ni1 . P2 . N2 . 123.45(9) yes
N1 . P2 . N2 . 88.48(12) yes
Ni2 . P3 . C26 . 108.27(10) yes
Ni2 . P3 . C27 . 115.81(10) yes
C26 . P3 . C27 . 101.48(14) yes
Ni2 . P3 . C33 . 123.84(10) yes
C26 . P3 . C33 . 104.55(14) yes
C27 . P3 . C33 . 100.25(13) yes
Ni2 . P4 . C39 . 127.16(10) yes
Ni2 . P4 . C45 . 115.94(10) yes
C39 . P4 . C45 . 96.46(14) yes
Ni2 . P4 . C51 . 110.57(10) yes
C39 . P4 . C51 . 100.79(14) yes
C45 . P4 . C51 . 102.39(14) yes
Ni2 . P5 . Ni3 . 85.97(3) yes
Ni2 . P5 . N3 . 115.89(10) yes
Ni3 . P5 . N3 . 124.03(10) yes
Ni2 . P5 . N4 . 130.28(10) yes
Ni3 . P5 . N4 . 116.45(9) yes
N3 . P5 . N4 . 88.67(13) yes
Ni3 . P6 . C64 . 113.58(10) yes
Ni3 . P6 . C65 . 115.08(10) yes
C64 . P6 . C65 . 102.95(14) yes
Ni3 . P6 . C71 . 121.44(10) yes
C64 . P6 . C71 . 99.96(14) yes
C65 . P6 . C71 . 101.19(14) yes
C84 . O1 . C85 . 105.9(6) yes
P2 . N1 . C18 . 127.5(2) yes
P2 . N1 . C19 . 114.5(2) yes
C18 . N1 . C19 . 117.5(2) yes
P2 . N2 . C20 . 112.40(19) yes
P2 . N2 . C21 . 127.3(2) yes
C20 . N2 . C21 . 119.6(2) yes
P5 . N3 . C56 . 124.6(2) yes
P5 . N3 . C57 . 113.9(2) yes
C56 . N3 . C57 . 119.8(3) yes
P5 . N4 . C58 . 114.7(2) yes
P5 . N4 . C59 . 125.6(2) yes
C58 . N4 . C59 . 119.6(2) yes
P1 . C1 . C2 . 122.6(2) yes
P1 . C1 . C6 . 118.5(2) yes
C2 . C1 . C6 . 118.6(3) yes
C1 . C2 . C3 . 120.4(3) yes
C1 . C2 . H21 . 118.9 no
C3 . C2 . H21 . 120.4 no
C2 . C3 . C4 . 120.4(3) yes
C2 . C3 . H31 . 120.3 no
C4 . C3 . H31 . 119.2 no
C3 . C4 . C5 . 119.6(3) yes
C3 . C4 . H41 . 121.4 no
C5 . C4 . H41 . 119.0 no
C4 . C5 . C6 . 120.4(3) yes
C4 . C5 . H51 . 120.7 no
C6 . C5 . H51 . 118.8 no
C5 . C6 . C1 . 120.5(3) yes
C5 . C6 . H61 . 121.8 no
C1 . C6 . H61 . 117.7 no
P1 . C7 . C8 . 123.3(3) yes
P1 . C7 . C12 . 117.7(3) yes
C8 . C7 . C12 . 119.0(3) yes
C7 . C8 . C9 . 120.6(4) yes
C7 . C8 . H81 . 118.7 no
C9 . C8 . H81 . 120.7 no
C8 . C9 . C10 . 120.3(4) yes
C8 . C9 . H91 . 118.5 no
C10 . C9 . H91 . 121.2 no
C9 . C10 . C11 . 119.9(3) yes
C9 . C10 . H101 . 131.5 no
C11 . C10 . H101 . 108.6 no
C10 . C11 . C12 . 120.1(4) yes
C10 . C11 . H111 . 121.1 no
C12 . C11 . H111 . 118.9 no
C11 . C12 . C7 . 120.1(4) yes
C11 . C12 . H121 . 119.8 no
C7 . C12 . H121 . 120.1 no
P1 . C13 . C14 . 122.1(2) yes
P1 . C13 . C18 . 118.7(2) yes
C14 . C13 . C18 . 118.3(3) yes
C13 . C14 . C15 . 122.1(3) yes
C13 . C14 . H141 . 119.4 no
C15 . C14 . H141 . 118.5 no
C14 . C15 . C16 . 119.1(3) yes
C14 . C15 . H151 . 122.2 no
C16 . C15 . H151 . 118.6 no
C15 . C16 . C17 . 120.1(3) yes
C15 . C16 . H161 . 120.5 no
C17 . C16 . H161 . 119.4 no
C16 . C17 . C18 . 120.8(3) yes
C16 . C17 . H171 . 114.8 no
C18 . C17 . H171 . 124.3 no
N1 . C18 . C13 . 122.2(3) yes
N1 . C18 . C17 . 118.4(3) yes
C13 . C18 . C17 . 119.2(3) yes
N1 . C19 . C20 . 103.5(2) yes
N1 . C19 . H191 . 108.6 no
C20 . C19 . H191 . 110.4 no
N1 . C19 . H192 . 112.5 no
C20 . C19 . H192 . 114.6 no
H191 . C19 . H192 . 107.2 no
C19 . C20 . N2 . 102.4(2) yes
C19 . C20 . H201 . 114.9 no
N2 . C20 . H201 . 101.5 no
C19 . C20 . H202 . 118.8 no
N2 . C20 . H202 . 105.8 no
H201 . C20 . H202 . 111.0 no
N2 . C21 . C22 . 119.7(3) yes
N2 . C21 . C26 . 121.1(3) yes
C22 . C21 . C26 . 119.1(3) yes
C21 . C22 . C23 . 120.4(3) yes
C21 . C22 . H221 . 118.2 no
C23 . C22 . H221 . 121.3 no
C22 . C23 . C24 . 120.7(3) yes
C22 . C23 . H231 . 114.2 no
C24 . C23 . H231 . 125.1 no
C23 . C24 . C25 . 119.5(3) yes
C23 . C24 . H241 . 122.7 no
C25 . C24 . H241 . 117.6 no
C24 . C25 . C26 . 121.5(3) yes
C24 . C25 . H251 . 119.6 no
C26 . C25 . H251 . 118.9 no
P3 . C26 . C21 . 117.3(2) yes
P3 . C26 . C25 . 124.1(2) yes
C21 . C26 . C25 . 118.6(3) yes
P3 . C27 . C28 . 123.0(2) yes
P3 . C27 . C32 . 118.5(2) yes
C28 . C27 . C32 . 118.5(3) yes
C27 . C28 . C29 . 120.2(3) yes
C27 . C28 . H281 . 118.5 no
C29 . C28 . H281 . 121.3 no
C28 . C29 . C30 . 120.5(3) yes
C28 . C29 . H291 . 119.4 no
C30 . C29 . H291 . 120.1 no
C29 . C30 . C31 . 120.1(3) yes
C29 . C30 . H301 . 119.9 no
C31 . C30 . H301 . 120.0 no
C30 . C31 . C32 . 119.9(3) yes
C30 . C31 . H311 . 121.7 no
C32 . C31 . H311 . 118.3 no
C27 . C32 . C31 . 120.8(3) yes
C27 . C32 . H321 . 118.5 no
C31 . C32 . H321 . 120.6 no
P3 . C33 . C34 . 123.0(2) yes
P3 . C33 . C38 . 118.7(2) yes
C34 . C33 . C38 . 118.2(3) yes
C33 . C34 . C35 . 120.6(3) yes
C33 . C34 . H341 . 120.7 no
C35 . C34 . H341 . 118.6 no
C34 . C35 . C36 . 120.1(3) yes
C34 . C35 . H351 . 122.4 no
C36 . C35 . H351 . 117.4 no
C35 . C36 . C37 . 120.1(3) yes
C35 . C36 . H361 . 115.2 no
C37 . C36 . H361 . 124.6 no
C36 . C37 . C38 . 119.8(3) yes
C36 . C37 . H371 . 118.8 no
C38 . C37 . H371 . 121.4 no
C33 . C38 . C37 . 121.0(3) yes
C33 . C38 . H381 . 120.2 no
C37 . C38 . H381 . 118.7 no
P4 . C39 . C40 . 120.0(2) yes
P4 . C39 . C44 . 121.3(2) yes
C40 . C39 . C44 . 118.6(3) yes
C39 . C40 . C41 . 120.5(3) yes
C39 . C40 . H401 . 122.5 no
C41 . C40 . H401 . 117.0 no
C40 . C41 . C42 . 119.9(3) yes
C40 . C41 . H411 . 121.9 no
C42 . C41 . H411 . 117.9 no
C41 . C42 . C43 . 120.0(3) yes
C41 . C42 . H421 . 120.5 no
C43 . C42 . H421 . 119.4 no
C42 . C43 . C44 . 119.9(3) yes
C42 . C43 . H431 . 116.6 no
C44 . C43 . H431 . 123.5 no
C43 . C44 . C39 . 121.1(3) yes
C43 . C44 . H441 . 122.1 no
C39 . C44 . H441 . 116.9 no
P4 . C45 . C46 . 124.9(2) yes
P4 . C45 . C50 . 116.5(2) yes
C46 . C45 . C50 . 118.5(3) yes
C45 . C46 . C47 . 120.6(3) yes
C45 . C46 . H461 . 123.2 no
C47 . C46 . H461 . 116.0 no
C46 . C47 . C48 . 120.2(3) yes
C46 . C47 . H471 . 117.8 no
C48 . C47 . H471 . 121.7 no
C47 . C48 . C49 . 120.0(3) yes
C47 . C48 . H481 . 119.7 no
C49 . C48 . H481 . 120.3 no
C48 . C49 . C50 . 119.8(3) yes
C48 . C49 . H491 . 122.3 no
C50 . C49 . H491 . 117.9 no
C45 . C50 . C49 . 120.9(3) yes
C45 . C50 . H501 . 121.2 no
C49 . C50 . H501 . 117.9 no
P4 . C51 . C52 . 123.1(3) yes
P4 . C51 . C56 . 118.8(2) yes
C52 . C51 . C56 . 118.1(3) yes
C51 . C52 . C53 . 121.8(3) yes
C51 . C52 . H521 . 119.0 no
C53 . C52 . H521 . 119.1 no
C52 . C53 . C54 . 119.4(3) yes
C52 . C53 . H531 . 119.0 no
C54 . C53 . H531 . 121.5 no
C53 . C54 . C55 . 120.4(3) yes
C53 . C54 . H541 . 122.3 no
C55 . C54 . H541 . 117.1 no
C54 . C55 . C56 . 120.5(3) yes
C54 . C55 . H551 . 121.3 no
C56 . C55 . H551 . 118.1 no
C51 . C56 . N3 . 120.1(3) yes
C51 . C56 . C55 . 119.6(3) yes
N3 . C56 . C55 . 120.2(3) yes
N3 . C57 . C58 . 103.0(3) yes
N3 . C57 . H571 . 109.6 no
C58 . C57 . H571 . 110.0 no
N3 . C57 . H572 . 110.0 no
C58 . C57 . H572 . 114.6 no
H571 . C57 . H572 . 109.4 no
C57 . C58 . N4 . 103.8(3) yes
C57 . C58 . H581 . 112.4 no
N4 . C58 . H581 . 111.1 no
C57 . C58 . H582 . 107.3 no
N4 . C58 . H582 . 115.0 no
H581 . C58 . H582 . 107.3 no
N4 . C59 . C60 . 120.4(3) yes
N4 . C59 . C64 . 119.8(3) yes
C60 . C59 . C64 . 119.7(3) yes
C59 . C60 . C61 . 120.8(3) yes
C59 . C60 . H601 . 117.8 no
C61 . C60 . H601 . 121.3 no
C60 . C61 . C62 . 119.7(3) yes
C60 . C61 . H611 . 121.1 no
C62 . C61 . H611 . 119.2 no
C61 . C62 . C63 . 120.1(3) yes
C61 . C62 . H621 . 124.3 no
C63 . C62 . H621 . 115.6 no
C62 . C63 . C64 . 121.1(3) yes
C62 . C63 . H631 . 117.4 no
C64 . C63 . H631 . 121.5 no
P6 . C64 . C59 . 118.1(2) yes
P6 . C64 . C63 . 123.4(2) yes
C59 . C64 . C63 . 118.5(3) yes
P6 . C65 . C66 . 116.8(2) yes
P6 . C65 . C70 . 123.8(2) yes
C66 . C65 . C70 . 119.1(3) yes
C65 . C66 . C67 . 120.6(3) yes
C65 . C66 . H661 . 122.7 no
C67 . C66 . H661 . 116.7 no
C66 . C67 . C68 . 119.3(3) yes
C66 . C67 . H671 . 124.1 no
C68 . C67 . H671 . 116.5 no
C67 . C68 . C69 . 120.4(3) yes
C67 . C68 . H681 . 117.5 no
C69 . C68 . H681 . 122.1 no
C68 . C69 . C70 . 120.3(4) yes
C68 . C69 . H691 . 116.0 no
C70 . C69 . H691 . 123.6 no
C65 . C70 . C69 . 120.3(3) yes
C65 . C70 . H701 . 116.7 no
C69 . C70 . H701 . 123.0 no
P6 . C71 . C72 . 122.8(3) yes
P6 . C71 . C76 . 117.6(2) yes
C72 . C71 . C76 . 119.3(3) yes
C71 . C72 . C73 . 120.3(3) yes
C71 . C72 . H721 . 121.9 no
C73 . C72 . H721 . 117.7 no
C72 . C73 . C74 . 119.9(3) yes
C72 . C73 . H731 . 117.8 no
C74 . C73 . H731 . 121.9 no
C73 . C74 . C75 . 120.2(3) yes
C73 . C74 . H741 . 120.1 no
C75 . C74 . H741 . 119.7 no
C74 . C75 . C76 . 120.4(4) yes
C74 . C75 . H751 . 117.9 no
C76 . C75 . H751 . 121.4 no
C71 . C76 . C75 . 119.8(3) yes
C71 . C76 . H761 . 121.2 no
C75 . C76 . H761 . 119.0 no
C78 . C77 . C82 . 116.1(7) yes
C78 . C77 . H771 . 123.9 no
C82 . C77 . H771 . 119.6 no
C77 . C78 . C79 . 120.5(7) yes
C77 . C78 . H781 . 117.2 no
C79 . C78 . H781 . 121.9 no
C78 . C79 . C80 . 121.1(6) yes
C78 . C79 . H791 . 122.5 no
C80 . C79 . H791 . 116.4 no
C79 . C80 . C81 . 120.2(7) yes
C79 . C80 . H801 . 124.4 no
C81 . C80 . H801 . 115.5 no
C80 . C81 . C82 . 120.1(7) yes
C80 . C81 . H811 . 116.3 no
C82 . C81 . H811 . 123.3 no
C77 . C82 . C81 . 122.1(7) yes
C77 . C82 . H821 . 117.4 no
C81 . C82 . H821 . 120.5 no
C84 . C83 . H831 . 109.2 no
C84 . C83 . H832 . 109.3 no
H831 . C83 . H832 . 109.5 no
C84 . C83 . H833 . 109.9 no
H831 . C83 . H833 . 109.5 no
H832 . C83 . H833 . 109.5 no
C83 . C84 . O1 . 109.9(7) yes
C83 . C84 . H841 . 109.8 no
O1 . C84 . H841 . 109.9 no
C83 . C84 . H842 . 109.2 no
O1 . C84 . H842 . 108.6 no
H841 . C84 . H842 . 109.5 no
O1 . C85 . C86 . 105.8(8) yes
O1 . C85 . H851 . 113.6 no
C86 . C85 . H851 . 115.1 no
O1 . C85 . H852 . 107.3 no
C86 . C85 . H852 . 105.0 no
H851 . C85 . H852 . 109.5 no
C85 . C86 . H861 . 106.6 no
C85 . C86 . H862 . 106.5 no
H861 . C86 . H862 . 109.5 no
C85 . C86 . H863 . 115.1 no
H861 . C86 . H863 . 109.5 no
H862 . C86 . H863 . 109.5 no


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 15/10/13 at 13:03:48
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   2,X'S) H   (  21,X'S) 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 171,X'S) 
RIDE C   (  19,X'S) H   ( 191,X'S) H   ( 192,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) 
RIDE C   (  31,X'S) H   ( 311,X'S) 
RIDE C   (  32,X'S) H   ( 321,X'S) 
RIDE C   (  34,X'S) H   ( 341,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  36,X'S) H   ( 361,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  38,X'S) H   ( 381,X'S) 
RIDE C   (  40,X'S) H   ( 401,X'S) 
RIDE C   (  41,X'S) H   ( 411,X'S) 
RIDE C   (  42,X'S) H   ( 421,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  44,X'S) H   ( 441,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  47,X'S) H   ( 471,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  49,X'S) H   ( 491,X'S) 
RIDE C   (  50,X'S) H   ( 501,X'S) 
RIDE C   (  52,X'S) H   ( 521,X'S) 
RIDE C   (  53,X'S) H   ( 531,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  55,X'S) H   ( 551,X'S) 
RIDE C   (  57,X'S) H   ( 571,X'S) H   ( 572,X'S) 
RIDE C   (  58,X'S) H   ( 581,X'S) H   ( 582,X'S) 
RIDE C   (  60,X'S) H   ( 601,X'S) 
RIDE C   (  61,X'S) H   ( 611,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  63,X'S) H   ( 631,X'S) 
RIDE C   (  66,X'S) H   ( 661,X'S) 
RIDE C   (  67,X'S) H   ( 671,X'S) 
RIDE C   (  68,X'S) H   ( 681,X'S) 
RIDE C   (  69,X'S) H   ( 691,X'S) 
RIDE C   (  70,X'S) H   ( 701,X'S) 
RIDE C   (  72,X'S) H   ( 721,X'S) 
RIDE C   (  73,X'S) H   ( 731,X'S) 
RIDE C   (  74,X'S) H   ( 741,X'S) 
RIDE C   (  75,X'S) H   ( 751,X'S) 
RIDE C   (  76,X'S) H   ( 761,X'S) 
RIDE C   (  77,X'S) H   ( 771,X'S) 
RIDE C   (  78,X'S) H   ( 781,X'S) 
RIDE C   (  79,X'S) H   ( 791,X'S) 
RIDE C   (  80,X'S) H   ( 801,X'S) 
RIDE C   (  81,X'S) H   ( 811,X'S) 
RIDE C   (  82,X'S) H   ( 821,X'S) 
RIDE C   (  83,X'S) H   ( 833,X'S) H   ( 832,X'S) H   ( 831,X'S) 
RIDE C   (  84,X'S) H   ( 841,X'S) H   ( 842,X'S) 
RIDE C   (  85,X'S) H   ( 851,X'S) H   ( 852,X'S) 
RIDE C   (  86,X'S) H   ( 863,X'S) H   ( 862,X'S) H   ( 861,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 15/10/13 at 13:03:48
#
#LIST     16                                                                    
NO 
DISTANCE 1.540000 , 0.010000 = C(85) TO C(86) 
END                                                                             
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.250 0.125 184 42 ' '
2 0.000 0.750 0.875 184 42 ' '
3 0.500 0.250 0.375 184 42 ' '
4 0.500 0.750 0.625 184 42 ' '
_platon_squeeze_details          
;
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Et2O, benzene'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_10
_database_code_depnum_ccdc_archive 'CCDC 1420819'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;
_audit_creation_date             2015-03-05
_audit_creation_method           CRYSTALS_ver_14.61

_oxford_structure_analysis_title 'dem4_162_0m in I-4c2'
_chemical_name_systematic        ?
_chemical_melting_point          ?

_cell_length_a                   16.6009(8)
_cell_length_b                   16.6009(8)
_cell_length_c                   25.9072(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7139.8(4)

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I -4 c 2 '
_symmetry_space_group_name_Hall  'I -4 -2c '
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
x+1/2,y+1/2,z+1/2
y,-x,-z
y+1/2,-x+1/2,-z+1/2
-x,-y,z
-x+1/2,-y+1/2,z+1/2
-y,x,-z
-y+1/2,x+1/2,-z+1/2
-x,y,z+1/2
-x+1/2,y+1/2,z+1
-y,-x,-z+1/2
-y+1/2,-x+1/2,-z+1
x,-y,z+1/2
x+1/2,-y+1/2,z+1
y,x,-z+1/2
y+1/2,x+1/2,-z+1

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C38 H32 N2 Ni1 P3 
# Dc =      1.24 Fooo =   2776.00 Mu =      7.05 M =    334.16
# Found Formula = C38 H32 N2 Ni1 P3 
# Dc =      1.24 FOOO =   2776.00 Mu =      7.05 M =    334.16

_chemical_formula_sum            'C38 H32 N2 Ni1 P3'
_chemical_formula_moiety         'C38 H32 N2 Ni1 P3'
_chemical_compound_source        ?
_chemical_formula_weight         668.32


_cell_measurement_reflns_used    9755
_cell_measurement_theta_min      3
_cell_measurement_theta_max      29
_cell_measurement_temperature    120

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_size_min          0.200
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_max          0.380

_exptl_crystal_density_diffrn    1.243
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2776
_exptl_absorpt_coefficient_mu    0.705

# Sheldrick geometric approximatio 0.82 0.87 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_T_max  0.87
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      120
_diffrn_reflns_number            4786
_reflns_number_total             4786
_diffrn_reflns_av_R_equivalents  0.065
# Number of reflections without Friedels Law is 4786 
# Number of reflections with Friedels Law is 2566 
# Theoretical number of reflections is about 2419 


_diffrn_reflns_theta_min         1.572
_diffrn_reflns_theta_max         29.206
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        28.622
_diffrn_measured_fraction_theta_full 0.998


_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       35
_reflns_limit_h_min              0
_reflns_limit_h_max              22
_reflns_limit_k_min              0
_reflns_limit_k_max              22
_reflns_limit_l_min              0
_reflns_limit_l_max              35

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.75
_refine_diff_density_max         0.84


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         4786
_refine_ls_number_restraints     0
_refine_ls_number_parameters     200
_oxford_refine_ls_R_factor_ref   0.0637
_refine_ls_wR_factor_ref         0.1284
_refine_ls_goodness_of_fit_ref   0.9777
_refine_ls_shift/su_max          0.0027460
_refine_ls_shift/su_mean         0.0007454


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        4786
_refine_ls_R_factor_all          0.0637
_refine_ls_wR_factor_all         0.1284

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                4015
_refine_ls_R_factor_gt           0.0514
_refine_ls_wR_factor_gt          0.1220

_refine_ls_abs_structure_Flack   0.010(15)
_refine_ls_abs_structure_details 'Flack (1983), 2220 Friedel-pairs'
# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration ad


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² +39.23P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.44645(2) 0.55355(2) 0.7500 0.0191 1.0000 Uani S T . . . .
P1 P 0.37241(5) 0.56729(5) 0.68233(4) 0.0218 1.0000 Uani . . . . . .
P2 P 0.42734(4) 0.42734(4) 0.7500 0.0206 1.0000 Uani S T . . . .
N1 N 0.36283(18) 0.38793(17) 0.70417(14) 0.0284 1.0000 Uani . . . . . .
C1 C 0.3780(2) 0.6598(2) 0.64361(17) 0.0281 1.0000 Uani . . . . . .
C2 C 0.4444(3) 0.7097(3) 0.6507(2) 0.0368 1.0000 Uani . . . . . .
C3 C 0.4501(3) 0.7830(3) 0.6246(3) 0.0625 1.0000 Uani . . . . . .
C4 C 0.3907(3) 0.8054(3) 0.5913(3) 0.0572 1.0000 Uani . . . . . .
C5 C 0.3256(3) 0.7569(3) 0.5832(2) 0.0512 1.0000 Uani . . . . . .
C6 C 0.3183(3) 0.6843(3) 0.60927(18) 0.0444 1.0000 Uani . . . . . .
C7 C 0.2618(2) 0.5621(2) 0.69102(16) 0.0234 1.0000 Uani . . . . . .
C8 C 0.2275(2) 0.6046(2) 0.73109(17) 0.0273 1.0000 Uani . . . . . .
C9 C 0.1437(2) 0.6070(2) 0.73749(17) 0.0309 1.0000 Uani . . . . . .
C10 C 0.0943(2) 0.5676(2) 0.70414(18) 0.0342 1.0000 Uani . . . . . .
C11 C 0.1278(2) 0.5226(3) 0.6645(2) 0.0465 1.0000 Uani . . . . . .
C12 C 0.2115(2) 0.5202(3) 0.6575(2) 0.0402 1.0000 Uani . . . . . .
C13 C 0.3844(2) 0.4868(2) 0.63527(16) 0.0268 1.0000 Uani . . . . . .
C14 C 0.3948(2) 0.5021(3) 0.58255(17) 0.0343 1.0000 Uani . . . . . .
C15 C 0.3899(3) 0.4424(3) 0.5461(2) 0.0490 1.0000 Uani . . . . . .
C16 C 0.3744(3) 0.3636(4) 0.5615(2) 0.0517 1.0000 Uani . . . . . .
C17 C 0.3660(3) 0.3450(3) 0.6149(2) 0.0435 1.0000 Uani . . . . . .
C18 C 0.3715(2) 0.4061(2) 0.65141(17) 0.0294 1.0000 Uani . . . . . .
C19 C 0.3252(3) 0.3125(2) 0.72122(18) 0.0365 1.0000 Uani . . . . . .
H21 H 0.4856 0.6933 0.6737 0.0442 1.0000 Uiso R . . . . .
H31 H 0.4947 0.8158 0.6307 0.0750 1.0000 Uiso R . . . . .
H41 H 0.3950 0.8550 0.5736 0.0691 1.0000 Uiso R . . . . .
H51 H 0.2856 0.7721 0.5598 0.0615 1.0000 Uiso R . . . . .
H61 H 0.2736 0.6512 0.6040 0.0530 1.0000 Uiso R . . . . .
H81 H 0.2606 0.6324 0.7541 0.0331 1.0000 Uiso R . . . . .
H91 H 0.1208 0.6351 0.7652 0.0367 1.0000 Uiso R . . . . .
H101 H 0.0386 0.5722 0.7074 0.0404 1.0000 Uiso R . . . . .
H111 H 0.0946 0.4940 0.6415 0.0560 1.0000 Uiso R . . . . .
H121 H 0.2337 0.4901 0.6310 0.0484 1.0000 Uiso R . . . . .
H141 H 0.4048 0.5554 0.5720 0.0415 1.0000 Uiso R . . . . .
H151 H 0.3964 0.4556 0.5112 0.0589 1.0000 Uiso R . . . . .
H161 H 0.3705 0.3235 0.5365 0.0622 1.0000 Uiso R . . . . .
H171 H 0.3561 0.2913 0.6257 0.0518 1.0000 Uiso R . . . . .
H191 H 0.2748 0.3027 0.7024 0.0441 1.0000 Uiso R . . . . .
H192 H 0.3612 0.2671 0.7154 0.0443 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.057406(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . P1 11_666 2.1532(11) yes
Ni1 . P2 5_665 2.1191(8) yes
Ni1 . Ni1 5_665 2.5146(10) yes
Ni1 . P1 . 2.1532(11) yes
Ni1 . P2 . 2.1191(8) yes
P1 . C1 . 1.836(4) yes
P1 . C7 . 1.852(3) yes
P1 . C13 . 1.820(4) yes
P2 . N1 15_556 1.728(3) yes
P2 . N1 . 1.728(3) yes
N1 . C18 . 1.407(6) yes
N1 . C19 . 1.467(5) yes
C1 . C2 . 1.391(5) yes
C1 . C6 . 1.393(6) yes
C2 . C3 . 1.395(6) yes
C2 . H21 . 0.947 no
C3 . C4 . 1.363(8) yes
C3 . H31 . 0.934 no
C4 . C5 . 1.365(8) yes
C4 . H41 . 0.944 no
C5 . C6 . 1.386(7) yes
C5 . H51 . 0.933 no
C6 . H61 . 0.935 no
C7 . C8 . 1.379(5) yes
C7 . C12 . 1.391(6) yes
C8 . C9 . 1.401(5) yes
C8 . H81 . 0.934 no
C9 . C10 . 1.359(6) yes
C9 . H91 . 0.937 no
C10 . C11 . 1.386(7) yes
C10 . H101 . 0.931 no
C11 . C12 . 1.403(5) yes
C11 . H111 . 0.940 no
C12 . H121 . 0.925 no
C13 . C14 . 1.400(6) yes
C13 . C18 . 1.419(5) yes
C14 . C15 . 1.373(7) yes
C14 . H141 . 0.940 no
C15 . C16 . 1.391(8) yes
C15 . H151 . 0.937 no
C16 . C17 . 1.424(7) yes
C16 . H161 . 0.933 no
C17 . C18 . 1.389(6) yes
C17 . H171 . 0.949 no
C19 . C19 15_556 1.520(9) yes
C19 . H191 . 0.981 no
C19 . H192 . 0.974 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P1 11_666 Ni1 . P2 5_665 91.11(2) yes
P1 11_666 Ni1 . Ni1 5_665 118.59(3) yes
P2 5_665 Ni1 . Ni1 5_665 53.606(19) yes
P1 11_666 Ni1 . P1 . 122.82(5) yes
P2 5_665 Ni1 . P1 . 123.27(2) yes
Ni1 5_665 Ni1 . P1 . 118.59(3) yes
P1 11_666 Ni1 . P2 . 123.27(2) yes
P2 5_665 Ni1 . P2 . 107.21(4) yes
Ni1 5_665 Ni1 . P2 . 53.606(19) yes
P1 . Ni1 . P2 . 91.11(2) yes
Ni1 . P1 . C1 . 120.30(13) yes
Ni1 . P1 . C7 . 117.52(14) yes
C1 . P1 . C7 . 98.96(16) yes
Ni1 . P1 . C13 . 113.90(13) yes
C1 . P1 . C13 . 104.04(19) yes
C7 . P1 . C13 . 98.95(16) yes
N1 15_556 P2 . Ni1 5_665 117.86(10) yes
N1 15_556 P2 . Ni1 . 132.03(11) yes
Ni1 5_665 P2 . Ni1 . 72.79(4) yes
N1 15_556 P2 . N1 . 90.2(2) yes
Ni1 5_665 P2 . N1 . 132.03(11) yes
Ni1 . P2 . N1 . 117.86(10) yes
P2 . N1 . C18 . 121.5(2) yes
P2 . N1 . C19 . 112.4(3) yes
C18 . N1 . C19 . 121.3(3) yes
P1 . C1 . C2 . 117.8(3) yes
P1 . C1 . C6 . 123.9(3) yes
C2 . C1 . C6 . 118.2(4) yes
C1 . C2 . C3 . 120.6(4) yes
C1 . C2 . H21 . 118.9 no
C3 . C2 . H21 . 120.5 no
C2 . C3 . C4 . 119.8(5) yes
C2 . C3 . H31 . 118.8 no
C4 . C3 . H31 . 121.4 no
C3 . C4 . C5 . 120.6(5) yes
C3 . C4 . H41 . 119.4 no
C5 . C4 . H41 . 120.0 no
C4 . C5 . C6 . 120.4(5) yes
C4 . C5 . H51 . 120.3 no
C6 . C5 . H51 . 119.3 no
C1 . C6 . C5 . 120.3(5) yes
C1 . C6 . H61 . 119.1 no
C5 . C6 . H61 . 120.5 no
P1 . C7 . C8 . 118.5(3) yes
P1 . C7 . C12 . 122.8(3) yes
C8 . C7 . C12 . 118.6(3) yes
C7 . C8 . C9 . 120.9(4) yes
C7 . C8 . H81 . 119.4 no
C9 . C8 . H81 . 119.7 no
C8 . C9 . C10 . 120.7(4) yes
C8 . C9 . H91 . 120.5 no
C10 . C9 . H91 . 118.7 no
C9 . C10 . C11 . 119.2(4) yes
C9 . C10 . H101 . 120.1 no
C11 . C10 . H101 . 120.7 no
C10 . C11 . C12 . 120.6(4) yes
C10 . C11 . H111 . 120.4 no
C12 . C11 . H111 . 118.9 no
C11 . C12 . C7 . 119.9(4) yes
C11 . C12 . H121 . 120.5 no
C7 . C12 . H121 . 119.6 no
P1 . C13 . C14 . 122.2(3) yes
P1 . C13 . C18 . 118.6(3) yes
C14 . C13 . C18 . 118.5(4) yes
C13 . C14 . C15 . 122.2(5) yes
C13 . C14 . H141 . 118.5 no
C15 . C14 . H141 . 119.3 no
C14 . C15 . C16 . 119.4(5) yes
C14 . C15 . H151 . 119.2 no
C16 . C15 . H151 . 121.4 no
C15 . C16 . C17 . 120.1(5) yes
C15 . C16 . H161 . 118.9 no
C17 . C16 . H161 . 121.0 no
C16 . C17 . C18 . 119.7(5) yes
C16 . C17 . H171 . 120.5 no
C18 . C17 . H171 . 119.8 no
C13 . C18 . N1 . 120.2(3) yes
C13 . C18 . C17 . 119.9(4) yes
N1 . C18 . C17 . 119.9(4) yes
C19 15_556 C19 . N1 . 103.7(3) yes
C19 15_556 C19 . H191 . 113.1 no
N1 . C19 . H191 . 110.8 no
C19 15_556 C19 . H192 . 110.1 no
N1 . C19 . H192 . 110.6 no
H191 . C19 . H192 . 108.4 no



# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 311 88 ' '
2 0.000 0.500 0.500 311 88 ' '
3 0.500 0.000 0.500 311 88 ' '
4 0.500 1.000 0.000 311 88 ' '
_platon_squeeze_details          
;
During the structure solution, electron density difference 
maps revealed that there were considerable disordered 
solvent molecules which could not be successfully modeled.  
From history, the remaining solvate was likely pentane in a 
volume of 1234.5 Å3 per unit cell (17.3%).  It appeared 
that the cavity area contained about eight pentane molecules, 
located in pairs near the four 222 positions at (0, 1/2, 0); 
(0, 1/2, 1/2); (1/2, 0, 1/2); (1/2, 1, 0). Modeling with or 
without restraints was unsuccessful, as was step by step 
acquisition of peaks using successive electron density 
difference maps. Thus, the structure factors were modified 
using the PLATON SQUEEZE technique, in order to produce a 
"solvate-free" structure factor set.  PLATON reported a 
total electron density of 350 e- per unit cell, likely 
representing eight pentane molecules, consistent with our 
earlier observations.  Use of the SQUEEZE technique resulted 
in a decrease of ca. 3.8 % in R.  
;
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane, benzene'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_refine_special_details          SQUEEZE
####################################################################### 
# 
# 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_12
_database_code_depnum_ccdc_archive 'CCDC 1420820'
_audit_update_record             
;
2015-08-26 deposited with the CCDC.
2015-10-06 downloaded from the CCDC.
;
_audit_creation_date             2014-07-28
_audit_creation_method           CRYSTALS_ver_14.52

_oxford_structure_analysis_title '4dem_50_0m in C2/c'
_chemical_name_systematic        ?
_chemical_melting_point          ?


_cell_length_a                   26.0844(7)
_cell_length_b                   13.0789(4)
_cell_length_c                   23.9074(7)
_cell_angle_alpha                90
_cell_angle_beta                 121.5730(11)
_cell_angle_gamma                90
_cell_volume                     6948.8(2)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1 '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476
0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            8

# Given Formula = C38 H32 F6 N2 Ni1 P4 
# Dc =      1.55 Fooo =   3328.00 Mu =      8.08 M =    813.28
# Found Formula = C38.00 H32 F6 N2 Ni1 P4 
# Dc =      1.55 FOOO =   3328.00 Mu =      8.08 M =    813.28

_chemical_formula_sum            'C38.00 H32 F6 N2 Ni1 P4'
_chemical_formula_moiety         'C38.00 H32 F6 N2 Ni1 P4'
_chemical_compound_source        ?
_chemical_formula_weight         813.28


_cell_measurement_reflns_used    9906
_cell_measurement_theta_min      2
_cell_measurement_theta_max      30
_cell_measurement_temperature    120

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_min          0.150
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_max          0.210

_exptl_crystal_density_diffrn    1.555
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             3328
_exptl_absorpt_coefficient_mu    0.808

# Sheldrick geometric approximatio 0.85 0.89 
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_T_max  0.89
_diffrn_measurement_device_type  'Bruker Kappa Apex2'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_structure_solution    'USER DEFINED STRUCTURE SOLUTION'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      120
_diffrn_reflns_number            41299
_reflns_number_total             10137
_diffrn_reflns_av_R_equivalents  0.032
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 10137 
# Theoretical number of reflections is about 20346 


_diffrn_reflns_theta_min         1.833
_diffrn_reflns_theta_max         30.042
_diffrn_measured_fraction_theta_max 0.996

_diffrn_reflns_theta_full        30.042
_diffrn_measured_fraction_theta_full 0.996


_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_reflns_limit_h_min              -36
_reflns_limit_h_max              31
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              33

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.93
_refine_diff_density_max         0.89


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_refine_ls_number_reflns         10137
_refine_ls_number_restraints     22
_refine_ls_number_parameters     508
_oxford_refine_ls_R_factor_ref   0.0520
_refine_ls_wR_factor_ref         0.1228
_refine_ls_goodness_of_fit_ref   0.9862
_refine_ls_shift/su_max          0.0080867
_refine_ls_shift/su_mean         0.0002723


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        10137
_refine_ls_R_factor_all          0.0520
_refine_ls_wR_factor_all         0.1228

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8321
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_gt          0.1089

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² +14.26P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Ni1 Ni 0.5000 0.78641(3) 0.7500 0.0199 1.0000 Uani S TU . . . .
Ni2 Ni 0.5000 0.59292(3) 0.7500 0.0163 1.0000 Uani S T . . . .
P1 P 0.56956(10) 0.88087(13) 0.83164(9) 0.0167(3) 0.474(9) Uiso . U P 1 1 .
P2 P 0.57384(2) 0.67634(4) 0.76953(2) 0.0179 1.0000 Uani . . . . . .
P3 P 0.49669(2) 0.51827(4) 0.66652(2) 0.0200 1.0000 Uani . . . . . .
P4 P 0.69705(3) 0.94041(5) 0.60862(3) 0.0367 1.0000 Uani . . . . . .
P11 P 0.57618(12) 0.88298(14) 0.82867(9) 0.0167(3) 0.463(9) Uiso . U P 1 2 .
P12 P 0.6037(5) 0.8973(6) 0.8379(4) 0.0182(3) 0.0626(16) Uiso D U P 1 3 .
F1 F 0.76608(7) 0.96383(13) 0.66080(9) 0.0526 1.0000 Uani . . . . . .
F2 F 0.71516(8) 0.82870(13) 0.59786(9) 0.0502 1.0000 Uani . . . . . .
F3 F 0.68865(11) 0.89603(15) 0.66588(10) 0.0652 1.0000 Uani . . . . . .
F4 F 0.67906(8) 1.05184(14) 0.61994(10) 0.0551 1.0000 Uani . . . . . .
F5 F 0.70584(7) 0.98417(14) 0.55228(8) 0.0504 1.0000 Uani . . . . . .
F6 F 0.62813(7) 0.91674(17) 0.55625(10) 0.0621 1.0000 Uani . . . . . .
N1 N 0.64182(7) 0.69713(14) 0.83317(8) 0.0241 1.0000 Uani . . . . . .
N2 N 0.59716(7) 0.67953(13) 0.71655(8) 0.0204 1.0000 Uani . . . . . .
C1 C 0.43168(9) 0.44102(16) 0.60994(10) 0.0257 1.0000 Uani . . . . . .
C2 C 0.43141(11) 0.3810(2) 0.56168(13) 0.0404 1.0000 Uani . . . . . .
C3 C 0.38362(12) 0.3153(2) 0.52377(15) 0.0480 1.0000 Uani . . . . . .
C4 C 0.33673(11) 0.3080(2) 0.53484(14) 0.0441 1.0000 Uani . . . . . .
C5 C 0.33581(11) 0.3682(2) 0.58114(14) 0.0398 1.0000 Uani . . . . . .
C6 C 0.38319(9) 0.43582(18) 0.61873(11) 0.0297 1.0000 Uani . . . . . .
C7 C 0.55999(9) 0.43302(16) 0.68669(11) 0.0276 1.0000 Uani . . . . . .
C8 C 0.59255(11) 0.4389(2) 0.65544(13) 0.0374 1.0000 Uani . . . . . .
C9 C 0.64051(12) 0.3720(2) 0.67359(15) 0.0467 1.0000 Uani . . . . . .
C10 C 0.65587(12) 0.2998(2) 0.72144(16) 0.0503 1.0000 Uani . . . . . .
C11 C 0.62323(13) 0.2922(2) 0.75179(16) 0.0468 1.0000 Uani . . . . . .
C12 C 0.57562(11) 0.35893(18) 0.73474(13) 0.0354 1.0000 Uani . . . . . .
C13 C 0.50612(9) 0.61400(16) 0.61742(9) 0.0217 1.0000 Uani . . . . . .
C14 C 0.46569(10) 0.62250(18) 0.54994(10) 0.0286 1.0000 Uani . . . . . .
C15 C 0.47613(11) 0.6892(2) 0.51199(11) 0.0368 1.0000 Uani . . . . . .
C16 C 0.52870(12) 0.7466(2) 0.54100(11) 0.0421 1.0000 Uani . . . . . .
C17 C 0.56918(10) 0.7411(2) 0.60833(10) 0.0344 1.0000 Uani . . . . . .
C18 C 0.55742(9) 0.67813(16) 0.64720(9) 0.0235 1.0000 Uani . . . . . .
C19 C 0.66145(10) 0.7033(2) 0.74620(11) 0.0403 1.0000 Uani . . . . . .
C20 C 0.69046(9) 0.70478(19) 0.82000(10) 0.0290 1.0000 Uani . . . . . .
C21 C 0.62050(9) 0.80258(15) 0.90296(9) 0.0225 1.0000 Uani . . . . . .
C22 C 0.65028(8) 0.71810(15) 0.89603(9) 0.0215 1.0000 Uani . . . . . .
C23 C 0.68793(9) 0.65650(17) 0.94945(10) 0.0257 1.0000 Uani . . . . . .
C24 C 0.69631(9) 0.67800(17) 1.01039(10) 0.0285 1.0000 Uani . . . . . .
C25 C 0.66822(10) 0.76207(18) 1.01801(10) 0.0289 1.0000 Uani . . . . . .
C26 C 0.63090(10) 0.82425(16) 0.96524(10) 0.0265 1.0000 Uani . . . . . .
C27 C 0.63018(11) 0.95530(17) 0.82653(11) 0.0280 0.9374 Uani . . . 1 4 .
C28 C 0.63002(13) 0.9654(2) 0.76899(13) 0.0364 0.9374 Uani . . . 1 4 .
C29 C 0.67544(15) 1.0217(3) 0.76845(16) 0.0482 0.9374 Uani . . . 1 4 .
C30 C 0.71983(15) 1.0677(3) 0.82497(19) 0.0528 0.9374 Uani . . . 1 4 .
C31 C 0.71945(15) 1.0590(3) 0.88245(16) 0.0544 0.9374 Uani . . . 1 4 .
C32 C 0.67513(14) 1.0033(2) 0.88361(14) 0.0400 0.9374 Uani . . . 1 4 .
C33 C 0.5412(3) 0.9821(5) 0.8521(3) 0.0205(12) 0.463(9) Uiso . . P 1 2 .
C34 C 0.5449(3) 1.0836(5) 0.8386(3) 0.0310(15) 0.463(9) Uiso . . P 1 2 .
C35 C 0.5142(3) 1.1552(5) 0.8516(3) 0.0353(15) 0.463(9) Uiso . . P 1 2 .
C36 C 0.4807(3) 1.1280(5) 0.8784(3) 0.0320(13) 0.463(9) Uiso . . P 1 2 .
C37 C 0.4776(3) 1.0278(6) 0.8944(3) 0.0341(13) 0.463(9) Uiso . . P 1 2 .
C38 C 0.5084(3) 0.9557(6) 0.8793(3) 0.0306(13) 0.463(9) Uiso . . P 1 2 .
C271 C 0.6611(17) 0.973(2) 0.8481(18) 0.016(3) 0.0626(16) Uiso . U P 1 3 .
C281 C 0.6654(19) 0.980(3) 0.785(2) 0.030(7) 0.0626(16) Uiso . . P 1 3 .
C291 C 0.7160(15) 1.036(2) 0.8004(16) 0.015(6) 0.0626(16) Uiso . . P 1 3 .
C301 C 0.7573(17) 1.092(3) 0.8547(18) 0.030(7) 0.0626(16) Uiso . . P 1 3 .
C311 C 0.748(2) 1.087(4) 0.908(3) 0.044(10) 0.0626(16) Uiso . . P 1 3 .
C321 C 0.700(2) 1.033(3) 0.8983(19) 0.026(7) 0.0626(16) Uiso . . P 1 3 .
C331 C 0.5333(2) 0.9674(4) 0.8593(2) 0.0174(11) 0.474(9) Uiso . . P 1 1 .
C332 C 0.5521(13) 0.976(2) 0.8525(17) 0.0181(6) 0.0626(16) Uiso D U P 1 3 .
C341 C 0.5297(3) 1.0729(4) 0.8453(3) 0.0276(12) 0.474(9) Uiso . . P 1 1 .
C342 C 0.5361(15) 1.073(2) 0.8249(16) 0.0181(8) 0.0626(16) Uiso D U P 1 3 .
C351 C 0.4963(3) 1.1365(4) 0.8622(3) 0.0319(13) 0.474(9) Uiso . . P 1 1 .
C352 C 0.499(2) 1.136(2) 0.837(2) 0.038(7) 0.0626(16) Uiso D U P 1 3 .
C361 C 0.4675(2) 1.0952(4) 0.8900(3) 0.0312(13) 0.474(9) Uiso . . P 1 1 .
C362 C 0.4726(19) 1.096(3) 0.870(2) 0.038(7) 0.0626(16) Uiso D U P 1 3 .
C371 C 0.4709(2) 0.9911(4) 0.9042(3) 0.0291(12) 0.474(9) Uiso . . P 1 1 .
C372 C 0.4849(18) 0.995(3) 0.893(2) 0.038(7) 0.0626(16) Uiso D U P 1 3 .
C381 C 0.5043(2) 0.9289(4) 0.8885(2) 0.0206(10) 0.474(9) Uiso . . P 1 1 .
C382 C 0.5239(17) 0.934(2) 0.883(2) 0.038(11) 0.0626(16) Uiso D . P 1 3 .
H21 H 0.4637 0.3830 0.5552 0.0484 1.0000 Uiso R . . . . .
H31 H 0.3843 0.2757 0.4916 0.0569 1.0000 Uiso R . . . . .
H41 H 0.3074 0.2620 0.5120 0.0534 1.0000 Uiso R . . . . .
H51 H 0.3035 0.3639 0.5877 0.0481 1.0000 Uiso R . . . . .
H61 H 0.3818 0.4780 0.6491 0.0354 1.0000 Uiso R . . . . .
H81 H 0.5829 0.4869 0.6226 0.0449 1.0000 Uiso R . . . . .
H91 H 0.6625 0.3772 0.6531 0.0559 1.0000 Uiso R . . . . .
H101 H 0.6877 0.2560 0.7319 0.0598 1.0000 Uiso R . . . . .
H111 H 0.6327 0.2426 0.7847 0.0560 1.0000 Uiso R . . . . .
H121 H 0.5542 0.3536 0.7563 0.0425 1.0000 Uiso R . . . . .
H141 H 0.4311 0.5821 0.5298 0.0343 1.0000 Uiso R . . . . .
H151 H 0.4478 0.6951 0.4672 0.0434 1.0000 Uiso R . . . . .
H161 H 0.5367 0.7907 0.5151 0.0509 1.0000 Uiso R . . . . .
H171 H 0.6035 0.7818 0.6271 0.0407 1.0000 Uiso R . . . . .
H191 H 0.6662 0.7699 0.7317 0.0495 1.0000 Uiso R . . . . .
H192 H 0.6799 0.6543 0.7340 0.0486 1.0000 Uiso R . . . . .
H201 H 0.7110 0.7697 0.8369 0.0353 1.0000 Uiso R . . . . .
H202 H 0.7180 0.6507 0.8393 0.0368 1.0000 Uiso R . . . . .
H231 H 0.7068 0.6031 0.9442 0.0303 1.0000 Uiso R . . . . .
H241 H 0.7206 0.6366 1.0459 0.0341 1.0000 Uiso R . . . . .
H251 H 0.6746 0.7784 1.0587 0.0356 1.0000 Uiso R . . . . .
H261 H 0.6130 0.8810 0.9709 0.0324 1.0000 Uiso R . . . . .
H281 H 0.5998 0.9338 0.7311 0.0438 0.9374 Uiso R . . 1 4 .
H291 H 0.6741 1.0277 0.7290 0.0584 0.9374 Uiso R . . 1 4 .
H301 H 0.7503 1.1040 0.8247 0.0627 0.9374 Uiso R . . 1 4 .
H311 H 0.7495 1.0919 0.9209 0.0647 0.9374 Uiso R . . 1 4 .
H321 H 0.6747 0.9982 0.9224 0.0477 0.9374 Uiso R . . 1 4 .
H341 H 0.5676 1.1020 0.8216 0.0365 0.463(9) Uiso R . P 1 2 .
H351 H 0.5164 1.2231 0.8422 0.0424 0.463(9) Uiso R . P 1 2 .
H361 H 0.4598 1.1784 0.8865 0.0385 0.463(9) Uiso R . P 1 2 .
H371 H 0.4561 1.0078 0.9137 0.0414 0.463(9) Uiso R . P 1 2 .
H381 H 0.5060 0.8873 0.8884 0.0365 0.463(9) Uiso R . P 1 2 .
H2811 H 0.6381 0.9526 0.7446 0.0361 0.0626(16) Uiso R . P 1 3 .
H2911 H 0.7246 1.0346 0.7673 0.0180 0.0626(16) Uiso R . P 1 3 .
H3011 H 0.7884 1.1288 0.8562 0.0360 0.0626(16) Uiso R . P 1 3 .
H3111 H 0.7734 1.1199 0.9471 0.0520 0.0626(16) Uiso R . P 1 3 .
H3211 H 0.6927 1.0377 0.9322 0.0311 0.0626(16) Uiso R . P 1 3 .
H3411 H 0.5502 1.0988 0.8257 0.0328 0.474(9) Uiso R . P 1 1 .
H3421 H 0.5500 1.0966 0.7985 0.0220 0.0626(16) Uiso R . P 1 3 .
H3511 H 0.4936 1.2071 0.8545 0.0381 0.474(9) Uiso R . P 1 1 .
H3521 H 0.4916 1.2034 0.8228 0.0450 0.0626(16) Uiso R . P 1 3 .
H3611 H 0.4443 1.1379 0.9004 0.0380 0.474(9) Uiso R . P 1 1 .
H3621 H 0.4467 1.1366 0.8765 0.0450 0.0626(16) Uiso R . P 1 3 .
H3711 H 0.4511 0.9639 0.9235 0.0347 0.474(9) Uiso R . P 1 1 .
H3721 H 0.4676 0.9688 0.9158 0.0449 0.0626(16) Uiso R . P 1 3 .
H3811 H 0.5074 0.8596 0.8980 0.0246 0.474(9) Uiso R . P 1 1 .
H3821 H 0.5307 0.8664 0.8970 0.0460 0.0626(16) Uiso R . P 1 3 .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.048097(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 . P2 5_656 2.2491(5) yes
Ni1 . P1 5_656 2.2180(18) yes
Ni1 . Ni2 . 2.5307(5) yes
Ni1 . P1 . 2.2180(18) yes
Ni1 . P2 . 2.2491(5) yes
Ni1 . P11 5_656 2.273(2) yes
Ni1 . P2 5_656 2.2491(5) yes
Ni1 . Ni2 . 2.5307(5) yes
Ni1 . P2 . 2.2491(5) yes
Ni1 . P11 . 2.273(2) yes
Ni1 . P12 5_656 2.808(10) yes
Ni1 . P2 5_656 2.2491(5) yes
Ni1 . Ni2 . 2.5307(5) yes
Ni1 . P2 . 2.2491(5) yes
Ni1 . P12 . 2.808(10) yes
Ni2 . P3 5_656 2.1826(5) yes
Ni2 . P2 5_656 2.0437(5) yes
Ni2 . P2 . 2.0437(5) yes
Ni2 . P3 . 2.1826(5) yes
P1 . C21 . 1.830(3) yes
P1 . C331 . 1.808(5) yes
P2 . N1 . 1.6454(16) yes
P2 . N2 . 1.6684(16) yes
P3 . C1 . 1.823(2) yes
P3 . C7 . 1.835(2) yes
P3 . C13 . 1.819(2) yes
P4 . F1 . 1.5938(16) yes
P4 . F2 . 1.5973(19) yes
P4 . F3 . 1.6038(18) yes
P4 . F4 . 1.597(2) yes
P4 . F5 . 1.5869(16) yes
P4 . F6 . 1.5931(17) yes
P11 . C21 . 1.857(3) yes
P11 . C33 . 1.834(6) yes
P12 . C21 . 1.852(8) yes
P12 . C271 . 1.70(4) yes
P12 . C332 . 1.863(17) yes
N1 . C20 . 1.462(3) yes
N1 . C22 . 1.427(2) yes
N2 . C18 . 1.423(2) yes
N2 . C19 . 1.472(3) yes
C1 . C2 . 1.393(3) yes
C1 . C6 . 1.388(3) yes
C2 . C3 . 1.389(3) yes
C2 . H21 . 0.933 no
C3 . C4 . 1.384(4) yes
C3 . H31 . 0.934 no
C4 . C5 . 1.369(4) yes
C4 . H41 . 0.899 no
C5 . C6 . 1.398(3) yes
C5 . H51 . 0.936 no
C6 . H61 . 0.928 no
C7 . C8 . 1.396(3) yes
C7 . C12 . 1.391(4) yes
C8 . C9 . 1.396(4) yes
C8 . H81 . 0.932 no
C9 . C10 . 1.372(5) yes
C9 . H91 . 0.930 no
C10 . C11 . 1.381(5) yes
C10 . H101 . 0.929 no
C11 . C12 . 1.393(3) yes
C11 . H111 . 0.948 no
C12 . H121 . 0.941 no
C13 . C14 . 1.395(3) yes
C13 . C18 . 1.415(3) yes
C14 . C15 . 1.385(3) yes
C14 . H141 . 0.934 no
C15 . C16 . 1.389(3) yes
C15 . H151 . 0.933 no
C16 . C17 . 1.390(3) yes
C16 . H161 . 0.946 no
C17 . C18 . 1.391(3) yes
C17 . H171 . 0.930 no
C19 . C20 . 1.513(3) yes
C19 . H191 . 0.969 no
C19 . H192 . 0.936 no
C20 . H201 . 0.972 no
C20 . H202 . 0.940 no
C21 . C22 . 1.409(3) yes
C21 . C26 . 1.396(3) yes
C21 . C22 . 1.409(3) yes
C21 . C26 . 1.396(3) yes
C21 . C22 . 1.409(3) yes
C21 . C26 . 1.396(3) yes
C22 . C23 . 1.390(3) yes
C23 . C24 . 1.384(3) yes
C23 . H231 . 0.901 no
C24 . C25 . 1.385(3) yes
C24 . H241 . 0.924 no
C25 . C26 . 1.384(3) yes
C25 . H251 . 0.922 no
C26 . H261 . 0.924 no
C27 . C28 . 1.380(3) yes
C27 . C32 . 1.399(3) yes
C28 . C29 . 1.401(4) yes
C28 . H281 . 0.931 no
C29 . C30 . 1.375(5) yes
C29 . H291 . 0.928 no
C30 . C31 . 1.384(5) yes
C30 . H301 . 0.928 no
C31 . C32 . 1.378(4) yes
C31 . H311 . 0.944 no
C32 . H321 . 0.935 no
C33 . C34 . 1.382(8) yes
C33 . C38 . 1.362(8) yes
C34 . C35 . 1.369(8) yes
C34 . H341 . 0.910 no
C35 . C36 . 1.374(8) yes
C35 . H351 . 0.924 no
C36 . C37 . 1.379(9) yes
C36 . H361 . 0.939 no
C37 . C38 . 1.403(9) yes
C37 . H371 . 0.932 no
C38 . H381 . 0.930 no
C271 . C281 . 1.56(5) yes
C271 . C321 . 1.35(5) yes
C281 . C291 . 1.38(5) yes
C281 . H2811 . 0.928 no
C291 . C301 . 1.39(5) yes
C291 . H2911 . 0.928 no
C301 . C311 . 1.41(6) yes
C301 . H3011 . 0.929 no
C311 . C321 . 1.34(7) yes
C311 . H3111 . 0.931 no
C321 . H3211 . 0.930 no
C331 . C341 . 1.411(7) yes
C331 . C381 . 1.366(7) yes
C332 . C342 . 1.396(16) yes
C332 . C382 . 1.390(16) yes
C341 . C351 . 1.407(8) yes
C341 . H3411 . 0.940 no
C342 . C352 . 1.420(16) yes
C342 . H3421 . 0.929 no
C351 . C361 . 1.349(8) yes
C351 . H3511 . 0.937 no
C352 . C362 . 1.382(16) yes
C352 . H3521 . 0.929 no
C361 . C371 . 1.394(8) yes
C361 . H3611 . 0.948 no
C362 . C372 . 1.405(16) yes
C362 . H3621 . 0.930 no
C371 . C381 . 1.381(7) yes
C371 . H3711 . 0.923 no
C372 . C382 . 1.412(16) yes
C372 . H3721 . 0.931 no
C381 . H3811 . 0.927 no
C382 . H3821 . 0.932 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P2 5_656 Ni1 . P1 5_656 87.52(5) yes
P2 5_656 Ni1 . Ni2 . 50.203(14) yes
P1 5_656 Ni1 . Ni2 . 123.85(4) yes
P2 5_656 Ni1 . P1 . 139.14(7) yes
P1 5_656 Ni1 . P1 . 112.30(9) yes
Ni2 . Ni1 . P1 . 123.85(4) yes
P2 5_656 Ni1 . P2 . 100.41(3) yes
P1 5_656 Ni1 . P2 . 139.14(7) yes
Ni2 . Ni1 . P2 . 50.203(14) yes
P1 . Ni1 . P2 . 87.52(5) yes
P11 5_656 Ni1 . P2 5_656 84.33(6) yes
P11 5_656 Ni1 . Ni2 . 123.75(4) yes
P2 5_656 Ni1 . Ni2 . 50.203(14) yes
P11 5_656 Ni1 . P2 . 144.10(7) yes
P2 5_656 Ni1 . P2 . 100.41(3) yes
Ni2 . Ni1 . P2 . 50.203(14) yes
P11 5_656 Ni1 . P11 . 112.50(9) yes
P2 5_656 Ni1 . P11 . 144.10(7) yes
Ni2 . Ni1 . P11 . 123.75(4) yes
P2 . Ni1 . P11 . 84.33(6) yes
P12 5_656 Ni1 . P2 5_656 77.92(17) yes
P12 5_656 Ni1 . Ni2 . 121.11(16) yes
P2 5_656 Ni1 . Ni2 . 50.203(14) yes
P12 5_656 Ni1 . P2 . 150.53(17) yes
P2 5_656 Ni1 . P2 . 100.41(3) yes
Ni2 . Ni1 . P2 . 50.203(14) yes
P12 5_656 Ni1 . P12 . 117.8(3) yes
P2 5_656 Ni1 . P12 . 150.53(17) yes
Ni2 . Ni1 . P12 . 121.11(16) yes
P2 . Ni1 . P12 . 77.92(17) yes
P3 5_656 Ni2 . Ni1 . 116.570(16) yes
P3 5_656 Ni2 . P2 5_656 91.664(18) yes
Ni1 . Ni2 . P2 5_656 57.731(16) yes
P3 5_656 Ni2 . P2 . 116.653(18) yes
Ni1 . Ni2 . P2 . 57.731(16) yes
P2 5_656 Ni2 . P2 . 115.46(3) yes
P3 5_656 Ni2 . P3 . 126.86(3) yes
Ni1 . Ni2 . P3 . 116.570(16) yes
P2 5_656 Ni2 . P3 . 116.653(18) yes
P2 . Ni2 . P3 . 91.664(18) yes
Ni1 . P1 . C21 . 111.63(10) yes
Ni1 . P1 . C331 . 109.08(17) yes
C21 . P1 . C331 . 105.86(19) yes
Ni1 . P2 . Ni2 . 72.066(18) yes
Ni1 . P2 . N1 . 118.51(7) yes
Ni2 . P2 . N1 . 136.88(7) yes
Ni1 . P2 . N2 . 116.07(6) yes
Ni2 . P2 . N2 . 120.97(6) yes
N1 . P2 . N2 . 93.04(8) yes
Ni2 . P3 . C1 . 120.16(7) yes
Ni2 . P3 . C7 . 115.60(7) yes
C1 . P3 . C7 . 102.57(9) yes
Ni2 . P3 . C13 . 109.16(6) yes
C1 . P3 . C13 . 106.87(9) yes
C7 . P3 . C13 . 100.42(10) yes
F1 . P4 . F2 . 89.63(10) yes
F1 . P4 . F3 . 90.27(11) yes
F2 . P4 . F3 . 89.46(11) yes
F1 . P4 . F4 . 90.22(10) yes
F2 . P4 . F4 . 179.56(11) yes
F3 . P4 . F4 . 90.13(11) yes
F1 . P4 . F5 . 89.36(10) yes
F2 . P4 . F5 . 90.38(10) yes
F3 . P4 . F5 . 179.60(11) yes
F4 . P4 . F5 . 90.03(10) yes
F1 . P4 . F6 . 179.73(12) yes
F2 . P4 . F6 . 90.16(11) yes
F3 . P4 . F6 . 89.90(11) yes
F4 . P4 . F6 . 89.99(11) yes
F5 . P4 . F6 . 90.46(10) yes
Ni1 . P11 . C21 . 108.27(11) yes
Ni1 . P11 . C33 . 106.6(2) yes
C21 . P11 . C33 . 105.6(2) yes
Ni1 . P12 . C21 . 89.7(4) yes
Ni1 . P12 . C271 . 146.8(13) yes
C21 . P12 . C271 . 117.7(12) yes
Ni1 . P12 . C332 . 85.2(12) yes
C21 . P12 . C332 . 95.0(10) yes
C271 . P12 . C332 . 108.9(15) yes
P2 . N1 . C20 . 116.66(13) yes
P2 . N1 . C22 . 120.21(14) yes
C20 . N1 . C22 . 122.73(16) yes
P2 . N2 . C18 . 123.47(13) yes
P2 . N2 . C19 . 114.58(13) yes
C18 . N2 . C19 . 121.02(16) yes
P3 . C1 . C2 . 121.77(17) yes
P3 . C1 . C6 . 118.82(16) yes
C2 . C1 . C6 . 119.20(19) yes
C1 . C2 . C3 . 120.2(2) yes
C1 . C2 . H21 . 120.5 no
C3 . C2 . H21 . 119.3 no
C2 . C3 . C4 . 119.9(3) yes
C2 . C3 . H31 . 118.9 no
C4 . C3 . H31 . 121.2 no
C3 . C4 . C5 . 120.4(2) yes
C3 . C4 . H41 . 119.2 no
C5 . C4 . H41 . 120.4 no
C4 . C5 . C6 . 120.0(2) yes
C4 . C5 . H51 . 119.9 no
C6 . C5 . H51 . 120.1 no
C5 . C6 . C1 . 120.2(2) yes
C5 . C6 . H61 . 119.7 no
C1 . C6 . H61 . 120.1 no
P3 . C7 . C8 . 122.80(19) yes
P3 . C7 . C12 . 118.34(17) yes
C8 . C7 . C12 . 118.9(2) yes
C7 . C8 . C9 . 119.7(3) yes
C7 . C8 . H81 . 121.1 no
C9 . C8 . H81 . 119.2 no
C8 . C9 . C10 . 120.9(3) yes
C8 . C9 . H91 . 119.3 no
C10 . C9 . H91 . 119.8 no
C9 . C10 . C11 . 119.8(2) yes
C9 . C10 . H101 . 118.5 no
C11 . C10 . H101 . 121.7 no
C10 . C11 . C12 . 120.1(3) yes
C10 . C11 . H111 . 121.5 no
C12 . C11 . H111 . 118.4 no
C11 . C12 . C7 . 120.6(3) yes
C11 . C12 . H121 . 119.2 no
C7 . C12 . H121 . 120.2 no
P3 . C13 . C14 . 121.70(15) yes
P3 . C13 . C18 . 119.67(14) yes
C14 . C13 . C18 . 118.53(19) yes
C13 . C14 . C15 . 121.3(2) yes
C13 . C14 . H141 . 119.5 no
C15 . C14 . H141 . 119.2 no
C14 . C15 . C16 . 119.7(2) yes
C14 . C15 . H151 . 119.6 no
C16 . C15 . H151 . 120.7 no
C15 . C16 . C17 . 120.2(2) yes
C15 . C16 . H161 . 120.1 no
C17 . C16 . H161 . 119.6 no
C16 . C17 . C18 . 120.3(2) yes
C16 . C17 . H171 . 119.0 no
C18 . C17 . H171 . 120.7 no
N2 . C18 . C13 . 120.93(18) yes
N2 . C18 . C17 . 119.33(18) yes
C13 . C18 . C17 . 119.74(18) yes
N2 . C19 . C20 . 108.21(17) yes
N2 . C19 . H191 . 110.2 no
C20 . C19 . H191 . 109.0 no
N2 . C19 . H192 . 110.4 no
C20 . C19 . H192 . 110.4 no
H191 . C19 . H192 . 108.7 no
C19 . C20 . N1 . 106.85(16) yes
C19 . C20 . H201 . 109.0 no
N1 . C20 . H201 . 108.8 no
C19 . C20 . H202 . 110.5 no
N1 . C20 . H202 . 111.7 no
H201 . C20 . H202 . 109.9 no
P1 . C21 . C22 . 120.34(15) yes
P1 . C21 . C26 . 121.41(17) yes
C22 . C21 . C26 . 118.25(18) yes
P11 . C21 . C22 . 115.91(15) yes
P11 . C21 . C26 . 125.56(17) yes
C22 . C21 . C26 . 118.25(18) yes
P12 . C21 . C22 . 109.2(3) yes
P12 . C21 . C26 . 126.0(3) yes
C22 . C21 . C26 . 118.25(18) yes
N1 . C22 . C21 . 118.93(17) yes
N1 . C22 . C23 . 120.12(19) yes
C21 . C22 . C23 . 120.95(18) yes
C22 . C23 . C24 . 119.7(2) yes
C22 . C23 . H231 . 119.7 no
C24 . C23 . H231 . 120.6 no
C23 . C24 . C25 . 119.79(19) yes
C23 . C24 . H241 . 120.1 no
C25 . C24 . H241 . 120.1 no
C24 . C25 . C26 . 120.98(19) yes
C24 . C25 . H251 . 120.4 no
C26 . C25 . H251 . 118.6 no
C21 . C26 . C25 . 120.3(2) yes
C21 . C26 . H261 . 119.2 no
C25 . C26 . H261 . 120.5 no
C28 . C27 . C32 . 119.6(3) yes
C27 . C28 . C29 . 119.9(3) yes
C27 . C28 . H281 . 119.2 no
C29 . C28 . H281 . 120.9 no
C28 . C29 . C30 . 120.2(3) yes
C28 . C29 . H291 . 118.1 no
C30 . C29 . H291 . 121.7 no
C29 . C30 . C31 . 119.9(3) yes
C29 . C30 . H301 . 120.0 no
C31 . C30 . H301 . 120.0 no
C30 . C31 . C32 . 120.4(3) yes
C30 . C31 . H311 . 119.8 no
C32 . C31 . H311 . 119.9 no
C27 . C32 . C31 . 120.1(3) yes
C27 . C32 . H321 . 119.7 no
C31 . C32 . H321 . 120.2 no
P11 . C33 . C34 . 120.1(5) yes
P11 . C33 . C38 . 120.2(5) yes
C34 . C33 . C38 . 119.6(6) yes
C33 . C34 . C35 . 118.9(6) yes
C33 . C34 . H341 . 120.0 no
C35 . C34 . H341 . 121.1 no
C34 . C35 . C36 . 121.3(6) yes
C34 . C35 . H351 . 118.9 no
C36 . C35 . H351 . 119.9 no
C35 . C36 . C37 . 121.3(6) yes
C35 . C36 . H361 . 119.7 no
C37 . C36 . H361 . 119.1 no
C36 . C37 . C38 . 116.3(6) yes
C36 . C37 . H371 . 122.7 no
C38 . C37 . H371 . 120.9 no
C37 . C38 . C33 . 122.6(6) yes
C37 . C38 . H381 . 118.0 no
C33 . C38 . H381 . 119.4 no
P12 . C271 . C281 . 114(3) yes
P12 . C271 . C321 . 132(3) yes
C281 . C271 . C321 . 115(3) yes
C271 . C281 . C291 . 109(3) yes
C271 . C281 . H2811 . 125.6 no
C291 . C281 . H2811 . 125.6 no
C281 . C291 . C301 . 134(3) yes
C281 . C291 . H2911 . 113.4 no
C301 . C291 . H2911 . 113.0 no
C291 . C301 . C311 . 114(4) yes
C291 . C301 . H3011 . 123.1 no
C311 . C301 . H3011 . 123.4 no
C301 . C311 . C321 . 117(5) yes
C301 . C311 . H3111 . 121.2 no
C321 . C311 . H3111 . 121.5 no
C271 . C321 . C311 . 131(4) yes
C271 . C321 . H3211 . 114.3 no
C311 . C321 . H3211 . 114.9 no
P1 . C331 . C341 . 120.5(4) yes
P1 . C331 . C381 . 119.5(4) yes
C341 . C331 . C381 . 119.7(5) yes
P12 . C332 . C342 . 118.6(17) yes
P12 . C332 . C382 . 121.2(17) yes
C342 . C332 . C382 . 119.7(3) yes
C331 . C341 . C351 . 119.0(5) yes
C331 . C341 . H3411 . 119.0 no
C351 . C341 . H3411 . 122.0 no
C332 . C342 . C352 . 119.9(3) yes
C332 . C342 . H3421 . 119.9 no
C352 . C342 . H3421 . 120.2 no
C341 . C351 . C361 . 119.5(5) yes
C341 . C351 . H3511 . 121.4 no
C361 . C351 . H3511 . 119.0 no
C342 . C352 . C362 . 119.9(3) yes
C342 . C352 . H3521 . 120.0 no
C362 . C352 . H3521 . 120.1 no
C351 . C361 . C371 . 122.1(5) yes
C351 . C361 . H3611 . 119.3 no
C371 . C361 . H3611 . 118.6 no
C352 . C362 . C372 . 119.9(3) yes
C352 . C362 . H3621 . 120.1 no
C372 . C362 . H3621 . 120.0 no
C361 . C371 . C381 . 118.5(5) yes
C361 . C371 . H3711 . 121.2 no
C381 . C371 . H3711 . 120.3 no
C362 . C372 . C382 . 120.0(3) yes
C362 . C372 . H3721 . 120.0 no
C382 . C372 . H3721 . 120.0 no
C371 . C381 . C331 . 121.3(5) yes
C371 . C381 . H3811 . 119.8 no
C331 . C381 . H3811 . 118.9 no
C372 . C382 . C332 . 120.0(3) yes
C372 . C382 . H3821 . 119.8 no
C332 . C382 . H3821 . 120.2 no


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: pentane, CH2Cl2'
_chemical_properties_physical    
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
