# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

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

data_AP13
_database_code_depnum_ccdc_archive 'CCDC 1486081'
#Added by publCIF



_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_publcif_datablock.id            {c4276b52-9cfa-4042-af9b-d9cf70b17d32}

_audit_creation_date             2016-01-08
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_chemical_formula_moiety         'C47 H48 N3 Ni P3, 2(B F4)'
_chemical_formula_sum            'C47 H48 B2 F8 N3 Ni P3'
_chemical_formula_weight         980.18
_chemical_oxdiff_formula         'Ni1 N4 C10 H10 P4 B2 F8'
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_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
Ni -2.97651 0.52496 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630
66.34210 1.03410005569
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.01920 0.00962 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
B 0.00963 0.00408 2.05450 1.33260 1.09790 0.70680 23.21850 1.02100 60.34980
0.14030 -0.193200007081
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
F 0.07537 0.05506 3.53920 2.64120 1.51700 1.02430 10.28250 4.29440 0.26150
26.14760 0.277599990368
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.03256 0.01839 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
P 0.30360 0.43703 6.43450 4.17910 1.78000 1.49080 1.90670 27.15700 0.52600
68.16450 1.11489999294
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y+1/2,-z+1/2
3 -x,-y,-z
4 x,-y-1/2,z-1/2

_symmetry_Int_Tables_number      14
_cell_length_a                   20.7166(5)
_cell_length_b                   12.4767(3)
_cell_length_c                   20.5881(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.315(2)
_cell_angle_gamma                90
_cell_volume                     5021.99(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7517
_cell_measurement_temperature    105.10(14)
_cell_measurement_theta_max      73.8700
_cell_measurement_theta_min      4.1760
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81628
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_density_diffrn    1.2963
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_F_000             2021.9415
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            13488
_diffrn_reflns_theta_full        74.0470
_diffrn_reflns_theta_max         74.05
_diffrn_reflns_theta_min         4.20
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      105.10(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4372
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.7723
_diffrn_measured_fraction_theta_max 0.7723
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -75.00   37.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2302   77.0000   30.0000 112

#__ type_ start__ end____ width___ exp.time_
  2 omega  -33.00   71.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2302  -57.0000  150.0000 104

#__ type_ start__ end____ width___ exp.time_
  3 omega   24.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000  150.0000 85

#__ type_ start__ end____ width___ exp.time_
  4 omega   33.00  122.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562 -125.0000  -60.0000 89

#__ type_ start__ end____ width___ exp.time_
  5 omega   78.00  154.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   30.0000   30.0000 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0328083000
_diffrn_orient_matrix_UB_12      -0.0979207000
_diffrn_orient_matrix_UB_13      0.0222863000
_diffrn_orient_matrix_UB_21      -0.0495359000
_diffrn_orient_matrix_UB_22      0.0745431000
_diffrn_orient_matrix_UB_23      0.0202102000
_diffrn_orient_matrix_UB_31      -0.0517915000
_diffrn_orient_matrix_UB_32      -0.0093135000
_diffrn_orient_matrix_UB_33      -0.0733818000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -24
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                7193
_reflns_number_total             7884
_reflns_odcompleteness_completeness 81.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_threshold_expression     I>=2u(I)
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_refine_diff_density_max         1.2717
_refine_diff_density_min         -0.8692
_refine_diff_density_rms         0.0695
_refine_ls_d_res_high            0.8018
_refine_ls_d_res_low             10.5175
_refine_ls_goodness_of_fit_ref   1.0492
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    85
_refine_ls_number_parameters     575
_refine_ls_number_reflns         7884
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0463
_refine_ls_restrained_S_all      1.0492
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0665P)²+6.5051P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1272
_olex2_refinement_description    
;
;
_atom_sites_solution_primary     iterative
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_refinement_flags_posn
Ni1 Ni 0.73166(2) 0.65191(4) 0.41621(2) 0.01914(12) Uani 1.000000 .
P2 P 0.80191(3) 0.52331(5) 0.46415(3) 0.01614(14) Uani 1.000000 .
P3 P 0.77546(3) 0.67301(5) 0.33345(3) 0.01579(14) Uani 1.000000 .
P10 P 0.84119(3) 0.40415(5) 0.24299(3) 0.01732(15) Uani 1.000000 .
F24 F 0.92816(10) 0.15398(17) 0.46866(9) 0.0450(5) Uani 1.000000 .
F22 F 1.04047(10) 0.2012(2) 0.49744(10) 0.0589(6) Uani 1.000000 .
C16 C 0.76174(13) 0.3297(2) 0.19982(12) 0.0191(5) Uani 1.000000 .
F25 F 0.99993(10) 0.13272(19) 0.57779(10) 0.0522(6) Uani 1.000000 .
N33 N 0.68466(11) 0.61881(19) 0.48026(11) 0.0242(5) Uani 1.000000 .
C36 C 0.75853(13) 0.3944(2) 0.44457(12) 0.0187(5) Uani 1.000000 .
C42 C 0.80625(14) 0.4692(2) 0.59762(13) 0.0256(6) Uani 1.000000 .
H42 H 0.77538(14) 0.4150(2) 0.57727(13) 0.0307(7) Uiso 1.000000 R
C5 C 0.91962(13) 0.2210(2) 0.31003(12) 0.0220(5) Uani 1.000000 .
H5 H 0.89909(13) 0.2273(2) 0.34376(12) 0.0264(6) Uiso 1.000000 R
C48 C 0.77827(13) 0.8165(2) 0.32090(12) 0.0187(5) Uani 1.000000 .
C34 C 0.65567(15) 0.5987(2) 0.51681(14) 0.0282(6) Uani 1.000000 .
F26 F 0.96763(12) 0.29663(17) 0.53593(13) 0.0653(7) Uani 1.000000 .
C17 C 0.71685(13) 0.2919(2) 0.23217(13) 0.0218(5) Uani 1.000000 .
H17 H 0.72660(13) 0.3032(2) 0.27909(13) 0.0261(6) Uiso 1.000000 R
C37 C 0.68933(14) 0.3887(2) 0.40717(12) 0.0224(6) Uani 1.000000 .
H37 H 0.66401(14) 0.4512(2) 0.39368(12) 0.0268(7) Uiso 1.000000 R
C21 C 0.74549(14) 0.3117(2) 0.12930(13) 0.0256(6) Uani 1.000000 .
H21 H 0.77467(14) 0.3370(2) 0.10679(13) 0.0307(7) Uiso 1.000000 R
N54 N 0.77953(13) 0.7967(2) 0.48089(12) 0.0286(5) Uani 1.000000 .
C13 C 0.95602(13) 0.4896(2) 0.37673(12) 0.0196(5) Uani 1.000000 .
H13a H 0.98573(18) 0.5432(9) 0.4047(8) 0.0294(8) Uiso 1.000000 GR
H13b H 0.9694(3) 0.4202(6) 0.3967(9) 0.0294(8) Uiso 1.000000 GR
H13c H 0.9592(2) 0.4912(15) 0.33126(16) 0.0294(8) Uiso 1.000000 GR
C55 C 0.81522(15) 0.8597(2) 0.51401(13) 0.0280(6) Uani 1.000000 .
C43 C 0.82852(16) 0.4833(3) 0.66877(14) 0.0322(7) Uani 1.000000 .
H43 H 0.81277(16) 0.4377(3) 0.69597(14) 0.0387(8) Uiso 1.000000 R
C14 C 0.88266(12) 0.5103(2) 0.44783(11) 0.0173(5) Uani 1.000000 .
H14a H 0.91242(12) 0.5676(2) 0.47244(11) 0.0208(6) Uiso 1.000000 R
H14b H 0.90353(12) 0.4434(2) 0.46821(11) 0.0208(6) Uiso 1.000000 R
C40 C 0.76409(15) 0.2012(2) 0.44794(14) 0.0289(6) Uani 1.000000 .
H40 H 0.78904(15) 0.1384(2) 0.46165(14) 0.0347(8) Uiso 1.000000 R
C49 C 0.83380(13) 0.8760(2) 0.36206(12) 0.0207(5) Uani 1.000000 .
H49 H 0.87149(13) 0.8411(2) 0.39233(12) 0.0248(6) Uiso 1.000000 R
C53 C 0.72175(14) 0.8698(2) 0.27588(13) 0.0225(5) Uani 1.000000 .
H53 H 0.68465(14) 0.8306(2) 0.24814(13) 0.0270(6) Uiso 1.000000 R
C50 C 0.83285(15) 0.9870(2) 0.35789(13) 0.0265(6) Uani 1.000000 .
H50 H 0.87007(15) 1.0266(2) 0.38499(13) 0.0319(7) Uiso 1.000000 R
C18 C 0.65766(14) 0.2374(2) 0.19504(14) 0.0268(6) Uani 1.000000 .
H18 H 0.62813(14) 0.2126(2) 0.21726(14) 0.0322(7) Uiso 1.000000 R
C11 C 0.83402(12) 0.4259(2) 0.32945(11) 0.0162(5) Uani 1.000000 .
H11a H 0.78725(12) 0.4459(2) 0.32393(11) 0.0194(6) Uiso 1.000000 R
H11b H 0.84348(12) 0.3587(2) 0.35457(11) 0.0194(6) Uiso 1.000000 R
C44 C 0.87363(16) 0.5641(3) 0.69910(13) 0.0328(7) Uani 1.000000 .
H44 H 0.88782(16) 0.5734(3) 0.74657(13) 0.0394(8) Uiso 1.000000 R
C51 C 0.77645(15) 1.0387(2) 0.31337(14) 0.0282(6) Uani 1.000000 .
H51 H 0.77579(15) 1.1132(2) 0.31083(14) 0.0338(7) Uiso 1.000000 R
C9 C 0.93540(13) 0.2836(2) 0.20587(12) 0.0220(5) Uani 1.000000 .
H9 H 0.92600(13) 0.3327(2) 0.16996(12) 0.0264(6) Uiso 1.000000 R
C12 C 0.88223(12) 0.5125(2) 0.37277(11) 0.0159(5) Uani 1.000000 .
N58 N 0.65070(13) 0.7276(2) 0.36171(13) 0.0313(6) Uani 1.000000 .
C46 C 0.87689(14) 0.6186(2) 0.58794(13) 0.0226(5) Uani 1.000000 .
H46 H 0.89348(14) 0.6638(2) 0.56119(13) 0.0271(7) Uiso 1.000000 R
C59 C 0.69673(17) 0.6101(3) 0.12784(14) 0.0383(8) Uani 1.000000 .
H59 H 0.70743(17) 0.6272(3) 0.08862(14) 0.0459(9) Uiso 1.000000 R
C8 C 0.98097(14) 0.2002(2) 0.20960(13) 0.0263(6) Uani 1.000000 .
H8 H 1.00097(14) 0.1928(2) 0.17552(13) 0.0316(7) Uiso 1.000000 R
C6 C 0.96599(14) 0.1386(2) 0.31429(13) 0.0251(6) Uani 1.000000 .
H6 H 0.97651(14) 0.0904(2) 0.35077(13) 0.0301(7) Uiso 1.000000 R
C39 C 0.69491(16) 0.1959(2) 0.40950(15) 0.0313(7) Uani 1.000000 .
H39 H 0.67377(16) 0.1298(2) 0.39710(15) 0.0376(8) Uiso 1.000000 R
C7 C 0.99673(14) 0.1284(2) 0.26365(13) 0.0256(6) Uani 1.000000 .
H7 H 1.02776(14) 0.0733(2) 0.26628(13) 0.0307(7) Uiso 1.000000 R
C20 C 0.68681(15) 0.2571(3) 0.09233(14) 0.0316(6) Uani 1.000000 .
H20 H 0.67705(15) 0.2452(3) 0.04546(14) 0.0380(8) Uiso 1.000000 R
C52 C 0.72084(15) 0.9803(2) 0.27247(14) 0.0272(6) Uani 1.000000 .
H52 H 0.68300(15) 1.0156(2) 0.24279(14) 0.0326(7) Uiso 1.000000 R
C61 C 0.72095(13) 0.6227(2) 0.25055(12) 0.0201(5) Uani 1.000000 .
C47 C 0.83076(13) 0.5373(2) 0.55712(12) 0.0194(5) Uani 1.000000 .
C41 C 0.79598(14) 0.2995(2) 0.46588(13) 0.0232(6) Uani 1.000000 .
H41 H 0.84214(14) 0.3026(2) 0.49201(13) 0.0278(7) Uiso 1.000000 R
C15 C 0.86197(12) 0.6255(2) 0.34313(12) 0.0172(5) Uani 1.000000 .
H15a H 0.86759(12) 0.6282(2) 0.29822(12) 0.0206(6) Uiso 1.000000 R
H15b H 0.89428(12) 0.6759(2) 0.37243(12) 0.0206(6) Uiso 1.000000 R
C4 C 0.90348(13) 0.2941(2) 0.25591(12) 0.0185(5) Uani 1.000000 .
C60 C 0.73757(15) 0.6479(2) 0.19169(13) 0.0285(6) Uani 1.000000 .
H60 H 0.77576(15) 0.6897(2) 0.19534(13) 0.0342(7) Uiso 1.000000 R
C62 C 0.66335(15) 0.5611(2) 0.24458(14) 0.0285(6) Uani 1.000000 .
H62 H 0.65166(15) 0.5450(2) 0.28337(14) 0.0343(7) Uiso 1.000000 R
C45 C 0.89791(15) 0.6316(2) 0.65895(13) 0.0284(6) Uani 1.000000 .
H45 H 0.92851(15) 0.6859(2) 0.67967(13) 0.0340(7) Uiso 1.000000 R
C19 C 0.64237(15) 0.2199(2) 0.12518(15) 0.0306(6) Uani 1.000000 .
H19 H 0.60267(15) 0.1836(2) 0.10041(15) 0.0368(7) Uiso 1.000000 R
C38 C 0.65774(15) 0.2892(2) 0.38982(14) 0.0280(6) Uani 1.000000 .
H38 H 0.61130(15) 0.2857(2) 0.36481(14) 0.0335(7) Uiso 1.000000 R
C64 C 0.64020(18) 0.5473(3) 0.12249(15) 0.0414(8) Uani 1.000000 .
H64 H 0.61357(18) 0.5208(3) 0.07980(15) 0.0496(10) Uiso 1.000000 R
C35 C 0.6203(2) 0.5730(3) 0.56522(19) 0.0496(9) Uani 1.000000 .
H35a H 0.5758(6) 0.545(2) 0.5406(2) 0.0744(14) Uiso 1.000000 GR
H35b H 0.6461(8) 0.5207(17) 0.5976(9) 0.0744(14) Uiso 1.000000 GR
H35c H 0.6155(13) 0.6368(6) 0.5894(10) 0.0744(14) Uiso 1.000000 GR
B23 B 0.98413(17) 0.1945(3) 0.51923(15) 0.0250(6) Uiso 1.000000 .
C63 C 0.62326(17) 0.5238(3) 0.18014(17) 0.0399(8) Uani 1.000000 .
H63 H 0.58470(17) 0.4826(3) 0.17602(17) 0.0479(9) Uiso 1.000000 R
C56 C 0.86224(18) 0.9377(3) 0.55726(17) 0.0429(8) Uani 1.000000 .
H56a H 0.8804(10) 0.9819(14) 0.5293(2) 0.0643(12) Uiso 1.000000 GR
H56b H 0.8383(4) 0.9817(14) 0.5801(10) 0.0643(12) Uiso 1.000000 GR
H56c H 0.8990(7) 0.9009(3) 0.5910(9) 0.0643(12) Uiso 1.000000 GR
C57 C 0.5988(2) 0.7593(4) 0.3333(2) 0.0658(14) Uani 1.000000 .
F1 F 0.54565(10) 0.4962(2) 0.31641(11) 0.0613(7) Uani 1.000000 .
F2 F 0.53461(15) 0.4490(3) 0.41689(15) 0.1015(11) Uani 1.000000 .
F3 F 0.44419(16) 0.4623(6) 0.32541(15) 0.209(3) Uani 1.000000 .
F4 F 0.5000(3) 0.5975(4) 0.3817(4) 0.207(3) Uani 1.000000 .
B5 B 0.5038(2) 0.4970(5) 0.3558(3) 0.0560(13) Uani 1.000000 .
C1 C 0.5301(3) 0.8002(7) 0.2947(4) 0.164(4) Uani 1.000000 .
H1a H 0.5072(17) 0.821(6) 0.3263(4) 0.245(6) Uiso 1.000000 GR
H1b H 0.5341(3) 0.861(4) 0.268(3) 0.245(6) Uiso 1.000000 GR
H1c H 0.5042(15) 0.745(2) 0.265(3) 0.245(6) Uiso 1.000000 GR


loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P2 2.1717(7) . ?
Ni1 P3 2.1951(7) . ?
Ni1 N33 1.925(2) . ?
Ni1 N54 2.268(3) . ?
Ni1 N58 1.928(3) . ?
P2 C36 1.822(3) . ?
P2 C14 1.819(2) . ?
P2 C47 1.815(2) . ?
P3 C48 1.812(3) . ?
P3 C61 1.819(3) . ?
P3 C15 1.835(2) . ?
P10 C16 1.842(3) . ?
P10 C11 1.854(2) . ?
P10 C4 1.842(3) . ?
F24 B23 1.373(4) . ?
F22 B23 1.384(4) . ?
C16 C17 1.393(3) . ?
C16 C21 1.396(3) . ?
F25 B23 1.376(4) . ?
N33 C34 1.135(3) . ?
C36 C37 1.387(4) . ?
C36 C41 1.404(4) . ?
C42 C43 1.394(4) . ?
C42 C47 1.398(4) . ?
C5 C6 1.390(4) . ?
C5 C4 1.393(4) . ?
C48 C49 1.395(4) . ?
C48 C53 1.398(4) . ?
C34 C35 1.455(4) . ?
F26 B23 1.392(4) . ?
C17 C18 1.389(4) . ?
C37 C38 1.393(4) . ?
C21 C20 1.382(4) . ?
N54 C55 1.139(4) . ?
C13 C12 1.531(3) . ?
C55 C56 1.454(4) . ?
C43 C44 1.376(5) . ?
C14 C12 1.543(3) . ?
C40 C39 1.391(5) . ?
C40 C41 1.383(4) . ?
C49 C50 1.388(4) . ?
C53 C52 1.381(4) . ?
C50 C51 1.383(4) . ?
C18 C19 1.384(4) . ?
C11 C12 1.540(3) . ?
C44 C45 1.386(4) . ?
C51 C52 1.388(4) . ?
C9 C8 1.389(4) . ?
C9 C4 1.402(3) . ?
C12 C15 1.539(3) . ?
N58 C57 1.113(4) . ?
C46 C47 1.394(4) . ?
C46 C45 1.390(3) . ?
C59 C60 1.389(4) . ?
C59 C64 1.383(5) . ?
C8 C7 1.381(4) . ?
C6 C7 1.396(4) . ?
C39 C38 1.380(4) . ?
C20 C19 1.390(4) . ?
C61 C60 1.401(4) . ?
C61 C62 1.390(4) . ?
C62 C63 1.392(4) . ?
C64 C63 1.376(5) . ?
C57 C1 1.473(6) . ?
F1 B5 1.369(4) . ?
F2 B5 1.348(5) . ?
F3 B5 1.262(6) . ?
F4 B5 1.374(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P3 Ni1 P2 93.12(3) . . ?
N33 Ni1 P2 86.85(7) . . ?
N33 Ni1 P3 171.84(8) . . ?
N54 Ni1 P2 102.97(7) . . ?
N54 Ni1 P3 98.48(6) . . ?
N54 Ni1 N33 89.47(9) . . ?
N58 Ni1 P2 161.68(9) . . ?
N58 Ni1 P3 89.59(7) . . ?
N58 Ni1 N33 87.93(9) . . ?
N58 Ni1 N54 94.53(11) . . ?
C36 P2 Ni1 110.14(9) . . ?
C14 P2 Ni1 120.06(8) . . ?
C14 P2 C36 107.28(11) . . ?
C47 P2 Ni1 110.21(8) . . ?
C47 P2 C36 106.54(11) . . ?
C47 P2 C14 101.61(11) . . ?
C48 P3 Ni1 105.67(8) . . ?
C61 P3 Ni1 113.53(9) . . ?
C61 P3 C48 104.28(12) . . ?
C15 P3 Ni1 121.10(8) . . ?
C15 P3 C48 104.97(12) . . ?
C15 P3 C61 105.74(11) . . ?
C11 P10 C16 101.22(11) . . ?
C4 P10 C16 99.52(11) . . ?
C4 P10 C11 104.19(11) . . ?
C17 C16 P10 124.84(19) . . ?
C21 C16 P10 116.9(2) . . ?
C21 C16 C17 118.2(2) . . ?
C34 N33 Ni1 178.5(2) . . ?
C37 C36 P2 120.8(2) . . ?
C41 C36 P2 119.6(2) . . ?
C41 C36 C37 119.6(2) . . ?
C47 C42 C43 119.4(3) . . ?
C4 C5 C6 120.9(2) . . ?
C49 C48 P3 119.8(2) . . ?
C53 C48 P3 120.3(2) . . ?
C53 C48 C49 119.4(2) . . ?
C35 C34 N33 178.4(3) . . ?
C18 C17 C16 120.7(2) . . ?
C38 C37 C36 120.0(3) . . ?
C20 C21 C16 121.2(3) . . ?
C55 N54 Ni1 166.6(2) . . ?
C56 C55 N54 178.3(3) . . ?
C44 C43 C42 120.6(3) . . ?
C12 C14 P2 118.85(17) . . ?
C41 C40 C39 120.4(3) . . ?
C50 C49 C48 120.1(3) . . ?
C52 C53 C48 120.2(3) . . ?
C51 C50 C49 119.9(3) . . ?
C19 C18 C17 120.4(3) . . ?
C12 C11 P10 114.60(15) . . ?
C45 C44 C43 120.0(2) . . ?
C52 C51 C50 120.5(3) . . ?
C4 C9 C8 120.4(2) . . ?
C14 C12 C13 105.59(18) . . ?
C11 C12 C13 110.2(2) . . ?
C11 C12 C14 110.84(19) . . ?
C15 C12 C13 109.2(2) . . ?
C15 C12 C14 108.89(18) . . ?
C15 C12 C11 111.94(19) . . ?
C57 N58 Ni1 169.4(3) . . ?
C45 C46 C47 119.5(3) . . ?
C64 C59 C60 120.1(3) . . ?
C7 C8 C9 120.4(2) . . ?
C7 C6 C5 119.8(2) . . ?
C38 C39 C40 119.8(3) . . ?
C6 C7 C8 119.9(3) . . ?
C19 C20 C21 120.0(2) . . ?
C51 C52 C53 119.9(3) . . ?
C60 C61 P3 118.7(2) . . ?
C62 C61 P3 121.5(2) . . ?
C62 C61 C60 119.8(2) . . ?
C42 C47 P2 120.8(2) . . ?
C46 C47 P2 119.15(18) . . ?
C46 C47 C42 120.0(2) . . ?
C40 C41 C36 119.9(3) . . ?
C12 C15 P3 117.88(16) . . ?
C5 C4 P10 125.11(18) . . ?
C9 C4 P10 116.21(19) . . ?
C9 C4 C5 118.7(2) . . ?
C61 C60 C59 119.7(3) . . ?
C63 C62 C61 119.6(3) . . ?
C46 C45 C44 120.5(3) . . ?
C20 C19 C18 119.5(3) . . ?
C39 C38 C37 120.4(3) . . ?
C63 C64 C59 120.2(3) . . ?
F22 B23 F24 111.6(2) . . ?
F25 B23 F24 110.8(3) . . ?
F25 B23 F22 109.6(3) . . ?
F26 B23 F24 108.0(3) . . ?
F26 B23 F22 109.1(3) . . ?
F26 B23 F25 107.6(2) . . ?
C64 C63 C62 120.6(3) . . ?
C1 C57 N58 179.0(6) . . ?
F2 B5 F1 110.6(3) . . ?
F3 B5 F1 114.3(4) . . ?
F3 B5 F2 113.2(5) . . ?
F4 B5 F1 111.4(4) . . ?
F4 B5 F2 96.5(5) . . ?
F4 B5 F3 109.5(5) . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.500 0.000 0.500 309.2 39.7 ?
2 0.500 0.500 1.000 309.2 39.7 ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_ap104
_database_code_depnum_ccdc_archive 'CCDC 1486082'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_publcif_datablock.id            {28239e12-f67a-482c-939e-7b890471db25}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Triphos(Si)Ni(CH2PPh2) BF4'
_chemical_name_common            'Triphos(Si)Ni(CH2PPh2) BF4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C53 H51 Ni P4 Si, B F4, C2 H3 N '

_chemical_formula_sum            'C55 H54 B F4 N Ni P4 Si'
_chemical_formula_weight         1026.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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

_cell_length_a                   10.33010(10)
_cell_length_b                   20.6239(2)
_cell_length_c                   23.6859(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.01(2)
_cell_angle_gamma                90.00
_cell_volume                     5046.21(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    18275
_cell_measurement_theta_min      4.2620
_cell_measurement_theta_max      74.0060

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_absorpt_coefficient_mu    2.413
_exptl_absorpt_correction_T_min  0.83981
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_measured_fraction_theta_max 0.933
_diffrn_reflns_theta_full        74.25
_diffrn_measured_fraction_theta_full 0.933
_refine_diff_density_max         1.105
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.050
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4372
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            26336
_diffrn_reflns_av_R_equivalents  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0141
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         4.28
_diffrn_reflns_theta_max         74.25
_reflns_number_total             9610
_reflns_number_gt                9272
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_structure_solution    SHELXS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0385P)²+4.4625P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9610
_refine_ls_number_parameters     645
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0838
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.66146(17) 0.48361(10) 0.17353(8) 0.0267(4) Uani 1 1 d . . .
H1 H 0.6364 0.5003 0.1387 0.032 Uiso 1 1 calc R . .
C2 C 0.91114(16) 0.65821(8) 0.23689(7) 0.0211(3) Uani 1 1 d . . .
H2A H 0.8749 0.6627 0.1993 0.025 Uiso 1 1 calc R . .
H2B H 0.8471 0.6591 0.2668 0.025 Uiso 1 1 calc R . .
C10 C 1.26094(17) 0.61900(9) 0.10029(8) 0.0240(4) Uani 1 1 d . . .
H10 H 1.2052 0.6526 0.1100 0.029 Uiso 1 1 calc R . .
C11 C 1.31938(15) 0.50638(9) 0.10327(7) 0.0199(3) Uani 1 1 d . . .
H11 H 1.3035 0.4641 0.1151 0.024 Uiso 1 1 calc R . .
C12 C 1.46031(16) 0.61405(9) 0.21334(7) 0.0210(3) Uani 1 1 d . . .
H12 H 1.4436 0.5792 0.1896 0.025 Uiso 1 1 calc R . .
C13 C 0.96884(15) 0.55759(8) 0.10231(6) 0.0166(3) Uani 1 1 d . . .
C14 C 1.2027(2) 0.60460(10) 0.39036(8) 0.0326(4) Uani 1 1 d . . .
H14 H 1.1424 0.6320 0.3737 0.039 Uiso 1 1 calc R . .
C15 C 0.91839(16) 0.50685(9) 0.07025(7) 0.0204(3) Uani 1 1 d . . .
H15 H 0.9410 0.4643 0.0787 0.024 Uiso 1 1 calc R . .
C16 C 1.23398(15) 0.55593(8) 0.11825(7) 0.0173(3) Uani 1 1 d . . .
C17 C 0.73684(17) 0.43366(9) 0.27694(8) 0.0247(4) Uani 1 1 d . . .
H17 H 0.7617 0.4168 0.3117 0.030 Uiso 1 1 calc R . .
C18 C 0.59633(17) 0.43104(9) 0.19618(9) 0.0286(4) Uani 1 1 d . . .
H18 H 0.5284 0.4120 0.1764 0.034 Uiso 1 1 calc R . .
C19 C 1.27200(16) 0.56168(8) 0.35700(7) 0.0176(3) Uani 1 1 d . . .
C20 C 0.93293(16) 0.62108(9) 0.08931(7) 0.0209(3) Uani 1 1 d . . .
H20 H 0.9656 0.6552 0.1106 0.025 Uiso 1 1 calc R . .
C21 C 0.84869(17) 0.63388(10) 0.04474(7) 0.0253(4) Uani 1 1 d . . .
H21 H 0.8249 0.6763 0.0365 0.030 Uiso 1 1 calc R . .
C23 C 1.42849(16) 0.51996(10) 0.07058(7) 0.0258(4) Uani 1 1 d . . .
H23 H 1.4845 0.4866 0.0605 0.031 Uiso 1 1 calc R . .
C24 C 0.80049(17) 0.58292(10) 0.01278(7) 0.0256(4) Uani 1 1 d . . .
H24 H 0.7453 0.5912 -0.0174 0.031 Uiso 1 1 calc R . .
C25 C 1.38961(16) 0.62094(8) 0.26303(7) 0.0175(3) Uani 1 1 d . . .
C26 C 0.80494(15) 0.48594(8) 0.25373(7) 0.0182(3) Uani 1 1 d . . .
C28 C 0.83442(17) 0.51963(10) 0.02573(7) 0.0245(4) Uani 1 1 d . . .
H28 H 0.8009 0.4856 0.0046 0.029 Uiso 1 1 calc R . .
C29 C 1.05829(17) 0.74306(8) 0.31524(7) 0.0199(3) Uani 1 1 d . . .
C30 C 1.41738(19) 0.67348(9) 0.29860(8) 0.0254(4) Uani 1 1 d . . .
H30 H 1.3713 0.6789 0.3320 0.030 Uiso 1 1 calc R . .
C31 C 1.14847(19) 0.79243(9) 0.32359(8) 0.0256(4) Uani 1 1 d . . .
H31 H 1.2049 0.8039 0.2947 0.031 Uiso 1 1 calc R . .
C32 C 1.37004(19) 0.63202(11) 0.06813(9) 0.0322(4) Uani 1 1 d . . .
H32 H 1.3871 0.6743 0.0565 0.039 Uiso 1 1 calc R . .
C33 C 0.76401(16) 0.51154(9) 0.20258(7) 0.0204(3) Uani 1 1 d . . .
H33 H 0.8056 0.5477 0.1876 0.024 Uiso 1 1 calc R . .
C34 C 1.3097(2) 0.56606(11) 0.47358(8) 0.0352(5) Uani 1 1 d . . .
H34 H 1.3240 0.5680 0.5123 0.042 Uiso 1 1 calc R . .
C35 C 1.04310(16) 0.44604(8) 0.30237(7) 0.0205(3) Uani 1 1 d . . .
H35A H 0.9863 0.4088 0.3059 0.025 Uiso 1 1 calc R . .
H35B H 1.0914 0.4504 0.3373 0.025 Uiso 1 1 calc R . .
C36 C 1.30304(15) 0.48705(8) 0.25414(7) 0.0167(3) Uani 1 1 d . . .
H36A H 1.3603 0.4668 0.2814 0.020 Uiso 1 1 calc R . .
H36B H 1.3506 0.4922 0.2191 0.020 Uiso 1 1 calc R . .
C37 C 1.24546(19) 0.75513(9) 0.18375(8) 0.0250(4) Uani 1 1 d . . .
H37 H 1.3034 0.7365 0.2090 0.030 Uiso 1 1 calc R . .
C38 C 1.0252(2) 0.77600(8) 0.15431(8) 0.0263(4) Uani 1 1 d . . .
H38 H 0.9365 0.7719 0.1599 0.032 Uiso 1 1 calc R . .
C39 C 0.7520(2) 0.57482(10) 0.35521(9) 0.0342(4) Uani 1 1 d . . .
H39 H 0.7102 0.5806 0.3208 0.041 Uiso 1 1 calc R . .
C40 C 1.2224(2) 0.60718(11) 0.44846(8) 0.0369(5) Uani 1 1 d . . .
H40 H 1.1764 0.6368 0.4703 0.044 Uiso 1 1 calc R . .
C42 C 1.55560(18) 0.65863(9) 0.19880(8) 0.0271(4) Uani 1 1 d . . .
H42 H 1.6014 0.6537 0.1653 0.033 Uiso 1 1 calc R . .
C43 C 1.1541(2) 0.82462(9) 0.37528(9) 0.0327(4) Uani 1 1 d . . .
H43 H 1.2144 0.8575 0.3807 0.039 Uiso 1 1 calc R . .
C44 C 1.0705(2) 0.80800(10) 0.41852(8) 0.0339(4) Uani 1 1 d . . .
H44 H 1.0748 0.8296 0.4530 0.041 Uiso 1 1 calc R . .
C45 C 0.9805(2) 0.75908(10) 0.41038(8) 0.0330(4) Uani 1 1 d . . .
H45 H 0.9238 0.7481 0.4394 0.040 Uiso 1 1 calc R . .
C46 C 1.45388(18) 0.58240(11) 0.05313(8) 0.0323(4) Uani 1 1 d . . .
H46 H 1.5268 0.5912 0.0314 0.039 Uiso 1 1 calc R . .
C47 C 0.97429(19) 0.72634(9) 0.35928(8) 0.0265(4) Uani 1 1 d . . .
H47 H 0.9142 0.6932 0.3543 0.032 Uiso 1 1 calc R . .
C48 C 1.0725(2) 0.80995(9) 0.10787(8) 0.0357(5) Uani 1 1 d . . .
H48 H 1.0152 0.8283 0.0822 0.043 Uiso 1 1 calc R . .
C49 C 1.3582(2) 0.51989(11) 0.38290(8) 0.0372(5) Uani 1 1 d . . .
H49 H 1.4046 0.4903 0.3613 0.045 Uiso 1 1 calc R . .
C50 C 1.11226(18) 0.74809(8) 0.19241(7) 0.0208(3) Uani 1 1 d . . .
C51 C 0.8728(3) 0.55739(15) 0.45806(10) 0.0613(8) Uani 1 1 d . . .
H51 H 0.9135 0.5516 0.4927 0.074 Uiso 1 1 calc R . .
C53 C 1.2918(2) 0.78976(10) 0.13774(8) 0.0332(4) Uani 1 1 d . . .
H53 H 1.3803 0.7950 0.1324 0.040 Uiso 1 1 calc R . .
C54 C 1.58233(19) 0.71020(10) 0.23411(9) 0.0313(4) Uani 1 1 d . . .
H54 H 1.6462 0.7400 0.2244 0.038 Uiso 1 1 calc R . .
C55 C 0.9302(2) 0.53260(11) 0.40924(8) 0.0395(5) Uani 1 1 d . . .
H55 H 1.0078 0.5099 0.4115 0.047 Uiso 1 1 calc R . .
C56 C 1.3758(3) 0.52189(13) 0.44096(9) 0.0508(7) Uani 1 1 d . . .
H56 H 1.4329 0.4931 0.4580 0.061 Uiso 1 1 calc R . .
C57 C 0.63262(18) 0.40680(9) 0.24843(9) 0.0290(4) Uani 1 1 d . . .
H57 H 0.5870 0.3725 0.2644 0.035 Uiso 1 1 calc R . .
C58 C 0.6965(3) 0.59860(14) 0.40431(11) 0.0529(7) Uani 1 1 d . . .
H58 H 0.6178 0.6204 0.4026 0.063 Uiso 1 1 calc R . .
C59 C 1.08007(15) 0.45664(8) 0.17260(7) 0.0175(3) Uani 1 1 d . . .
H59A H 1.1234 0.4344 0.1418 0.021 Uiso 1 1 calc R . .
H59B H 0.9905 0.4425 0.1730 0.021 Uiso 1 1 calc R . .
C60 C 1.2046(3) 0.81647(10) 0.09985(8) 0.0388(5) Uani 1 1 d . . .
H60 H 1.2352 0.8391 0.0686 0.047 Uiso 1 1 calc R . .
C61 C 0.7571(3) 0.59024(16) 0.45558(12) 0.0666(9) Uani 1 1 d . . .
H61 H 0.7200 0.6067 0.4883 0.080 Uiso 1 1 calc R . .
C62 C 1.5137(2) 0.71746(10) 0.28404(9) 0.0323(4) Uani 1 1 d . . .
H62 H 1.5323 0.7520 0.3080 0.039 Uiso 1 1 calc R . .
C63 C 0.87090(19) 0.54196(9) 0.35721(8) 0.0256(4) Uani 1 1 d . . .
C64 C 1.21326(19) 0.34732(9) 0.23728(9) 0.0299(4) Uani 1 1 d . . .
H64A H 1.2748 0.3428 0.2071 0.045 Uiso 1 1 calc R . .
H64B H 1.1400 0.3199 0.2301 0.045 Uiso 1 1 calc R . .
H64C H 1.2530 0.3350 0.2723 0.045 Uiso 1 1 calc R . .
Si6 Si 1.15939(4) 0.43279(2) 0.241601(19) 0.01719(10) Uani 1 1 d . . .
P2 P 1.08536(4) 0.543985(19) 0.159686(16) 0.01371(9) Uani 1 1 d . . .
P3 P 1.25428(4) 0.566609(19) 0.280210(16) 0.01384(9) Uani 1 1 d . . .
P4 P 1.05568(4) 0.69737(2) 0.249776(17) 0.01726(9) Uani 1 1 d . . .
P5 P 0.94647(4) 0.519063(19) 0.290482(16) 0.01527(9) Uani 1 1 d . . .
Ni1 Ni 1.06253(2) 0.594130(13) 0.246219(11) 0.01372(7) Uani 1 1 d . . .
N1 N 0.4220(3) 0.34217(12) 0.08853(11) 0.0644(7) Uani 1 1 d . . .
C99 C 0.4674(4) 0.29837(13) 0.06799(11) 0.0610(8) Uani 1 1 d . . .
C100 C 0.5385(5) 0.24196(15) 0.04346(14) 0.0850(12) Uani 1 1 d . . .
H101 H 0.5776 0.2545 0.0084 0.127 Uiso 1 1 calc R . .
H100 H 0.4790 0.2070 0.0369 0.127 Uiso 1 1 calc R . .
H103 H 0.6044 0.2281 0.0693 0.127 Uiso 1 1 calc R . .
B1 B 0.6613(4) 0.8332(2) 0.10481(15) 0.0491(10) Uani 0.796(4) 1 d PD A 1
F2 F 0.7710(3) 0.8701(2) 0.09465(16) 0.0531(9) Uani 0.796(4) 1 d PD A 1
F3 F 0.59948(18) 0.85568(9) 0.15174(7) 0.0509(6) Uani 0.796(4) 1 d PD A 1
F1 F 0.5771(5) 0.8359(3) 0.0610(2) 0.112(2) Uani 0.796(4) 1 d PD A 1
F4 F 0.7056(3) 0.76934(14) 0.11861(15) 0.0824(10) Uani 0.796(4) 1 d PD A 1
B1B B 0.6856(14) 0.8195(7) 0.0841(6) 0.0491(10) Uani 0.204(4) 1 d PD A 2
F1B F 0.7574(10) 0.7904(4) 0.0387(3) 0.072(3) Uani 0.204(4) 1 d PD A 2
F3B F 0.6373(14) 0.7658(5) 0.0972(5) 0.082(4) Uani 0.204(4) 1 d PD A 2
F4B F 0.5717(11) 0.8568(5) 0.0613(6) 0.029(2) Uani 0.204(4) 1 d PD A 2
F2B F 0.771(2) 0.8621(11) 0.1015(11) 0.120(10) Uani 0.204(4) 1 d PD A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C18 1.384(3) . ?
C1 C33 1.388(2) . ?
C1 H1 0.9300 . ?
C2 P4 1.7248(18) . ?
C2 Ni1 2.0593(16) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C10 C32 1.387(3) . ?
C10 C16 1.397(3) . ?
C10 H10 0.9300 . ?
C11 C23 1.396(3) . ?
C11 C16 1.396(2) . ?
C11 H11 0.9300 . ?
C12 C42 1.390(3) . ?
C12 C25 1.392(2) . ?
C12 H12 0.9300 . ?
C13 C15 1.394(2) . ?
C13 C20 1.395(2) . ?
C13 P2 1.8369(16) . ?
C14 C19 1.386(3) . ?
C14 C40 1.392(3) . ?
C14 H14 0.9300 . ?
C15 C28 1.391(2) . ?
C15 H15 0.9300 . ?
C16 P2 1.8387(17) . ?
C17 C57 1.386(3) . ?
C17 C26 1.400(2) . ?
C17 H17 0.9300 . ?
C18 C57 1.386(3) . ?
C18 H18 0.9300 . ?
C19 C49 1.383(2) . ?
C19 P3 1.8308(16) . ?
C20 C21 1.393(2) . ?
C20 H20 0.9300 . ?
C21 C24 1.388(3) . ?
C21 H21 0.9300 . ?
C23 C46 1.378(3) . ?
C23 H23 0.9300 . ?
C24 C28 1.386(3) . ?
C24 H24 0.9300 . ?
C25 C30 1.402(2) . ?
C25 P3 1.8372(17) . ?
C26 C33 1.387(2) . ?
C26 P5 1.8336(17) . ?
C28 H28 0.9300 . ?
C29 C31 1.394(3) . ?
C29 C47 1.400(3) . ?
C29 P4 1.8145(17) . ?
C30 C62 1.390(3) . ?
C30 H30 0.9300 . ?
C31 C43 1.394(3) . ?
C31 H31 0.9300 . ?
C32 C46 1.387(3) . ?
C32 H32 0.9300 . ?
C33 H33 0.9300 . ?
C34 C40 1.374(3) . ?
C34 C56 1.376(3) . ?
C34 H34 0.9300 . ?
C35 P5 1.8286(17) . ?
C35 Si6 1.8946(18) . ?
C35 H35A 0.9700 . ?
C35 H35B 0.9700 . ?
C36 P3 1.8241(16) . ?
C36 Si6 1.8821(16) . ?
C36 H36A 0.9700 . ?
C36 H36B 0.9700 . ?
C37 C53 1.388(3) . ?
C37 C50 1.399(3) . ?
C37 H37 0.9300 . ?
C38 C48 1.392(3) . ?
C38 C50 1.398(2) . ?
C38 H38 0.9300 . ?
C39 C58 1.386(3) . ?
C39 C63 1.404(3) . ?
C39 H39 0.9300 . ?
C40 H40 0.9300 . ?
C42 C54 1.381(3) . ?
C42 H42 0.9300 . ?
C43 C44 1.382(3) . ?
C43 H43 0.9300 . ?
C44 C45 1.386(3) . ?
C44 H44 0.9300 . ?
C45 C47 1.387(3) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
C47 H47 0.9300 . ?
C48 C60 1.383(3) . ?
C48 H48 0.9300 . ?
C49 C56 1.388(3) . ?
C49 H49 0.9300 . ?
C50 P4 1.8115(17) . ?
C51 C61 1.375(5) . ?
C51 C55 1.396(3) . ?
C51 H51 0.9300 . ?
C53 C60 1.386(3) . ?
C53 H53 0.9300 . ?
C54 C62 1.387(3) . ?
C54 H54 0.9300 . ?
C55 C63 1.390(3) . ?
C55 H55 0.9300 . ?
C56 H56 0.9300 . ?
C57 H57 0.9300 . ?
C58 C61 1.377(4) . ?
C58 H58 0.9300 . ?
C59 P2 1.8281(17) . ?
C59 Si6 1.8933(16) . ?
C59 H59A 0.9700 . ?
C59 H59B 0.9700 . ?
C60 H60 0.9300 . ?
C61 H61 0.9300 . ?
C62 H62 0.9300 . ?
C63 P5 1.8250(18) . ?
C64 Si6 1.8514(18) . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
P2 Ni1 2.3078(5) . ?
P3 Ni1 2.2123(4) . ?
P4 Ni1 2.1321(5) . ?
P5 Ni1 2.2211(5) . ?
N1 C99 1.128(4) . ?
C99 C100 1.493(5) . ?
C100 H101 0.9600 . ?
C100 H100 0.9600 . ?
C100 H103 0.9600 . ?
B1 F1 1.355(5) . ?
B1 F3 1.363(5) . ?
B1 F2 1.385(5) . ?
B1 F4 1.433(6) . ?
B1B F3B 1.252(15) . ?
B1B F2B 1.309(16) . ?
B1B F1B 1.438(15) . ?
B1B F4B 1.506(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C18 C1 C33 120.25(17) . . ?
C18 C1 H1 119.9 . . ?
C33 C1 H1 119.9 . . ?
P4 C2 Ni1 67.92(6) . . ?
P4 C2 H2A 116.9 . . ?
Ni1 C2 H2A 116.9 . . ?
P4 C2 H2B 116.9 . . ?
Ni1 C2 H2B 116.9 . . ?
H2A C2 H2B 113.9 . . ?
C32 C10 C16 120.65(18) . . ?
C32 C10 H10 119.7 . . ?
C16 C10 H10 119.7 . . ?
C23 C11 C16 120.30(17) . . ?
C23 C11 H11 119.9 . . ?
C16 C11 H11 119.9 . . ?
C42 C12 C25 120.88(16) . . ?
C42 C12 H12 119.6 . . ?
C25 C12 H12 119.6 . . ?
C15 C13 C20 118.99(15) . . ?
C15 C13 P2 122.23(13) . . ?
C20 C13 P2 118.74(12) . . ?
C19 C14 C40 120.87(18) . . ?
C19 C14 H14 119.6 . . ?
C40 C14 H14 119.6 . . ?
C28 C15 C13 120.27(17) . . ?
C28 C15 H15 119.9 . . ?
C13 C15 H15 119.9 . . ?
C11 C16 C10 118.58(16) . . ?
C11 C16 P2 124.43(14) . . ?
C10 C16 P2 116.99(13) . . ?
C57 C17 C26 120.44(17) . . ?
C57 C17 H17 119.8 . . ?
C26 C17 H17 119.8 . . ?
C1 C18 C57 119.80(17) . . ?
C1 C18 H18 120.1 . . ?
C57 C18 H18 120.1 . . ?
C49 C19 C14 118.52(16) . . ?
C49 C19 P3 122.67(14) . . ?
C14 C19 P3 118.65(13) . . ?
C21 C20 C13 120.74(16) . . ?
C21 C20 H20 119.6 . . ?
C13 C20 H20 119.6 . . ?
C24 C21 C20 119.60(17) . . ?
C24 C21 H21 120.2 . . ?
C20 C21 H21 120.2 . . ?
C46 C23 C11 120.52(17) . . ?
C46 C23 H23 119.7 . . ?
C11 C23 H23 119.7 . . ?
C28 C24 C21 120.12(15) . . ?
C28 C24 H24 119.9 . . ?
C21 C24 H24 119.9 . . ?
C12 C25 C30 118.65(16) . . ?
C12 C25 P3 121.61(12) . . ?
C30 C25 P3 119.60(13) . . ?
C33 C26 C17 118.87(16) . . ?
C33 C26 P5 121.05(13) . . ?
C17 C26 P5 120.07(13) . . ?
C24 C28 C15 120.27(17) . . ?
C24 C28 H28 119.9 . . ?
C15 C28 H28 119.9 . . ?
C31 C29 C47 119.23(16) . . ?
C31 C29 P4 120.69(13) . . ?
C47 C29 P4 119.97(14) . . ?
C62 C30 C25 120.11(17) . . ?
C62 C30 H30 119.9 . . ?
C25 C30 H30 119.9 . . ?
C43 C31 C29 120.01(18) . . ?
C43 C31 H31 120.0 . . ?
C29 C31 H31 120.0 . . ?
C10 C32 C46 120.36(19) . . ?
C10 C32 H32 119.8 . . ?
C46 C32 H32 119.8 . . ?
C26 C33 C1 120.49(17) . . ?
C26 C33 H33 119.8 . . ?
C1 C33 H33 119.8 . . ?
C40 C34 C56 119.43(18) . . ?
C40 C34 H34 120.3 . . ?
C56 C34 H34 120.3 . . ?
P5 C35 Si6 110.36(8) . . ?
P5 C35 H35A 109.6 . . ?
Si6 C35 H35A 109.6 . . ?
P5 C35 H35B 109.6 . . ?
Si6 C35 H35B 109.6 . . ?
H35A C35 H35B 108.1 . . ?
P3 C36 Si6 111.75(8) . . ?
P3 C36 H36A 109.3 . . ?
Si6 C36 H36A 109.3 . . ?
P3 C36 H36B 109.3 . . ?
Si6 C36 H36B 109.3 . . ?
H36A C36 H36B 107.9 . . ?
C53 C37 C50 120.50(18) . . ?
C53 C37 H37 119.7 . . ?
C50 C37 H37 119.7 . . ?
C48 C38 C50 119.43(19) . . ?
C48 C38 H38 120.3 . . ?
C50 C38 H38 120.3 . . ?
C58 C39 C63 120.3(2) . . ?
C58 C39 H39 119.9 . . ?
C63 C39 H39 119.9 . . ?
C34 C40 C14 120.02(19) . . ?
C34 C40 H40 120.0 . . ?
C14 C40 H40 120.0 . . ?
C54 C42 C12 120.06(18) . . ?
C54 C42 H42 120.0 . . ?
C12 C42 H42 120.0 . . ?
C44 C43 C31 120.45(19) . . ?
C44 C43 H43 119.8 . . ?
C31 C43 H43 119.8 . . ?
C43 C44 C45 119.76(18) . . ?
C43 C44 H44 120.1 . . ?
C45 C44 H44 120.1 . . ?
C44 C45 C47 120.45(19) . . ?
C44 C45 H45 119.8 . . ?
C47 C45 H45 119.8 . . ?
C23 C46 C32 119.60(18) . . ?
C23 C46 H46 120.2 . . ?
C32 C46 H46 120.2 . . ?
C45 C47 C29 120.10(18) . . ?
C45 C47 H47 119.9 . . ?
C29 C47 H47 119.9 . . ?
C60 C48 C38 120.23(19) . . ?
C60 C48 H48 119.9 . . ?
C38 C48 H48 119.9 . . ?
C19 C49 C56 120.37(19) . . ?
C19 C49 H49 119.8 . . ?
C56 C49 H49 119.8 . . ?
C38 C50 C37 119.68(17) . . ?
C38 C50 P4 120.97(15) . . ?
C37 C50 P4 119.17(13) . . ?
C61 C51 C55 120.9(2) . . ?
C61 C51 H51 119.5 . . ?
C55 C51 H51 119.5 . . ?
C60 C53 C37 119.3(2) . . ?
C60 C53 H53 120.4 . . ?
C37 C53 H53 120.4 . . ?
C42 C54 C62 119.84(18) . . ?
C42 C54 H54 120.1 . . ?
C62 C54 H54 120.1 . . ?
C63 C55 C51 119.8(2) . . ?
C63 C55 H55 120.1 . . ?
C51 C55 H55 120.1 . . ?
C34 C56 C49 120.74(19) . . ?
C34 C56 H56 119.6 . . ?
C49 C56 H56 119.6 . . ?
C17 C57 C18 120.05(18) . . ?
C17 C57 H57 120.0 . . ?
C18 C57 H57 120.0 . . ?
C61 C58 C39 120.5(3) . . ?
C61 C58 H58 119.7 . . ?
C39 C58 H58 119.7 . . ?
P2 C59 Si6 112.80(8) . . ?
P2 C59 H59A 109.0 . . ?
Si6 C59 H59A 109.0 . . ?
P2 C59 H59B 109.0 . . ?
Si6 C59 H59B 109.0 . . ?
H59A C59 H59B 107.8 . . ?
C48 C60 C53 120.87(19) . . ?
C48 C60 H60 119.6 . . ?
C53 C60 H60 119.6 . . ?
C51 C61 C58 119.6(2) . . ?
C51 C61 H61 120.2 . . ?
C58 C61 H61 120.2 . . ?
C54 C62 C30 120.46(17) . . ?
C54 C62 H62 119.8 . . ?
C30 C62 H62 119.8 . . ?
C55 C63 C39 118.86(19) . . ?
C55 C63 P5 122.93(16) . . ?
C39 C63 P5 118.03(15) . . ?
Si6 C64 H64A 109.5 . . ?
Si6 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
Si6 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C64 Si6 C36 109.74(8) . . ?
C64 Si6 C59 109.25(8) . . ?
C36 Si6 C59 108.84(7) . . ?
C64 Si6 C35 111.71(9) . . ?
C36 Si6 C35 107.12(7) . . ?
C59 Si6 C35 110.12(7) . . ?
C59 P2 C13 104.76(7) . . ?
C59 P2 C16 104.26(8) . . ?
C13 P2 C16 97.57(7) . . ?
C59 P2 Ni1 106.85(5) . . ?
C13 P2 Ni1 121.44(5) . . ?
C16 P2 Ni1 119.95(5) . . ?
C36 P3 C19 105.00(8) . . ?
C36 P3 C25 105.28(8) . . ?
C19 P3 C25 100.24(7) . . ?
C36 P3 Ni1 110.78(5) . . ?
C19 P3 Ni1 117.73(6) . . ?
C25 P3 Ni1 116.37(5) . . ?
C2 P4 C50 114.64(8) . . ?
C2 P4 C29 114.03(8) . . ?
C50 P4 C29 109.65(8) . . ?
C2 P4 Ni1 63.52(6) . . ?
C50 P4 Ni1 122.43(6) . . ?
C29 P4 Ni1 123.50(6) . . ?
C63 P5 C35 108.25(8) . . ?
C63 P5 C26 99.58(8) . . ?
C35 P5 C26 101.63(8) . . ?
C63 P5 Ni1 117.34(6) . . ?
C35 P5 Ni1 110.62(6) . . ?
C26 P5 Ni1 117.77(6) . . ?
C2 Ni1 P4 48.56(5) . . ?
C2 Ni1 P3 152.09(5) . . ?
P4 Ni1 P3 105.757(18) . . ?
C2 Ni1 P5 95.05(5) . . ?
P4 Ni1 P5 131.26(2) . . ?
P3 Ni1 P5 97.625(17) . . ?
C2 Ni1 P2 105.66(5) . . ?
P4 Ni1 P2 119.078(18) . . ?
P3 Ni1 P2 96.703(17) . . ?
P5 Ni1 P2 99.324(17) . . ?
N1 C99 C100 174.9(4) . . ?
C99 C100 H101 109.5 . . ?
C99 C100 H100 109.5 . . ?
H101 C100 H100 109.5 . . ?
C99 C100 H103 109.5 . . ?
H101 C100 H103 109.5 . . ?
H100 C100 H103 109.5 . . ?
F1 B1 F3 108.1(4) . . ?
F1 B1 F2 111.7(4) . . ?
F3 B1 F2 109.8(3) . . ?
F1 B1 F4 114.7(4) . . ?
F3 B1 F4 106.0(3) . . ?
F2 B1 F4 106.4(4) . . ?
F3B B1B F2B 141.5(17) . . ?
F3B B1B F1B 91.2(11) . . ?
F2B B1B F1B 99.7(15) . . ?
F3B B1B F4B 103.2(11) . . ?
F2B B1B F4B 107.1(15) . . ?
F1B B1B F4B 110.3(10) . . ?
####################################################################### 
# 
# 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_xxx
_database_code_depnum_ccdc_archive 'CCDC 1486083'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_publcif_datablock.id            {12080ffe-f243-4989-b96c-a9770601d576}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Triphos(C)NiCl
_chemical_name_common            Triphos(C)NiCl
_chemical_melting_point          ?
_chemical_formula_moiety         'C41 H39 Cl Ni P3'
_chemical_formula_sum            'C41 H39 Cl Ni P3'
_chemical_formula_weight         718.79

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pna21
_symmetry_space_group_name_Hall  'P 2c -2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   20.70(2)
_cell_length_b                   10.259(11)
_cell_length_c                   16.853(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3579(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7665
_cell_measurement_temperature    293
_cell_measurement_theta_max      26.4
_cell_measurement_theta_min      2.0

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1500
_exptl_absorpt_coefficient_mu    0.779
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)'

_exptl_special_details           ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000


_diffrn_reflns_number            29335
_diffrn_reflns_av_R_equivalents  0.1148
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.22
_diffrn_reflns_theta_max         25.00
_reflns_number_total             6292
_reflns_number_gt                5125
_reflns_threshold_expression     >2σ(I)



_diffrn_ambient_temperature      293
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 13.6612

_diffrn_measurement_details      
;
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 0.0000
	             XTD: 50.1911
	          2theta: 29.9399
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 120.0000
	             XTD: 50.1911
	          2theta: 29.9399
scan:
	Number of images: 180
	           Slice: -60.0000 - 120.0000
	     Image width: 1.0000
	        Exp time: 25.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 54.0000
	             Phi: 240.0000
	             XTD: 50.1911
	          2theta: 29.9399
;
_diffrn_measurement_device       
;
XtaLABmini: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  
;
Rigaku Mercury375R (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.009052
_diffrn_orient_matrix_UB_12      -0.080601
_diffrn_orient_matrix_UB_13      0.054071
_diffrn_orient_matrix_UB_21      0.026449
_diffrn_orient_matrix_UB_22      -0.027544
_diffrn_orient_matrix_UB_23      -0.045417
_diffrn_orient_matrix_UB_31      0.042982
_diffrn_orient_matrix_UB_32      0.015553
_diffrn_orient_matrix_UB_33      0.015641
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           12.0
_diffrn_source_power             0.6
_diffrn_source_voltage           50.0

_computing_cell_refinement       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection       
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction        
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0549P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_number_reflns         6292
_refine_ls_number_parameters     416
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0550
_refine_ls_wR_factor_ref         0.1412
_refine_ls_wR_factor_gt          0.1183
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni2 Ni 0.43418(3) 0.92324(6) 0.40090(5) 0.02934(17) Uani 1 1 d . . .
Cl15 Cl 0.38956(10) 1.00375(17) 0.28895(10) 0.0540(5) Uani 1 1 d . . .
P6 P 0.53864(7) 0.87083(14) 0.40507(10) 0.0301(3) Uani 1 1 d . . .
P8 P 0.44204(7) 1.02045(14) 0.51819(9) 0.0286(3) Uani 1 1 d . . .
P14 P 0.40033(8) 0.73012(14) 0.44852(9) 0.0311(3) Uani 1 1 d . . .
C1B C 0.5174(3) 1.2279(6) 0.4698(4) 0.0417(16) Uani 1 1 d . . .
H1B H 0.4947 1.2179 0.4225 0.050 Uiso 1 1 calc R . .
C1F C 0.5875(4) 1.2572(8) 0.6098(5) 0.062(2) Uani 1 1 d . . .
H1F H 0.6108 1.2669 0.6566 0.075 Uiso 1 1 calc R . .
C1P C 0.2295(3) 0.8060(8) 0.5674(5) 0.063(2) Uani 1 1 d . . .
H1P H 0.2008 0.8754 0.5723 0.076 Uiso 1 1 calc R . .
C1R C 0.5983(4) 1.3417(7) 0.5466(6) 0.063(2) Uani 1 1 d . . .
H1R H 0.6291 1.4073 0.5508 0.075 Uiso 1 1 calc R . .
C6 C 0.5340(3) 0.7125(6) 0.6350(3) 0.0327(13) Uani 1 1 d . . .
H6A H 0.5620 0.7736 0.6610 0.049 Uiso 1 1 calc R . .
H6B H 0.5583 0.6371 0.6195 0.049 Uiso 1 1 calc R . .
H6C H 0.5002 0.6869 0.6707 0.049 Uiso 1 1 calc R . .
C12 C 0.5416(3) 1.1576(7) 0.6031(4) 0.0493(18) Uani 1 1 d . . .
H12 H 0.5347 1.1005 0.6451 0.059 Uiso 1 1 calc R . .
C13 C 0.4640(3) 0.6689(5) 0.5163(3) 0.0294(12) Uani 1 1 d . . .
H13A H 0.4438 0.6133 0.5558 0.035 Uiso 1 1 calc R . .
H13B H 0.4936 0.6153 0.4859 0.035 Uiso 1 1 calc R . .
C16 C 0.2839(3) 0.8178(6) 0.5177(5) 0.055(2) Uani 1 1 d . . .
H16 H 0.2905 0.8942 0.4891 0.067 Uiso 1 1 calc R . .
C17 C 0.5062(3) 1.1444(5) 0.5327(3) 0.0326(13) Uani 1 1 d . . .
C18 C 0.5631(3) 1.3277(7) 0.4776(5) 0.054(2) Uani 1 1 d . . .
H18 H 0.5699 1.3852 0.4358 0.065 Uiso 1 1 calc R . .
C30 C 0.5846(3) 1.0777(6) 0.3161(4) 0.0392(15) Uani 1 1 d . . .
H30 H 0.5436 1.0766 0.2936 0.047 Uiso 1 1 calc R . .
C33 C 0.5256(3) 0.6954(6) 0.2811(4) 0.0426(16) Uani 1 1 d . . .
H33 H 0.4878 0.7417 0.2711 0.051 Uiso 1 1 calc R . .
C35 C 0.6007(3) 0.9884(6) 0.3765(3) 0.0305(13) Uani 1 1 d . . .
C36 C 0.2593(4) 0.5918(7) 0.6015(4) 0.0535(19) Uani 1 1 d . . .
H36 H 0.2506 0.5149 0.6287 0.064 Uiso 1 1 calc R . .
C37 C 0.6304(4) 1.1673(7) 0.2902(4) 0.0534(19) Uani 1 1 d . . .
H37 H 0.6193 1.2283 0.2516 0.064 Uiso 1 1 calc R . .
C38 C 0.6628(3) 0.9904(5) 0.4074(4) 0.0373(13) Uani 1 1 d . . .
H38 H 0.6741 0.9320 0.4471 0.045 Uiso 1 1 calc R . .
C40 C 0.5997(4) 0.5272(7) 0.2444(4) 0.058(2) Uani 1 1 d . . .
H40 H 0.6117 0.4596 0.2108 0.070 Uiso 1 1 calc R . .
C44 C 0.3514(3) 0.6209(7) 0.3119(3) 0.0391(15) Uani 1 1 d . . .
H44 H 0.3380 0.7057 0.3013 0.047 Uiso 1 1 calc R . .
C45 C 0.3364(3) 0.5213(7) 0.2591(4) 0.0453(17) Uani 1 1 d . . .
H45 H 0.3134 0.5400 0.2131 0.054 Uiso 1 1 calc R . .
C51 C 0.3138(4) 1.1775(7) 0.6788(5) 0.0513(18) Uani 1 1 d . . .
H51 H 0.3096 1.1829 0.7336 0.062 Uiso 1 1 calc R . .
C58 C 0.3733(3) 1.1042(5) 0.5645(3) 0.0303(13) Uani 1 1 d . . .
C68 C 0.3868(3) 0.5934(6) 0.3815(3) 0.0321(14) Uani 1 1 d . . .
C69 C 0.5633(3) 0.7288(6) 0.3462(4) 0.0358(14) Uani 1 1 d . . .
C70 C 0.2735(4) 1.2213(7) 0.5494(5) 0.061(2) Uani 1 1 d . . .
H70 H 0.2419 1.2573 0.5169 0.073 Uiso 1 1 calc R . .
C72 C 0.2673(4) 1.2316(7) 0.6306(5) 0.056(2) Uani 1 1 d . . .
H72 H 0.2321 1.2747 0.6525 0.067 Uiso 1 1 calc R . .
C83 C 0.3668(3) 1.1149(6) 0.6460(4) 0.0409(15) Uani 1 1 d . . .
H83 H 0.3982 1.0798 0.6791 0.049 Uiso 1 1 calc R . .
C91 C 0.4055(3) 0.4649(5) 0.3950(4) 0.0372(13) Uani 1 1 d . . .
H91 H 0.4289 0.4446 0.4405 0.045 Uiso 1 1 calc R . .
C103 C 0.3148(3) 0.6004(7) 0.5540(4) 0.0432(16) Uani 1 1 d . . .
H103 H 0.3431 0.5301 0.5507 0.052 Uiso 1 1 calc R . .
C106 C 0.7078(3) 1.0781(6) 0.3796(4) 0.0452(18) Uani 1 1 d . . .
H106 H 0.7493 1.0776 0.4007 0.054 Uiso 1 1 calc R . .
C107 C 0.6923(4) 1.1668(7) 0.3211(4) 0.0503(18) Uani 1 1 d . . .
H107 H 0.7231 1.2255 0.3027 0.060 Uiso 1 1 calc R . .
C111 C 0.3276(3) 0.7156(6) 0.5113(4) 0.0343(13) Uani 1 1 d . . .
C114 C 0.3261(3) 1.1585(6) 0.5151(4) 0.0439(16) Uani 1 1 d . . .
H114 H 0.3298 1.1526 0.4602 0.053 Uiso 1 1 calc R . .
C115 C 0.3898(3) 0.3660(7) 0.3416(4) 0.0443(16) Uani 1 1 d . . .
H115 H 0.4026 0.2807 0.3516 0.053 Uiso 1 1 calc R . .
C118 C 0.2185(4) 0.6933(8) 0.6084(5) 0.058(2) Uani 1 1 d . . .
H118 H 0.1826 0.6866 0.6413 0.070 Uiso 1 1 calc R . .
C119 C 0.3554(3) 0.3949(7) 0.2744(4) 0.0433(17) Uani 1 1 d . . .
H119 H 0.3447 0.3289 0.2389 0.052 Uiso 1 1 calc R . .
C122 C 0.5040(3) 0.7769(5) 0.5606(3) 0.0291(13) Uani 1 1 d . . .
C135 C 0.6393(4) 0.5594(7) 0.3084(4) 0.058(2) Uani 1 1 d . . .
H135 H 0.6777 0.5143 0.3171 0.069 Uiso 1 1 calc R . .
C155 C 0.5433(5) 0.5931(7) 0.2302(5) 0.059(2) Uani 1 1 d . . .
H155 H 0.5171 0.5705 0.1875 0.071 Uiso 1 1 calc R . .
C169 C 0.6207(4) 0.6609(6) 0.3595(4) 0.0506(18) Uani 1 1 d . . .
H169 H 0.6467 0.6829 0.4025 0.061 Uiso 1 1 calc R . .
C204 C 0.4608(3) 0.8916(6) 0.5909(3) 0.0316(13) Uani 1 1 d . . .
H20A H 0.4823 0.9316 0.6359 0.038 Uiso 1 1 calc R . .
H20B H 0.4204 0.8553 0.6099 0.038 Uiso 1 1 calc R . .
C233 C 0.5602(3) 0.8270(6) 0.5092(3) 0.0330(13) Uani 1 1 d . . .
H23A H 0.5935 0.7606 0.5077 0.040 Uiso 1 1 calc R . .
H23B H 0.5786 0.9033 0.5347 0.040 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni2 P8 2.220(2) . ?
Ni2 P6 2.229(3) . ?
Ni2 P14 2.250(2) . ?
Ni2 Cl15 2.257(2) . ?
P6 C35 1.826(6) . ?
P6 C69 1.836(6) . ?
P6 C233 1.866(6) . ?
P8 C58 1.836(6) . ?
P8 C204 1.844(6) . ?
P8 C17 1.854(6) . ?
P14 C68 1.822(6) . ?
P14 C111 1.845(6) . ?
P14 C13 1.853(6) . ?
C1B C17 1.383(9) . ?
C1B C18 1.401(9) . ?
C1B H1B 0.9300 . ?
C1F C1R 1.392(12) . ?
C1F C12 1.399(10) . ?
C1F H1F 0.9300 . ?
C1P C118 1.366(12) . ?
C1P C16 1.409(11) . ?
C1P H1P 0.9300 . ?
C1R C18 1.379(11) . ?
C1R H1R 0.9300 . ?
C6 C122 1.547(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C12 C17 1.401(9) . ?
C12 H12 0.9300 . ?
C13 C122 1.572(8) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C16 C111 1.390(8) . ?
C16 H16 0.9300 . ?
C18 H18 0.9300 . ?
C30 C37 1.391(9) . ?
C30 C35 1.409(8) . ?
C30 H30 0.9300 . ?
C33 C69 1.388(9) . ?
C33 C155 1.404(10) . ?
C33 H33 0.9300 . ?
C35 C38 1.386(8) . ?
C36 C118 1.345(10) . ?
C36 C103 1.403(9) . ?
C36 H36 0.9300 . ?
C37 C107 1.384(11) . ?
C37 H37 0.9300 . ?
C38 C106 1.377(8) . ?
C38 H38 0.9300 . ?
C40 C155 1.371(12) . ?
C40 C135 1.395(11) . ?
C40 H40 0.9300 . ?
C44 C45 1.389(9) . ?
C44 C68 1.413(8) . ?
C44 H44 0.9300 . ?
C45 C119 1.378(10) . ?
C45 H45 0.9300 . ?
C51 C72 1.376(11) . ?
C51 C83 1.386(9) . ?
C51 H51 0.9300 . ?
C58 C83 1.385(8) . ?
C58 C114 1.400(9) . ?
C68 C91 1.393(8) . ?
C69 C169 1.396(9) . ?
C70 C72 1.377(12) . ?
C70 C114 1.391(10) . ?
C70 H70 0.9300 . ?
C72 H72 0.9300 . ?
C83 H83 0.9300 . ?
C91 C115 1.395(8) . ?
C91 H91 0.9300 . ?
C103 C111 1.410(9) . ?
C103 H103 0.9300 . ?
C106 C107 1.379(9) . ?
C106 H106 0.9300 . ?
C107 H107 0.9300 . ?
C114 H114 0.9300 . ?
C115 C119 1.371(9) . ?
C115 H115 0.9300 . ?
C118 H118 0.9300 . ?
C119 H119 0.9300 . ?
C122 C233 1.539(8) . ?
C122 C204 1.564(8) . ?
C135 C169 1.406(9) . ?
C135 H135 0.9300 . ?
C155 H155 0.9300 . ?
C169 H169 0.9300 . ?
C204 H20A 0.9700 . ?
C204 H20B 0.9700 . ?
C233 H23A 0.9700 . ?
C233 H23B 0.9700 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P8 Ni2 P6 90.53(6) . . ?
P8 Ni2 P14 95.78(8) . . ?
P6 Ni2 P14 94.50(7) . . ?
P8 Ni2 Cl15 127.58(9) . . ?
P6 Ni2 Cl15 120.77(8) . . ?
P14 Ni2 Cl15 119.54(8) . . ?
C35 P6 C69 100.8(3) . . ?
C35 P6 C233 103.8(3) . . ?
C69 P6 C233 104.5(3) . . ?
C35 P6 Ni2 121.0(2) . . ?
C69 P6 Ni2 116.3(2) . . ?
C233 P6 Ni2 108.68(19) . . ?
C58 P8 C204 102.5(3) . . ?
C58 P8 C17 100.2(3) . . ?
C204 P8 C17 104.7(3) . . ?
C58 P8 Ni2 122.1(2) . . ?
C204 P8 Ni2 106.6(2) . . ?
C17 P8 Ni2 118.6(2) . . ?
C68 P14 C111 99.6(3) . . ?
C68 P14 C13 103.3(3) . . ?
C111 P14 C13 101.5(3) . . ?
C68 P14 Ni2 120.3(2) . . ?
C111 P14 Ni2 122.0(2) . . ?
C13 P14 Ni2 107.27(19) . . ?
C17 C1B C18 119.6(7) . . ?
C17 C1B H1B 120.2 . . ?
C18 C1B H1B 120.2 . . ?
C1R C1F C12 120.1(8) . . ?
C1R C1F H1F 119.9 . . ?
C12 C1F H1F 119.9 . . ?
C118 C1P C16 120.4(7) . . ?
C118 C1P H1P 119.8 . . ?
C16 C1P H1P 119.8 . . ?
C18 C1R C1F 119.7(7) . . ?
C18 C1R H1R 120.2 . . ?
C1F C1R H1R 120.2 . . ?
C122 C6 H6A 109.5 . . ?
C122 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C122 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1F C12 C17 119.7(7) . . ?
C1F C12 H12 120.2 . . ?
C17 C12 H12 120.2 . . ?
C122 C13 P14 115.4(4) . . ?
C122 C13 H13A 108.4 . . ?
P14 C13 H13A 108.4 . . ?
C122 C13 H13B 108.4 . . ?
P14 C13 H13B 108.4 . . ?
H13A C13 H13B 107.5 . . ?
C111 C16 C1P 120.2(7) . . ?
C111 C16 H16 119.9 . . ?
C1P C16 H16 119.9 . . ?
C1B C17 C12 120.1(6) . . ?
C1B C17 P8 116.3(5) . . ?
C12 C17 P8 123.6(5) . . ?
C1R C18 C1B 120.8(7) . . ?
C1R C18 H18 119.6 . . ?
C1B C18 H18 119.6 . . ?
C37 C30 C35 119.8(6) . . ?
C37 C30 H30 120.1 . . ?
C35 C30 H30 120.1 . . ?
C69 C33 C155 121.4(7) . . ?
C69 C33 H33 119.3 . . ?
C155 C33 H33 119.3 . . ?
C38 C35 C30 118.6(6) . . ?
C38 C35 P6 124.3(5) . . ?
C30 C35 P6 117.0(5) . . ?
C118 C36 C103 121.0(7) . . ?
C118 C36 H36 119.5 . . ?
C103 C36 H36 119.5 . . ?
C107 C37 C30 120.6(6) . . ?
C107 C37 H37 119.7 . . ?
C30 C37 H37 119.7 . . ?
C106 C38 C35 120.7(6) . . ?
C106 C38 H38 119.7 . . ?
C35 C38 H38 119.7 . . ?
C155 C40 C135 121.3(7) . . ?
C155 C40 H40 119.3 . . ?
C135 C40 H40 119.3 . . ?
C45 C44 C68 120.0(6) . . ?
C45 C44 H44 120.0 . . ?
C68 C44 H44 120.0 . . ?
C119 C45 C44 120.6(6) . . ?
C119 C45 H45 119.7 . . ?
C44 C45 H45 119.7 . . ?
C72 C51 C83 120.3(7) . . ?
C72 C51 H51 119.8 . . ?
C83 C51 H51 119.8 . . ?
C83 C58 C114 119.4(6) . . ?
C83 C58 P8 122.3(5) . . ?
C114 C58 P8 118.3(5) . . ?
C91 C68 C44 118.0(6) . . ?
C91 C68 P14 125.8(4) . . ?
C44 C68 P14 116.2(5) . . ?
C33 C69 C169 118.9(6) . . ?
C33 C69 P6 117.8(5) . . ?
C169 C69 P6 123.0(5) . . ?
C72 C70 C114 121.5(7) . . ?
C72 C70 H70 119.3 . . ?
C114 C70 H70 119.3 . . ?
C51 C72 C70 119.3(7) . . ?
C51 C72 H72 120.3 . . ?
C70 C72 H72 120.3 . . ?
C58 C83 C51 120.6(6) . . ?
C58 C83 H83 119.7 . . ?
C51 C83 H83 119.7 . . ?
C68 C91 C115 121.2(6) . . ?
C68 C91 H91 119.4 . . ?
C115 C91 H91 119.4 . . ?
C36 C103 C111 119.9(6) . . ?
C36 C103 H103 120.1 . . ?
C111 C103 H103 120.1 . . ?
C38 C106 C107 121.1(7) . . ?
C38 C106 H106 119.4 . . ?
C107 C106 H106 119.4 . . ?
C106 C107 C37 119.1(7) . . ?
C106 C107 H107 120.4 . . ?
C37 C107 H107 120.4 . . ?
C16 C111 C103 118.0(6) . . ?
C16 C111 P14 121.0(5) . . ?
C103 C111 P14 120.9(5) . . ?
C70 C114 C58 118.9(7) . . ?
C70 C114 H114 120.6 . . ?
C58 C114 H114 120.6 . . ?
C119 C115 C91 119.8(6) . . ?
C119 C115 H115 120.1 . . ?
C91 C115 H115 120.1 . . ?
C36 C118 C1P 120.4(7) . . ?
C36 C118 H118 119.8 . . ?
C1P C118 H118 119.8 . . ?
C115 C119 C45 120.3(6) . . ?
C115 C119 H119 119.8 . . ?
C45 C119 H119 119.8 . . ?
C233 C122 C6 107.2(5) . . ?
C233 C122 C204 111.4(5) . . ?
C6 C122 C204 106.6(4) . . ?
C233 C122 C13 111.5(5) . . ?
C6 C122 C13 107.2(4) . . ?
C204 C122 C13 112.5(5) . . ?
C40 C135 C169 119.2(8) . . ?
C40 C135 H135 120.4 . . ?
C169 C135 H135 120.4 . . ?
C40 C155 C33 119.0(7) . . ?
C40 C155 H155 120.5 . . ?
C33 C155 H155 120.5 . . ?
C69 C169 C135 120.3(7) . . ?
C69 C169 H169 119.9 . . ?
C135 C169 H169 119.9 . . ?
C122 C204 P8 116.3(4) . . ?
C122 C204 H20A 108.2 . . ?
P8 C204 H20A 108.2 . . ?
C122 C204 H20B 108.2 . . ?
P8 C204 H20B 108.2 . . ?
H20A C204 H20B 107.4 . . ?
C122 C233 P6 115.4(4) . . ?
C122 C233 H23A 108.4 . . ?
P6 C233 H23A 108.4 . . ?
C122 C233 H23B 108.4 . . ?
P6 C233 H23B 108.4 . . ?
H23A C233 H23B 107.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P8 Ni2 P6 C35 -82.0(2) . . . . ?
P14 Ni2 P6 C35 -177.9(2) . . . . ?
Cl15 Ni2 P6 C35 53.6(2) . . . . ?
P8 Ni2 P6 C69 155.3(2) . . . . ?
P14 Ni2 P6 C69 59.4(2) . . . . ?
Cl15 Ni2 P6 C69 -69.1(2) . . . . ?
P8 Ni2 P6 C233 37.7(2) . . . . ?
P14 Ni2 P6 C233 -58.2(2) . . . . ?
Cl15 Ni2 P6 C233 173.3(2) . . . . ?
P6 Ni2 P8 C58 177.8(2) . . . . ?
P14 Ni2 P8 C58 -87.7(2) . . . . ?
Cl15 Ni2 P8 C58 47.0(2) . . . . ?
P6 Ni2 P8 C204 -65.3(2) . . . . ?
P14 Ni2 P8 C204 29.3(2) . . . . ?
Cl15 Ni2 P8 C204 164.0(2) . . . . ?
P6 Ni2 P8 C17 52.3(2) . . . . ?
P14 Ni2 P8 C17 146.9(2) . . . . ?
Cl15 Ni2 P8 C17 -78.5(2) . . . . ?
P8 Ni2 P14 C68 -177.2(2) . . . . ?
P6 Ni2 P14 C68 -86.2(2) . . . . ?
Cl15 Ni2 P14 C68 43.1(2) . . . . ?
P8 Ni2 P14 C111 56.4(2) . . . . ?
P6 Ni2 P14 C111 147.3(2) . . . . ?
Cl15 Ni2 P14 C111 -83.3(3) . . . . ?
P8 Ni2 P14 C13 -59.7(2) . . . . ?
P6 Ni2 P14 C13 31.3(2) . . . . ?
Cl15 Ni2 P14 C13 160.6(2) . . . . ?
C12 C1F C1R C18 0.7(12) . . . . ?
C1R C1F C12 C17 -0.7(12) . . . . ?
C68 P14 C13 C122 158.6(4) . . . . ?
C111 P14 C13 C122 -98.4(4) . . . . ?
Ni2 P14 C13 C122 30.5(5) . . . . ?
C118 C1P C16 C111 -1.3(11) . . . . ?
C18 C1B C17 C12 -1.6(9) . . . . ?
C18 C1B C17 P8 177.3(5) . . . . ?
C1F C12 C17 C1B 1.2(10) . . . . ?
C1F C12 C17 P8 -177.6(6) . . . . ?
C58 P8 C17 C1B -95.7(5) . . . . ?
C204 P8 C17 C1B 158.4(5) . . . . ?
Ni2 P8 C17 C1B 39.8(5) . . . . ?
C58 P8 C17 C12 83.2(6) . . . . ?
C204 P8 C17 C12 -22.8(6) . . . . ?
Ni2 P8 C17 C12 -141.3(5) . . . . ?
C1F C1R C18 C1B -1.1(11) . . . . ?
C17 C1B C18 C1R 1.6(10) . . . . ?
C37 C30 C35 C38 -1.6(9) . . . . ?
C37 C30 C35 P6 -178.2(5) . . . . ?
C69 P6 C35 C38 -79.5(5) . . . . ?
C233 P6 C35 C38 28.6(6) . . . . ?
Ni2 P6 C35 C38 150.7(4) . . . . ?
C69 P6 C35 C30 96.9(5) . . . . ?
C233 P6 C35 C30 -155.1(5) . . . . ?
Ni2 P6 C35 C30 -33.0(5) . . . . ?
C35 C30 C37 C107 2.4(11) . . . . ?
C30 C35 C38 C106 0.2(9) . . . . ?
P6 C35 C38 C106 176.6(5) . . . . ?
C68 C44 C45 C119 0.6(10) . . . . ?
C204 P8 C58 C83 32.3(6) . . . . ?
C17 P8 C58 C83 -75.4(5) . . . . ?
Ni2 P8 C58 C83 151.2(4) . . . . ?
C204 P8 C58 C114 -147.5(5) . . . . ?
C17 P8 C58 C114 104.8(5) . . . . ?
Ni2 P8 C58 C114 -28.6(5) . . . . ?
C45 C44 C68 C91 -0.2(9) . . . . ?
C45 C44 C68 P14 -177.2(5) . . . . ?
C111 P14 C68 C91 -87.1(6) . . . . ?
C13 P14 C68 C91 17.3(6) . . . . ?
Ni2 P14 C68 C91 136.8(5) . . . . ?
C111 P14 C68 C44 89.7(5) . . . . ?
C13 P14 C68 C44 -166.0(5) . . . . ?
Ni2 P14 C68 C44 -46.5(5) . . . . ?
C155 C33 C69 C169 1.7(10) . . . . ?
C155 C33 C69 P6 176.0(5) . . . . ?
C35 P6 C69 C33 -107.6(5) . . . . ?
C233 P6 C69 C33 144.9(5) . . . . ?
Ni2 P6 C69 C33 25.1(6) . . . . ?
C35 P6 C69 C169 66.5(6) . . . . ?
C233 P6 C69 C169 -41.0(6) . . . . ?
Ni2 P6 C69 C169 -160.8(5) . . . . ?
C83 C51 C72 C70 0.9(11) . . . . ?
C114 C70 C72 C51 -0.6(12) . . . . ?
C114 C58 C83 C51 0.6(10) . . . . ?
P8 C58 C83 C51 -179.2(5) . . . . ?
C72 C51 C83 C58 -1.0(11) . . . . ?
C44 C68 C91 C115 -0.1(9) . . . . ?
P14 C68 C91 C115 176.6(5) . . . . ?
C118 C36 C103 C111 -1.4(11) . . . . ?
C35 C38 C106 C107 0.5(9) . . . . ?
C38 C106 C107 C37 0.2(10) . . . . ?
C30 C37 C107 C106 -1.6(11) . . . . ?
C1P C16 C111 C103 1.7(10) . . . . ?
C1P C16 C111 P14 -178.5(5) . . . . ?
C36 C103 C111 C16 -0.3(9) . . . . ?
C36 C103 C111 P14 179.8(5) . . . . ?
C68 P14 C111 C16 -121.6(5) . . . . ?
C13 P14 C111 C16 132.6(5) . . . . ?
Ni2 P14 C111 C16 13.6(6) . . . . ?
C68 P14 C111 C103 58.3(6) . . . . ?
C13 P14 C111 C103 -47.6(6) . . . . ?
Ni2 P14 C111 C103 -166.5(4) . . . . ?
C72 C70 C114 C58 0.3(11) . . . . ?
C83 C58 C114 C70 -0.3(9) . . . . ?
P8 C58 C114 C70 179.5(5) . . . . ?
C68 C91 C115 C119 0.1(10) . . . . ?
C103 C36 C118 C1P 1.7(12) . . . . ?
C16 C1P C118 C36 -0.4(12) . . . . ?
C91 C115 C119 C45 0.2(10) . . . . ?
C44 C45 C119 C115 -0.6(10) . . . . ?
P14 C13 C122 C233 -84.5(5) . . . . ?
P14 C13 C122 C6 158.4(4) . . . . ?
P14 C13 C122 C204 41.5(6) . . . . ?
C155 C40 C135 C169 0.5(12) . . . . ?
C135 C40 C155 C33 0.3(12) . . . . ?
C69 C33 C155 C40 -1.4(11) . . . . ?
C33 C69 C169 C135 -0.8(10) . . . . ?
P6 C69 C169 C135 -174.9(5) . . . . ?
C40 C135 C169 C69 -0.3(11) . . . . ?
C233 C122 C204 P8 42.4(6) . . . . ?
C6 C122 C204 P8 159.1(4) . . . . ?
C13 C122 C204 P8 -83.7(5) . . . . ?
C58 P8 C204 C122 163.3(4) . . . . ?
C17 P8 C204 C122 -92.5(5) . . . . ?
Ni2 P8 C204 C122 33.9(5) . . . . ?
C6 C122 C233 P6 165.2(4) . . . . ?
C204 C122 C233 P6 -78.5(5) . . . . ?
C13 C122 C233 P6 48.1(6) . . . . ?
C35 P6 C233 C122 155.5(4) . . . . ?
C69 P6 C233 C122 -99.3(4) . . . . ?
Ni2 P6 C233 C122 25.6(5) . . . . ?


_refine_diff_density_max         0.370
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_ap225sq
_database_code_depnum_ccdc_archive 'CCDC 1486084'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
# 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 -0.001 -0.001 -0.001 9147 1577 'one disordered molecule THF per formula unit'
_platon_squeeze_details          
;
;
_publcif_datablock.id            {55c7935b-4d26-4e4a-b34c-bea152f975b8}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'Triphos_C_NiCl BF4'
_chemical_name_common            'Triphos_C_NiCl BF4'
_chemical_melting_point          ?
_chemical_formula_moiety         '(C41 H39 Cl Ni P3) (B F4)'
_chemical_formula_sum            'C41 H39 B Cl F4 Ni P3'
_chemical_formula_weight         805.60

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F d-3'
_symmetry_space_group_name_Hall  '-F 2uv 2vw'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/4, -y+1/4, z'
'x, -y+1/4, -z+1/4'
'-x+1/4, y, -z+1/4'
'z, x, y'
'-z+1/4, -x+1/4, y'
'z, -x+1/4, -y+1/4'
'-z+1/4, x, -y+1/4'
'y, z, x'
'y, -z+1/4, -x+1/4'
'-y+1/4, z, -x+1/4'
'-y+1/4, -z+1/4, x'
'x, y+1/2, z+1/2'
'-x+1/4, -y+3/4, z+1/2'
'x, -y+3/4, -z+3/4'
'-x+1/4, y+1/2, -z+3/4'
'z, x+1/2, y+1/2'
'-z+1/4, -x+3/4, y+1/2'
'z, -x+3/4, -y+3/4'
'-z+1/4, x+1/2, -y+3/4'
'y, z+1/2, x+1/2'
'y, -z+3/4, -x+3/4'
'-y+1/4, z+1/2, -x+3/4'
'-y+1/4, -z+3/4, x+1/2'
'x+1/2, y, z+1/2'
'-x+3/4, -y+1/4, z+1/2'
'x+1/2, -y+1/4, -z+3/4'
'-x+3/4, y, -z+3/4'
'z+1/2, x, y+1/2'
'-z+3/4, -x+1/4, y+1/2'
'z+1/2, -x+1/4, -y+3/4'
'-z+3/4, x, -y+3/4'
'y+1/2, z, x+1/2'
'y+1/2, -z+1/4, -x+3/4'
'-y+3/4, z, -x+3/4'
'-y+3/4, -z+1/4, x+1/2'
'x+1/2, y+1/2, z'
'-x+3/4, -y+3/4, z'
'x+1/2, -y+3/4, -z+1/4'
'-x+3/4, y+1/2, -z+1/4'
'z+1/2, x+1/2, y'
'-z+3/4, -x+3/4, y'
'z+1/2, -x+3/4, -y+1/4'
'-z+3/4, x+1/2, -y+1/4'
'y+1/2, z+1/2, x'
'y+1/2, -z+3/4, -x+1/4'
'-y+3/4, z+1/2, -x+1/4'
'-y+3/4, -z+3/4, x'
'-x, -y, -z'
'x-1/4, y-1/4, -z'
'-x, y-1/4, z-1/4'
'x-1/4, -y, z-1/4'
'-z, -x, -y'
'z-1/4, x-1/4, -y'
'-z, x-1/4, y-1/4'
'z-1/4, -x, y-1/4'
'-y, -z, -x'
'-y, z-1/4, x-1/4'
'y-1/4, -z, x-1/4'
'y-1/4, z-1/4, -x'
'-x, -y+1/2, -z+1/2'
'x-1/4, y+1/4, -z+1/2'
'-x, y+1/4, z+1/4'
'x-1/4, -y+1/2, z+1/4'
'-z, -x+1/2, -y+1/2'
'z-1/4, x+1/4, -y+1/2'
'-z, x+1/4, y+1/4'
'z-1/4, -x+1/2, y+1/4'
'-y, -z+1/2, -x+1/2'
'-y, z+1/4, x+1/4'
'y-1/4, -z+1/2, x+1/4'
'y-1/4, z+1/4, -x+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/4, y-1/4, -z+1/2'
'-x+1/2, y-1/4, z+1/4'
'x+1/4, -y, z+1/4'
'-z+1/2, -x, -y+1/2'
'z+1/4, x-1/4, -y+1/2'
'-z+1/2, x-1/4, y+1/4'
'z+1/4, -x, y+1/4'
'-y+1/2, -z, -x+1/2'
'-y+1/2, z-1/4, x+1/4'
'y+1/4, -z, x+1/4'
'y+1/4, z-1/4, -x+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/4, y+1/4, -z'
'-x+1/2, y+1/4, z-1/4'
'x+1/4, -y+1/2, z-1/4'
'-z+1/2, -x+1/2, -y'
'z+1/4, x+1/4, -y'
'-z+1/2, x+1/4, y-1/4'
'z+1/4, -x+1/2, y-1/4'
'-y+1/2, -z+1/2, -x'
'-y+1/2, z+1/4, x-1/4'
'y+1/4, -z+1/2, x-1/4'
'y+1/4, z+1/4, -x'

_cell_length_a                   33.558(2)
_cell_length_b                   33.558(2)
_cell_length_c                   33.558(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     37791(4)
_cell_formula_units_Z            32
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8000
_cell_measurement_theta_min      2.1
_cell_measurement_theta_max      23.7

_exptl_crystal_description       plate
_exptl_crystal_colour            green
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.133
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13312
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8236
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_process_details   
;
 [X-Red (Stoe & Cie, 2001) and X-Shape (Stoe & Cie, 1999)]
;


_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            52558
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_sigmaI/netI    0.0821
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         1.72
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2517
_reflns_number_gt                1406
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0503P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2517
_refine_ls_number_parameters     158
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0401
_refine_ls_wR_factor_ref         0.0984
_refine_ls_wR_factor_gt          0.0890
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_restrained_S_all      0.825
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.249124(14) 0.249124(14) 0.249124(14) 0.03106(19) Uani 1 3 d S . .
Cl2 Cl 0.21205(3) 0.21205(3) 0.21205(3) 0.0701(6) Uani 1 3 d S . .
P1 P 0.22948(3) 0.27584(3) 0.30756(3) 0.0317(2) Uani 1 1 d . . .
C1 C 0.33528(12) 0.33528(12) 0.33528(12) 0.0355(18) Uani 1 3 d S . .
C7 C 0.30884(11) 0.30884(11) 0.30884(11) 0.0304(15) Uani 1 3 d S . .
C8 C 0.21499(11) 0.19813(12) 0.33042(12) 0.0397(10) Uani 1 1 d . . .
H8 H 0.2079 0.1948 0.3038 0.048 Uiso 1 1 calc R . .
C9 C 0.18053(11) 0.29942(12) 0.30938(11) 0.0374(10) Uani 1 1 d . . .
C11 C 0.23837(11) 0.23997(11) 0.38346(11) 0.0400(10) Uani 1 1 d . . .
H11 H 0.2469 0.2646 0.3928 0.048 Uiso 1 1 calc R . .
C15 C 0.26577(10) 0.31326(11) 0.32470(11) 0.0329(9) Uani 1 1 d . . .
H15A H 0.2560 0.3394 0.3172 0.040 Uiso 1 1 calc R . .
H15B H 0.2667 0.3124 0.3536 0.040 Uiso 1 1 calc R . .
C17 C 0.17401(13) 0.33784(13) 0.32175(12) 0.0504(12) Uani 1 1 d . . .
H17 H 0.1952 0.3529 0.3314 0.060 Uiso 1 1 calc R . .
C19 C 0.21309(12) 0.16629(12) 0.35614(14) 0.0473(11) Uani 1 1 d . . .
H19 H 0.2045 0.1416 0.3470 0.057 Uiso 1 1 calc R . .
C25 C 0.22747(10) 0.23532(11) 0.34379(11) 0.0316(9) Uani 1 1 d . . .
C31 C 0.23650(13) 0.20769(13) 0.40895(13) 0.0522(12) Uani 1 1 d . . .
H31 H 0.2438 0.2108 0.4355 0.063 Uiso 1 1 calc R . .
C33 C 0.22392(13) 0.17092(13) 0.39545(15) 0.0555(12) Uani 1 1 d . . .
H33 H 0.2228 0.1494 0.4128 0.067 Uiso 1 1 calc R . .
C34 C 0.11073(14) 0.29336(17) 0.29470(15) 0.0693(14) Uani 1 1 d . . .
H34 H 0.0894 0.2780 0.2859 0.083 Uiso 1 1 calc R . .
C40 C 0.14855(13) 0.27711(14) 0.29590(14) 0.0568(13) Uani 1 1 d . . .
H40 H 0.1525 0.2510 0.2876 0.068 Uiso 1 1 calc R . .
C45 C 0.10455(14) 0.33202(17) 0.30639(14) 0.0633(14) Uani 1 1 d . . .
H45 H 0.0792 0.3430 0.3051 0.076 Uiso 1 1 calc R . .
C46 C 0.13598(15) 0.35442(15) 0.32002(14) 0.0631(14) Uani 1 1 d . . .
H46 H 0.1319 0.3806 0.3281 0.076 Uiso 1 1 calc R . .
F3 F 0.02688(7) 0.02688(7) 0.52688(7) 0.0635(12) Uani 1 3 d S . .
F4 F 0.07618(7) 0.07306(7) 0.52656(7) 0.0584(7) Uani 1 1 d . . .
B13 B 0.05016(15) 0.05016(15) 0.55016(15) 0.047(2) Uani 1 3 d S . .
H1 H 0.3240(9) 0.3615(9) 0.3363(10) 0.032(10) Uiso 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Cl2 2.155(2) . ?
Ni1 P1 2.2547(11) 9 ?
Ni1 P1 2.2547(11) 5 ?
Ni1 P1 2.2547(11) . ?
P1 C9 1.824(4) . ?
P1 C25 1.826(4) . ?
P1 C15 1.841(4) . ?
C1 C7 1.537(9) . ?
C1 H1 0.96(3) . ?
C7 C15 1.547(4) . ?
C7 C15 1.547(4) 9 ?
C7 C15 1.547(4) 5 ?
C8 C19 1.375(5) . ?
C8 C25 1.391(5) . ?
C8 H8 0.9300 . ?
C9 C17 1.372(5) . ?
C9 C40 1.385(5) . ?
C11 C31 1.382(5) . ?
C11 C25 1.389(5) . ?
C11 H11 0.9300 . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C17 C46 1.393(6) . ?
C17 H17 0.9300 . ?
C19 C33 1.377(6) . ?
C19 H19 0.9300 . ?
C31 C33 1.381(6) . ?
C31 H31 0.9300 . ?
C33 H33 0.9300 . ?
C34 C45 1.371(6) . ?
C34 C40 1.382(6) . ?
C34 H34 0.9300 . ?
C40 H40 0.9300 . ?
C45 C46 1.373(7) . ?
C45 H45 0.9300 . ?
C46 H46 0.9300 . ?
F3 B13 1.354(9) . ?
F4 B13 1.407(4) . ?
B13 F4 1.407(4) 21_545 ?
B13 F4 1.407(4) 29_455 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Ni1 P1 124.26(3) . 9 ?
Cl2 Ni1 P1 124.26(3) . 5 ?
P1 Ni1 P1 91.41(4) 9 5 ?
Cl2 Ni1 P1 124.26(3) . . ?
P1 Ni1 P1 91.41(4) 9 . ?
P1 Ni1 P1 91.41(4) 5 . ?
C9 P1 C25 105.51(17) . . ?
C9 P1 C15 106.82(18) . . ?
C25 P1 C15 108.93(17) . . ?
C9 P1 Ni1 117.70(13) . . ?
C25 P1 Ni1 107.09(12) . . ?
C15 P1 Ni1 110.46(11) . . ?
C7 C1 H1 109(2) . . ?
C1 C7 C15 106.6(3) . . ?
C1 C7 C15 106.6(3) . 9 ?
C15 C7 C15 112.2(2) . 9 ?
C1 C7 C15 106.6(3) . 5 ?
C15 C7 C15 112.2(2) . 5 ?
C15 C7 C15 112.2(2) 9 5 ?
C19 C8 C25 120.6(4) . . ?
C19 C8 H8 119.7 . . ?
C25 C8 H8 119.7 . . ?
C17 C9 C40 118.9(4) . . ?
C17 C9 P1 124.1(3) . . ?
C40 C9 P1 116.9(3) . . ?
C31 C11 C25 119.6(4) . . ?
C31 C11 H11 120.2 . . ?
C25 C11 H11 120.2 . . ?
C7 C15 P1 116.4(3) . . ?
C7 C15 H15A 108.2 . . ?
P1 C15 H15A 108.2 . . ?
C7 C15 H15B 108.2 . . ?
P1 C15 H15B 108.2 . . ?
H15A C15 H15B 107.3 . . ?
C9 C17 C46 120.6(4) . . ?
C9 C17 H17 119.7 . . ?
C46 C17 H17 119.7 . . ?
C8 C19 C33 120.1(4) . . ?
C8 C19 H19 120.0 . . ?
C33 C19 H19 120.0 . . ?
C11 C25 C8 119.3(3) . . ?
C11 C25 P1 123.0(3) . . ?
C8 C25 P1 117.7(3) . . ?
C33 C31 C11 120.8(4) . . ?
C33 C31 H31 119.6 . . ?
C11 C31 H31 119.6 . . ?
C19 C33 C31 119.7(4) . . ?
C19 C33 H33 120.1 . . ?
C31 C33 H33 120.1 . . ?
C45 C34 C40 120.3(5) . . ?
C45 C34 H34 119.9 . . ?
C40 C34 H34 119.9 . . ?
C34 C40 C9 120.5(4) . . ?
C34 C40 H40 119.7 . . ?
C9 C40 H40 119.7 . . ?
C34 C45 C46 119.8(4) . . ?
C34 C45 H45 120.1 . . ?
C46 C45 H45 120.1 . . ?
C45 C46 C17 119.9(5) . . ?
C45 C46 H46 120.0 . . ?
C17 C46 H46 120.0 . . ?
F3 B13 F4 110.4(3) . 21_545 ?
F3 B13 F4 110.4(3) . 29_455 ?
F4 B13 F4 108.5(4) 21_545 29_455 ?
F3 B13 F4 110.4(3) . . ?
F4 B13 F4 108.5(4) 21_545 . ?
F4 B13 F4 108.5(4) 29_455 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 Ni1 P1 C9 -45.62(15) . . . . ?
P1 Ni1 P1 C9 88.65(16) 9 . . . ?
P1 Ni1 P1 C9 -179.90(15) 5 . . . ?
Cl2 Ni1 P1 C25 72.89(13) . . . . ?
P1 Ni1 P1 C25 -152.83(12) 9 . . . ?
P1 Ni1 P1 C25 -61.38(14) 5 . . . ?
Cl2 Ni1 P1 C15 -168.62(12) . . . . ?
P1 Ni1 P1 C15 -34.35(13) 9 . . . ?
P1 Ni1 P1 C15 57.10(13) 5 . . . ?
C25 P1 C9 C17 115.4(3) . . . . ?
C15 P1 C9 C17 -0.4(4) . . . . ?
Ni1 P1 C9 C17 -125.2(3) . . . . ?
C25 P1 C9 C40 -67.0(3) . . . . ?
C15 P1 C9 C40 177.1(3) . . . . ?
Ni1 P1 C9 C40 52.3(3) . . . . ?
C1 C7 C15 P1 -164.97(16) . . . . ?
C15 C7 C15 P1 78.7(3) 9 . . . ?
C15 C7 C15 P1 -48.7(4) 5 . . . ?
C9 P1 C15 C7 -153.2(2) . . . . ?
C25 P1 C15 C7 93.3(3) . . . . ?
Ni1 P1 C15 C7 -24.1(3) . . . . ?
C40 C9 C17 C46 -1.3(6) . . . . ?
P1 C9 C17 C46 176.2(3) . . . . ?
C25 C8 C19 C33 -0.6(6) . . . . ?
C31 C11 C25 C8 -0.2(5) . . . . ?
C31 C11 C25 P1 -179.2(3) . . . . ?
C19 C8 C25 C11 0.6(6) . . . . ?
C19 C8 C25 P1 179.5(3) . . . . ?
C9 P1 C25 C11 -90.8(3) . . . . ?
C15 P1 C25 C11 23.6(3) . . . . ?
Ni1 P1 C25 C11 143.1(3) . . . . ?
C9 P1 C25 C8 90.3(3) . . . . ?
C15 P1 C25 C8 -155.3(3) . . . . ?
Ni1 P1 C25 C8 -35.8(3) . . . . ?
C25 C11 C31 C33 0.0(6) . . . . ?
C8 C19 C33 C31 0.3(6) . . . . ?
C11 C31 C33 C19 0.0(7) . . . . ?
C45 C34 C40 C9 0.8(7) . . . . ?
C17 C9 C40 C34 0.4(6) . . . . ?
P1 C9 C40 C34 -177.3(4) . . . . ?
C40 C34 C45 C46 -1.2(8) . . . . ?
C34 C45 C46 C17 0.3(7) . . . . ?
C9 C17 C46 C45 1.0(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.055
####################################################################### 
# 
# 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_ap245c
_database_code_depnum_ccdc_archive 'CCDC 1486085'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_publcif_datablock.id            {d8ec3d61-3187-4d96-97fd-c1299d6ace31}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        TriphosNiBr
_chemical_name_common            TrophosNiBr
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H39 Br Ni P3 Si'
_chemical_formula_sum            'C40 H39 Br Ni P3 Si'
_chemical_formula_weight         779.33

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21
_symmetry_space_group_name_Hall  'P 2yb'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   10.2603(18)
_cell_length_b                   17.719(2)
_cell_length_c                   10.385(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 105.514(15)
_cell_angle_gamma                90.00
_cell_volume                     1819.1(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    170(2)
_cell_measurement_reflns_used    3614
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      27.8

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             802
_exptl_absorpt_coefficient_mu    1.824
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6696
_exptl_absorpt_correction_T_max  0.8275
_exptl_absorpt_process_details   
;
 [X-Red (Stoe & Cie, 2001) and X-Shape (Stoe & Cie, 1999)]
;



_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            9961
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0739
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.73
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5979
_reflns_number_gt                4848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'


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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0306P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.013(8)
_refine_ls_number_reflns         5979
_refine_ls_number_parameters     416
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0335
_refine_ls_wR_factor_ref         0.0692
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_restrained_S_all      0.882
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.45943(5) 0.23489(3) 0.60143(5) 0.01974(12) Uani 1 1 d . . .
P3 P 0.36191(9) 0.22713(7) 0.38083(11) 0.0217(2) Uani 1 1 d . . .
P4 P 0.29423(10) 0.28181(7) 0.68486(12) 0.0217(2) Uani 1 1 d . . .
Si5 Si 0.27926(11) 0.38802(7) 0.44437(13) 0.0231(3) Uani 1 1 d . . .
P6 P 0.57075(10) 0.34060(6) 0.58723(12) 0.0206(2) Uani 1 1 d . . .
C1 C 0.5149(4) 0.1180(3) 0.3014(5) 0.0371(12) Uani 1 1 d . . .
H1 H 0.5077 0.0933 0.3805 0.044 Uiso 1 1 calc R . .
C2 C 0.7039(4) 0.3689(3) 0.7364(5) 0.0232(10) Uani 1 1 d . . .
C3 C 0.1812(4) 0.1217(3) 0.4364(5) 0.0332(11) Uani 1 1 d . . .
H3 H 0.2455 0.1177 0.5210 0.040 Uiso 1 1 calc R . .
C4 C 0.1830(4) 0.3371(3) 0.5508(5) 0.0251(10) Uani 1 1 d . . .
H4A H 0.1337 0.3747 0.5906 0.030 Uiso 1 1 calc R . .
H4B H 0.1154 0.3032 0.4933 0.030 Uiso 1 1 calc R . .
C5 C 0.6684(4) 0.3437(3) 0.4621(5) 0.0245(10) Uani 1 1 d . . .
C6 C 0.6026(4) 0.1213(3) 0.1087(5) 0.0362(11) Uani 1 1 d . . .
H6 H 0.6539 0.0990 0.0549 0.043 Uiso 1 1 calc R . .
C7 C 0.4516(4) 0.4196(3) 0.5473(5) 0.0258(10) Uani 1 1 d . . .
H7A H 0.4873 0.4583 0.4971 0.031 Uiso 1 1 calc R . .
H7B H 0.4429 0.4428 0.6312 0.031 Uiso 1 1 calc R . .
C8 C 0.2036(4) 0.1713(3) 0.3379(5) 0.0250(10) Uani 1 1 d . . .
C9 C 0.1108(4) 0.1751(3) 0.2152(5) 0.0337(12) Uani 1 1 d . . .
H9 H 0.1270 0.2077 0.1484 0.040 Uiso 1 1 calc R . .
C10 C 0.7824(5) 0.4063(4) 0.3159(6) 0.0454(15) Uani 1 1 d . . .
H10 H 0.7998 0.4507 0.2719 0.055 Uiso 1 1 calc R . .
C13 C 0.3895(5) 0.4469(3) 1.0454(5) 0.0382(12) Uani 1 1 d . . .
H13 H 0.4101 0.4808 1.1189 0.046 Uiso 1 1 calc R . .
C15 C 0.7675(4) 0.3124(3) 0.8220(5) 0.0330(12) Uani 1 1 d . . .
H15 H 0.7421 0.2613 0.8019 0.040 Uiso 1 1 calc R . .
C16 C 0.3072(4) 0.3209(3) 0.3133(5) 0.0285(11) Uani 1 1 d . . .
H16A H 0.2220 0.3160 0.2414 0.034 Uiso 1 1 calc R . .
H16B H 0.3766 0.3423 0.2733 0.034 Uiso 1 1 calc R . .
C18 C 0.6953(4) 0.4097(3) 0.4010(5) 0.0338(12) Uani 1 1 d . . .
H18 H 0.6558 0.4563 0.4162 0.041 Uiso 1 1 calc R . .
C19 C 0.0369(5) 0.1048(3) 0.8332(5) 0.0368(13) Uani 1 1 d . . .
H19 H -0.0136 0.0684 0.8668 0.044 Uiso 1 1 calc R . .
C20 C 0.1849(4) 0.2132(2) 0.7384(5) 0.0249(11) Uani 1 1 d . . .
C21 C 0.8682(5) 0.3296(4) 0.9373(6) 0.0454(14) Uani 1 1 d . . .
H21 H 0.9113 0.2903 0.9954 0.054 Uiso 1 1 calc R . .
C22 C 0.4612(4) 0.3603(3) 0.9004(5) 0.0295(11) Uani 1 1 d . . .
H22 H 0.5320 0.3343 0.8761 0.035 Uiso 1 1 calc R . .
C23 C 0.5898(5) 0.0841(3) 0.2222(6) 0.0445(15) Uani 1 1 d . . .
H23 H 0.6312 0.0363 0.2459 0.053 Uiso 1 1 calc R . .
C25 C 0.4518(4) 0.1862(3) 0.2665(5) 0.0253(10) Uani 1 1 d . . .
C26 C -0.0288(5) 0.1612(3) 0.7502(6) 0.0392(13) Uani 1 1 d . . .
H26 H -0.1249 0.1627 0.7251 0.047 Uiso 1 1 calc R . .
C27 C -0.0070(4) 0.1318(3) 0.1872(6) 0.0393(13) Uani 1 1 d . . .
H27 H -0.0714 0.1350 0.1025 0.047 Uiso 1 1 calc R . .
C28 C 0.9054(5) 0.4033(4) 0.9673(6) 0.0515(17) Uani 1 1 d . . .
H28 H 0.9730 0.4154 1.0468 0.062 Uiso 1 1 calc R . .
C29 C 0.2563(5) 0.4348(3) 0.9749(6) 0.0385(13) Uani 1 1 d . . .
H29 H 0.1856 0.4600 1.0008 0.046 Uiso 1 1 calc R . .
C30 C 0.0641(5) 0.0791(3) 0.4075(6) 0.0421(14) Uani 1 1 d . . .
H30 H 0.0478 0.0461 0.4737 0.051 Uiso 1 1 calc R . .
C32 C 0.1762(5) 0.1009(3) 0.8680(6) 0.0389(13) Uani 1 1 d . . .
H32 H 0.2220 0.0620 0.9254 0.047 Uiso 1 1 calc R . .
C33 C 0.8432(5) 0.4596(4) 0.8804(6) 0.0468(15) Uani 1 1 d . . .
H33 H 0.8701 0.5106 0.8997 0.056 Uiso 1 1 calc R . .
C34 C 0.3289(4) 0.3488(3) 0.8273(5) 0.0231(10) Uani 1 1 d . . .
C36 C 0.7284(4) 0.2760(3) 0.4412(5) 0.0315(12) Uani 1 1 d . . .
H36 H 0.7109 0.2312 0.4839 0.038 Uiso 1 1 calc R . .
C38 C 0.0435(4) 0.2164(3) 0.7021(5) 0.0315(11) Uani 1 1 d . . .
H38 H -0.0027 0.2555 0.6455 0.038 Uiso 1 1 calc R . .
C39 C 0.2258(4) 0.3862(3) 0.8667(5) 0.0322(12) Uani 1 1 d . . .
H39 H 0.1341 0.3782 0.8188 0.039 Uiso 1 1 calc R . .
C41 C -0.0289(5) 0.0834(3) 0.2858(7) 0.0457(15) Uani 1 1 d . . .
H41 H -0.1085 0.0535 0.2681 0.055 Uiso 1 1 calc R . .
C42 C 0.8413(5) 0.3402(4) 0.2967(6) 0.0464(15) Uani 1 1 d . . .
H42 H 0.9015 0.3393 0.2413 0.056 Uiso 1 1 calc R . .
C43 C 0.8153(5) 0.2740(4) 0.3563(6) 0.0433(14) Uani 1 1 d . . .
H43 H 0.8553 0.2279 0.3402 0.052 Uiso 1 1 calc R . .
C44 C 0.4661(4) 0.2235(3) 0.1514(5) 0.0389(13) Uani 1 1 d . . .
H44 H 0.4247 0.2711 0.1263 0.047 Uiso 1 1 calc R . .
C46 C 0.2490(5) 0.1546(3) 0.8182(5) 0.0331(12) Uani 1 1 d . . .
H46 H 0.3448 0.1508 0.8395 0.040 Uiso 1 1 calc R . .
C47 C 0.7425(5) 0.4430(3) 0.7660(5) 0.0361(12) Uani 1 1 d . . .
H47 H 0.6999 0.4825 0.7079 0.043 Uiso 1 1 calc R . .
C50 C 0.4926(5) 0.4096(3) 1.0092(5) 0.0412(13) Uani 1 1 d . . .
H50 H 0.5841 0.4175 1.0579 0.049 Uiso 1 1 calc R . .
C53 C 0.5431(5) 0.1886(3) 0.0742(5) 0.0394(13) Uani 1 1 d . . .
H53 H 0.5531 0.2132 -0.0039 0.047 Uiso 1 1 calc R . .
C67 C 0.1807(5) 0.4715(3) 0.3657(6) 0.0375(13) Uani 1 1 d . . .
H67A H 0.0897 0.4556 0.3160 0.056 Uiso 1 1 calc R . .
H67B H 0.2260 0.4953 0.3043 0.056 Uiso 1 1 calc R . .
H67C H 0.1743 0.5076 0.4351 0.056 Uiso 1 1 calc R . .
Br1 Br 0.56331(5) 0.11888(3) 0.69635(6) 0.03776(14) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 P6 2.2193(12) . ?
Ni1 P3 2.2454(13) . ?
Ni1 P4 2.2584(12) . ?
Ni1 Br1 2.4022(8) . ?
P3 C16 1.832(5) . ?
P3 C25 1.836(4) . ?
P3 C8 1.851(4) . ?
P4 C4 1.830(5) . ?
P4 C20 1.838(4) . ?
P4 C34 1.855(5) . ?
Si5 C67 1.853(5) . ?
Si5 C16 1.886(5) . ?
Si5 C7 1.889(4) . ?
Si5 C4 1.896(4) . ?
P6 C7 1.831(4) . ?
P6 C2 1.840(5) . ?
P6 C5 1.841(4) . ?
C1 C25 1.374(7) . ?
C1 C23 1.402(7) . ?
C1 H1 0.9500 . ?
C2 C15 1.382(7) . ?
C2 C47 1.382(7) . ?
C3 C30 1.383(7) . ?
C3 C8 1.414(7) . ?
C3 H3 0.9500 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C36 1.391(7) . ?
C5 C18 1.394(7) . ?
C6 C53 1.344(8) . ?
C6 C23 1.386(8) . ?
C6 H6 0.9500 . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.373(7) . ?
C9 C27 1.396(7) . ?
C9 H9 0.9500 . ?
C10 C42 1.357(9) . ?
C10 C18 1.417(7) . ?
C10 H10 0.9500 . ?
C13 C50 1.382(7) . ?
C13 C29 1.384(7) . ?
C13 H13 0.9500 . ?
C15 C21 1.390(7) . ?
C15 H15 0.9500 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C18 H18 0.9500 . ?
C19 C26 1.373(8) . ?
C19 C32 1.379(7) . ?
C19 H19 0.9500 . ?
C20 C46 1.381(7) . ?
C20 C38 1.398(6) . ?
C21 C28 1.373(9) . ?
C21 H21 0.9500 . ?
C22 C34 1.382(6) . ?
C22 C50 1.396(7) . ?
C22 H22 0.9500 . ?
C23 H23 0.9500 . ?
C25 C44 1.407(7) . ?
C26 C38 1.398(7) . ?
C26 H26 0.9500 . ?
C27 C41 1.398(8) . ?
C27 H27 0.9500 . ?
C28 C33 1.382(9) . ?
C28 H28 0.9500 . ?
C29 C39 1.383(7) . ?
C29 H29 0.9500 . ?
C30 C41 1.367(8) . ?
C30 H30 0.9500 . ?
C32 C46 1.392(7) . ?
C32 H32 0.9500 . ?
C33 C47 1.381(8) . ?
C33 H33 0.9500 . ?
C34 C39 1.399(6) . ?
C36 C43 1.412(7) . ?
C36 H36 0.9500 . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C41 H41 0.9500 . ?
C42 C43 1.385(9) . ?
C42 H42 0.9500 . ?
C43 H43 0.9500 . ?
C44 C53 1.410(7) . ?
C44 H44 0.9500 . ?
C46 H46 0.9500 . ?
C47 H47 0.9500 . ?
C50 H50 0.9500 . ?
C53 H53 0.9500 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P6 Ni1 P3 94.63(5) . . ?
P6 Ni1 P4 99.63(5) . . ?
P3 Ni1 P4 103.80(5) . . ?
P6 Ni1 Br1 124.73(4) . . ?
P3 Ni1 Br1 113.21(4) . . ?
P4 Ni1 Br1 116.98(4) . . ?
C16 P3 C25 105.4(2) . . ?
C16 P3 C8 103.5(2) . . ?
C25 P3 C8 101.1(2) . . ?
C16 P3 Ni1 110.02(17) . . ?
C25 P3 Ni1 121.33(15) . . ?
C8 P3 Ni1 113.67(16) . . ?
C4 P4 C20 106.1(2) . . ?
C4 P4 C34 102.2(2) . . ?
C20 P4 C34 100.6(2) . . ?
C4 P4 Ni1 106.54(14) . . ?
C20 P4 Ni1 117.00(14) . . ?
C34 P4 Ni1 122.53(13) . . ?
C67 Si5 C16 110.8(2) . . ?
C67 Si5 C7 109.3(2) . . ?
C16 Si5 C7 107.1(2) . . ?
C67 Si5 C4 109.2(2) . . ?
C16 Si5 C4 108.9(2) . . ?
C7 Si5 C4 111.4(2) . . ?
C7 P6 C2 106.4(2) . . ?
C7 P6 C5 105.9(2) . . ?
C2 P6 C5 99.44(19) . . ?
C7 P6 Ni1 109.61(14) . . ?
C2 P6 Ni1 116.99(15) . . ?
C5 P6 Ni1 117.29(16) . . ?
C25 C1 C23 121.0(5) . . ?
C25 C1 H1 119.5 . . ?
C23 C1 H1 119.5 . . ?
C15 C2 C47 119.2(4) . . ?
C15 C2 P6 117.4(4) . . ?
C47 C2 P6 123.4(4) . . ?
C30 C3 C8 118.9(5) . . ?
C30 C3 H3 120.6 . . ?
C8 C3 H3 120.6 . . ?
P4 C4 Si5 112.5(2) . . ?
P4 C4 H4A 109.1 . . ?
Si5 C4 H4A 109.1 . . ?
P4 C4 H4B 109.1 . . ?
Si5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.8 . . ?
C36 C5 C18 120.2(4) . . ?
C36 C5 P6 115.6(4) . . ?
C18 C5 P6 123.9(4) . . ?
C53 C6 C23 120.6(5) . . ?
C53 C6 H6 119.7 . . ?
C23 C6 H6 119.7 . . ?
P6 C7 Si5 111.7(2) . . ?
P6 C7 H7A 109.3 . . ?
Si5 C7 H7A 109.3 . . ?
P6 C7 H7B 109.3 . . ?
Si5 C7 H7B 109.3 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 C3 119.7(4) . . ?
C9 C8 P3 122.9(4) . . ?
C3 C8 P3 117.4(4) . . ?
C8 C9 C27 120.9(5) . . ?
C8 C9 H9 119.6 . . ?
C27 C9 H9 119.6 . . ?
C42 C10 C18 120.6(5) . . ?
C42 C10 H10 119.7 . . ?
C18 C10 H10 119.7 . . ?
C50 C13 C29 120.1(5) . . ?
C50 C13 H13 120.0 . . ?
C29 C13 H13 120.0 . . ?
C2 C15 C21 120.6(5) . . ?
C2 C15 H15 119.7 . . ?
C21 C15 H15 119.7 . . ?
P3 C16 Si5 112.7(3) . . ?
P3 C16 H16A 109.1 . . ?
Si5 C16 H16A 109.1 . . ?
P3 C16 H16B 109.1 . . ?
Si5 C16 H16B 109.1 . . ?
H16A C16 H16B 107.8 . . ?
C5 C18 C10 118.9(5) . . ?
C5 C18 H18 120.6 . . ?
C10 C18 H18 120.6 . . ?
C26 C19 C32 120.1(4) . . ?
C26 C19 H19 119.9 . . ?
C32 C19 H19 119.9 . . ?
C46 C20 C38 119.1(4) . . ?
C46 C20 P4 116.6(3) . . ?
C38 C20 P4 124.4(4) . . ?
C28 C21 C15 120.1(6) . . ?
C28 C21 H21 119.9 . . ?
C15 C21 H21 119.9 . . ?
C34 C22 C50 121.1(4) . . ?
C34 C22 H22 119.4 . . ?
C50 C22 H22 119.4 . . ?
C6 C23 C1 119.2(5) . . ?
C6 C23 H23 120.4 . . ?
C1 C23 H23 120.4 . . ?
C1 C25 C44 119.2(4) . . ?
C1 C25 P3 117.4(4) . . ?
C44 C25 P3 123.3(4) . . ?
C19 C26 C38 121.0(4) . . ?
C19 C26 H26 119.5 . . ?
C38 C26 H26 119.5 . . ?
C9 C27 C41 119.0(5) . . ?
C9 C27 H27 120.5 . . ?
C41 C27 H27 120.5 . . ?
C21 C28 C33 119.2(5) . . ?
C21 C28 H28 120.4 . . ?
C33 C28 H28 120.4 . . ?
C39 C29 C13 120.2(5) . . ?
C39 C29 H29 119.9 . . ?
C13 C29 H29 119.9 . . ?
C41 C30 C3 121.4(5) . . ?
C41 C30 H30 119.3 . . ?
C3 C30 H30 119.3 . . ?
C19 C32 C46 119.4(5) . . ?
C19 C32 H32 120.3 . . ?
C46 C32 H32 120.3 . . ?
C47 C33 C28 121.1(6) . . ?
C47 C33 H33 119.5 . . ?
C28 C33 H33 119.5 . . ?
C22 C34 C39 118.5(4) . . ?
C22 C34 P4 118.9(3) . . ?
C39 C34 P4 122.5(3) . . ?
C5 C36 C43 119.9(5) . . ?
C5 C36 H36 120.1 . . ?
C43 C36 H36 120.1 . . ?
C26 C38 C20 119.1(5) . . ?
C26 C38 H38 120.4 . . ?
C20 C38 H38 120.4 . . ?
C29 C39 C34 120.5(4) . . ?
C29 C39 H39 119.7 . . ?
C34 C39 H39 119.7 . . ?
C30 C41 C27 120.2(5) . . ?
C30 C41 H41 119.9 . . ?
C27 C41 H41 119.9 . . ?
C10 C42 C43 121.3(4) . . ?
C10 C42 H42 119.4 . . ?
C43 C42 H42 119.4 . . ?
C42 C43 C36 119.2(5) . . ?
C42 C43 H43 120.4 . . ?
C36 C43 H43 120.4 . . ?
C25 C44 C53 118.6(5) . . ?
C25 C44 H44 120.7 . . ?
C53 C44 H44 120.7 . . ?
C20 C46 C32 121.3(4) . . ?
C20 C46 H46 119.4 . . ?
C32 C46 H46 119.4 . . ?
C33 C47 C2 119.9(5) . . ?
C33 C47 H47 120.1 . . ?
C2 C47 H47 120.1 . . ?
C13 C50 C22 119.5(5) . . ?
C13 C50 H50 120.3 . . ?
C22 C50 H50 120.3 . . ?
C6 C53 C44 121.4(5) . . ?
C6 C53 H53 119.3 . . ?
C44 C53 H53 119.3 . . ?
Si5 C67 H67A 109.5 . . ?
Si5 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
Si5 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P6 Ni1 P3 C16 -40.88(15) . . . . ?
P4 Ni1 P3 C16 60.23(15) . . . . ?
Br1 Ni1 P3 C16 -171.92(14) . . . . ?
P6 Ni1 P3 C25 82.71(18) . . . . ?
P4 Ni1 P3 C25 -176.18(18) . . . . ?
Br1 Ni1 P3 C25 -48.33(18) . . . . ?
P6 Ni1 P3 C8 -156.37(16) . . . . ?
P4 Ni1 P3 C8 -55.26(16) . . . . ?
Br1 Ni1 P3 C8 72.60(16) . . . . ?
P6 Ni1 P4 C4 70.02(16) . . . . ?
P3 Ni1 P4 C4 -27.21(16) . . . . ?
Br1 Ni1 P4 C4 -152.69(15) . . . . ?
P6 Ni1 P4 C20 -171.56(18) . . . . ?
P3 Ni1 P4 C20 91.21(18) . . . . ?
Br1 Ni1 P4 C20 -34.27(18) . . . . ?
P6 Ni1 P4 C34 -46.79(18) . . . . ?
P3 Ni1 P4 C34 -144.02(17) . . . . ?
Br1 Ni1 P4 C34 90.50(18) . . . . ?
P3 Ni1 P6 C7 71.37(17) . . . . ?
P4 Ni1 P6 C7 -33.49(17) . . . . ?
Br1 Ni1 P6 C7 -166.14(17) . . . . ?
P3 Ni1 P6 C2 -167.39(15) . . . . ?
P4 Ni1 P6 C2 87.75(15) . . . . ?
Br1 Ni1 P6 C2 -44.90(15) . . . . ?
P3 Ni1 P6 C5 -49.37(17) . . . . ?
P4 Ni1 P6 C5 -154.23(16) . . . . ?
Br1 Ni1 P6 C5 73.12(17) . . . . ?
C7 P6 C2 C15 150.5(3) . . . . ?
C5 P6 C2 C15 -99.7(4) . . . . ?
Ni1 P6 C2 C15 27.6(4) . . . . ?
C7 P6 C2 C47 -29.5(4) . . . . ?
C5 P6 C2 C47 80.3(4) . . . . ?
Ni1 P6 C2 C47 -152.4(3) . . . . ?
C20 P4 C4 Si5 -161.1(2) . . . . ?
C34 P4 C4 Si5 93.9(3) . . . . ?
Ni1 P4 C4 Si5 -35.8(3) . . . . ?
C67 Si5 C4 P4 -155.3(3) . . . . ?
C16 Si5 C4 P4 83.6(3) . . . . ?
C7 Si5 C4 P4 -34.4(3) . . . . ?
C7 P6 C5 C36 -157.5(3) . . . . ?
C2 P6 C5 C36 92.3(4) . . . . ?
Ni1 P6 C5 C36 -34.8(4) . . . . ?
C7 P6 C5 C18 29.4(5) . . . . ?
C2 P6 C5 C18 -80.9(4) . . . . ?
Ni1 P6 C5 C18 152.0(3) . . . . ?
C2 P6 C7 Si5 -157.6(2) . . . . ?
C5 P6 C7 Si5 97.2(3) . . . . ?
Ni1 P6 C7 Si5 -30.2(3) . . . . ?
C67 Si5 C7 P6 -163.3(2) . . . . ?
C16 Si5 C7 P6 -43.1(3) . . . . ?
C4 Si5 C7 P6 75.9(3) . . . . ?
C30 C3 C8 C9 -1.4(7) . . . . ?
C30 C3 C8 P3 -179.9(4) . . . . ?
C16 P3 C8 C9 43.6(4) . . . . ?
C25 P3 C8 C9 -65.5(4) . . . . ?
Ni1 P3 C8 C9 162.9(3) . . . . ?
C16 P3 C8 C3 -138.0(4) . . . . ?
C25 P3 C8 C3 113.0(4) . . . . ?
Ni1 P3 C8 C3 -18.7(4) . . . . ?
C3 C8 C9 C27 1.4(7) . . . . ?
P3 C8 C9 C27 179.8(4) . . . . ?
C47 C2 C15 C21 0.6(6) . . . . ?
P6 C2 C15 C21 -179.4(3) . . . . ?
C25 P3 C16 Si5 -156.0(2) . . . . ?
C8 P3 C16 Si5 98.2(3) . . . . ?
Ni1 P3 C16 Si5 -23.6(3) . . . . ?
C67 Si5 C16 P3 -164.3(2) . . . . ?
C7 Si5 C16 P3 76.5(3) . . . . ?
C4 Si5 C16 P3 -44.2(3) . . . . ?
C36 C5 C18 C10 1.1(7) . . . . ?
P6 C5 C18 C10 174.0(4) . . . . ?
C42 C10 C18 C5 -1.5(8) . . . . ?
C4 P4 C20 C46 166.4(4) . . . . ?
C34 P4 C20 C46 -87.5(4) . . . . ?
Ni1 P4 C20 C46 47.7(4) . . . . ?
C4 P4 C20 C38 -12.7(5) . . . . ?
C34 P4 C20 C38 93.5(4) . . . . ?
Ni1 P4 C20 C38 -131.3(4) . . . . ?
C2 C15 C21 C28 0.1(7) . . . . ?
C53 C6 C23 C1 -0.6(8) . . . . ?
C25 C1 C23 C6 1.6(8) . . . . ?
C23 C1 C25 C44 -1.8(8) . . . . ?
C23 C1 C25 P3 -177.7(4) . . . . ?
C16 P3 C25 C1 174.0(4) . . . . ?
C8 P3 C25 C1 -78.5(4) . . . . ?
Ni1 P3 C25 C1 48.3(4) . . . . ?
C16 P3 C25 C44 -1.7(5) . . . . ?
C8 P3 C25 C44 105.8(4) . . . . ?
Ni1 P3 C25 C44 -127.4(4) . . . . ?
C32 C19 C26 C38 -1.5(8) . . . . ?
C8 C9 C27 C41 -0.7(7) . . . . ?
C15 C21 C28 C33 -1.1(8) . . . . ?
C50 C13 C29 C39 -0.9(8) . . . . ?
C8 C3 C30 C41 0.8(8) . . . . ?
C26 C19 C32 C46 0.0(8) . . . . ?
C21 C28 C33 C47 1.5(8) . . . . ?
C50 C22 C34 C39 -1.6(7) . . . . ?
C50 C22 C34 P4 -179.4(4) . . . . ?
C4 P4 C34 C22 -130.6(4) . . . . ?
C20 P4 C34 C22 120.2(4) . . . . ?
Ni1 P4 C34 C22 -11.7(4) . . . . ?
C4 P4 C34 C39 51.6(4) . . . . ?
C20 P4 C34 C39 -57.6(4) . . . . ?
Ni1 P4 C34 C39 170.5(3) . . . . ?
C18 C5 C36 C43 -0.9(7) . . . . ?
P6 C5 C36 C43 -174.3(4) . . . . ?
C19 C26 C38 C20 0.7(8) . . . . ?
C46 C20 C38 C26 1.6(7) . . . . ?
P4 C20 C38 C26 -179.4(4) . . . . ?
C13 C29 C39 C34 0.0(8) . . . . ?
C22 C34 C39 C29 1.2(7) . . . . ?
P4 C34 C39 C29 179.0(4) . . . . ?
C3 C30 C41 C27 -0.2(8) . . . . ?
C9 C27 C41 C30 0.1(8) . . . . ?
C18 C10 C42 C43 1.8(8) . . . . ?
C10 C42 C43 C36 -1.6(8) . . . . ?
C5 C36 C43 C42 1.1(8) . . . . ?
C1 C25 C44 C53 1.1(8) . . . . ?
P3 C25 C44 C53 176.8(4) . . . . ?
C38 C20 C46 C32 -3.1(8) . . . . ?
P4 C20 C46 C32 177.8(4) . . . . ?
C19 C32 C46 C20 2.3(8) . . . . ?
C28 C33 C47 C2 -0.8(7) . . . . ?
C15 C2 C47 C33 -0.2(6) . . . . ?
P6 C2 C47 C33 179.8(4) . . . . ?
C29 C13 C50 C22 0.5(8) . . . . ?
C34 C22 C50 C13 0.7(8) . . . . ?
C23 C6 C53 C44 0.0(9) . . . . ?
C25 C44 C53 C6 -0.2(8) . . . . ?

_diffrn_measured_fraction_theta_max 0.978
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.978
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.059
####################################################################### 
# 
# 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_ap270
_database_code_depnum_ccdc_archive 'CCDC 1486086'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_publcif_datablock.id            {a51d96d5-b804-42f1-84a0-7c596061e3ee}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H47 Ni O6 P5, 2(B F4)'
_chemical_formula_sum            'C15 H47 B2 F8 Ni O6 P5'
_chemical_formula_weight         710.69

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'
'x+1/2, -y+1/2, z'

_cell_length_a                   21.1905(6)
_cell_length_b                   13.5221(4)
_cell_length_c                   11.3801(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3260.85(16)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    19053
_cell_measurement_theta_min      3.1660
_cell_measurement_theta_max      34.2990
_cell_measurement_temperature    170(2)

_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    0.913
_exptl_absorpt_correction_T_min  0.86849
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_diffrn_ambient_temperature      170(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Sapphire2-CCD, Oxford Diffraction'
_diffrn_measurement_method       '288 images at 1.0 deg. in ω and 40 sec.'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            44950
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         25.00
_reflns_number_total             5730
_reflns_number_gt                5359
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'CrysAlis CCD 171_33_34d, Oxford Diffraction'
_computing_cell_refinement       'CrysAlis RED 171_33_34d, Oxford Diffraction'
_computing_data_reduction        'CrysAlis RED 171_33_34d, Oxford Diffraction'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0914P)²+3.5196P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.118(18)
_refine_ls_number_reflns         5730
_refine_ls_number_parameters     313
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1398
_refine_ls_wR_factor_gt          0.1347
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.16519(2) -0.23731(3) -0.0417(3) 0.02218(14) Uani 1 1 d . B .
P0AA P -0.04570(6) -0.30922(9) 0.1174(3) 0.0303(3) Uani 1 1 d . . .
P3 P -0.08338(6) -0.27907(11) -0.2801(3) 0.0376(3) Uani 1 1 d . . .
P4 P -0.24441(6) -0.19151(10) 0.2010(3) 0.0349(3) Uani 1 1 d . . .
O10 O -0.07982(15) -0.2957(3) 0.0031(4) 0.0330(7) Uani 1 1 d . . .
O11 O -0.25299(15) -0.1888(3) -0.0867(4) 0.0328(8) Uani 1 1 d . . .
O12 O -0.18726(18) -0.2181(4) 0.1331(4) 0.0517(11) Uani 1 1 d . . .
O14 O -0.14364(19) -0.2554(3) -0.2160(4) 0.0490(10) Uani 1 1 d . . .
C6 C 0.0308(2) -0.3589(5) 0.0892(6) 0.0451(13) Uani 1 1 d . . .
H6A H 0.0267 -0.4204 0.0476 0.068 Uiso 1 1 calc R . .
H6B H 0.0522 -0.3702 0.1624 0.068 Uiso 1 1 calc R . .
H6C H 0.0546 -0.3131 0.0426 0.068 Uiso 1 1 calc R . .
C3AA C -0.0837(2) -0.3945(4) 0.2140(6) 0.0439(12) Uani 1 1 d . . .
H3AA H -0.1254 -0.3710 0.2321 0.066 Uiso 1 1 calc R . .
H3AB H -0.0597 -0.4004 0.2852 0.066 Uiso 1 1 calc R . .
H3AC H -0.0866 -0.4580 0.1766 0.066 Uiso 1 1 calc R . .
C9 C -0.0536(3) -0.3982(5) -0.2480(6) 0.0513(14) Uani 1 1 d . . .
H9A H -0.0443 -0.4027 -0.1656 0.077 Uiso 1 1 calc R . .
H9B H -0.0158 -0.4095 -0.2925 0.077 Uiso 1 1 calc R . .
H9C H -0.0846 -0.4471 -0.2684 0.077 Uiso 1 1 calc R . .
C10 C -0.3095(3) -0.2721(6) 0.1731(7) 0.0574(17) Uani 1 1 d . . .
H10A H -0.3217 -0.2667 0.0921 0.086 Uiso 1 1 calc R . .
H10B H -0.3444 -0.2538 0.2223 0.086 Uiso 1 1 calc R . .
H10C H -0.2973 -0.3390 0.1898 0.086 Uiso 1 1 calc R . .
C12 C -0.2527(3) -0.0871(6) -0.2982(8) 0.068(2) Uani 1 1 d . . .
H12A H -0.2577 -0.0229 -0.2632 0.102 Uiso 1 1 calc R . .
H12B H -0.2740 -0.0886 -0.3726 0.102 Uiso 1 1 calc R . .
H12C H -0.2087 -0.1006 -0.3095 0.102 Uiso 1 1 calc R . .
C13 C -0.2891(3) -0.2916(5) -0.2836(7) 0.0572(16) Uani 1 1 d . . .
H13A H -0.2470 -0.3143 -0.2987 0.086 Uiso 1 1 calc R . .
H13B H -0.3105 -0.2806 -0.3568 0.086 Uiso 1 1 calc R . .
H13C H -0.3115 -0.3406 -0.2390 0.086 Uiso 1 1 calc R . .
C1AA C -0.0334(3) -0.1978(5) 0.1972(7) 0.0529(15) Uani 1 1 d . . .
H1AA H -0.0125 -0.1505 0.1478 0.079 Uiso 1 1 calc R . .
H1AB H -0.0077 -0.2112 0.2648 0.079 Uiso 1 1 calc R . .
H1AC H -0.0733 -0.1717 0.2221 0.079 Uiso 1 1 calc R . .
C2AA C -0.3669(2) -0.1463(6) -0.1794(6) 0.0515(15) Uani 1 1 d . . .
H2AA H -0.3883 -0.1996 -0.1405 0.077 Uiso 1 1 calc R . .
H2AB H -0.3868 -0.1336 -0.2536 0.077 Uiso 1 1 calc R . .
H2AC H -0.3690 -0.0880 -0.1314 0.077 Uiso 1 1 calc R . .
C18 C -0.2739(4) -0.0716(6) 0.1740(8) 0.076(2) Uani 1 1 d . . .
H18A H -0.2430 -0.0235 0.1974 0.114 Uiso 1 1 calc R . .
H18B H -0.3119 -0.0618 0.2183 0.114 Uiso 1 1 calc R . .
H18C H -0.2827 -0.0643 0.0917 0.114 Uiso 1 1 calc R . .
C19 C -0.2284(3) -0.1974(6) 0.3549(6) 0.0589(17) Uani 1 1 d . . .
H19A H -0.2221 -0.2651 0.3776 0.088 Uiso 1 1 calc R . .
H19B H -0.2635 -0.1705 0.3977 0.088 Uiso 1 1 calc R . .
H19C H -0.1911 -0.1599 0.3721 0.088 Uiso 1 1 calc R . .
C20 C -0.0219(3) -0.1952(6) -0.2520(7) 0.0619(18) Uani 1 1 d . . .
H20A H -0.0314 -0.1329 -0.2884 0.093 Uiso 1 1 calc R . .
H20B H 0.0168 -0.2207 -0.2836 0.093 Uiso 1 1 calc R . .
H20C H -0.0176 -0.1861 -0.1688 0.093 Uiso 1 1 calc R . .
B5 B -0.0867(2) -0.6278(4) -0.0382(6) 0.0308(10) Uani 1 1 d . . .
F6 F -0.13338(19) -0.5616(3) -0.0344(8) 0.117(2) Uani 1 1 d . . .
F9 F -0.0321(3) -0.5806(4) -0.0184(10) 0.169(4) Uani 1 1 d . . .
F0AA F -0.0962(5) -0.7029(5) 0.0340(8) 0.183(5) Uani 1 1 d . . .
F11 F -0.0805(4) -0.6636(7) -0.1432(6) 0.170(4) Uani 1 1 d . . .
C0AA C -0.0967(4) -0.2748(8) -0.4353(6) 0.078(3) Uani 1 1 d . . .
H0AA H -0.1290 -0.3213 -0.4560 0.117 Uiso 1 1 calc R . .
H0AB H -0.0584 -0.2913 -0.4758 0.117 Uiso 1 1 calc R . .
H0AC H -0.1098 -0.2094 -0.4573 0.117 Uiso 1 1 calc R . .
F4 F -0.4101(2) -0.3713(3) -0.0399(7) 0.0983(15) Uani 1 1 d . . .
F5 F -0.32106(17) -0.4573(4) -0.0374(7) 0.1016(16) Uani 1 1 d . . .
B9 B -0.3841(3) -0.4618(5) -0.0319(9) 0.0558(17) Uani 1 1 d . . .
F10 F -0.3997(5) -0.4975(9) 0.0728(10) 0.204(5) Uani 1 1 d . . .
F13 F -0.4068(3) -0.5210(7) -0.1121(12) 0.208(5) Uani 1 1 d . . .
P1 P -0.28619(5) -0.17923(9) -0.2028(3) 0.0307(3) Uani 1 1 d . . .
O3 O -0.19972(16) -0.3821(2) -0.0341(6) 0.0605(12) Uani 1 1 d . . .
H3A H -0.1775 -0.4279 -0.0802 0.091 Uiso 1 1 d R . .
H3B H -0.2417 -0.3883 -0.0591 0.091 Uiso 1 1 d R . .
O5 O -0.1264(2) -0.0977(3) -0.0485(7) 0.0718(13) Uani 1 1 d . . .
C8 C -0.1886 0.0667 -0.0563 0.117 Uani 1 1 d . . .
H8A H -0.2225 0.0242 -0.0803 0.175 Uiso 1 1 calc R A 1
H8B H -0.1838 0.1193 -0.1122 0.175 Uiso 1 1 calc R A 1
H8C H -0.1978 0.0940 0.0196 0.175 Uiso 1 1 calc R A 1
P2A P -0.1091 -0.0108 -0.0478 0.076 Uani 0.412(6) 1 d P B 1
C14A C -0.0966 0.0326 0.1174 0.117 Uani 0.412(6) 1 d P B 1
H14A H -0.1332 0.0156 0.1630 0.175 Uiso 0.412(6) 1 calc PR B 1
H14B H -0.0904 0.1029 0.1195 0.175 Uiso 0.412(6) 1 calc PR B 1
H14C H -0.0602 0.0001 0.1496 0.175 Uiso 0.412(6) 1 calc PR B 1
C17A C -0.0638 0.0696 -0.0766 0.117 Uani 0.412(6) 1 d P B 1
H17A H -0.0237 0.0413 -0.0967 0.175 Uiso 0.412(6) 1 calc PR B 1
H17B H -0.0589 0.1122 -0.0097 0.175 Uiso 0.412(6) 1 calc PR B 1
H17C H -0.0795 0.1072 -0.1419 0.175 Uiso 0.412(6) 1 calc PR B 1
P2B P -0.1180 0.0068 -0.0432 0.076 Uani 0.588(6) 1 d P B 2
C14B C -0.0637 0.0576 0.0485 0.117 Uani 0.588(6) 1 d P B 2
H14D H -0.0840 0.0779 0.1200 0.175 Uiso 0.588(6) 1 calc PR B 2
H14E H -0.0448 0.1140 0.0113 0.175 Uiso 0.588(6) 1 calc PR B 2
H14F H -0.0317 0.0097 0.0660 0.175 Uiso 0.588(6) 1 calc PR B 2
C17B C -0.0716 0.0498 -0.1573 0.117 Uani 0.588(6) 1 d P B 2
H17D H -0.0331 0.0765 -0.1262 0.175 Uiso 0.588(6) 1 calc PR B 2
H17E H -0.0939 0.1006 -0.1992 0.175 Uiso 0.588(6) 1 calc PR B 2
H17F H -0.0621 -0.0037 -0.2098 0.175 Uiso 0.588(6) 1 calc PR B 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 O10 2.038(3) . ?
Ni1 O11 2.038(3) . ?
Ni1 O14 2.051(4) . ?
Ni1 O12 2.059(4) . ?
Ni1 O5 2.060(4) . ?
Ni1 O3 2.092(3) . ?
P0AA O10 1.500(3) . ?
P0AA C1AA 1.778(6) . ?
P0AA C6 1.784(5) . ?
P0AA C3AA 1.785(5) . ?
P3 O14 1.505(4) . ?
P3 C20 1.757(7) . ?
P3 C9 1.768(6) . ?
P3 C0AA 1.789(7) . ?
P4 O12 1.481(4) . ?
P4 C18 1.764(8) . ?
P4 C19 1.785(6) . ?
P4 C10 1.786(7) . ?
O11 P1 1.502(3) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C3AA H3AA 0.9600 . ?
C3AA H3AB 0.9600 . ?
C3AA H3AC 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C12 P1 1.798(6) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 P1 1.778(6) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C1AA H1AA 0.9600 . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?
C2AA P1 1.788(5) . ?
C2AA H2AA 0.9600 . ?
C2AA H2AB 0.9600 . ?
C2AA H2AC 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
B5 F11 1.296(8) . ?
B5 F0AA 1.322(8) . ?
B5 F6 1.335(6) . ?
B5 F9 1.340(7) . ?
C0AA H0AA 0.9600 . ?
C0AA H0AB 0.9600 . ?
C0AA H0AC 0.9600 . ?
F4 B9 1.345(8) . ?
F5 B9 1.340(7) . ?
B9 F13 1.305(11) . ?
B9 F10 1.327(12) . ?
O3 H3A 0.9384 . ?
O3 H3B 0.9374 . ?
O5 P2A 1.232(4) . ?
O5 P2B 1.426(4) . ?
C8 P2B 1.7065 . ?
C8 P2A 1.9852 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
P2A C17A 1.4871 . ?
P2A C14A 1.9877 . ?
C14A H14A 0.9600 . ?
C14A H14B 0.9600 . ?
C14A H14C 0.9600 . ?
C17A H17A 0.9600 . ?
C17A H17B 0.9600 . ?
C17A H17C 0.9600 . ?
P2B C14B 1.6994 . ?
P2B C17B 1.7300 . ?
C14B H14D 0.9600 . ?
C14B H14E 0.9600 . ?
C14B H14F 0.9600 . ?
C17B H17D 0.9600 . ?
C17B H17E 0.9600 . ?
C17B H17F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O10 Ni1 O11 175.99(15) . . ?
O10 Ni1 O14 89.88(14) . . ?
O11 Ni1 O14 89.89(14) . . ?
O10 Ni1 O12 90.52(14) . . ?
O11 Ni1 O12 89.72(14) . . ?
O14 Ni1 O12 179.53(19) . . ?
O10 Ni1 O5 90.59(17) . . ?
O11 Ni1 O5 93.41(17) . . ?
O14 Ni1 O5 89.1(2) . . ?
O12 Ni1 O5 90.7(2) . . ?
O10 Ni1 O3 86.44(15) . . ?
O11 Ni1 O3 89.56(14) . . ?
O14 Ni1 O3 90.3(2) . . ?
O12 Ni1 O3 89.9(2) . . ?
O5 Ni1 O3 176.98(16) . . ?
O10 P0AA C1AA 114.2(3) . . ?
O10 P0AA C6 109.2(2) . . ?
C1AA P0AA C6 106.1(3) . . ?
O10 P0AA C3AA 113.3(2) . . ?
C1AA P0AA C3AA 107.4(3) . . ?
C6 P0AA C3AA 106.1(3) . . ?
O14 P3 C20 113.8(3) . . ?
O14 P3 C9 113.3(3) . . ?
C20 P3 C9 106.6(3) . . ?
O14 P3 C0AA 109.7(3) . . ?
C20 P3 C0AA 106.0(4) . . ?
C9 P3 C0AA 106.8(4) . . ?
O12 P4 C18 114.9(4) . . ?
O12 P4 C19 110.2(3) . . ?
C18 P4 C19 106.2(4) . . ?
O12 P4 C10 112.9(3) . . ?
C18 P4 C10 104.9(4) . . ?
C19 P4 C10 107.1(3) . . ?
P0AA O10 Ni1 133.8(2) . . ?
P1 O11 Ni1 132.6(2) . . ?
P4 O12 Ni1 136.1(2) . . ?
P3 O14 Ni1 133.1(2) . . ?
P0AA C6 H6A 109.5 . . ?
P0AA C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
P0AA C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
P0AA C3AA H3AA 109.5 . . ?
P0AA C3AA H3AB 109.5 . . ?
H3AA C3AA H3AB 109.5 . . ?
P0AA C3AA H3AC 109.5 . . ?
H3AA C3AA H3AC 109.5 . . ?
H3AB C3AA H3AC 109.5 . . ?
P3 C9 H9A 109.5 . . ?
P3 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
P3 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
P4 C10 H10A 109.5 . . ?
P4 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
P4 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
P1 C12 H12A 109.5 . . ?
P1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
P1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
P1 C13 H13A 109.5 . . ?
P1 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
P1 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
P0AA C1AA H1AA 109.5 . . ?
P0AA C1AA H1AB 109.5 . . ?
H1AA C1AA H1AB 109.5 . . ?
P0AA C1AA H1AC 109.5 . . ?
H1AA C1AA H1AC 109.5 . . ?
H1AB C1AA H1AC 109.5 . . ?
P1 C2AA H2AA 109.5 . . ?
P1 C2AA H2AB 109.5 . . ?
H2AA C2AA H2AB 109.5 . . ?
P1 C2AA H2AC 109.5 . . ?
H2AA C2AA H2AC 109.5 . . ?
H2AB C2AA H2AC 109.5 . . ?
P4 C18 H18A 109.5 . . ?
P4 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P4 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P4 C19 H19A 109.5 . . ?
P4 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P4 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P3 C20 H20A 109.5 . . ?
P3 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P3 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
F11 B5 F0AA 107.5(7) . . ?
F11 B5 F6 110.8(7) . . ?
F0AA B5 F6 112.4(6) . . ?
F11 B5 F9 104.3(8) . . ?
F0AA B5 F9 113.2(8) . . ?
F6 B5 F9 108.4(5) . . ?
P3 C0AA H0AA 109.5 . . ?
P3 C0AA H0AB 109.5 . . ?
H0AA C0AA H0AB 109.5 . . ?
P3 C0AA H0AC 109.5 . . ?
H0AA C0AA H0AC 109.5 . . ?
H0AB C0AA H0AC 109.5 . . ?
F13 B9 F10 108.3(9) . . ?
F13 B9 F5 111.3(8) . . ?
F10 B9 F5 107.9(8) . . ?
F13 B9 F4 111.1(8) . . ?
F10 B9 F4 106.8(9) . . ?
F5 B9 F4 111.3(5) . . ?
O11 P1 C13 113.4(3) . . ?
O11 P1 C2AA 109.8(2) . . ?
C13 P1 C2AA 104.9(3) . . ?
O11 P1 C12 113.9(3) . . ?
C13 P1 C12 107.1(4) . . ?
C2AA P1 C12 107.1(3) . . ?
Ni1 O3 H3A 114.7 . . ?
Ni1 O3 H3B 113.7 . . ?
H3A O3 H3B 104.4 . . ?
P2A O5 P2B 10.36(4) . . ?
P2A O5 Ni1 173.3(4) . . ?
P2B O5 Ni1 163.0(3) . . ?
P2B C8 P2A 4.1 . . ?
P2B C8 H8A 113.4 . . ?
P2A C8 H8A 109.5 . . ?
P2B C8 H8B 108.5 . . ?
P2A C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
P2B C8 H8C 106.5 . . ?
P2A C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O5 P2A C17A 152.7(2) . . ?
O5 P2A C8 104.5(2) . . ?
C17A P2A C8 98.726(2) . . ?
O5 P2A C14A 109.1(4) . . ?
C17A P2A C14A 84.628(1) . . ?
C8 P2A C14A 90.190(1) . . ?
P2A C14A H14A 109.5 . . ?
P2A C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
P2A C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
P2A C17A H17A 109.5 . . ?
P2A C17A H17B 109.5 . . ?
H17A C17A H17B 109.5 . . ?
P2A C17A H17C 109.5 . . ?
H17A C17A H17C 109.5 . . ?
H17B C17A H17C 109.5 . . ?
O5 P2B C14B 120.8(3) . . ?
O5 P2B C8 110.95(18) . . ?
C14B P2B C8 117.048(2) . . ?
O5 P2B C17B 111.9(3) . . ?
C14B P2B C17B 86.526(2) . . ?
C8 P2B C17B 105.849(1) . . ?
P2B C14B H14D 109.5 . . ?
P2B C14B H14E 109.5 . . ?
H14D C14B H14E 109.5 . . ?
P2B C14B H14F 109.5 . . ?
H14D C14B H14F 109.5 . . ?
H14E C14B H14F 109.5 . . ?
P2B C17B H17D 109.5 . . ?
P2B C17B H17E 109.5 . . ?
H17D C17B H17E 109.5 . . ?
P2B C17B H17F 109.5 . . ?
H17D C17B H17F 109.5 . . ?
H17E C17B H17F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1AA P0AA O10 Ni1 -57.5(4) . . . . ?
C6 P0AA O10 Ni1 -176.1(3) . . . . ?
C3AA P0AA O10 Ni1 65.9(4) . . . . ?
O11 Ni1 O10 P0AA -98(2) . . . . ?
O14 Ni1 O10 P0AA 174.7(3) . . . . ?
O12 Ni1 O10 P0AA -5.0(3) . . . . ?
O5 Ni1 O10 P0AA 85.7(4) . . . . ?
O3 Ni1 O10 P0AA -94.9(4) . . . . ?
O10 Ni1 O11 P1 -83(2) . . . . ?
O14 Ni1 O11 P1 3.6(3) . . . . ?
O12 Ni1 O11 P1 -176.7(3) . . . . ?
O5 Ni1 O11 P1 92.7(3) . . . . ?
O3 Ni1 O11 P1 -86.7(3) . . . . ?
C18 P4 O12 Ni1 -64.0(6) . . . . ?
C19 P4 O12 Ni1 176.0(4) . . . . ?
C10 P4 O12 Ni1 56.3(5) . . . . ?
O10 Ni1 O12 P4 -169.9(4) . . . . ?
O11 Ni1 O12 P4 6.1(4) . . . . ?
O14 Ni1 O12 P4 42(27) . . . . ?
O5 Ni1 O12 P4 99.5(5) . . . . ?
O3 Ni1 O12 P4 -83.5(4) . . . . ?
C20 P3 O14 Ni1 -57.0(5) . . . . ?
C9 P3 O14 Ni1 65.1(5) . . . . ?
C0AA P3 O14 Ni1 -175.6(5) . . . . ?
O10 Ni1 O14 P3 -12.5(4) . . . . ?
O11 Ni1 O14 P3 171.5(4) . . . . ?
O12 Ni1 O14 P3 135(27) . . . . ?
O5 Ni1 O14 P3 78.1(4) . . . . ?
O3 Ni1 O14 P3 -98.9(4) . . . . ?
Ni1 O11 P1 C13 55.6(4) . . . . ?
Ni1 O11 P1 C2AA 172.5(3) . . . . ?
Ni1 O11 P1 C12 -67.3(4) . . . . ?
O10 Ni1 O5 P2A -143(5) . . . . ?
O11 Ni1 O5 P2A 37(5) . . . . ?
O14 Ni1 O5 P2A 127(5) . . . . ?
O12 Ni1 O5 P2A -53(5) . . . . ?
O3 Ni1 O5 P2A -154(4) . . . . ?
O10 Ni1 O5 P2B -149.9(16) . . . . ?
O11 Ni1 O5 P2B 30.3(17) . . . . ?
O14 Ni1 O5 P2B 120.2(17) . . . . ?
O12 Ni1 O5 P2B -59.4(16) . . . . ?
O3 Ni1 O5 P2B -161(4) . . . . ?
P2B O5 P2A C17A -162.1(9) . . . . ?
Ni1 O5 P2A C17A -173(4) . . . . ?
P2B O5 P2A C8 -14.53(15) . . . . ?
Ni1 O5 P2A C8 -25(5) . . . . ?
P2B O5 P2A C14A 80.8(2) . . . . ?
Ni1 O5 P2A C14A 70(5) . . . . ?
P2B C8 P2A O5 148.0(4) . . . . ?
P2B C8 P2A C17A -46.397(2) . . . . ?
P2B C8 P2A C14A 38.2 . . . . ?
P2A O5 P2B C14B -55.0(4) . . . . ?
Ni1 O5 P2B C14B 120.8(15) . . . . ?
P2A O5 P2B C8 162.39(18) . . . . ?
Ni1 O5 P2B C8 -21.8(17) . . . . ?
P2A O5 P2B C17B 44.4(4) . . . . ?
Ni1 O5 P2B C17B -139.8(15) . . . . ?
P2A C8 P2B O5 -28.3(3) . . . . ?
P2A C8 P2B C14B -172.503(1) . . . . ?
P2A C8 P2B C17B 93.239(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.717
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.105
####################################################################### 
# 
# 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_upa-pg-10sq
_database_code_depnum_ccdc_archive 'CCDC 1486087'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
# SQUEEZE RESULTS (APPEND TO CIF)
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
1 0.155 0.000 0.000 15.0 3.6
2 0.345 0.000 0.000 15.0 3.6
3 0.655 0.000 0.000 15.0 3.6
4 0.845 0.000 0.000 15.0 3.6
5 0.000 0.000 0.155 15.0 3.7
6 0.500 0.000 0.155 15.0 3.7
7 0.000 0.000 0.345 15.0 3.6
8 0.500 0.000 0.345 15.0 3.5
9 0.155 0.000 0.500 15.0 3.6
10 0.845 0.000 0.500 14.9 3.6
11 0.345 0.000 0.500 15.0 3.6
12 0.655 0.000 0.500 15.0 3.6
13 0.000 0.000 0.655 15.0 3.7
14 0.500 0.000 0.655 15.0 3.7
15 0.000 0.000 0.845 15.0 3.5
16 0.500 0.000 0.845 15.0 3.6
17 0.250 0.250 0.250 789.9 122.4
18 0.750 0.250 0.250 790.0 122.7
19 0.750 0.250 0.750 789.9 122.4
20 0.250 0.250 0.750 790.0 122.7
21 0.000 0.155 0.000 15.0 3.6
22 0.500 0.155 0.000 15.0 3.6
23 0.000 0.155 0.500 15.0 3.6
24 0.500 0.155 0.500 15.0 3.6
25 0.000 0.345 0.000 15.0 3.6
26 0.500 0.345 0.000 15.0 3.6
27 0.000 0.345 0.500 15.0 3.6
28 0.500 0.345 0.500 15.0 3.6
29 0.345 0.500 0.000 15.0 3.6
30 0.655 0.500 0.000 15.0 3.6
31 0.000 0.500 0.155 15.0 3.7
32 0.500 0.500 0.345 15.0 3.6
33 0.155 0.500 0.500 15.0 3.6
34 0.845 0.500 0.500 15.0 3.6
35 0.500 0.500 0.655 15.0 3.7
36 0.000 0.500 0.845 15.0 3.6
37 0.155 0.500 0.000 15.0 3.6
38 0.845 0.500 0.000 14.9 3.6
39 0.500 0.500 0.155 15.0 3.7
40 0.000 0.500 0.345 14.9 3.5
41 0.345 0.500 0.500 14.9 3.6
42 0.655 0.500 0.500 15.0 3.6
43 0.000 0.500 0.655 15.0 3.7
44 0.500 0.500 0.845 14.9 3.5
45 0.750 0.750 0.250 789.9 122.4
46 0.250 0.750 0.250 790.0 122.7
47 0.250 0.750 0.750 789.9 122.4
48 0.750 0.750 0.750 790.0 122.7
49 0.000 0.655 0.000 15.0 3.6
50 0.500 0.655 0.000 15.0 3.6
51 0.000 0.655 0.500 15.0 3.6
52 0.500 0.655 0.500 15.0 3.6
53 0.000 0.845 0.000 15.0 3.6
54 0.500 0.845 0.000 15.0 3.6
55 0.000 0.845 0.500 15.0 3.6
56 0.500 0.845 0.500 15.0 3.6
_platon_squeeze_details          
;
;
_publcif_datablock.id            {266aba0d-b8ef-409a-8a21-3aa5df2916a9}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        'TriphosNiCl ClO4'

_chemical_name_common            'TriphosNiCl ClO4'
_chemical_melting_point          ?
_chemical_formula_moiety         'C40 H38.97 Cl Ni P3 Si, Cl O4 '
_chemical_formula_sum            'C40 H39 Cl2 Ni O4 P3 Si'
_chemical_formula_weight         834.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   'F -4 3 c'
_symmetry_space_group_name_Hall  'F -4c 2 3'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'y, -x, -z+1/2'
'-x, -y, z'
'-y, x, -z+1/2'
'x, -y, -z'
'-y, -x, z+1/2'
'-x, y, -z'
'y, x, z+1/2'
'z, x, y'
'x, -z, -y+1/2'
'-z, -x, y'
'-x, z, -y+1/2'
'z, -x, -y'
'-x, -z, y+1/2'
'-z, x, -y'
'x, z, y+1/2'
'y, z, x'
'z+1/2, y, x'
'z+1/2, -y, -x'
'-z+1/2, -y, x'
'-z+1/2, y, -x'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'x, y+1/2, z+1/2'
'y, -x+1/2, -z+1'
'-x, -y+1/2, z+1/2'
'-y, x+1/2, -z+1'
'x, -y+1/2, -z+1/2'
'-y, -x+1/2, z+1'
'-x, y+1/2, -z+1/2'
'y, x+1/2, z+1'
'z, x+1/2, y+1/2'
'x, -z+1/2, -y+1'
'-z, -x+1/2, y+1/2'
'-x, z+1/2, -y+1'
'z, -x+1/2, -y+1/2'
'-x, -z+1/2, y+1'
'-z, x+1/2, -y+1/2'
'x, z+1/2, y+1'
'y, z+1/2, x+1/2'
'z+1/2, y+1/2, x+1/2'
'z+1/2, -y+1/2, -x+1/2'
'-z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, -x+1/2'
'y, -z+1, -x+1'
'-y, -z+1, x+1'
'-y, z+1, -x+1'
'x+1/2, y, z+1/2'
'y+1/2, -x, -z+1'
'-x+1/2, -y, z+1/2'
'-y+1/2, x, -z+1'
'x+1/2, -y, -z+1/2'
'-y+1/2, -x, z+1'
'-x+1/2, y, -z+1/2'
'y+1/2, x, z+1'
'z+1/2, x, y+1/2'
'x+1/2, -z, -y+1'
'-z+1/2, -x, y+1/2'
'-x+1/2, z, -y+1'
'z+1/2, -x, -y+1/2'
'-x+1/2, -z, y+1'
'-z+1/2, x, -y+1/2'
'x+1/2, z, y+1'
'y+1/2, z, x+1/2'
'z+1, y, x+1/2'
'z+1, -y, -x+1/2'
'-z+1, -y, x+1/2'
'-z+1, y, -x+1/2'
'y+1/2, -z+1/2, -x+1'
'-y+1/2, -z+1/2, x+1'
'-y+1/2, z+1/2, -x+1'
'x+1/2, y+1/2, z'
'y+1/2, -x+1/2, -z+1/2'
'-x+1/2, -y+1/2, z'
'-y+1/2, x+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z'
'y+1/2, x+1/2, z+1/2'
'z+1/2, x+1/2, y'
'x+1/2, -z+1/2, -y+1/2'
'-z+1/2, -x+1/2, y'
'-x+1/2, z+1/2, -y+1/2'
'z+1/2, -x+1/2, -y'
'-x+1/2, -z+1/2, y+1/2'
'-z+1/2, x+1/2, -y'
'x+1/2, z+1/2, y+1/2'
'y+1/2, z+1/2, x'
'z+1, y+1/2, x'
'z+1, -y+1/2, -x'
'-z+1, -y+1/2, x'
'-z+1, y+1/2, -x'
'y+1/2, -z+1, -x+1/2'
'-y+1/2, -z+1, x+1/2'
'-y+1/2, z+1, -x+1/2'

_cell_length_a                   33.108(3)
_cell_length_b                   33.108(3)
_cell_length_c                   33.108(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     36291(6)
_cell_formula_units_Z            32
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    12836
_cell_measurement_theta_min      2.15
_cell_measurement_theta_max      24.1

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             13824
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_process_details   
;
 [X-Red (Stoe & Cie, 2001) and X-Shape (Stoe & Cie, 1999)]
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'STOE IPDS I'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            61209
_diffrn_reflns_av_R_equivalents  0.2376
_diffrn_reflns_av_sigmaI/netI    0.0759
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_theta_min         2.13
_diffrn_reflns_theta_max         24.98
_reflns_number_total             2683
_reflns_number_gt                1373
_reflns_threshold_expression     >2σ(I)

_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_structure_solution    'SIR92 (Altomare 1994)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Diamond (Brandenburg 2011)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1474P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.000040(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(6)
_refine_ls_number_reflns         2683
_refine_ls_number_parameters     144
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1110
_refine_ls_R_factor_gt           0.0830
_refine_ls_wR_factor_ref         0.2451
_refine_ls_wR_factor_gt          0.2256
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_restrained_S_all      0.923
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.63656(3) 0.36344(3) 0.36344(3) 0.0759(6) Uani 1 3 d S . .
Cl11 Cl 0.67464(7) 0.32536(7) 0.32536(7) 0.1001(13) Uani 1 3 d S . .
P10 P 0.57789(8) 0.33952(7) 0.39034(7) 0.0760(6) Uani 1 1 d . . .
Si3 Si 0.57374(8) 0.42626(8) 0.42626(8) 0.0752(11) Uani 1 3 d S . .
C1AA C 0.5413(3) 0.4587(3) 0.4587(3) 0.093(5) Uani 1 3 d S . .
H1AA H 0.5407 0.4479 0.4856 0.139 Uiso 0.33 1 calc PR A -1
H1AB H 0.5144 0.4593 0.4479 0.139 Uiso 0.33 1 calc PR A -1
H1AC H 0.5521 0.4856 0.4593 0.139 Uiso 0.33 1 calc PR A -1
C0AA C 0.5595(3) 0.3707(3) 0.4318(3) 0.075(2) Uani 1 1 d . . .
H0AA H 0.5705 0.3605 0.4570 0.090 Uiso 1 1 calc R . .
H0AB H 0.5303 0.3684 0.4333 0.090 Uiso 1 1 calc R . .
C51 C 0.5389(3) 0.3385(3) 0.3505(3) 0.089(3) Uani 1 1 d . . .
Cl10 Cl 0.42111(7) 0.57889(7) 0.57889(7) 0.0816(10) Uani 1 3 d S . .
O1 O 0.3956(2) 0.6044(2) 0.6044(2) 0.100(4) Uani 1 3 d S . .
O5 O 0.4436(3) 0.5512(3) 0.6029(2) 0.108(2) Uani 1 1 d . . .
C61 C 0.5451(2) 0.2726(2) 0.4301(3) 0.118(4) Uani 1 1 d G . .
H61 H 0.5236 0.2895 0.4366 0.142 Uiso 1 1 calc R . .
C62 C 0.5773(2) 0.28733(15) 0.4076(2) 0.095(3) Uani 1 1 d G . .
C66 C 0.60940(19) 0.2620(2) 0.3979(3) 0.109(4) Uani 1 1 d G . .
H66 H 0.6310 0.2719 0.3828 0.131 Uiso 1 1 calc R . .
C65 C 0.6092(2) 0.22202(19) 0.4106(3) 0.115(4) Uani 1 1 d G . .
H65 H 0.6306 0.2051 0.4040 0.138 Uiso 1 1 calc R . .
C64 C 0.5769(3) 0.20730(16) 0.4330(3) 0.122(4) Uani 1 1 d G . .
H64 H 0.5768 0.1805 0.4415 0.146 Uiso 1 1 calc R . .
C63 C 0.5449(3) 0.2326(2) 0.4428(3) 0.135(5) Uani 1 1 d G . .
H63 H 0.5233 0.2227 0.4578 0.163 Uiso 1 1 calc R . .
C1 C 0.4994(3) 0.3539(3) 0.3565(3) 0.085(3) Uani 1 1 d . . .
H1 H 0.4922 0.3658 0.3809 0.102 Uiso 1 1 calc R . .
C2 C 0.5490(3) 0.3215(3) 0.3154(3) 0.090(3) Uani 1 1 d . . .
H2 H 0.5748 0.3110 0.3120 0.108 Uiso 1 1 calc R . .
C4 C 0.5213(4) 0.3193(4) 0.2839(4) 0.102(3) Uani 1 1 d . . .
H4 H 0.5286 0.3082 0.2591 0.123 Uiso 1 1 calc R . .
C5 C 0.4830(4) 0.3340(4) 0.2901(4) 0.111(4) Uani 1 1 d . . .
H5 H 0.4638 0.3325 0.2697 0.133 Uiso 1 1 calc R . .
C7 C 0.4731(4) 0.3510(4) 0.3265(4) 0.111(4) Uani 1 1 d . . .
H7 H 0.4470 0.3607 0.3304 0.133 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 Cl11 2.183(5) . ?
Ni1 P10 2.279(3) 48_645 ?
Ni1 P10 2.279(3) 11_665 ?
Ni1 P10 2.279(3) . ?
P10 C62 1.820(5) . ?
P10 C0AA 1.823(9) . ?
P10 C51 1.847(11) . ?
Si3 C1AA 1.860(15) . ?
Si3 C0AA 1.909(10) . ?
Si3 C0AA 1.909(10) 48_645 ?
Si3 C0AA 1.909(10) 11_665 ?
C1AA H1AA 0.9600 . ?
C1AA H1AB 0.9600 . ?
C1AA H1AC 0.9600 . ?
C0AA H0AA 0.9700 . ?
C0AA H0AB 0.9700 . ?
C51 C2 1.331(14) . ?
C51 C1 1.416(14) . ?
Cl10 O5 1.424(8) . ?
Cl10 O5 1.424(8) 11_665 ?
Cl10 O5 1.424(8) 48_645 ?
Cl10 O1 1.464(12) . ?
C61 C62 1.3900 . ?
C61 C63 1.3900 . ?
C61 H61 0.9300 . ?
C62 C66 1.3900 . ?
C66 C65 1.3900 . ?
C66 H66 0.9300 . ?
C65 C64 1.3900 . ?
C65 H65 0.9300 . ?
C64 C63 1.3900 . ?
C64 H64 0.9300 . ?
C63 H63 0.9300 . ?
C1 C7 1.325(16) . ?
C1 H1 0.9300 . ?
C2 C4 1.391(15) . ?
C2 H2 0.9300 . ?
C4 C5 1.377(18) . ?
C4 H4 0.9300 . ?
C5 C7 1.369(18) . ?
C5 H5 0.9300 . ?
C7 H7 0.9300 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl11 Ni1 P10 121.14(7) . 48_645 ?
Cl11 Ni1 P10 121.14(7) . 11_665 ?
P10 Ni1 P10 95.67(9) 48_645 11_665 ?
Cl11 Ni1 P10 121.14(7) . . ?
P10 Ni1 P10 95.67(9) 48_645 . ?
P10 Ni1 P10 95.67(9) 11_665 . ?
C62 P10 C0AA 107.3(4) . . ?
C62 P10 C51 101.6(4) . . ?
C0AA P10 C51 108.4(4) . . ?
C62 P10 Ni1 117.5(3) . . ?
C0AA P10 Ni1 112.5(3) . . ?
C51 P10 Ni1 108.8(4) . . ?
C1AA Si3 C0AA 111.0(3) . . ?
C1AA Si3 C0AA 111.0(3) . 48_645 ?
C0AA Si3 C0AA 107.9(3) . 48_645 ?
C1AA Si3 C0AA 111.0(3) . 11_665 ?
C0AA Si3 C0AA 107.9(3) . 11_665 ?
C0AA Si3 C0AA 107.9(3) 48_645 11_665 ?
Si3 C1AA H1AA 109.5 . . ?
Si3 C1AA H1AB 109.5 . . ?
Si3 C1AA H1AC 109.5 . . ?
P10 C0AA Si3 113.0(5) . . ?
P10 C0AA H0AA 109.0 . . ?
Si3 C0AA H0AA 109.0 . . ?
P10 C0AA H0AB 109.0 . . ?
Si3 C0AA H0AB 109.0 . . ?
H0AA C0AA H0AB 107.8 . . ?
C2 C51 C1 120.4(10) . . ?
C2 C51 P10 117.0(8) . . ?
C1 C51 P10 122.5(9) . . ?
O5 Cl10 O5 108.3(3) . 11_665 ?
O5 Cl10 O5 108.3(3) . 48_645 ?
O5 Cl10 O5 108.3(3) 11_665 48_645 ?
O5 Cl10 O1 110.6(3) . . ?
O5 Cl10 O1 110.6(3) 11_665 . ?
O5 Cl10 O1 110.6(3) 48_645 . ?
C62 C61 C63 120.0 . . ?
C62 C61 H61 120.0 . . ?
C63 C61 H61 120.0 . . ?
C61 C62 C66 120.0 . . ?
C61 C62 P10 120.6(4) . . ?
C66 C62 P10 119.4(4) . . ?
C65 C66 C62 120.0 . . ?
C65 C66 H66 120.0 . . ?
C62 C66 H66 120.0 . . ?
C64 C65 C66 120.0 . . ?
C64 C65 H65 120.0 . . ?
C66 C65 H65 120.0 . . ?
C65 C64 C63 120.0 . . ?
C65 C64 H64 120.0 . . ?
C63 C64 H64 120.0 . . ?
C64 C63 C61 120.0 . . ?
C64 C63 H63 120.0 . . ?
C61 C63 H63 120.0 . . ?
C7 C1 C51 118.5(11) . . ?
C7 C1 H1 120.8 . . ?
C51 C1 H1 120.8 . . ?
C51 C2 C4 120.8(10) . . ?
C51 C2 H2 119.6 . . ?
C4 C2 H2 119.6 . . ?
C5 C4 C2 118.4(11) . . ?
C5 C4 H4 120.8 . . ?
C2 C4 H4 120.8 . . ?
C7 C5 C4 119.9(11) . . ?
C7 C5 H5 120.0 . . ?
C4 C5 H5 120.0 . . ?
C1 C7 C5 122.1(12) . . ?
C1 C7 H7 119.0 . . ?
C5 C7 H7 119.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl11 Ni1 P10 C62 37.9(3) . . . . ?
P10 Ni1 P10 C62 -94.0(3) 48_645 . . . ?
P10 Ni1 P10 C62 169.8(3) 11_665 . . . ?
Cl11 Ni1 P10 C0AA 163.2(3) . . . . ?
P10 Ni1 P10 C0AA 31.3(3) 48_645 . . . ?
P10 Ni1 P10 C0AA -65.0(3) 11_665 . . . ?
Cl11 Ni1 P10 C51 -76.7(4) . . . . ?
P10 Ni1 P10 C51 151.5(3) 48_645 . . . ?
P10 Ni1 P10 C51 55.2(4) 11_665 . . . ?
C62 P10 C0AA Si3 161.2(4) . . . . ?
C51 P10 C0AA Si3 -89.9(5) . . . . ?
Ni1 P10 C0AA Si3 30.5(5) . . . . ?
C1AA Si3 C0AA P10 161.5(3) . . . . ?
C0AA Si3 C0AA P10 -76.7(4) 48_645 . . . ?
C0AA Si3 C0AA P10 39.6(6) 11_665 . . . ?
C62 P10 C51 C2 -75.7(10) . . . . ?
C0AA P10 C51 C2 171.5(9) . . . . ?
Ni1 P10 C51 C2 48.8(10) . . . . ?
C62 P10 C51 C1 102.7(9) . . . . ?
C0AA P10 C51 C1 -10.1(10) . . . . ?
Ni1 P10 C51 C1 -132.8(8) . . . . ?
C63 C61 C62 C66 0.0 . . . . ?
C63 C61 C62 P10 179.4(6) . . . . ?
C0AA P10 C62 C61 41.8(6) . . . . ?
C51 P10 C62 C61 -71.8(6) . . . . ?
Ni1 P10 C62 C61 169.6(4) . . . . ?
C0AA P10 C62 C66 -138.8(5) . . . . ?
C51 P10 C62 C66 107.6(6) . . . . ?
Ni1 P10 C62 C66 -10.9(6) . . . . ?
C61 C62 C66 C65 0.0 . . . . ?
P10 C62 C66 C65 -179.4(6) . . . . ?
C62 C66 C65 C64 0.0 . . . . ?
C66 C65 C64 C63 0.0 . . . . ?
C65 C64 C63 C61 0.0 . . . . ?
C62 C61 C63 C64 0.0 . . . . ?
C2 C51 C1 C7 0.1(16) . . . . ?
P10 C51 C1 C7 -178.3(9) . . . . ?
C1 C51 C2 C4 1.3(17) . . . . ?
P10 C51 C2 C4 179.7(9) . . . . ?
C51 C2 C4 C5 -1.9(18) . . . . ?
C2 C4 C5 C7 1.1(19) . . . . ?
C51 C1 C7 C5 -0.8(18) . . . . ?
C4 C5 C7 C1 0(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        24.98
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.079
####################################################################### 
# 
# 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_upa159
_database_code_depnum_ccdc_archive 'CCDC 1486088'
_audit_update_record             
;
2016-06-16 deposited with the CCDC.
2016-12-08 downloaded from the CCDC.
;
_publcif_datablock.id            {043af71d-75df-4730-93a2-8b5d46d01bf4}

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H39 N Ni P4, 2(B F4)'
_chemical_formula_sum            'C14 H39 B2 F8 N Ni P4'
_chemical_formula_weight         577.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.1498(3)
_cell_length_b                   16.0585(6)
_cell_length_c                   19.1814(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 121.948(2)
_cell_angle_gamma                90.00
_cell_volume                     2652.83(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    108(2)
_cell_measurement_reflns_used    6997
_cell_measurement_theta_min      3.8370
_cell_measurement_theta_max      73.8190


_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1200
_exptl_absorpt_coefficient_mu    3.891
_exptl_crystal_description       prism
_exptl_absorpt_correction_T_min  0.82920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      108.2(6)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Atlas
_diffrn_detector_area_resol_mean 10.4372
_diffrn_reflns_number            14353
_diffrn_reflns_theta_min         3.8670
_diffrn_reflns_theta_max         74.2490
_diffrn_measured_fraction_theta_max 0.8816
_diffrn_reflns_theta_full        66.9682
_diffrn_measured_fraction_theta_full 0.9120
_diffrn_orient_matrix_UB_11      0.1134761000
_diffrn_orient_matrix_UB_12      -0.0635838000
_diffrn_orient_matrix_UB_13      0.0040453000
_diffrn_orient_matrix_UB_21      -0.0998410000
_diffrn_orient_matrix_UB_22      -0.0716581000
_diffrn_orient_matrix_UB_23      -0.0099569000
_diffrn_orient_matrix_UB_31      0.0147711000
_diffrn_orient_matrix_UB_32      0.0048612000
_diffrn_orient_matrix_UB_33      -0.0939989000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega -124.00  -79.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -99.0000   30.0000 45

#__ type_ start__ end____ width___ exp.time_
  2 omega  -32.00   71.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -       41.4802  -57.0000  150.0000 103

#__ type_ start__ end____ width___ exp.time_
  3 omega   24.00  109.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -94.0000    0.0000 85

#__ type_ start__ end____ width___ exp.time_
  4 omega   31.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000  -90.0000 38

#__ type_ start__ end____ width___ exp.time_
  5 omega   31.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -150.0000 38

#__ type_ start__ end____ width___ exp.time_
  6 omega   34.00   77.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -45.0000    0.0000 43

#__ type_ start__ end____ width___ exp.time_
  7 omega   31.00   69.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562  -30.0000 -120.0000 38

#__ type_ start__ end____ width___ exp.time_
  8 omega   75.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000   30.0000 83

#__ type_ start__ end____ width___ exp.time_
  9 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -57.0000 -150.0000 103

#__ type_ start__ end____ width___ exp.time_
 10 omega -115.00  -12.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.4802  -57.0000   90.0000 103

#__ type_ start__ end____ width___ exp.time_
 11 omega   75.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -90.0000 83

#__ type_ start__ end____ width___ exp.time_
 12 omega   81.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   45.0000 -180.0000 77

#__ type_ start__ end____ width___ exp.time_
 13 omega   75.00  158.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.4562   77.0000  -30.0000 83

;
_diffrn_measurement_method       'ω scans'

_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23

_reflns_number_total             4798
_reflns_number_gt                4300
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0608P)²+5.0530P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4798
_refine_ls_number_parameters     282
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0460
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1200
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.001

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.64467(5) 0.26991(3) -0.40711(3) 0.02002(14) Uani 1 1 d . . .
P2 P -0.72434(9) 0.34574(4) -0.34388(5) 0.02226(18) Uani 1 1 d . . .
P3 P -0.78139(9) 0.34614(4) -0.52844(5) 0.02248(18) Uani 1 1 d . . .
P4 P -0.76003(9) 0.15180(4) -0.39482(5) 0.02386(18) Uani 1 1 d . . .
P5 P -0.38447(8) 0.30231(5) -0.31710(5) 0.02307(18) Uani 1 1 d . . .
N9 N -0.5668(3) 0.20363(15) -0.45902(16) 0.0232(5) Uani 1 1 d . . .
C14 C -0.6349(4) 0.32245(19) -0.23564(19) 0.0269(6) Uani 1 1 d . . .
H14A H -0.6241 0.2632 -0.2276 0.040 Uiso 1 1 calc R . .
H14B H -0.6989 0.3436 -0.2166 0.040 Uiso 1 1 calc R . .
H14C H -0.5344 0.3481 -0.2053 0.040 Uiso 1 1 calc R . .
C16 C -0.5115(4) 0.16422(17) -0.48585(19) 0.0234(6) Uani 1 1 d . . .
C17 C -0.8285(4) 0.2829(2) -0.6178(2) 0.0317(7) Uani 1 1 d . . .
H17A H -0.7343 0.2637 -0.6128 0.048 Uiso 1 1 calc R . .
H17B H -0.8861 0.3158 -0.6667 0.048 Uiso 1 1 calc R . .
H17C H -0.8898 0.2359 -0.6208 0.048 Uiso 1 1 calc R . .
C18 C -0.6743(4) 0.43147(19) -0.5381(2) 0.0321(7) Uani 1 1 d . . .
H18A H -0.6521 0.4729 -0.4972 0.048 Uiso 1 1 calc R . .
H18B H -0.7355 0.4558 -0.5918 0.048 Uiso 1 1 calc R . .
H18C H -0.5788 0.4108 -0.5304 0.048 Uiso 1 1 calc R . .
C19 C -0.9306(4) 0.3413(2) -0.3818(2) 0.0325(7) Uani 1 1 d . . .
H19A H -0.9891 0.3557 -0.4390 0.049 Uiso 1 1 calc R . .
H19B H -0.9540 0.3799 -0.3516 0.049 Uiso 1 1 calc R . .
H19C H -0.9575 0.2860 -0.3748 0.049 Uiso 1 1 calc R . .
C20 C -0.2944(4) 0.3646(2) -0.2233(2) 0.0358(7) Uani 1 1 d . . .
H20A H -0.3476 0.4169 -0.2342 0.054 Uiso 1 1 calc R . .
H20B H -0.1874 0.3744 -0.2047 0.054 Uiso 1 1 calc R . .
H20C H -0.3007 0.3352 -0.1815 0.054 Uiso 1 1 calc R . .
C21 C -0.4382(4) 0.11321(19) -0.5187(2) 0.0300(7) Uani 1 1 d . . .
H21A H -0.3613 0.0781 -0.4760 0.045 Uiso 1 1 calc R . .
H21B H -0.3896 0.1486 -0.5390 0.045 Uiso 1 1 calc R . .
H21C H -0.5153 0.0793 -0.5626 0.045 Uiso 1 1 calc R . .
C24 C -0.6574(5) 0.0573(2) -0.3912(3) 0.0499(11) Uani 1 1 d . . .
H24A H -0.6629 0.0506 -0.4424 0.075 Uiso 1 1 calc R . .
H24B H -0.7046 0.0102 -0.3821 0.075 Uiso 1 1 calc R . .
H24C H -0.5507 0.0614 -0.3473 0.075 Uiso 1 1 calc R . .
C25 C -0.3051(5) 0.3525(3) -0.3714(3) 0.0506(11) Uani 1 1 d . . .
H25A H -0.3327 0.3211 -0.4199 0.076 Uiso 1 1 calc R . .
H25B H -0.1940 0.3552 -0.3365 0.076 Uiso 1 1 calc R . .
H25C H -0.3463 0.4079 -0.3867 0.076 Uiso 1 1 calc R . .
C26 C -0.6897(4) 0.45637(19) -0.3442(2) 0.0312(7) Uani 1 1 d . . .
H26A H -0.5820 0.4657 -0.3242 0.047 Uiso 1 1 calc R . .
H26B H -0.7168 0.4846 -0.3094 0.047 Uiso 1 1 calc R . .
H26C H -0.7520 0.4775 -0.3992 0.047 Uiso 1 1 calc R . .
C27 C -0.9513(4) 0.1336(2) -0.4858(2) 0.0420(9) Uani 1 1 d . . .
H27A H -1.0165 0.1810 -0.4954 0.063 Uiso 1 1 calc R . .
H27B H -0.9967 0.0850 -0.4776 0.063 Uiso 1 1 calc R . .
H27C H -0.9417 0.1251 -0.5325 0.063 Uiso 1 1 calc R . .
C29 C -0.9698(4) 0.3948(2) -0.5653(2) 0.0374(8) Uani 1 1 d . . .
H29A H -1.0417 0.3536 -0.5689 0.056 Uiso 1 1 calc R . .
H29B H -1.0081 0.4185 -0.6186 0.056 Uiso 1 1 calc R . .
H29C H -0.9586 0.4378 -0.5278 0.056 Uiso 1 1 calc R . .
C31 C -0.2687(4) 0.2076(2) -0.2763(3) 0.0436(9) Uani 1 1 d . . .
H31A H -0.2931 0.1806 -0.2399 0.065 Uiso 1 1 calc R . .
H31B H -0.1604 0.2217 -0.2468 0.065 Uiso 1 1 calc R . .
H31C H -0.2917 0.1708 -0.3208 0.065 Uiso 1 1 calc R . .
C37 C -0.7895(5) 0.1299(2) -0.3110(3) 0.0466(9) Uani 1 1 d . . .
H37A H -0.6909 0.1283 -0.2601 0.070 Uiso 1 1 calc R . .
H37B H -0.8405 0.0771 -0.3201 0.070 Uiso 1 1 calc R . .
H37C H -0.8528 0.1728 -0.3084 0.070 Uiso 1 1 calc R . .
F6 F -0.4715(2) 0.19773(13) -0.07698(14) 0.0404(5) Uani 1 1 d . . .
F8 F -0.2533(3) 0.23740(14) -0.07101(18) 0.0536(6) Uani 1 1 d . . .
F10 F -0.2710(2) 0.10612(11) -0.03297(12) 0.0331(4) Uani 1 1 d . . .
F11 F -0.4134(3) 0.14459(15) -0.16643(14) 0.0575(7) Uani 1 1 d . . .
B23 B -0.3518(4) 0.1708(2) -0.0867(2) 0.0272(7) Uani 1 1 d . . .
F7 F -0.7270(3) 0.49957(14) -0.16635(16) 0.0490(6) Uani 1 1 d . A .
B22 B -0.8767(4) 0.4855(2) -0.1820(2) 0.0316(8) Uani 1 1 d . . .
F12 F -0.8856(4) 0.5036(2) -0.1150(2) 0.0581(5) Uani 0.847(3) 1 d P A 1
F13 F -0.9159(4) 0.40195(19) -0.2036(2) 0.0581(5) Uani 0.847(3) 1 d P A 1
F15 F -0.9832(4) 0.5335(2) -0.2476(2) 0.0581(5) Uani 0.847(3) 1 d P A 1
F12B F -0.892(2) 0.5667(11) -0.1481(11) 0.0581(5) Uani 0.153(3) 1 d P A 2
F15B F -0.978(2) 0.4872(12) -0.2624(12) 0.0581(5) Uani 0.153(3) 1 d P A 2
F13B F -0.840(2) 0.4617(13) -0.1039(12) 0.0581(5) Uani 0.153(3) 1 d P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N9 1.892(2) . ?
Ni1 P2 2.1556(8) . ?
Ni1 P4 2.3057(8) . ?
Ni1 P5 2.3239(9) . ?
Ni1 P3 2.3287(9) . ?
P2 C14 1.811(3) . ?
P2 C26 1.812(3) . ?
P2 C19 1.818(3) . ?
P3 C18 1.818(3) . ?
P3 C17 1.825(3) . ?
P3 C29 1.826(3) . ?
P4 C37 1.819(4) . ?
P4 C24 1.820(4) . ?
P4 C27 1.821(4) . ?
P5 C25 1.810(4) . ?
P5 C31 1.825(4) . ?
P5 C20 1.826(3) . ?
N9 C16 1.134(4) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C16 C21 1.454(4) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
F6 B23 1.391(4) . ?
F8 B23 1.384(4) . ?
F10 B23 1.385(4) . ?
F11 B23 1.377(4) . ?
F7 B22 1.403(4) . ?
B22 F15B 1.32(2) . ?
B22 F12 1.366(5) . ?
B22 F15 1.380(5) . ?
B22 F13B 1.393(19) . ?
B22 F13 1.399(5) . ?
B22 F12B 1.499(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N9 Ni1 P2 177.78(8) . . ?
N9 Ni1 P4 88.12(8) . . ?
P2 Ni1 P4 92.59(3) . . ?
N9 Ni1 P5 83.69(8) . . ?
P2 Ni1 P5 94.17(3) . . ?
P4 Ni1 P5 123.17(3) . . ?
N9 Ni1 P3 87.93(8) . . ?
P2 Ni1 P3 93.60(3) . . ?
P4 Ni1 P3 117.93(3) . . ?
P5 Ni1 P3 117.83(3) . . ?
C14 P2 C26 103.06(15) . . ?
C14 P2 C19 102.90(15) . . ?
C26 P2 C19 102.78(16) . . ?
C14 P2 Ni1 114.75(10) . . ?
C26 P2 Ni1 114.89(11) . . ?
C19 P2 Ni1 116.63(11) . . ?
C18 P3 C17 101.40(16) . . ?
C18 P3 C29 101.43(17) . . ?
C17 P3 C29 100.03(17) . . ?
C18 P3 Ni1 115.19(12) . . ?
C17 P3 Ni1 111.54(12) . . ?
C29 P3 Ni1 124.05(12) . . ?
C37 P4 C24 99.4(2) . . ?
C37 P4 C27 103.0(2) . . ?
C24 P4 C27 101.6(2) . . ?
C37 P4 Ni1 125.40(13) . . ?
C24 P4 Ni1 112.21(12) . . ?
C27 P4 Ni1 112.07(13) . . ?
C25 P5 C31 103.7(2) . . ?
C25 P5 C20 100.38(19) . . ?
C31 P5 C20 99.24(18) . . ?
C25 P5 Ni1 110.44(13) . . ?
C31 P5 Ni1 110.65(13) . . ?
C20 P5 Ni1 129.38(12) . . ?
C16 N9 Ni1 175.8(3) . . ?
P2 C14 H14A 109.5 . . ?
P2 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
P2 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N9 C16 C21 178.9(4) . . ?
P3 C17 H17A 109.5 . . ?
P3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P3 C18 H18A 109.5 . . ?
P3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
P2 C19 H19A 109.5 . . ?
P2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
P2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
P5 C20 H20A 109.5 . . ?
P5 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
P5 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
P4 C24 H24A 109.5 . . ?
P4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
P4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
P5 C25 H25A 109.5 . . ?
P5 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
P5 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
P2 C26 H26A 109.5 . . ?
P2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
P2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
P4 C27 H27A 109.5 . . ?
P4 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
P4 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
P3 C29 H29A 109.5 . . ?
P3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
P3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
P5 C31 H31A 109.5 . . ?
P5 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
P5 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
P4 C37 H37A 109.5 . . ?
P4 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
P4 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
F11 B23 F8 109.1(3) . . ?
F11 B23 F10 109.8(3) . . ?
F8 B23 F10 110.0(3) . . ?
F11 B23 F6 109.2(3) . . ?
F8 B23 F6 108.2(3) . . ?
F10 B23 F6 110.4(3) . . ?
F15B B22 F12 134.0(9) . . ?
F15B B22 F15 34.7(8) . . ?
F12 B22 F15 109.2(3) . . ?
F15B B22 F13B 149.2(12) . . ?
F12 B22 F13B 32.8(8) . . ?
F15 B22 F13B 140.2(9) . . ?
F15B B22 F13 75.6(9) . . ?
F12 B22 F13 109.5(3) . . ?
F15 B22 F13 107.6(3) . . ?
F13B B22 F13 85.9(9) . . ?
F15B B22 F7 109.2(8) . . ?
F12 B22 F7 111.6(3) . . ?
F15 B22 F7 110.0(3) . . ?
F13B B22 F7 99.9(8) . . ?
F13 B22 F7 108.8(3) . . ?
F15B B22 F12B 107.0(11) . . ?
F12 B22 F12B 48.3(7) . . ?
F15 B22 F12B 72.5(7) . . ?
F13B B22 F12B 78.6(11) . . ?
F13 B22 F12B 152.2(7) . . ?
F7 B22 F12B 96.6(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N9 Ni1 P2 C14 -40(2) . . . . ?
P4 Ni1 P2 C14 68.50(12) . . . . ?
P5 Ni1 P2 C14 -55.03(12) . . . . ?
P3 Ni1 P2 C14 -173.30(12) . . . . ?
N9 Ni1 P2 C26 79(2) . . . . ?
P4 Ni1 P2 C26 -172.27(13) . . . . ?
P5 Ni1 P2 C26 64.20(13) . . . . ?
P3 Ni1 P2 C26 -54.07(13) . . . . ?
N9 Ni1 P2 C19 -160(2) . . . . ?
P4 Ni1 P2 C19 -51.91(13) . . . . ?
P5 Ni1 P2 C19 -175.44(13) . . . . ?
P3 Ni1 P2 C19 66.29(13) . . . . ?
N9 Ni1 P3 C18 -86.65(14) . . . . ?
P2 Ni1 P3 C18 91.73(12) . . . . ?
P4 Ni1 P3 C18 -173.42(12) . . . . ?
P5 Ni1 P3 C18 -4.90(13) . . . . ?
N9 Ni1 P3 C17 28.22(14) . . . . ?
P2 Ni1 P3 C17 -153.40(12) . . . . ?
P4 Ni1 P3 C17 -58.56(12) . . . . ?
P5 Ni1 P3 C17 109.97(12) . . . . ?
N9 Ni1 P3 C29 147.74(18) . . . . ?
P2 Ni1 P3 C29 -33.87(17) . . . . ?
P4 Ni1 P3 C29 60.97(17) . . . . ?
P5 Ni1 P3 C29 -130.51(16) . . . . ?
N9 Ni1 P4 C37 147.3(2) . . . . ?
P2 Ni1 P4 C37 -30.60(19) . . . . ?
P5 Ni1 P4 C37 66.09(19) . . . . ?
P3 Ni1 P4 C37 -126.05(19) . . . . ?
N9 Ni1 P4 C24 26.79(19) . . . . ?
P2 Ni1 P4 C24 -151.10(18) . . . . ?
P5 Ni1 P4 C24 -54.42(18) . . . . ?
P3 Ni1 P4 C24 113.44(18) . . . . ?
N9 Ni1 P4 C27 -86.77(17) . . . . ?
P2 Ni1 P4 C27 95.34(15) . . . . ?
P5 Ni1 P4 C27 -167.98(15) . . . . ?
P3 Ni1 P4 C27 -0.11(16) . . . . ?
N9 Ni1 P5 C25 61.03(19) . . . . ?
P2 Ni1 P5 C25 -119.55(18) . . . . ?
P4 Ni1 P5 C25 144.61(18) . . . . ?
P3 Ni1 P5 C25 -23.26(18) . . . . ?
N9 Ni1 P5 C31 -53.18(17) . . . . ?
P2 Ni1 P5 C31 126.24(15) . . . . ?
P4 Ni1 P5 C31 30.40(16) . . . . ?
P3 Ni1 P5 C31 -137.47(15) . . . . ?
N9 Ni1 P5 C20 -175.28(18) . . . . ?
P2 Ni1 P5 C20 4.14(17) . . . . ?
P4 Ni1 P5 C20 -91.69(17) . . . . ?
P3 Ni1 P5 C20 100.44(17) . . . . ?
P2 Ni1 N9 C16 3(5) . . . . ?
P4 Ni1 N9 C16 -106(3) . . . . ?
P5 Ni1 N9 C16 18(3) . . . . ?
P3 Ni1 N9 C16 136(3) . . . . ?
Ni1 N9 C16 C21 25(20) . . . . ?




_refine_diff_density_max         1.104
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.078
