# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_jyy148
_database_code_depnum_ccdc_archive 'CCDC 1827010'
_audit_update_record             
;
2018-03-02 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[CoTPAP(Cl)] '
_chemical_name_common            '[CoTPAP(Cl)] '
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H30 Cl Co N7 P'
_chemical_formula_weight         541.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   9.1020(16)
_cell_length_b                   16.434(3)
_cell_length_c                   33.454(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5004.1(16)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9922
_cell_measurement_theta_min      2.44
_cell_measurement_theta_max      28.81

_exptl_crystal_description       irregular
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             2256
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.164
_exptl_absorpt_coefficient_mu    0.884
_shelx_estimated_absorpt_T_min   0.777
_shelx_estimated_absorpt_T_max   0.869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6892
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
60785 Corrected reflections written to file jyy148s.hkl 
Estimated minimum and maximum transmission:  0.6892  0.7458 
The ratio (0.9241) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.2000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            56948
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_theta_min         1.217
_diffrn_reflns_theta_max         28.820
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6257
_reflns_number_gt                5454
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A purple crystal of approximate dimensions 0.164 x 0.180 x 0.301 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters and 
for data collection (60 sec/frame scan time for a sphere of diffraction data).  
The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was mmm and the systematic absences were consistent with 
the orthorhombic space group Pbca that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis. Hydrogen atoms were included using a riding 
model.

Least-squares analysis yielded wR2 = 0.0776 and Goof = 1.052 for 307 variables 
refined against 6257 data (0.74 Å), R1 = 0.0315 for those 5454 data 
with I > 2.0sigma(I).  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0343P)²+4.1355P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         6257
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0745
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.64432(2) 0.75899(2) 0.34442(2) 0.01292(6) Uani 1 1 d . . . . .
Cl1 Cl 0.54021(4) 0.86650(2) 0.31332(2) 0.02206(9) Uani 1 1 d . . . . .
P1 P 0.66101(4) 0.69301(2) 0.40034(2) 0.01105(8) Uani 1 1 d . . . . .
N1 N 0.74936(15) 0.57822(8) 0.47627(4) 0.0155(3) Uani 1 1 d . . . . .
N2 N 0.81122(14) 0.72558(7) 0.42648(4) 0.0127(2) Uani 1 1 d . . . . .
N3 N 0.69682(15) 0.59418(7) 0.39045(4) 0.0137(3) Uani 1 1 d . . . . .
N4 N 0.52860(14) 0.68992(8) 0.43563(4) 0.0143(3) Uani 1 1 d . . . . .
N5 N 0.86221(14) 0.78567(8) 0.34152(4) 0.0149(3) Uani 1 1 d . . . . .
N6 N 0.61500(16) 0.65724(8) 0.30952(4) 0.0186(3) Uani 1 1 d . . . . .
N7 N 0.26032(15) 0.57736(9) 0.44101(4) 0.0198(3) Uani 1 1 d . . . . .
C1 C 0.88319(17) 0.62486(9) 0.47858(4) 0.0154(3) Uani 1 1 d . . . . .
H1A H 0.9644 0.5877 0.4860 0.019 Uiso 1 1 calc R U . . .
H1B H 0.8729 0.6653 0.5003 0.019 Uiso 1 1 calc R U . . .
C2 C 0.92618(16) 0.66986(9) 0.44018(5) 0.0145(3) Uani 1 1 d . . . . .
H2A H 1.0175 0.7010 0.4450 0.017 Uiso 1 1 calc R U . . .
H2B H 0.9465 0.6295 0.4189 0.017 Uiso 1 1 calc R U . . .
C3 C 0.74111(17) 0.50824(9) 0.45020(5) 0.0158(3) Uani 1 1 d . . . . .
H3A H 0.7000 0.4616 0.4652 0.019 Uiso 1 1 calc R U . . .
H3B H 0.8414 0.4933 0.4414 0.019 Uiso 1 1 calc R U . . .
C4 C 0.64550(18) 0.52440(9) 0.41337(5) 0.0154(3) Uani 1 1 d . . . . .
H4A H 0.6460 0.4756 0.3960 0.018 Uiso 1 1 calc R U . . .
H4B H 0.5430 0.5342 0.4220 0.018 Uiso 1 1 calc R U . . .
C5 C 0.61650(18) 0.60777(10) 0.49473(5) 0.0169(3) Uani 1 1 d . . . . .
H5A H 0.6346 0.6139 0.5238 0.020 Uiso 1 1 calc R U . . .
H5B H 0.5391 0.5660 0.4914 0.020 Uiso 1 1 calc R U . . .
C6 C 0.55809(18) 0.68853(9) 0.47868(4) 0.0165(3) Uani 1 1 d . . . . .
H6A H 0.4661 0.7019 0.4930 0.020 Uiso 1 1 calc R U . . .
H6B H 0.6304 0.7317 0.4849 0.020 Uiso 1 1 calc R U . . .
C7 C 0.86207(17) 0.80624(9) 0.41371(5) 0.0145(3) Uani 1 1 d . . . . .
H7A H 0.9286 0.8282 0.4345 0.017 Uiso 1 1 calc R U . . .
H7B H 0.7761 0.8430 0.4120 0.017 Uiso 1 1 calc R U . . .
C8 C 0.94154(17) 0.80801(9) 0.37402(4) 0.0143(3) Uani 1 1 d . . . . .
C9 C 1.08709(18) 0.83218(10) 0.37076(5) 0.0207(3) Uani 1 1 d . . . . .
H9 H 1.1404 0.8472 0.3940 0.025 Uiso 1 1 calc R U . . .
C10 C 1.15501(19) 0.83457(11) 0.33367(6) 0.0258(4) Uani 1 1 d . . . . .
H10 H 1.2548 0.8508 0.3311 0.031 Uiso 1 1 calc R U . . .
C11 C 1.0735(2) 0.81271(11) 0.30045(5) 0.0246(4) Uani 1 1 d . . . . .
H11 H 1.1161 0.8141 0.2745 0.030 Uiso 1 1 calc R U . . .
C12 C 0.92908(19) 0.78885(10) 0.30560(5) 0.0201(3) Uani 1 1 d . . . . .
H12 H 0.8741 0.7739 0.2826 0.024 Uiso 1 1 calc R U . . .
C13 C 0.77538(17) 0.57838(9) 0.35310(5) 0.0160(3) Uani 1 1 d . . . . .
H13A H 0.8207 0.5237 0.3542 0.019 Uiso 1 1 calc R U . . .
H13B H 0.8550 0.6189 0.3498 0.019 Uiso 1 1 calc R U . . .
C14 C 0.67301(18) 0.58291(10) 0.31769(5) 0.0180(3) Uani 1 1 d . . . . .
C15 C 0.6366(2) 0.51438(11) 0.29557(5) 0.0284(4) Uani 1 1 d . . . . .
H15 H 0.6797 0.4632 0.3017 0.034 Uiso 1 1 calc R U . . .
C16 C 0.5371(3) 0.52099(13) 0.26446(6) 0.0432(6) Uani 1 1 d . . . . .
H16 H 0.5110 0.4747 0.2490 0.052 Uiso 1 1 calc R U . . .
C17 C 0.4767(3) 0.59615(13) 0.25642(6) 0.0458(6) Uani 1 1 d . . . . .
H17 H 0.4075 0.6024 0.2354 0.055 Uiso 1 1 calc R U . . .
C18 C 0.5179(2) 0.66236(12) 0.27927(5) 0.0298(4) Uani 1 1 d . . . . .
H18 H 0.4758 0.7139 0.2734 0.036 Uiso 1 1 calc R U . . .
C19 C 0.37819(17) 0.70382(10) 0.42173(5) 0.0178(3) Uani 1 1 d . . . . .
H19A H 0.3813 0.7401 0.3981 0.021 Uiso 1 1 calc R U . . .
H19B H 0.3229 0.7323 0.4430 0.021 Uiso 1 1 calc R U . . .
C20 C 0.29603(17) 0.62695(10) 0.41059(5) 0.0174(3) Uani 1 1 d . . . . .
C21 C 0.2609(2) 0.60928(11) 0.37111(5) 0.0242(4) Uani 1 1 d . . . . .
H21 H 0.2889 0.6454 0.3503 0.029 Uiso 1 1 calc R U . . .
C22 C 0.1847(2) 0.53842(12) 0.36240(6) 0.0287(4) Uani 1 1 d . . . . .
H22 H 0.1591 0.5253 0.3356 0.034 Uiso 1 1 calc R U . . .
C23 C 0.14653(19) 0.48716(11) 0.39356(6) 0.0259(4) Uani 1 1 d . . . . .
H23 H 0.0939 0.4382 0.3887 0.031 Uiso 1 1 calc R U . . .
C24 C 0.18718(18) 0.50919(11) 0.43202(5) 0.0220(3) Uani 1 1 d . . . . .
H24 H 0.1615 0.4737 0.4533 0.026 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N5 2.0334(14) . ?
Co1 N6 2.0568(14) . ?
Co1 P1 2.1675(5) . ?
Co1 Cl1 2.2589(5) . ?
P1 N4 1.6879(13) . ?
P1 N3 1.6892(13) . ?
P1 N2 1.7089(13) . ?
P1 N1 3.2647(14) . ?
N1 C1 1.441(2) . ?
N1 C5 1.442(2) . ?
N1 C3 1.445(2) . ?
N2 C2 1.4640(19) . ?
N2 C7 1.4677(19) . ?
N3 C4 1.4563(19) . ?
N3 C13 1.4629(19) . ?
N4 C19 1.4638(19) . ?
N4 C6 1.4651(19) . ?
N5 C12 1.348(2) . ?
N5 C8 1.3557(19) . ?
N6 C18 1.346(2) . ?
N6 C14 1.358(2) . ?
N7 C24 1.337(2) . ?
N7 C20 1.344(2) . ?
C1 C2 1.533(2) . ?
C3 C4 1.532(2) . ?
C5 C6 1.527(2) . ?
C7 C8 1.512(2) . ?
C8 C9 1.387(2) . ?
C9 C10 1.387(2) . ?
C10 C11 1.384(3) . ?
C11 C12 1.383(2) . ?
C13 C14 1.509(2) . ?
C14 C15 1.388(2) . ?
C15 C16 1.384(3) . ?
C16 C17 1.379(3) . ?
C17 C18 1.382(3) . ?
C19 C20 1.515(2) . ?
C20 C21 1.389(2) . ?
C21 C22 1.387(3) . ?
C22 C23 1.384(3) . ?
C23 C24 1.387(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Co1 N6 105.95(6) . . ?
N5 Co1 P1 94.63(4) . . ?
N6 Co1 P1 95.30(4) . . ?
N5 Co1 Cl1 102.62(4) . . ?
N6 Co1 Cl1 108.66(4) . . ?
P1 Co1 Cl1 144.910(18) . . ?
N4 P1 N3 104.23(7) . . ?
N4 P1 N2 102.87(7) . . ?
N3 P1 N2 104.30(7) . . ?
N4 P1 Co1 124.66(5) . . ?
N3 P1 Co1 109.00(5) . . ?
N2 P1 Co1 109.94(5) . . ?
N4 P1 N1 67.31(5) . . ?
N3 P1 N1 63.21(5) . . ?
N2 P1 N1 65.53(5) . . ?
Co1 P1 N1 167.92(3) . . ?
C1 N1 C5 120.44(13) . . ?
C1 N1 C3 119.96(13) . . ?
C5 N1 C3 118.87(13) . . ?
C1 N1 P1 86.71(8) . . ?
C5 N1 P1 86.11(8) . . ?
C3 N1 P1 88.70(8) . . ?
C2 N2 C7 115.51(12) . . ?
C2 N2 P1 122.42(10) . . ?
C7 N2 P1 112.72(10) . . ?
C4 N3 C13 117.82(12) . . ?
C4 N3 P1 126.31(10) . . ?
C13 N3 P1 115.61(10) . . ?
C19 N4 C6 119.08(12) . . ?
C19 N4 P1 116.16(10) . . ?
C6 N4 P1 123.87(11) . . ?
C12 N5 C8 117.63(14) . . ?
C12 N5 Co1 119.42(11) . . ?
C8 N5 Co1 122.66(11) . . ?
C18 N6 C14 117.55(14) . . ?
C18 N6 Co1 117.46(12) . . ?
C14 N6 Co1 124.50(11) . . ?
C24 N7 C20 117.27(15) . . ?
N1 C1 C2 115.29(12) . . ?
N2 C2 C1 112.43(12) . . ?
N1 C3 C4 112.15(12) . . ?
N3 C4 C3 112.19(13) . . ?
N1 C5 C6 115.72(13) . . ?
N4 C6 C5 115.02(13) . . ?
N2 C7 C8 115.08(12) . . ?
N5 C8 C9 121.54(15) . . ?
N5 C8 C7 116.36(14) . . ?
C9 C8 C7 122.10(14) . . ?
C10 C9 C8 120.28(16) . . ?
C11 C10 C9 118.18(16) . . ?
C12 C11 C10 118.90(16) . . ?
N5 C12 C11 123.46(16) . . ?
N3 C13 C14 111.09(13) . . ?
N6 C14 C15 121.98(16) . . ?
N6 C14 C13 116.25(13) . . ?
C15 C14 C13 121.74(15) . . ?
C16 C15 C14 119.58(18) . . ?
C17 C16 C15 118.57(18) . . ?
C16 C17 C18 119.28(19) . . ?
N6 C18 C17 123.03(18) . . ?
N4 C19 C20 114.20(13) . . ?
N7 C20 C21 122.51(16) . . ?
N7 C20 C19 116.03(14) . . ?
C21 C20 C19 121.46(15) . . ?
C22 C21 C20 119.38(16) . . ?
C23 C22 C21 118.57(17) . . ?
C22 C23 C24 118.22(17) . . ?
N7 C24 C23 124.06(16) . . ?

_refine_diff_density_max         0.698
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.063


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl Ether'
####################################################################### 
# 
# 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_jyy18
_database_code_depnum_ccdc_archive 'CCDC 1827011'
_audit_update_record             
;
2018-03-02 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[NiTPAP(COD)]'
_chemical_name_common            '[NiTPAP(COD)]'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H42 N7 Ni P'
_chemical_formula_weight         614.40

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   9.5307(6)
_cell_length_b                   28.5152(19)
_cell_length_c                   11.3412(8)
_cell_angle_alpha                90
_cell_angle_beta                 106.0248(9)
_cell_angle_gamma                90
_cell_volume                     2962.4(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    7495
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      25.84

_exptl_crystal_description       prism
_exptl_crystal_colour            green
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             1304
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.125
_exptl_absorpt_coefficient_mu    0.744
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7475
_exptl_absorpt_correction_T_max  0.8013
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
32647 Corrected reflections written to file jyy18s.hkl 
Estimated minimum and maximum transmission:  0.7475  0.8013 
The ratio (0.9329) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.1500 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32225
_diffrn_reflns_av_unetI/netI     0.0318
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.428
_diffrn_reflns_theta_max         26.412
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6048
_reflns_number_gt                4981
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A green crystal of approximate dimensions 0.125 x 0.137 x 0.182 mm was 
mounted on a glass fiber and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (35 sec/frame scan time for 
a sphere of diffraction data).  The raw frame data was processed using 
SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  The diffraction 
symmetry was 2/m and the systematic absences were consistent with the 
monoclinic space group P21/c that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering factors 
for neutral atoms were used throughout the analysis.  Hydrogen atoms 
were included using a riding model.

Least-squares analysis yielded wR2 = 0.0819 and Goof = 1.042 for 370 
variables refined against 6048 data (0.80 Å), R1 = 0.0331 for those 
4981 data with I > 2.0sigma(I).  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0380P)²+1.3668P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         6048
_refine_ls_number_parameters     370
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0449
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0819
_refine_ls_wR_factor_gt          0.0764
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.35188(3) 0.89633(2) 0.99843(2) 0.01682(8) Uani 1 1 d . . . . .
P1 P 0.48284(5) 0.86046(2) 0.89808(4) 0.01415(11) Uani 1 1 d . . . . .
N1 N 0.73824(17) 0.79882(6) 0.80617(15) 0.0194(4) Uani 1 1 d . . . . .
N2 N 0.66029(16) 0.86575(5) 0.98415(14) 0.0166(3) Uani 1 1 d . . . . .
N3 N 0.49972(17) 0.87680(5) 0.75881(14) 0.0167(3) Uani 1 1 d . . . . .
N4 N 0.45011(16) 0.80201(5) 0.87666(14) 0.0159(3) Uani 1 1 d . . . . .
N5 N 0.48947(18) 0.88367(6) 1.16361(15) 0.0197(4) Uani 1 1 d . . . . .
N6 N 0.2037(2) 0.92624(7) 0.50745(17) 0.0328(4) Uani 1 1 d . . . . .
N7 N 0.22274(19) 0.71654(6) 0.97890(16) 0.0284(4) Uani 1 1 d . . . . .
C1 C 0.8342(2) 0.81225(7) 0.92346(18) 0.0198(4) Uani 1 1 d . . . . .
H1A H 0.8942 0.8391 0.9108 0.024 Uiso 1 1 calc R U . . .
H1B H 0.9015 0.7858 0.9553 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7589(2) 0.82573(7) 1.02037(17) 0.0186(4) Uani 1 1 d . . . . .
H2A H 0.7026 0.7985 1.0367 0.022 Uiso 1 1 calc R U . . .
H2B H 0.8339 0.8335 1.0975 0.022 Uiso 1 1 calc R U . . .
C3 C 0.7074(2) 0.83178(7) 0.70600(18) 0.0205(4) Uani 1 1 d . . . . .
H3A H 0.6409 0.8165 0.6335 0.025 Uiso 1 1 calc R U . . .
H3B H 0.7997 0.8386 0.6855 0.025 Uiso 1 1 calc R U . . .
C4 C 0.6386(2) 0.87877(7) 0.72737(18) 0.0191(4) Uani 1 1 d . . . . .
H4A H 0.7099 0.8956 0.7941 0.023 Uiso 1 1 calc R U . . .
H4B H 0.6238 0.8979 0.6521 0.023 Uiso 1 1 calc R U . . .
C5 C 0.6408(2) 0.75958(7) 0.80042(18) 0.0210(4) Uani 1 1 d . . . . .
H5A H 0.6731 0.7417 0.8781 0.025 Uiso 1 1 calc R U . . .
H5B H 0.6488 0.7385 0.7332 0.025 Uiso 1 1 calc R U . . .
C6 C 0.4818(2) 0.77306(7) 0.77967(18) 0.0186(4) Uani 1 1 d . . . . .
H6A H 0.4493 0.7903 0.7011 0.022 Uiso 1 1 calc R U . . .
H6B H 0.4231 0.7440 0.7711 0.022 Uiso 1 1 calc R U . . .
C7 C 0.6854(2) 0.90431(7) 1.07293(17) 0.0184(4) Uani 1 1 d . . . . .
H7A H 0.6324 0.9325 1.0331 0.022 Uiso 1 1 calc R U . . .
H7B H 0.7909 0.9119 1.0992 0.022 Uiso 1 1 calc R U . . .
C8 C 0.6351(2) 0.89199(7) 1.18390(18) 0.0196(4) Uani 1 1 d . . . . .
C9 C 0.7333(2) 0.88705(7) 1.29894(19) 0.0241(5) Uani 1 1 d . . . . .
H9A H 0.8336 0.8942 1.3106 0.029 Uiso 1 1 calc R U . . .
C10 C 0.6848(3) 0.87169(8) 1.3971(2) 0.0300(5) Uani 1 1 d . . . . .
H10A H 0.7509 0.8675 1.4760 0.036 Uiso 1 1 calc R U . . .
C11 C 0.5378(3) 0.86265(8) 1.37668(19) 0.0297(5) Uani 1 1 d . . . . .
H11A H 0.5009 0.8519 1.4416 0.036 Uiso 1 1 calc R U . . .
C12 C 0.4451(2) 0.86936(7) 1.26097(19) 0.0254(5) Uani 1 1 d . . . . .
H12A H 0.3440 0.8636 1.2490 0.031 Uiso 1 1 calc R U . . .
C13 C 0.3656(2) 0.87871(7) 0.65989(17) 0.0184(4) Uani 1 1 d . . . . .
H13A H 0.2842 0.8685 0.6923 0.022 Uiso 1 1 calc R U . . .
H13B H 0.3731 0.8559 0.5961 0.022 Uiso 1 1 calc R U . . .
C14 C 0.3275(2) 0.92613(7) 0.59982(18) 0.0200(4) Uani 1 1 d . . . . .
C15 C 0.4112(2) 0.96593(7) 0.63678(19) 0.0239(4) Uani 1 1 d . . . . .
H15A H 0.4982 0.9645 0.7025 0.029 Uiso 1 1 calc R U . . .
C16 C 0.3662(3) 1.00780(8) 0.5764(2) 0.0323(5) Uani 1 1 d . . . . .
H16A H 0.4221 1.0356 0.5997 0.039 Uiso 1 1 calc R U . . .
C17 C 0.2393(3) 1.00861(9) 0.4823(2) 0.0405(6) Uani 1 1 d . . . . .
H17A H 0.2053 1.0369 0.4396 0.049 Uiso 1 1 calc R U . . .
C18 C 0.1628(3) 0.96747(9) 0.4516(2) 0.0406(6) Uani 1 1 d . . . . .
H18A H 0.0752 0.9683 0.3865 0.049 Uiso 1 1 calc R U . . .
C19 C 0.3955(2) 0.77628(7) 0.96462(17) 0.0191(4) Uani 1 1 d . . . . .
H19A H 0.3831 0.7983 1.0284 0.023 Uiso 1 1 calc R U . . .
H19B H 0.4695 0.7528 1.0054 0.023 Uiso 1 1 calc R U . . .
C20 C 0.2518(2) 0.75134(7) 0.91021(18) 0.0191(4) Uani 1 1 d . . . . .
C21 C 0.1562(2) 0.76443(7) 0.79847(18) 0.0202(4) Uani 1 1 d . . . . .
H21A H 0.1819 0.7885 0.7504 0.024 Uiso 1 1 calc R U . . .
C22 C 0.0237(2) 0.74185(7) 0.75869(19) 0.0235(4) Uani 1 1 d . . . . .
H22A H -0.0438 0.7503 0.6832 0.028 Uiso 1 1 calc R U . . .
C23 C -0.0093(2) 0.70667(7) 0.8305(2) 0.0271(5) Uani 1 1 d . . . . .
H23A H -0.1005 0.6909 0.8062 0.033 Uiso 1 1 calc R U . . .
C24 C 0.0931(2) 0.69509(8) 0.9378(2) 0.0327(5) Uani 1 1 d . . . . .
H24A H 0.0708 0.6704 0.9859 0.039 Uiso 1 1 calc R U . . .
C25 C 0.3028(2) 0.96388(7) 0.91653(19) 0.0224(4) Uani 1 1 d . . . . .
H25A H 0.3781 0.9766 0.8787 0.027 Uiso 1 1 calc R U . . .
C26 C 0.3384(2) 0.96760(7) 1.0427(2) 0.0229(4) Uani 1 1 d . . . . .
H26A H 0.4350 0.9828 1.0804 0.028 Uiso 1 1 calc R U . . .
C27 C 0.2319(2) 0.97105(8) 1.1194(2) 0.0285(5) Uani 1 1 d . . . . .
H27A H 0.1903 1.0031 1.1116 0.034 Uiso 1 1 calc R U . . .
H27B H 0.2853 0.9661 1.2067 0.034 Uiso 1 1 calc R U . . .
C28 C 0.1061(2) 0.93523(8) 1.0824(2) 0.0285(5) Uani 1 1 d . . . . .
H28A H 0.0703 0.9283 1.1546 0.034 Uiso 1 1 calc R U . . .
H28B H 0.0245 0.9493 1.0184 0.034 Uiso 1 1 calc R U . . .
C29 C 0.1517(2) 0.88952(7) 1.0337(2) 0.0242(5) Uani 1 1 d . . . . .
H29A H 0.1408 0.8609 1.0813 0.029 Uiso 1 1 calc R U . . .
C30 C 0.1384(2) 0.88180(7) 0.9100(2) 0.0229(4) Uani 1 1 d . . . . .
H30A H 0.1199 0.8483 0.8840 0.027 Uiso 1 1 calc R U . . .
C31 C 0.0749(2) 0.91703(8) 0.8093(2) 0.0263(5) Uani 1 1 d . . . . .
H31A H -0.0309 0.9204 0.8004 0.032 Uiso 1 1 calc R U . . .
H31B H 0.0864 0.9048 0.7308 0.032 Uiso 1 1 calc R U . . .
C32 C 0.1475(2) 0.96562(8) 0.8340(2) 0.0279(5) Uani 1 1 d . . . . .
H32A H 0.1481 0.9801 0.7548 0.034 Uiso 1 1 calc R U . . .
H32B H 0.0883 0.9859 0.8726 0.034 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N5 2.0008(17) . ?
Ni1 C30 2.047(2) . ?
Ni1 C29 2.0636(19) . ?
Ni1 C26 2.1057(19) . ?
Ni1 C25 2.134(2) . ?
Ni1 P1 2.1642(5) . ?
P1 N3 1.6965(16) . ?
P1 N4 1.7007(16) . ?
P1 N2 1.7101(16) . ?
P1 N1 3.3915(17) . ?
N1 C3 1.441(2) . ?
N1 C1 1.443(2) . ?
N1 C5 1.444(2) . ?
N2 C2 1.463(2) . ?
N2 C7 1.465(2) . ?
N3 C13 1.450(2) . ?
N3 C4 1.464(2) . ?
N4 C19 1.446(2) . ?
N4 C6 1.472(2) . ?
N5 C12 1.350(3) . ?
N5 C8 1.363(3) . ?
N6 C18 1.341(3) . ?
N6 C14 1.344(3) . ?
N7 C20 1.337(3) . ?
N7 C24 1.341(3) . ?
C1 C2 1.519(3) . ?
C3 C4 1.540(3) . ?
C5 C6 1.518(3) . ?
C7 C8 1.507(3) . ?
C8 C9 1.387(3) . ?
C9 C10 1.389(3) . ?
C10 C11 1.380(3) . ?
C11 C12 1.378(3) . ?
C13 C14 1.513(3) . ?
C14 C15 1.384(3) . ?
C15 C16 1.384(3) . ?
C16 C17 1.375(3) . ?
C17 C18 1.374(4) . ?
C19 C20 1.515(3) . ?
C20 C21 1.392(3) . ?
C21 C22 1.378(3) . ?
C22 C23 1.382(3) . ?
C23 C24 1.374(3) . ?
C25 C26 1.381(3) . ?
C25 C32 1.519(3) . ?
C26 C27 1.512(3) . ?
C27 C28 1.543(3) . ?
C28 C29 1.525(3) . ?
C29 C30 1.391(3) . ?
C30 C31 1.516(3) . ?
C31 C32 1.539(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Ni1 C30 136.72(8) . . ?
N5 Ni1 C29 101.74(8) . . ?
C30 Ni1 C29 39.55(8) . . ?
N5 Ni1 C26 91.04(7) . . ?
C30 Ni1 C26 101.22(8) . . ?
C29 Ni1 C26 85.65(8) . . ?
N5 Ni1 C25 125.36(7) . . ?
C30 Ni1 C25 84.31(8) . . ?
C29 Ni1 C25 93.80(8) . . ?
C26 Ni1 C25 38.00(8) . . ?
N5 Ni1 P1 94.76(5) . . ?
C30 Ni1 P1 106.64(6) . . ?
C29 Ni1 P1 139.09(6) . . ?
C26 Ni1 P1 131.56(6) . . ?
C25 Ni1 P1 106.66(6) . . ?
N3 P1 N4 101.36(8) . . ?
N3 P1 N2 100.03(8) . . ?
N4 P1 N2 106.35(8) . . ?
N3 P1 Ni1 125.20(6) . . ?
N4 P1 Ni1 115.38(6) . . ?
N2 P1 Ni1 106.33(6) . . ?
N3 P1 N1 66.15(6) . . ?
N4 P1 N1 64.35(6) . . ?
N2 P1 N1 62.65(6) . . ?
Ni1 P1 N1 166.82(3) . . ?
C3 N1 C1 119.56(16) . . ?
C3 N1 C5 118.75(16) . . ?
C1 N1 C5 118.92(16) . . ?
C3 N1 P1 84.06(10) . . ?
C1 N1 P1 84.56(10) . . ?
C5 N1 P1 84.74(10) . . ?
C2 N2 C7 114.96(15) . . ?
C2 N2 P1 123.28(13) . . ?
C7 N2 P1 113.99(12) . . ?
C13 N3 C4 118.23(15) . . ?
C13 N3 P1 116.15(12) . . ?
C4 N3 P1 124.18(13) . . ?
C19 N4 C6 114.71(15) . . ?
C19 N4 P1 119.05(12) . . ?
C6 N4 P1 126.10(12) . . ?
C12 N5 C8 116.66(18) . . ?
C12 N5 Ni1 123.23(14) . . ?
C8 N5 Ni1 120.01(13) . . ?
C18 N6 C14 116.6(2) . . ?
C20 N7 C24 117.08(18) . . ?
N1 C1 C2 115.35(15) . . ?
N2 C2 C1 112.92(16) . . ?
N1 C3 C4 116.53(16) . . ?
N3 C4 C3 117.24(16) . . ?
N1 C5 C6 114.40(16) . . ?
N4 C6 C5 115.35(16) . . ?
N2 C7 C8 111.69(15) . . ?
N5 C8 C9 122.17(19) . . ?
N5 C8 C7 116.33(17) . . ?
C9 C8 C7 121.42(18) . . ?
C8 C9 C10 119.9(2) . . ?
C11 C10 C9 118.2(2) . . ?
C12 C11 C10 119.2(2) . . ?
N5 C12 C11 123.9(2) . . ?
N3 C13 C14 115.65(16) . . ?
N6 C14 C15 122.87(19) . . ?
N6 C14 C13 113.78(17) . . ?
C15 C14 C13 123.34(18) . . ?
C14 C15 C16 118.9(2) . . ?
C17 C16 C15 119.0(2) . . ?
C18 C17 C16 118.3(2) . . ?
N6 C18 C17 124.3(2) . . ?
N4 C19 C20 114.47(16) . . ?
N7 C20 C21 122.72(18) . . ?
N7 C20 C19 114.86(17) . . ?
C21 C20 C19 122.41(17) . . ?
C22 C21 C20 118.90(18) . . ?
C21 C22 C23 118.90(19) . . ?
C24 C23 C22 118.37(19) . . ?
N7 C24 C23 124.0(2) . . ?
C26 C25 C32 123.73(19) . . ?
C26 C25 Ni1 69.90(12) . . ?
C32 C25 Ni1 110.91(13) . . ?
C25 C26 C27 126.14(19) . . ?
C25 C26 Ni1 72.09(11) . . ?
C27 C26 Ni1 107.15(14) . . ?
C26 C27 C28 113.27(17) . . ?
C29 C28 C27 112.76(16) . . ?
C30 C29 C28 123.0(2) . . ?
C30 C29 Ni1 69.57(11) . . ?
C28 C29 Ni1 111.16(14) . . ?
C29 C30 C31 124.14(19) . . ?
C29 C30 Ni1 70.88(12) . . ?
C31 C30 Ni1 111.77(13) . . ?
C30 C31 C32 113.17(17) . . ?
C25 C32 C31 113.29(17) . . ?

_refine_diff_density_max         0.400
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Diethyl Ether'
####################################################################### 
# 
# 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_jyy24
_database_code_depnum_ccdc_archive 'CCDC 1827013'
_audit_update_record             
;
2018-03-02 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[PdTPAP(CH3CN)][BF4]2 '
_chemical_name_common            '[PdTPAP(CH3CN)][BF4]2'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 B2 F8 N9 P Pd'
_chemical_formula_weight         809.65

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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.9669(6)
_cell_length_b                   12.4170(7)
_cell_length_c                   25.3468(14)
_cell_angle_alpha                77.9589(6)
_cell_angle_beta                 87.3208(7)
_cell_angle_gamma                81.2206(7)
_cell_volume                     3335.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      28.61

_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_F_000             1640
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.136
_exptl_absorpt_coefficient_mu    0.685
_shelx_estimated_absorpt_T_min   0.766
_shelx_estimated_absorpt_T_max   0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7163
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
39746 Corrected reflections written to file jyy24s.hkl 
Estimated minimum and maximum transmission:  0.7163  0.8015 
The ratio (0.8937) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.1500 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            39746
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.643
_diffrn_reflns_theta_max         28.734
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.903
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.903
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             15613
_reflns_number_gt                13905
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
An orange crystal of approximate dimensions 0.136 x 0.265 x 0.410 mm was mounted 
on a glass fiber and transferred to a Bruker SMART APEX II diffractometer.  The 
APEX2 program package was used to determine the unit-cell parameters and for 
data collection (20 sec/frame scan time for a sphere of diffraction data).  The 
raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
There were no systematic absences nor any diffraction symmetry other than the 
Friedel condition.  The centrosymmetric triclinic space group P-1 was assigned and 
later determined to be correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis.  Hydrogen atoms were included using a riding 
model.  There were two molecules of the formula-unit present (Z = 4).  There was 
one molecule of acetonitrile solvent present per formula-unit.  
Atoms C(54), F(5), F(6), F(7) and F(8) were disordered and included using multiple 
components with partial site-occupancy-factors.

Least-squares analysis yielded wR2 = 0.0682 and Goof = 1.042 for 934 variables 
refined against 15613 data (0.74 Å), R1 = 0.0288 for those 13905 data 
with I > 2.0sigma(I).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0260P)²+3.2106P] 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         15613
_refine_ls_number_parameters     934
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0340
_refine_ls_R_factor_gt           0.0288
_refine_ls_wR_factor_ref         0.0682
_refine_ls_wR_factor_gt          0.0659
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.82222(2) 1.28812(2) 0.12297(2) 0.01601(4) Uani 1 1 d . . . . .
P1 P 0.67601(4) 1.40404(4) 0.15513(2) 0.01616(10) Uani 1 1 d . . . . .
N1 N 0.48841(15) 1.53824(15) 0.18939(7) 0.0224(4) Uani 1 1 d . . . . .
N2 N 0.72022(15) 1.53009(14) 0.14304(7) 0.0198(3) Uani 1 1 d . . . . .
N3 N 0.65825(15) 1.35402(14) 0.22031(6) 0.0196(3) Uani 1 1 d . . . . .
N4 N 0.55459(14) 1.40109(14) 0.11912(7) 0.0183(3) Uani 1 1 d . . . . .
N5 N 0.83707(14) 1.41477(14) 0.05751(6) 0.0185(3) Uani 1 1 d . . . . .
N6 N 0.79823(15) 1.15608(14) 0.18565(6) 0.0183(3) Uani 1 1 d . . . . .
N7 N 0.65160(17) 1.20691(18) 0.06169(8) 0.0330(5) Uani 1 1 d . . . . .
N8 N 0.96753(16) 1.18528(14) 0.08836(7) 0.0223(4) Uani 1 1 d . . . . .
C1 C 0.54298(19) 1.64031(17) 0.17876(9) 0.0248(4) Uani 1 1 d . . . . .
H1A H 0.5156 1.6845 0.2066 0.030 Uiso 1 1 calc R U . . .
H1B H 0.5174 1.6858 0.1430 0.030 Uiso 1 1 calc R U . . .
C2 C 0.68187(19) 1.60780(18) 0.17992(9) 0.0247(4) Uani 1 1 d . . . . .
H2A H 0.7223 1.6752 0.1686 0.030 Uiso 1 1 calc R U . . .
H2B H 0.7078 1.5717 0.2171 0.030 Uiso 1 1 calc R U . . .
C3 C 0.48159(19) 1.47918(19) 0.24481(8) 0.0257(4) Uani 1 1 d . . . . .
H3A H 0.3946 1.4842 0.2575 0.031 Uiso 1 1 calc R U . . .
H3B H 0.5281 1.5127 0.2682 0.031 Uiso 1 1 calc R U . . .
C4 C 0.53655(18) 1.35788(18) 0.24785(8) 0.0233(4) Uani 1 1 d . . . . .
H4A H 0.5457 1.3188 0.2860 0.028 Uiso 1 1 calc R U . . .
H4B H 0.4814 1.3205 0.2302 0.028 Uiso 1 1 calc R U . . .
C5 C 0.39362(18) 1.53073(19) 0.15256(9) 0.0244(4) Uani 1 1 d . . . . .
H5A H 0.3395 1.6031 0.1426 0.029 Uiso 1 1 calc R U . . .
H5B H 0.3422 1.4735 0.1696 0.029 Uiso 1 1 calc R U . . .
C6 C 0.46139(18) 1.49868(18) 0.10261(8) 0.0230(4) Uani 1 1 d . . . . .
H6A H 0.4017 1.4819 0.0784 0.028 Uiso 1 1 calc R U . . .
H6B H 0.5014 1.5616 0.0826 0.028 Uiso 1 1 calc R U . . .
C7 C 0.84503(18) 1.53924(18) 0.11837(8) 0.0220(4) Uani 1 1 d . . . . .
H7A H 0.9074 1.4839 0.1402 0.026 Uiso 1 1 calc R U . . .
H7B H 0.8658 1.6144 0.1177 0.026 Uiso 1 1 calc R U . . .
C8 C 0.84698(17) 1.51909(17) 0.06230(8) 0.0196(4) Uani 1 1 d . . . . .
C9 C 0.85787(18) 1.60235(18) 0.01730(9) 0.0246(4) Uani 1 1 d . . . . .
H9A H 0.8659 1.6752 0.0215 0.030 Uiso 1 1 calc R U . . .
C10 C 0.85700(19) 1.57926(18) -0.03373(9) 0.0262(5) Uani 1 1 d . . . . .
H10A H 0.8643 1.6357 -0.0649 0.031 Uiso 1 1 calc R U . . .
C11 C 0.84525(18) 1.47215(18) -0.03845(8) 0.0248(4) Uani 1 1 d . . . . .
H11A H 0.8438 1.4540 -0.0730 0.030 Uiso 1 1 calc R U . . .
C12 C 0.83561(18) 1.39197(18) 0.00792(8) 0.0224(4) Uani 1 1 d . . . . .
H12A H 0.8277 1.3185 0.0046 0.027 Uiso 1 1 calc R U . . .
C13 C 0.76444(18) 1.28153(17) 0.24825(8) 0.0198(4) Uani 1 1 d . . . . .
H13A H 0.7550 1.2784 0.2876 0.024 Uiso 1 1 calc R U . . .
H13B H 0.8410 1.3129 0.2358 0.024 Uiso 1 1 calc R U . . .
C14 C 0.77476(17) 1.16579(17) 0.23746(8) 0.0195(4) Uani 1 1 d . . . . .
C15 C 0.7567(2) 1.07489(18) 0.27723(8) 0.0252(4) Uani 1 1 d . . . . .
H15A H 0.7411 1.0832 0.3135 0.030 Uiso 1 1 calc R U . . .
C16 C 0.7614(2) 0.97147(19) 0.26406(9) 0.0299(5) Uani 1 1 d . . . . .
H16A H 0.7480 0.9084 0.2910 0.036 Uiso 1 1 calc R U . . .
C17 C 0.7859(2) 0.96142(18) 0.21118(9) 0.0274(5) Uani 1 1 d . . . . .
H17A H 0.7906 0.8913 0.2012 0.033 Uiso 1 1 calc R U . . .
C18 C 0.80355(19) 1.05531(17) 0.17304(8) 0.0229(4) Uani 1 1 d . . . . .
H18A H 0.8200 1.0485 0.1367 0.027 Uiso 1 1 calc R U . . .
C19 C 0.51387(18) 1.29144(17) 0.12383(8) 0.0211(4) Uani 1 1 d . . . . .
H19A H 0.4248 1.2980 0.1332 0.025 Uiso 1 1 calc R U . . .
H19B H 0.5587 1.2379 0.1536 0.025 Uiso 1 1 calc R U . . .
C20 C 0.53547(18) 1.24633(17) 0.07267(8) 0.0209(4) Uani 1 1 d . . . . .
C21 C 0.4381(2) 1.2443(2) 0.04029(10) 0.0352(5) Uani 1 1 d . . . . .
H21A H 0.3561 1.2717 0.0497 0.042 Uiso 1 1 calc R U . . .
C22 C 0.4619(2) 1.2016(2) -0.00600(11) 0.0441(7) Uani 1 1 d . . . . .
H22A H 0.3967 1.1995 -0.0290 0.053 Uiso 1 1 calc R U . . .
C23 C 0.5821(2) 1.1622(2) -0.01818(10) 0.0388(6) Uani 1 1 d . . . . .
H23A H 0.6018 1.1335 -0.0500 0.047 Uiso 1 1 calc R U . . .
C24 C 0.6726(2) 1.1655(2) 0.01676(11) 0.0399(6) Uani 1 1 d . . . . .
H24A H 0.7551 1.1367 0.0087 0.048 Uiso 1 1 calc R U . . .
C25 C 1.0481(2) 1.13755(17) 0.06929(9) 0.0265(4) Uani 1 1 d . . . . .
C26 C 1.1524(3) 1.0781(2) 0.04437(13) 0.0464(7) Uani 1 1 d . . . . .
H26A H 1.1399 1.0909 0.0054 0.070 Uiso 1 1 calc R U . . .
H26B H 1.1591 0.9983 0.0598 0.070 Uiso 1 1 calc R U . . .
H26C H 1.2284 1.1052 0.0511 0.070 Uiso 1 1 calc R U . . .
Pd2 Pd 1.22665(2) 0.69320(2) 0.38423(2) 0.01637(4) Uani 1 1 d . . . . .
P2 P 1.11612(4) 0.58813(4) 0.34939(2) 0.01517(9) Uani 1 1 d . . . . .
N9 N 0.97833(15) 0.45997(14) 0.31392(7) 0.0226(4) Uani 1 1 d . . . . .
N10 N 1.18156(15) 0.45807(13) 0.37019(7) 0.0206(3) Uani 1 1 d . . . . .
N11 N 1.12080(15) 0.62799(13) 0.28233(6) 0.0185(3) Uani 1 1 d . . . . .
N12 N 0.97511(15) 0.61671(14) 0.37405(7) 0.0192(3) Uani 1 1 d . . . . .
N13 N 1.29369(14) 0.56295(14) 0.44590(6) 0.0181(3) Uani 1 1 d . . . . .
N14 N 1.15439(15) 0.82584(14) 0.32685(7) 0.0225(4) Uani 1 1 d . . . . .
N15 N 1.0100(2) 0.73031(17) 0.48855(8) 0.0351(5) Uani 1 1 d . . . . .
N16 N 1.32949(16) 0.80050(14) 0.41501(7) 0.0216(3) Uani 1 1 d . . . . .
C27 C 1.0434(2) 0.35115(17) 0.33826(9) 0.0255(4) Uani 1 1 d . . . . .
H27A H 1.1041 0.3232 0.3123 0.031 Uiso 1 1 calc R U . . .
H27B H 0.9845 0.2972 0.3492 0.031 Uiso 1 1 calc R U . . .
C28 C 1.1086(2) 0.36628(17) 0.38739(9) 0.0258(4) Uani 1 1 d . . . . .
H28A H 1.0472 0.3839 0.4154 0.031 Uiso 1 1 calc R U . . .
H28B H 1.1633 0.2968 0.4028 0.031 Uiso 1 1 calc R U . . .
C29 C 0.99507(18) 0.50074(18) 0.25656(8) 0.0224(4) Uani 1 1 d . . . . .
H29A H 0.9268 0.5605 0.2428 0.027 Uiso 1 1 calc R U . . .
H29B H 0.9953 0.4397 0.2369 0.027 Uiso 1 1 calc R U . . .
C30 C 1.11697(19) 0.54527(18) 0.24790(8) 0.0230(4) Uani 1 1 d . . . . .
H30A H 1.1857 0.4833 0.2572 0.028 Uiso 1 1 calc R U . . .
H30B H 1.1268 0.5809 0.2095 0.028 Uiso 1 1 calc R U . . .
C31 C 0.85990(19) 0.49584(19) 0.33747(9) 0.0270(5) Uani 1 1 d . . . . .
H31A H 0.8471 0.4464 0.3727 0.032 Uiso 1 1 calc R U . . .
H31B H 0.7921 0.4945 0.3133 0.032 Uiso 1 1 calc R U . . .
C32 C 0.86329(18) 0.61386(18) 0.34469(9) 0.0246(4) Uani 1 1 d . . . . .
H32A H 0.8634 0.6647 0.3090 0.030 Uiso 1 1 calc R U . . .
H32B H 0.7891 0.6392 0.3651 0.030 Uiso 1 1 calc R U . . .
C33 C 1.31290(18) 0.43875(17) 0.38296(8) 0.0216(4) Uani 1 1 d . . . . .
H33A H 1.3571 0.4894 0.3560 0.026 Uiso 1 1 calc R U . . .
H33B H 1.3479 0.3612 0.3812 0.026 Uiso 1 1 calc R U . . .
C34 C 1.33139(17) 0.45857(17) 0.43859(8) 0.0187(4) Uani 1 1 d . . . . .
C35 C 1.37887(19) 0.37431(18) 0.48033(8) 0.0240(4) Uani 1 1 d . . . . .
H35A H 1.4047 0.3012 0.4743 0.029 Uiso 1 1 calc R U . . .
C36 C 1.38862(19) 0.39728(19) 0.53122(8) 0.0265(5) Uani 1 1 d . . . . .
H36A H 1.4214 0.3404 0.5603 0.032 Uiso 1 1 calc R U . . .
C37 C 1.34984(18) 0.50405(19) 0.53869(8) 0.0249(4) Uani 1 1 d . . . . .
H37A H 1.3557 0.5219 0.5731 0.030 Uiso 1 1 calc R U . . .
C38 C 1.30224(18) 0.58488(18) 0.49544(8) 0.0212(4) Uani 1 1 d . . . . .
H38A H 1.2747 0.6582 0.5008 0.025 Uiso 1 1 calc R U . . .
C39 C 1.20144(19) 0.71233(17) 0.25920(8) 0.0233(4) Uani 1 1 d . . . . .
H39A H 1.2043 0.7218 0.2194 0.028 Uiso 1 1 calc R U . . .
H39B H 1.2863 0.6858 0.2726 0.028 Uiso 1 1 calc R U . . .
C40 C 1.15572(19) 0.82199(17) 0.27404(9) 0.0244(4) Uani 1 1 d . . . . .
C41 C 1.1160(2) 0.91603(19) 0.23534(11) 0.0344(5) Uani 1 1 d . . . . .
H41A H 1.1169 0.9121 0.1983 0.041 Uiso 1 1 calc R U . . .
C42 C 1.0752(2) 1.0154(2) 0.25114(13) 0.0443(7) Uani 1 1 d . . . . .
H42A H 1.0501 1.0811 0.2250 0.053 Uiso 1 1 calc R U . . .
C43 C 1.0713(2) 1.01822(19) 0.30519(13) 0.0423(7) Uani 1 1 d . . . . .
H43A H 1.0420 1.0856 0.3169 0.051 Uiso 1 1 calc R U . . .
C44 C 1.1104(2) 0.92181(19) 0.34228(11) 0.0330(5) Uani 1 1 d . . . . .
H44A H 1.1061 0.9234 0.3796 0.040 Uiso 1 1 calc R U . . .
C45 C 0.96262(19) 0.60924(17) 0.43252(8) 0.0215(4) Uani 1 1 d . . . . .
H45A H 1.0389 0.5662 0.4499 0.026 Uiso 1 1 calc R U . . .
H45B H 0.8935 0.5678 0.4463 0.026 Uiso 1 1 calc R U . . .
C46 C 0.93948(19) 0.72152(18) 0.44869(8) 0.0222(4) Uani 1 1 d . . . . .
C47 C 0.8509(2) 0.8064(2) 0.42498(12) 0.0408(6) Uani 1 1 d . . . . .
H47A H 0.8038 0.7975 0.3960 0.049 Uiso 1 1 calc R U . . .
C48 C 0.8310(2) 0.9044(2) 0.44362(13) 0.0452(7) Uani 1 1 d . . . . .
H48A H 0.7710 0.9644 0.4275 0.054 Uiso 1 1 calc R U . . .
C49 C 0.8996(3) 0.9136(2) 0.48590(11) 0.0425(6) Uani 1 1 d . . . . .
H49A H 0.8859 0.9787 0.5007 0.051 Uiso 1 1 calc R U . . .
C50 C 0.9888(3) 0.8261(2) 0.50634(11) 0.0481(7) Uani 1 1 d . . . . .
H50A H 1.0382 0.8340 0.5347 0.058 Uiso 1 1 calc R U . . .
C51 C 1.3920(2) 0.85336(17) 0.42920(8) 0.0241(4) Uani 1 1 d . . . . .
C52 C 1.4745(3) 0.9186(2) 0.44781(11) 0.0393(6) Uani 1 1 d . . . . .
H52A H 1.5056 0.8802 0.4835 0.059 Uiso 1 1 calc R U . . .
H52B H 1.4294 0.9920 0.4502 0.059 Uiso 1 1 calc R U . . .
H52C H 1.5440 0.9276 0.4223 0.059 Uiso 1 1 calc R U . . .
N17 N 0.6104(4) 0.9109(3) 0.10633(15) 0.0888(12) Uani 1 1 d . . . . .
C53 C 0.5330(5) 0.9396(3) 0.13370(15) 0.0692(11) Uani 1 1 d . . . . .
C54 C 0.4617(8) 0.9823(8) 0.1725(4) 0.076(3) Uani 0.53 1 d . . P A 1
H54A H 0.4258 0.9224 0.1966 0.113 Uiso 0.53 1 calc R U P A 1
H54B H 0.3954 1.0390 0.1552 0.113 Uiso 0.53 1 calc R U P A 1
H54C H 0.5129 1.0160 0.1933 0.113 Uiso 0.53 1 calc R U P A 1
C54B C 0.4026(11) 0.9542(9) 0.1648(4) 0.075(3) Uani 0.47 1 d . . P A 2
H54D H 0.3461 0.9121 0.1516 0.112 Uiso 0.47 1 calc R U P A 2
H54E H 0.3675 1.0332 0.1583 0.112 Uiso 0.47 1 calc R U P A 2
H54F H 0.4145 0.9262 0.2036 0.112 Uiso 0.47 1 calc R U P A 2
N18 N 1.2750(3) 0.1275(3) 0.37915(14) 0.0743(9) Uani 1 1 d . . . . .
C55 C 1.3327(3) 0.1041(2) 0.34388(14) 0.0473(7) Uani 1 1 d . . . . .
C56 C 1.4066(3) 0.0705(2) 0.30030(13) 0.0516(7) Uani 1 1 d . . . . .
H56A H 1.4895 0.0902 0.3015 0.077 Uiso 1 1 calc R U . . .
H56B H 1.3685 0.1086 0.2659 0.077 Uiso 1 1 calc R U . . .
H56C H 1.4123 -0.0101 0.3037 0.077 Uiso 1 1 calc R U . . .
B1 B 0.1723(2) 1.2881(2) 0.18515(10) 0.0240(5) Uani 1 1 d . . . . .
F1 F 0.21748(13) 1.21371(12) 0.15218(6) 0.0410(3) Uani 1 1 d . . . . .
F2 F 0.05934(12) 1.26514(11) 0.20713(7) 0.0396(3) Uani 1 1 d . . . . .
F3 F 0.25507(14) 1.28114(13) 0.22570(6) 0.0433(4) Uani 1 1 d . . . . .
F4 F 0.15730(15) 1.39601(11) 0.15495(5) 0.0394(3) Uani 1 1 d . . . . .
B2 B 1.0399(4) 1.8058(2) 0.10538(12) 0.0448(8) Uani 1 1 d . . . . .
F5 F 0.9761(5) 1.7469(5) 0.15056(17) 0.0539(13) Uani 0.620(15) 1 d . . P B 1
F6 F 1.0179(5) 1.7640(6) 0.0615(2) 0.0578(14) Uani 0.620(15) 1 d . . P B 1
F7 F 1.1667(10) 1.7978(9) 0.1142(4) 0.102(3) Uani 0.620(15) 1 d . . P B 1
F8 F 0.9728(5) 1.9149(4) 0.0967(4) 0.0548(16) Uani 0.620(15) 1 d . . P B 1
F5B F 1.0353(16) 1.7065(8) 0.1327(5) 0.084(5) Uani 0.380(15) 1 d . . P B 2
F6B F 1.0519(10) 1.8130(10) 0.0485(3) 0.061(3) Uani 0.380(15) 1 d . . P B 2
F7B F 1.1632(13) 1.8148(8) 0.1151(4) 0.051(3) Uani 0.380(15) 1 d . . P B 2
F8B F 0.9989(10) 1.8941(10) 0.1191(4) 0.061(2) Uani 0.380(15) 1 d . . P B 2
B3 B 0.6707(3) 0.2127(2) 0.40298(10) 0.0318(6) Uani 1 1 d . . . . .
F9 F 0.79122(15) 0.19671(15) 0.38398(6) 0.0497(4) Uani 1 1 d . . . . .
F10 F 0.61693(19) 0.31968(13) 0.38073(7) 0.0587(5) Uani 1 1 d . . . . .
F11 F 0.6712(2) 0.19646(16) 0.45827(6) 0.0670(6) Uani 1 1 d . . . . .
F12 F 0.60853(15) 0.13627(14) 0.38742(7) 0.0503(4) Uani 1 1 d . . . . .
B4 B 1.5540(2) 0.74630(19) 0.31325(9) 0.0220(5) Uani 1 1 d . . . . .
F13 F 1.44409(11) 0.80464(11) 0.29043(5) 0.0322(3) Uani 1 1 d . . . . .
F14 F 1.64332(12) 0.74067(13) 0.27286(5) 0.0357(3) Uani 1 1 d . . . . .
F15 F 1.53549(15) 0.64025(11) 0.33930(6) 0.0418(4) Uani 1 1 d . . . . .
F16 F 1.59350(11) 0.80202(10) 0.35060(5) 0.0257(3) 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
Pd1 N5 2.0535(16) . ?
Pd1 N6 2.0706(16) . ?
Pd1 N8 2.1577(17) . ?
Pd1 P1 2.2294(5) . ?
P1 N3 1.6528(17) . ?
P1 N4 1.6583(16) . ?
P1 N2 1.6722(17) . ?
P1 N1 2.6747(18) . ?
N1 C3 1.447(3) . ?
N1 C1 1.453(3) . ?
N1 C5 1.455(3) . ?
N2 C2 1.482(2) . ?
N2 C7 1.488(2) . ?
N3 C13 1.469(2) . ?
N3 C4 1.476(2) . ?
N4 C6 1.462(3) . ?
N4 C19 1.477(2) . ?
N5 C12 1.346(3) . ?
N5 C8 1.347(3) . ?
N6 C18 1.347(3) . ?
N6 C14 1.353(2) . ?
N7 C20 1.331(3) . ?
N7 C24 1.341(3) . ?
N8 C25 1.134(3) . ?
C1 C2 1.515(3) . ?
C3 C4 1.522(3) . ?
C5 C6 1.531(3) . ?
C7 C8 1.492(3) . ?
C8 C9 1.385(3) . ?
C9 C10 1.383(3) . ?
C10 C11 1.386(3) . ?
C11 C12 1.384(3) . ?
C13 C14 1.505(3) . ?
C14 C15 1.380(3) . ?
C15 C16 1.386(3) . ?
C16 C17 1.382(3) . ?
C17 C18 1.383(3) . ?
C19 C20 1.512(3) . ?
C20 C21 1.383(3) . ?
C21 C22 1.384(3) . ?
C22 C23 1.379(4) . ?
C23 C24 1.371(4) . ?
C25 C26 1.456(3) . ?
Pd2 N14 2.0410(17) . ?
Pd2 N13 2.0711(16) . ?
Pd2 N16 2.1517(17) . ?
Pd2 P2 2.2394(5) . ?
P2 N10 1.6515(17) . ?
P2 N12 1.6561(17) . ?
P2 N11 1.6691(17) . ?
P2 N9 2.6613(18) . ?
N9 C29 1.449(3) . ?
N9 C31 1.450(3) . ?
N9 C27 1.454(3) . ?
N10 C33 1.464(3) . ?
N10 C28 1.472(3) . ?
N11 C39 1.483(2) . ?
N11 C30 1.486(2) . ?
N12 C45 1.467(2) . ?
N12 C32 1.473(2) . ?
N13 C34 1.347(3) . ?
N13 C38 1.350(2) . ?
N14 C44 1.344(3) . ?
N14 C40 1.349(3) . ?
N15 C46 1.333(3) . ?
N15 C50 1.342(3) . ?
N16 C51 1.135(3) . ?
C27 C28 1.523(3) . ?
C29 C30 1.513(3) . ?
C31 C32 1.520(3) . ?
C33 C34 1.509(3) . ?
C34 C35 1.382(3) . ?
C35 C36 1.390(3) . ?
C36 C37 1.378(3) . ?
C37 C38 1.384(3) . ?
C39 C40 1.495(3) . ?
C40 C41 1.386(3) . ?
C41 C42 1.380(4) . ?
C42 C43 1.376(4) . ?
C43 C44 1.383(3) . ?
C45 C46 1.516(3) . ?
C46 C47 1.376(3) . ?
C47 C48 1.380(3) . ?
C48 C49 1.371(4) . ?
C49 C50 1.376(4) . ?
C51 C52 1.457(3) . ?
N17 C53 1.133(5) . ?
C53 C54 1.370(11) . ?
C53 C54B 1.605(13) . ?
N18 C55 1.133(4) . ?
C55 C56 1.434(4) . ?
B1 F2 1.380(3) . ?
B1 F3 1.383(3) . ?
B1 F4 1.387(3) . ?
B1 F1 1.393(3) . ?
B2 F8B 1.232(10) . ?
B2 F5B 1.290(6) . ?
B2 F6 1.369(5) . ?
B2 F7 1.404(11) . ?
B2 F7B 1.412(13) . ?
B2 F8 1.418(6) . ?
B2 F6B 1.427(7) . ?
B2 F5 1.438(5) . ?
B3 F11 1.374(3) . ?
B3 F12 1.378(3) . ?
B3 F10 1.382(3) . ?
B3 F9 1.386(3) . ?
B4 F15 1.385(3) . ?
B4 F14 1.389(3) . ?
B4 F13 1.391(3) . ?
B4 F16 1.402(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Pd1 N6 175.70(6) . . ?
N5 Pd1 N8 88.94(6) . . ?
N6 Pd1 N8 90.78(6) . . ?
N5 Pd1 P1 87.49(5) . . ?
N6 Pd1 P1 92.86(5) . . ?
N8 Pd1 P1 176.25(5) . . ?
N3 P1 N4 113.37(9) . . ?
N3 P1 N2 112.24(9) . . ?
N4 P1 N2 112.06(9) . . ?
N3 P1 Pd1 107.91(6) . . ?
N4 P1 Pd1 102.38(6) . . ?
N2 P1 Pd1 108.21(6) . . ?
N3 P1 N1 73.70(7) . . ?
N4 P1 N1 73.38(7) . . ?
N2 P1 N1 74.40(7) . . ?
Pd1 P1 N1 175.71(4) . . ?
C3 N1 C1 117.82(17) . . ?
C3 N1 C5 118.27(17) . . ?
C1 N1 C5 116.80(18) . . ?
C3 N1 P1 98.62(12) . . ?
C1 N1 P1 98.69(11) . . ?
C5 N1 P1 99.52(11) . . ?
C2 N2 C7 113.73(15) . . ?
C2 N2 P1 120.59(14) . . ?
C7 N2 P1 116.83(13) . . ?
C13 N3 C4 118.70(16) . . ?
C13 N3 P1 116.94(13) . . ?
C4 N3 P1 122.90(14) . . ?
C6 N4 C19 116.44(16) . . ?
C6 N4 P1 122.42(13) . . ?
C19 N4 P1 116.30(13) . . ?
C12 N5 C8 119.12(17) . . ?
C12 N5 Pd1 118.15(14) . . ?
C8 N5 Pd1 122.73(13) . . ?
C18 N6 C14 118.84(17) . . ?
C18 N6 Pd1 117.01(13) . . ?
C14 N6 Pd1 124.12(13) . . ?
C20 N7 C24 117.4(2) . . ?
C25 N8 Pd1 175.19(17) . . ?
N1 C1 C2 107.50(17) . . ?
N2 C2 C1 109.75(16) . . ?
N1 C3 C4 108.63(16) . . ?
N3 C4 C3 108.57(17) . . ?
N1 C5 C6 106.42(16) . . ?
N4 C6 C5 109.62(17) . . ?
N2 C7 C8 109.60(16) . . ?
N5 C8 C9 121.24(19) . . ?
N5 C8 C7 116.34(17) . . ?
C9 C8 C7 122.42(19) . . ?
C10 C9 C8 119.9(2) . . ?
C9 C10 C11 118.64(19) . . ?
C12 C11 C10 119.0(2) . . ?
N5 C12 C11 122.1(2) . . ?
N3 C13 C14 110.89(16) . . ?
N6 C14 C15 121.35(19) . . ?
N6 C14 C13 116.03(17) . . ?
C15 C14 C13 122.57(18) . . ?
C14 C15 C16 119.7(2) . . ?
C17 C16 C15 119.0(2) . . ?
C16 C17 C18 118.8(2) . . ?
N6 C18 C17 122.32(19) . . ?
N4 C19 C20 113.05(16) . . ?
N7 C20 C21 122.7(2) . . ?
N7 C20 C19 116.40(18) . . ?
C21 C20 C19 120.92(19) . . ?
C20 C21 C22 119.0(2) . . ?
C23 C22 C21 118.8(2) . . ?
C24 C23 C22 118.3(2) . . ?
N7 C24 C23 123.9(2) . . ?
N8 C25 C26 179.0(3) . . ?
N14 Pd2 N13 176.55(7) . . ?
N14 Pd2 N16 89.40(7) . . ?
N13 Pd2 N16 89.42(6) . . ?
N14 Pd2 P2 88.03(5) . . ?
N13 Pd2 P2 93.15(5) . . ?
N16 Pd2 P2 177.43(5) . . ?
N10 P2 N12 114.22(9) . . ?
N10 P2 N11 112.30(9) . . ?
N12 P2 N11 111.59(8) . . ?
N10 P2 Pd2 106.04(6) . . ?
N12 P2 Pd2 103.96(6) . . ?
N11 P2 Pd2 108.03(6) . . ?
N10 P2 N9 73.20(7) . . ?
N12 P2 N9 73.52(7) . . ?
N11 P2 N9 75.32(7) . . ?
Pd2 P2 N9 176.49(4) . . ?
C29 N9 C31 116.80(17) . . ?
C29 N9 C27 118.36(17) . . ?
C31 N9 C27 117.46(17) . . ?
C29 N9 P2 98.13(11) . . ?
C31 N9 P2 99.85(12) . . ?
C27 N9 P2 99.38(12) . . ?
C33 N10 C28 118.89(16) . . ?
C33 N10 P2 117.63(13) . . ?
C28 N10 P2 122.07(14) . . ?
C39 N11 C30 112.59(15) . . ?
C39 N11 P2 117.19(13) . . ?
C30 N11 P2 119.91(13) . . ?
C45 N12 C32 117.29(16) . . ?
C45 N12 P2 117.09(13) . . ?
C32 N12 P2 122.74(13) . . ?
C34 N13 C38 118.77(17) . . ?
C34 N13 Pd2 123.17(13) . . ?
C38 N13 Pd2 118.04(14) . . ?
C44 N14 C40 119.31(19) . . ?
C44 N14 Pd2 118.33(16) . . ?
C40 N14 Pd2 122.26(14) . . ?
C46 N15 C50 116.8(2) . . ?
C51 N16 Pd2 174.39(17) . . ?
N9 C27 C28 106.61(16) . . ?
N10 C28 C27 108.24(17) . . ?
N9 C29 C30 108.06(16) . . ?
N11 C30 C29 109.58(16) . . ?
N9 C31 C32 106.20(16) . . ?
N12 C32 C31 109.53(17) . . ?
N10 C33 C34 110.69(16) . . ?
N13 C34 C35 121.65(18) . . ?
N13 C34 C33 115.85(17) . . ?
C35 C34 C33 122.44(18) . . ?
C34 C35 C36 119.5(2) . . ?
C37 C36 C35 118.8(2) . . ?
C36 C37 C38 119.1(2) . . ?
N13 C38 C37 122.2(2) . . ?
N11 C39 C40 111.44(17) . . ?
N14 C40 C41 121.1(2) . . ?
N14 C40 C39 117.20(18) . . ?
C41 C40 C39 121.7(2) . . ?
C42 C41 C40 119.4(2) . . ?
C43 C42 C41 119.2(2) . . ?
C42 C43 C44 119.2(2) . . ?
N14 C44 C43 121.7(2) . . ?
N12 C45 C46 113.61(16) . . ?
N15 C46 C47 122.9(2) . . ?
N15 C46 C45 114.46(19) . . ?
C47 C46 C45 122.65(19) . . ?
C46 C47 C48 119.4(2) . . ?
C49 C48 C47 118.6(2) . . ?
C48 C49 C50 118.4(2) . . ?
N15 C50 C49 123.9(3) . . ?
N16 C51 C52 178.5(3) . . ?
N17 C53 C54 166.3(6) . . ?
N17 C53 C54B 162.2(5) . . ?
N18 C55 C56 178.0(3) . . ?
F2 B1 F3 110.14(19) . . ?
F2 B1 F4 108.56(19) . . ?
F3 B1 F4 108.37(18) . . ?
F2 B1 F1 110.01(18) . . ?
F3 B1 F1 109.98(19) . . ?
F4 B1 F1 109.74(19) . . ?
F8B B2 F5B 127.1(8) . . ?
F6 B2 F7 111.8(5) . . ?
F8B B2 F7B 93.3(8) . . ?
F5B B2 F7B 99.3(7) . . ?
F6 B2 F8 105.7(4) . . ?
F7 B2 F8 115.7(6) . . ?
F8B B2 F6B 114.8(5) . . ?
F5B B2 F6B 114.1(5) . . ?
F7B B2 F6B 97.6(7) . . ?
F6 B2 F5 107.0(3) . . ?
F7 B2 F5 112.7(5) . . ?
F8 B2 F5 103.2(3) . . ?
F11 B3 F12 110.1(2) . . ?
F11 B3 F10 110.6(2) . . ?
F12 B3 F10 110.2(2) . . ?
F11 B3 F9 109.0(2) . . ?
F12 B3 F9 108.0(2) . . ?
F10 B3 F9 108.8(2) . . ?
F15 B4 F14 110.26(18) . . ?
F15 B4 F13 109.56(18) . . ?
F14 B4 F13 109.14(18) . . ?
F15 B4 F16 109.32(18) . . ?
F14 B4 F16 108.96(17) . . ?
F13 B4 F16 109.58(17) . . ?

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
N3 P1 N2 C2 -30.60(18) . . . . ?
N4 P1 N2 C2 98.31(16) . . . . ?
Pd1 P1 N2 C2 -149.56(13) . . . . ?
N1 P1 N2 C2 34.01(14) . . . . ?
N3 P1 N2 C7 114.78(14) . . . . ?
N4 P1 N2 C7 -116.32(14) . . . . ?
Pd1 P1 N2 C7 -4.18(15) . . . . ?
N1 P1 N2 C7 179.38(15) . . . . ?
N4 P1 N3 C13 137.82(14) . . . . ?
N2 P1 N3 C13 -93.96(15) . . . . ?
Pd1 P1 N3 C13 25.17(15) . . . . ?
N1 P1 N3 C13 -158.99(15) . . . . ?
N4 P1 N3 C4 -28.19(18) . . . . ?
N2 P1 N3 C4 100.03(17) . . . . ?
Pd1 P1 N3 C4 -140.84(14) . . . . ?
N1 P1 N3 C4 35.00(15) . . . . ?
N3 P1 N4 C6 98.39(17) . . . . ?
N2 P1 N4 C6 -29.92(18) . . . . ?
Pd1 P1 N4 C6 -145.64(14) . . . . ?
N1 P1 N4 C6 35.01(15) . . . . ?
N3 P1 N4 C19 -56.07(16) . . . . ?
N2 P1 N4 C19 175.62(13) . . . . ?
Pd1 P1 N4 C19 59.90(14) . . . . ?
N1 P1 N4 C19 -119.45(14) . . . . ?
C3 N1 C1 C2 79.3(2) . . . . ?
C5 N1 C1 C2 -130.62(18) . . . . ?
P1 N1 C1 C2 -25.28(17) . . . . ?
C7 N2 C2 C1 149.07(18) . . . . ?
P1 N2 C2 C1 -64.6(2) . . . . ?
N1 C1 C2 N2 52.8(2) . . . . ?
C1 N1 C3 C4 -128.77(18) . . . . ?
C5 N1 C3 C4 81.6(2) . . . . ?
P1 N1 C3 C4 -24.13(16) . . . . ?
C13 N3 C4 C3 130.46(18) . . . . ?
P1 N3 C4 C3 -63.8(2) . . . . ?
N1 C3 C4 N3 50.2(2) . . . . ?
C3 N1 C5 C6 -129.61(19) . . . . ?
C1 N1 C5 C6 80.5(2) . . . . ?
P1 N1 C5 C6 -24.38(17) . . . . ?
C19 N4 C6 C5 89.2(2) . . . . ?
P1 N4 C6 C5 -65.2(2) . . . . ?
N1 C5 C6 N4 51.3(2) . . . . ?
C2 N2 C7 C8 -145.23(18) . . . . ?
P1 N2 C7 C8 67.07(19) . . . . ?
C12 N5 C8 C9 -1.2(3) . . . . ?
Pd1 N5 C8 C9 179.46(14) . . . . ?
C12 N5 C8 C7 178.60(17) . . . . ?
Pd1 N5 C8 C7 -0.8(2) . . . . ?
N2 C7 C8 N5 -68.2(2) . . . . ?
N2 C7 C8 C9 111.6(2) . . . . ?
N5 C8 C9 C10 0.9(3) . . . . ?
C7 C8 C9 C10 -178.88(18) . . . . ?
C8 C9 C10 C11 -0.1(3) . . . . ?
C9 C10 C11 C12 -0.4(3) . . . . ?
C8 N5 C12 C11 0.7(3) . . . . ?
Pd1 N5 C12 C11 -179.93(15) . . . . ?
C10 C11 C12 N5 0.1(3) . . . . ?
C4 N3 C13 C14 87.7(2) . . . . ?
P1 N3 C13 C14 -78.88(18) . . . . ?
C18 N6 C14 C15 0.2(3) . . . . ?
Pd1 N6 C14 C15 178.40(15) . . . . ?
C18 N6 C14 C13 -177.34(17) . . . . ?
Pd1 N6 C14 C13 0.9(2) . . . . ?
N3 C13 C14 N6 64.3(2) . . . . ?
N3 C13 C14 C15 -113.2(2) . . . . ?
N6 C14 C15 C16 -0.6(3) . . . . ?
C13 C14 C15 C16 176.76(19) . . . . ?
C14 C15 C16 C17 0.9(3) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
C14 N6 C18 C17 0.0(3) . . . . ?
Pd1 N6 C18 C17 -178.39(16) . . . . ?
C16 C17 C18 N6 0.3(3) . . . . ?
C6 N4 C19 C20 92.6(2) . . . . ?
P1 N4 C19 C20 -111.36(17) . . . . ?
C24 N7 C20 C21 1.0(4) . . . . ?
C24 N7 C20 C19 179.4(2) . . . . ?
N4 C19 C20 N7 74.6(2) . . . . ?
N4 C19 C20 C21 -107.0(2) . . . . ?
N7 C20 C21 C22 -1.3(4) . . . . ?
C19 C20 C21 C22 -179.6(2) . . . . ?
C20 C21 C22 C23 0.2(4) . . . . ?
C21 C22 C23 C24 1.0(4) . . . . ?
C20 N7 C24 C23 0.4(4) . . . . ?
C22 C23 C24 N7 -1.4(5) . . . . ?
N12 P2 N10 C33 -140.12(14) . . . . ?
N11 P2 N10 C33 91.52(15) . . . . ?
Pd2 P2 N10 C33 -26.25(15) . . . . ?
N9 P2 N10 C33 157.32(16) . . . . ?
N12 P2 N10 C28 26.17(19) . . . . ?
N11 P2 N10 C28 -102.19(16) . . . . ?
Pd2 P2 N10 C28 140.04(14) . . . . ?
N9 P2 N10 C28 -36.39(15) . . . . ?
N10 P2 N11 C39 -111.21(15) . . . . ?
N12 P2 N11 C39 119.06(15) . . . . ?
Pd2 P2 N11 C39 5.38(15) . . . . ?
N9 P2 N11 C39 -175.72(15) . . . . ?
N10 P2 N11 C30 31.33(17) . . . . ?
N12 P2 N11 C30 -98.40(15) . . . . ?
Pd2 P2 N11 C30 147.91(13) . . . . ?
N9 P2 N11 C30 -33.18(14) . . . . ?
N10 P2 N12 C45 64.53(16) . . . . ?
N11 P2 N12 C45 -166.75(14) . . . . ?
Pd2 P2 N12 C45 -50.56(15) . . . . ?
N9 P2 N12 C45 126.91(15) . . . . ?
N10 P2 N12 C32 -95.71(17) . . . . ?
N11 P2 N12 C32 33.01(18) . . . . ?
Pd2 P2 N12 C32 149.20(15) . . . . ?
N9 P2 N12 C32 -33.33(15) . . . . ?
C29 N9 C27 C28 129.65(19) . . . . ?
C31 N9 C27 C28 -81.3(2) . . . . ?
P2 N9 C27 C28 25.05(17) . . . . ?
C33 N10 C28 C27 -126.82(19) . . . . ?
P2 N10 C28 C27 67.1(2) . . . . ?
N9 C27 C28 N10 -52.3(2) . . . . ?
C31 N9 C29 C30 131.50(18) . . . . ?
C27 N9 C29 C30 -79.2(2) . . . . ?
P2 N9 C29 C30 26.09(16) . . . . ?
C39 N11 C30 C29 -152.28(17) . . . . ?
P2 N11 C30 C29 63.6(2) . . . . ?
N9 C29 C30 N11 -53.5(2) . . . . ?
C29 N9 C31 C32 -78.5(2) . . . . ?
C27 N9 C31 C32 131.99(19) . . . . ?
P2 N9 C31 C32 25.93(18) . . . . ?
C45 N12 C32 C31 -96.4(2) . . . . ?
P2 N12 C32 C31 63.8(2) . . . . ?
N9 C31 C32 N12 -51.9(2) . . . . ?
C28 N10 C33 C34 -86.1(2) . . . . ?
P2 N10 C33 C34 80.65(19) . . . . ?
C38 N13 C34 C35 -0.4(3) . . . . ?
Pd2 N13 C34 C35 178.15(14) . . . . ?
C38 N13 C34 C33 176.89(17) . . . . ?
Pd2 N13 C34 C33 -4.6(2) . . . . ?
N10 C33 C34 N13 -62.5(2) . . . . ?
N10 C33 C34 C35 114.7(2) . . . . ?
N13 C34 C35 C36 -0.2(3) . . . . ?
C33 C34 C35 C36 -177.26(19) . . . . ?
C34 C35 C36 C37 0.3(3) . . . . ?
C35 C36 C37 C38 0.2(3) . . . . ?
C34 N13 C38 C37 0.8(3) . . . . ?
Pd2 N13 C38 C37 -177.75(15) . . . . ?
C36 C37 C38 N13 -0.7(3) . . . . ?
C30 N11 C39 C40 148.78(17) . . . . ?
P2 N11 C39 C40 -66.0(2) . . . . ?
C44 N14 C40 C41 2.0(3) . . . . ?
Pd2 N14 C40 C41 -174.23(16) . . . . ?
C44 N14 C40 C39 -177.92(18) . . . . ?
Pd2 N14 C40 C39 5.9(2) . . . . ?
N11 C39 C40 N14 63.6(2) . . . . ?
N11 C39 C40 C41 -116.2(2) . . . . ?
N14 C40 C41 C42 0.4(3) . . . . ?
C39 C40 C41 C42 -179.7(2) . . . . ?
C40 C41 C42 C43 -1.9(4) . . . . ?
C41 C42 C43 C44 1.1(4) . . . . ?
C40 N14 C44 C43 -2.8(3) . . . . ?
Pd2 N14 C44 C43 173.52(18) . . . . ?
C42 C43 C44 N14 1.3(4) . . . . ?
C32 N12 C45 C46 -94.0(2) . . . . ?
P2 N12 C45 C46 104.65(17) . . . . ?
C50 N15 C46 C47 1.9(4) . . . . ?
C50 N15 C46 C45 -176.6(2) . . . . ?
N12 C45 C46 N15 -132.67(19) . . . . ?
N12 C45 C46 C47 48.8(3) . . . . ?
N15 C46 C47 C48 -1.6(4) . . . . ?
C45 C46 C47 C48 176.8(2) . . . . ?
C46 C47 C48 C49 -0.8(4) . . . . ?
C47 C48 C49 C50 2.6(4) . . . . ?
C46 N15 C50 C49 0.1(4) . . . . ?
C48 C49 C50 N15 -2.4(5) . . . . ?

_refine_diff_density_max         0.862
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.064


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile / Diethyl Ether'
####################################################################### 
# 
# 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_jyy156
_database_code_depnum_ccdc_archive 'CCDC 1827012'
_audit_update_record             
;
2018-03-02 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[NiTPAP(CH3CN)][BF4]2'
_chemical_name_common            '[NiTPAP(CH3CN)][BF4]2'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H36 B2 F8 N9 Ni P'
_chemical_formula_weight         761.96

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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   9.0563(17)
_cell_length_b                   20.118(4)
_cell_length_c                   18.435(4)
_cell_angle_alpha                90
_cell_angle_beta                 98.9026(17)
_cell_angle_gamma                90
_cell_volume                     3318.3(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9904
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      28.88

_exptl_crystal_description       Irregular
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_F_000             1568
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.437
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.178
_exptl_absorpt_coefficient_mu    0.714
_shelx_estimated_absorpt_T_min   0.745
_shelx_estimated_absorpt_T_max   0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
 Reflections not merged 
   82592 Corrected reflections written to file jyy156s.hkl 
 Estimated minimum and maximum transmission:  0.6681  0.7458 
 The ratio (0.8958) of these values is more reliable than their absolute values! 
 Additional spherical absorption correction applied with mu*r =  0.2000 
 Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            40781
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.025
_diffrn_reflns_theta_max         29.077
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8456
_reflns_number_gt                6941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.1-1, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
An orange crystal of approximate dimensions 0.178 x 0.238 x 0.437 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters and 
for data collection (60 sec/frame scan time for a sphere of diffraction data).  
The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were consistent with 
the monoclinic space group P21/c that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis. Hydrogen atoms were included using a riding 
model. There was one molecule of free acetonitrile solvent present per formula-unit.  
Atoms F(7) and F(8) were disordered and included using multiple components with 
partial site-occupancy-factors.

Least-squares analysis yielded wR2 = 0.1267 and Goof = 1.030 for 462 variables 
refined against 8456 data (0.73 Å), R1 = 0.0454 for those 6941 data 
with I > 2.0sigma(I)
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²+4.5044P] 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         8456
_refine_ls_number_parameters     462
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0454
_refine_ls_wR_factor_ref         0.1267
_refine_ls_wR_factor_gt          0.1187
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.67919(3) 0.34643(2) 0.66702(2) 0.02101(9) Uani 1 1 d . . . . .
P1 P 0.61141(6) 0.30064(3) 0.56069(3) 0.01794(12) Uani 1 1 d . . . . .
F1 F -0.0830(2) 0.37589(11) 0.95149(14) 0.0668(7) Uani 1 1 d . . . . .
F2 F 0.1598(2) 0.34759(9) 0.99008(10) 0.0492(5) Uani 1 1 d . . . . .
F3 F 0.0046(2) 0.27486(9) 0.92339(10) 0.0475(4) Uani 1 1 d . . . . .
F4 F 0.0764(2) 0.36946(9) 0.87034(9) 0.0427(4) Uani 1 1 d . . . . .
F5 F -0.0858(2) 0.56685(11) 0.56360(12) 0.0570(5) Uani 1 1 d . . . . .
F6 F -0.2898(3) 0.52661(18) 0.60502(12) 0.1036(12) Uani 1 1 d . . . A 1
F7 F -0.0318(5) 0.4975(2) 0.6539(3) 0.0609(12) Uani 0.5 1 d . . P A 2
F7B F -0.1338(6) 0.4612(2) 0.6070(3) 0.0730(14) Uani 0.5 1 d . . P A 1
F8 F -0.1553(5) 0.5913(2) 0.6687(3) 0.0596(11) Uani 0.5 1 d . . P A 2
F8B F -0.0892(6) 0.5429(3) 0.6901(3) 0.0854(19) Uani 0.5 1 d . . P A .
N1 N 0.5185(2) 0.24721(10) 0.41175(10) 0.0248(4) Uani 1 1 d . . . . .
N2 N 0.7484(2) 0.31145(11) 0.51234(10) 0.0256(4) Uani 1 1 d . . . . .
N3 N 0.4613(2) 0.33968(9) 0.51926(10) 0.0197(4) Uani 1 1 d . . . . .
N4 N 0.5793(2) 0.22028(9) 0.56658(9) 0.0190(4) Uani 1 1 d . . . . .
N5 N 0.8660(2) 0.30033(10) 0.67462(10) 0.0226(4) Uani 1 1 d . . . . .
N6 N 0.4781(2) 0.37180(10) 0.67412(10) 0.0240(4) Uani 1 1 d . . . . .
N7 N 0.4402(2) 0.12328(10) 0.71106(11) 0.0250(4) Uani 1 1 d . . . . .
N8 N 0.7511(2) 0.40412(11) 0.75021(11) 0.0300(4) Uani 1 1 d . . . . .
N9 N 0.5134(7) 0.4897(2) 0.9001(3) 0.1074(17) Uani 1 1 d . . . . .
B1 B 0.0387(3) 0.34204(15) 0.93417(16) 0.0288(6) Uani 1 1 d . . . . .
B2 B -0.1426(4) 0.53535(18) 0.61986(18) 0.0386(7) Uani 1 1 d . . . . .
C1 C 0.6507(3) 0.27364(13) 0.38667(12) 0.0266(5) Uani 1 1 d . . . . .
H1A H 0.6244 0.2889 0.3352 0.032 Uiso 1 1 calc R U . . .
H1B H 0.7265 0.2380 0.3879 0.032 Uiso 1 1 calc R U . . .
C2 C 0.7169(3) 0.33165(14) 0.43447(12) 0.0288(5) Uani 1 1 d . . . . .
H2A H 0.8105 0.3466 0.4181 0.035 Uiso 1 1 calc R U . . .
H2B H 0.6457 0.3693 0.4290 0.035 Uiso 1 1 calc R U . . .
C3 C 0.3804(2) 0.28455(12) 0.40071(12) 0.0226(4) Uani 1 1 d . . . . .
H3A H 0.3001 0.2570 0.3731 0.027 Uiso 1 1 calc R U . . .
H3B H 0.3927 0.3247 0.3711 0.027 Uiso 1 1 calc R U . . .
C4 C 0.3354(2) 0.30535(11) 0.47433(11) 0.0201(4) Uani 1 1 d . . . . .
H4A H 0.2477 0.3353 0.4656 0.024 Uiso 1 1 calc R U . . .
H4B H 0.3073 0.2656 0.5007 0.024 Uiso 1 1 calc R U . . .
C5 C 0.5181(3) 0.17950(12) 0.43803(12) 0.0260(5) Uani 1 1 d . . . . .
H5A H 0.5537 0.1494 0.4019 0.031 Uiso 1 1 calc R U . . .
H5B H 0.4147 0.1664 0.4429 0.031 Uiso 1 1 calc R U . . .
C6 C 0.6186(3) 0.17204(12) 0.51238(12) 0.0244(5) Uani 1 1 d . . . . .
H6A H 0.6088 0.1264 0.5311 0.029 Uiso 1 1 calc R U . . .
H6B H 0.7241 0.1787 0.5059 0.029 Uiso 1 1 calc R U . . .
C7 C 0.9032(3) 0.32223(15) 0.54832(13) 0.0310(5) Uani 1 1 d . . . . .
H7A H 0.9187 0.3704 0.5576 0.037 Uiso 1 1 calc R U . . .
H7B H 0.9720 0.3082 0.5144 0.037 Uiso 1 1 calc R U . . .
C8 C 0.9434(2) 0.28563(13) 0.61940(12) 0.0257(5) Uani 1 1 d . . . . .
C9 C 1.0594(3) 0.24008(14) 0.62935(14) 0.0307(5) Uani 1 1 d . . . . .
H9 H 1.1107 0.2296 0.5896 0.037 Uiso 1 1 calc R U . . .
C10 C 1.1013(3) 0.20968(14) 0.69679(15) 0.0322(5) Uani 1 1 d . . . . .
H10 H 1.1801 0.1780 0.7037 0.039 Uiso 1 1 calc R U . . .
C11 C 1.0253(3) 0.22665(13) 0.75419(14) 0.0300(5) Uani 1 1 d . . . . .
H11 H 1.0527 0.2076 0.8015 0.036 Uiso 1 1 calc R U . . .
C12 C 0.9094(3) 0.27174(13) 0.74107(12) 0.0262(5) Uani 1 1 d . . . . .
H12 H 0.8578 0.2833 0.7804 0.031 Uiso 1 1 calc R U . . .
C13 C 0.4362(3) 0.40661(11) 0.54721(13) 0.0234(4) Uani 1 1 d . . . . .
H13A H 0.3616 0.4306 0.5118 0.028 Uiso 1 1 calc R U . . .
H13B H 0.5307 0.4323 0.5538 0.028 Uiso 1 1 calc R U . . .
C14 C 0.3805(3) 0.39942(11) 0.61957(13) 0.0232(4) Uani 1 1 d . . . . .
C15 C 0.2355(3) 0.41525(12) 0.62994(15) 0.0288(5) Uani 1 1 d . . . . .
H15 H 0.1680 0.4352 0.5915 0.035 Uiso 1 1 calc R U . . .
C16 C 0.1906(3) 0.40147(13) 0.69726(17) 0.0362(6) Uani 1 1 d . . . . .
H16 H 0.0921 0.4121 0.7052 0.043 Uiso 1 1 calc R U . . .
C17 C 0.2898(3) 0.37236(14) 0.75233(15) 0.0361(6) Uani 1 1 d . . . . .
H17 H 0.2605 0.3620 0.7983 0.043 Uiso 1 1 calc R U . . .
C18 C 0.4328(3) 0.35852(14) 0.73916(14) 0.0319(5) Uani 1 1 d . . . . .
H18 H 0.5018 0.3389 0.7772 0.038 Uiso 1 1 calc R U . . .
C19 C 0.4729(2) 0.19760(11) 0.61351(11) 0.0194(4) Uani 1 1 d . . . . .
H19A H 0.3889 0.1747 0.5827 0.023 Uiso 1 1 calc R U . . .
H19B H 0.4316 0.2368 0.6359 0.023 Uiso 1 1 calc R U . . .
C20 C 0.5407(2) 0.15100(10) 0.67403(11) 0.0190(4) Uani 1 1 d . . . . .
C21 C 0.6930(3) 0.13845(12) 0.69002(12) 0.0242(5) Uani 1 1 d . . . . .
H21 H 0.7608 0.1590 0.6625 0.029 Uiso 1 1 calc R U . . .
C22 C 0.7444(3) 0.09514(12) 0.74715(13) 0.0313(6) Uani 1 1 d . . . . .
H22 H 0.8480 0.0856 0.7596 0.038 Uiso 1 1 calc R U . . .
C23 C 0.6420(4) 0.06637(12) 0.78524(14) 0.0364(6) Uani 1 1 d . . . . .
H23 H 0.6740 0.0365 0.8244 0.044 Uiso 1 1 calc R U . . .
C24 C 0.4919(3) 0.08137(12) 0.76597(14) 0.0327(6) Uani 1 1 d . . . . .
H24 H 0.4223 0.0611 0.7927 0.039 Uiso 1 1 calc R U . . .
C25 C 0.7925(3) 0.44649(14) 0.78929(14) 0.0347(6) Uani 1 1 d . . . . .
C26 C 0.8460(4) 0.50172(17) 0.83812(19) 0.0573(10) Uani 1 1 d . . . . .
H26A H 0.9252 0.5256 0.8182 0.086 Uiso 1 1 calc R U . . .
H26B H 0.8856 0.4844 0.8869 0.086 Uiso 1 1 calc R U . . .
H26C H 0.7630 0.5322 0.8419 0.086 Uiso 1 1 calc R U . . .
C27 C 0.3866(6) 0.49373(19) 0.9188(3) 0.0693(12) Uani 1 1 d . . . . .
C28 C 0.2427(5) 0.5004(2) 0.9453(3) 0.0906(17) Uani 1 1 d . . . . .
H28A H 0.1761 0.4642 0.9254 0.136 Uiso 1 1 calc R U . . .
H28B H 0.1971 0.5432 0.9291 0.136 Uiso 1 1 calc R U . . .
H28C H 0.2586 0.4984 0.9990 0.136 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N6 1.915(2) . ?
Ni1 N5 1.916(2) . ?
Ni1 N8 1.953(2) . ?
Ni1 P1 2.1670(7) . ?
P1 N4 1.649(2) . ?
P1 N2 1.6500(19) . ?
P1 N3 1.6511(19) . ?
P1 N1 2.948(2) . ?
F1 B1 1.374(3) . ?
F2 B1 1.388(3) . ?
F3 B1 1.394(4) . ?
F4 B1 1.389(3) . ?
F5 B2 1.381(4) . ?
F6 B2 1.331(4) . ?
F7 F8B 1.288(8) . ?
F7 B2 1.337(4) . ?
F7B B2 1.514(6) . ?
F8 F8B 1.178(7) . ?
F8 B2 1.458(5) . ?
F8B B2 1.319(5) . ?
N1 C3 1.446(3) . ?
N1 C5 1.446(3) . ?
N1 C1 1.450(3) . ?
N2 C7 1.472(3) . ?
N2 C2 1.477(3) . ?
N3 C13 1.472(3) . ?
N3 C4 1.473(3) . ?
N4 C19 1.464(3) . ?
N4 C6 1.476(3) . ?
N5 C8 1.355(3) . ?
N5 C12 1.355(3) . ?
N6 C14 1.352(3) . ?
N6 C18 1.353(3) . ?
N7 C20 1.341(3) . ?
N7 C24 1.345(3) . ?
N8 C25 1.141(3) . ?
N9 C27 1.252(7) . ?
C1 C2 1.528(4) . ?
C3 C4 1.535(3) . ?
C5 C6 1.531(3) . ?
C7 C8 1.498(3) . ?
C8 C9 1.385(4) . ?
C9 C10 1.385(4) . ?
C10 C11 1.391(4) . ?
C11 C12 1.380(4) . ?
C13 C14 1.504(3) . ?
C14 C15 1.393(3) . ?
C15 C16 1.392(4) . ?
C16 C17 1.378(4) . ?
C17 C18 1.382(4) . ?
C19 C20 1.513(3) . ?
C20 C21 1.389(3) . ?
C21 C22 1.390(3) . ?
C22 C23 1.374(4) . ?
C23 C24 1.385(4) . ?
C25 C26 1.465(4) . ?
C27 C28 1.467(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
N6 Ni1 N5 164.27(9) . . ?
N6 Ni1 N8 89.59(8) . . ?
N5 Ni1 N8 92.69(8) . . ?
N6 Ni1 P1 92.06(6) . . ?
N5 Ni1 P1 89.06(6) . . ?
N8 Ni1 P1 167.53(7) . . ?
N4 P1 N2 108.66(10) . . ?
N4 P1 N3 110.83(9) . . ?
N2 P1 N3 108.74(10) . . ?
N4 P1 Ni1 112.67(7) . . ?
N2 P1 Ni1 107.53(7) . . ?
N3 P1 Ni1 108.30(7) . . ?
N4 P1 N1 71.09(7) . . ?
N2 P1 N1 71.04(8) . . ?
N3 P1 N1 69.30(8) . . ?
Ni1 P1 N1 176.21(5) . . ?
F8B F7 B2 60.3(3) . . ?
F8B F8 B2 58.9(3) . . ?
F8 F8B F7 129.7(5) . . ?
F8 F8B B2 71.2(4) . . ?
F7 F8B B2 61.7(3) . . ?
C3 N1 C5 119.33(19) . . ?
C3 N1 C1 120.2(2) . . ?
C5 N1 C1 119.8(2) . . ?
C3 N1 P1 93.31(13) . . ?
C5 N1 P1 92.67(12) . . ?
C1 N1 P1 91.85(13) . . ?
C7 N2 C2 115.14(18) . . ?
C7 N2 P1 121.30(15) . . ?
C2 N2 P1 120.88(15) . . ?
C13 N3 C4 118.52(17) . . ?
C13 N3 P1 115.71(14) . . ?
C4 N3 P1 123.18(15) . . ?
C19 N4 C6 116.42(18) . . ?
C19 N4 P1 118.92(14) . . ?
C6 N4 P1 122.46(15) . . ?
C8 N5 C12 118.4(2) . . ?
C8 N5 Ni1 127.18(16) . . ?
C12 N5 Ni1 113.63(16) . . ?
C14 N6 C18 119.2(2) . . ?
C14 N6 Ni1 125.33(16) . . ?
C18 N6 Ni1 115.49(17) . . ?
C20 N7 C24 117.3(2) . . ?
C25 N8 Ni1 167.6(2) . . ?
F1 B1 F2 110.9(3) . . ?
F1 B1 F4 108.1(2) . . ?
F2 B1 F4 109.1(2) . . ?
F1 B1 F3 110.2(2) . . ?
F2 B1 F3 108.4(2) . . ?
F4 B1 F3 110.0(2) . . ?
F8B B2 F6 114.8(4) . . ?
F8B B2 F7 58.0(4) . . ?
F8B B2 F5 124.2(4) . . ?
F6 B2 F5 112.6(2) . . ?
F7 B2 F5 105.9(3) . . ?
F8B B2 F8 49.9(4) . . ?
F7 B2 F8 106.0(4) . . ?
F5 B2 F8 100.6(3) . . ?
F8B B2 F7B 104.3(4) . . ?
F6 B2 F7B 85.0(3) . . ?
F5 B2 F7B 107.4(3) . . ?
N1 C1 C2 111.47(19) . . ?
N2 C2 C1 110.5(2) . . ?
N1 C3 C4 111.07(17) . . ?
N3 C4 C3 109.66(18) . . ?
N1 C5 C6 111.1(2) . . ?
N4 C6 C5 111.68(18) . . ?
N2 C7 C8 114.0(2) . . ?
N5 C8 C9 121.0(2) . . ?
N5 C8 C7 117.8(2) . . ?
C9 C8 C7 121.2(2) . . ?
C10 C9 C8 120.5(2) . . ?
C9 C10 C11 118.4(2) . . ?
C12 C11 C10 118.7(2) . . ?
N5 C12 C11 122.9(2) . . ?
N3 C13 C14 108.28(18) . . ?
N6 C14 C15 120.9(2) . . ?
N6 C14 C13 115.4(2) . . ?
C15 C14 C13 123.5(2) . . ?
C16 C15 C14 119.2(3) . . ?
C17 C16 C15 119.7(2) . . ?
C16 C17 C18 118.5(3) . . ?
N6 C18 C17 122.5(3) . . ?
N4 C19 C20 113.59(17) . . ?
N7 C20 C21 123.1(2) . . ?
N7 C20 C19 113.79(19) . . ?
C21 C20 C19 123.1(2) . . ?
C20 C21 C22 118.7(2) . . ?
C23 C22 C21 118.6(2) . . ?
C22 C23 C24 119.4(2) . . ?
N7 C24 C23 122.9(3) . . ?
N8 C25 C26 178.8(3) . . ?
N9 C27 C28 176.2(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
B2 F8 F8B F7 21.0(5) . . . . ?
B2 F7 F8B F8 -22.6(6) . . . . ?
N4 P1 N2 C7 -98.1(2) . . . . ?
N3 P1 N2 C7 141.2(2) . . . . ?
Ni1 P1 N2 C7 24.1(2) . . . . ?
N1 P1 N2 C7 -159.6(2) . . . . ?
N4 P1 N2 C2 101.4(2) . . . . ?
N3 P1 N2 C2 -19.4(2) . . . . ?
Ni1 P1 N2 C2 -136.43(18) . . . . ?
N1 P1 N2 C2 39.88(19) . . . . ?
N4 P1 N3 C13 143.97(15) . . . . ?
N2 P1 N3 C13 -96.66(17) . . . . ?
Ni1 P1 N3 C13 19.91(17) . . . . ?
N1 P1 N3 C13 -156.99(17) . . . . ?
N4 P1 N3 C4 -17.5(2) . . . . ?
N2 P1 N3 C4 101.91(18) . . . . ?
Ni1 P1 N3 C4 -141.53(15) . . . . ?
N1 P1 N3 C4 41.58(16) . . . . ?
N2 P1 N4 C19 173.61(15) . . . . ?
N3 P1 N4 C19 -66.97(17) . . . . ?
Ni1 P1 N4 C19 54.56(16) . . . . ?
N1 P1 N4 C19 -124.95(16) . . . . ?
N2 P1 N4 C6 -23.85(19) . . . . ?
N3 P1 N4 C6 95.57(18) . . . . ?
Ni1 P1 N4 C6 -142.90(15) . . . . ?
N1 P1 N4 C6 37.58(15) . . . . ?
F8 F8B B2 F7 161.8(5) . . . . ?
F8 F8B B2 F5 73.7(5) . . . . ?
F7 F8B B2 F5 -88.1(5) . . . . ?
F7 F8B B2 F8 -161.8(5) . . . . ?
F8B F7 B2 F5 120.7(4) . . . . ?
F8B F7 B2 F8 14.4(4) . . . . ?
F8B F8 B2 F7 -16.0(4) . . . . ?
F8B F8 B2 F5 -126.1(4) . . . . ?
C3 N1 C1 C2 72.1(3) . . . . ?
C5 N1 C1 C2 -116.9(2) . . . . ?
P1 N1 C1 C2 -22.77(19) . . . . ?
C7 N2 C2 C1 124.9(2) . . . . ?
P1 N2 C2 C1 -73.4(3) . . . . ?
N1 C1 C2 N2 55.5(3) . . . . ?
C5 N1 C3 C4 73.6(3) . . . . ?
C1 N1 C3 C4 -115.5(2) . . . . ?
P1 N1 C3 C4 -21.38(18) . . . . ?
C13 N3 C4 C3 125.0(2) . . . . ?
P1 N3 C4 C3 -74.0(2) . . . . ?
N1 C3 C4 N3 52.6(2) . . . . ?
C3 N1 C5 C6 -118.0(2) . . . . ?
C1 N1 C5 C6 71.0(3) . . . . ?
P1 N1 C5 C6 -22.69(18) . . . . ?
C19 N4 C6 C5 92.8(2) . . . . ?
P1 N4 C6 C5 -70.1(2) . . . . ?
N1 C5 C6 N4 53.7(3) . . . . ?
C2 N2 C7 C8 -164.5(2) . . . . ?
P1 N2 C7 C8 33.9(3) . . . . ?
C12 N5 C8 C9 3.1(3) . . . . ?
Ni1 N5 C8 C9 -165.90(18) . . . . ?
C12 N5 C8 C7 -174.5(2) . . . . ?
Ni1 N5 C8 C7 16.5(3) . . . . ?
N2 C7 C8 N5 -61.4(3) . . . . ?
N2 C7 C8 C9 121.0(3) . . . . ?
N5 C8 C9 C10 -1.6(4) . . . . ?
C7 C8 C9 C10 175.9(2) . . . . ?
C8 C9 C10 C11 -0.8(4) . . . . ?
C9 C10 C11 C12 1.5(4) . . . . ?
C8 N5 C12 C11 -2.3(3) . . . . ?
Ni1 N5 C12 C11 168.10(19) . . . . ?
C10 C11 C12 N5 0.0(4) . . . . ?
C4 N3 C13 C14 87.7(2) . . . . ?
P1 N3 C13 C14 -74.6(2) . . . . ?
C18 N6 C14 C15 1.1(3) . . . . ?
Ni1 N6 C14 C15 179.05(16) . . . . ?
C18 N6 C14 C13 -174.6(2) . . . . ?
Ni1 N6 C14 C13 3.3(3) . . . . ?
N3 C13 C14 N6 64.6(2) . . . . ?
N3 C13 C14 C15 -111.0(2) . . . . ?
N6 C14 C15 C16 -0.9(3) . . . . ?
C13 C14 C15 C16 174.5(2) . . . . ?
C14 C15 C16 C17 -0.2(4) . . . . ?
C15 C16 C17 C18 0.9(4) . . . . ?
C14 N6 C18 C17 -0.3(4) . . . . ?
Ni1 N6 C18 C17 -178.4(2) . . . . ?
C16 C17 C18 N6 -0.7(4) . . . . ?
C6 N4 C19 C20 76.0(2) . . . . ?
P1 N4 C19 C20 -120.47(17) . . . . ?
C24 N7 C20 C21 -0.2(3) . . . . ?
C24 N7 C20 C19 -179.8(2) . . . . ?
N4 C19 C20 N7 -171.73(18) . . . . ?
N4 C19 C20 C21 8.7(3) . . . . ?
N7 C20 C21 C22 0.0(3) . . . . ?
C19 C20 C21 C22 179.5(2) . . . . ?
C20 C21 C22 C23 0.2(3) . . . . ?
C21 C22 C23 C24 -0.2(4) . . . . ?
C20 N7 C24 C23 0.2(4) . . . . ?
C22 C23 C24 N7 0.0(4) . . . . ?

_refine_diff_density_max         1.173
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.077


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile / Diethyl Ether'
####################################################################### 
# 
# 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_15073z
_database_code_depnum_ccdc_archive 'CCDC 1841335'
_audit_update_record             
;
2018-05-04 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_chemical_name_systematic        Co(TPAP)Cl
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H30 Cl Co N7 P'
_chemical_formula_sum            'C24 H30 Cl Co N7 P'
_chemical_formula_weight         541.90

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   9.8827(5)
_cell_length_b                   14.0100(7)
_cell_length_c                   17.8800(9)
_cell_angle_alpha                90
_cell_angle_beta                 100.490(2)
_cell_angle_gamma                90
_cell_volume                     2434.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9913
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      68.43

_exptl_crystal_description       Block
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   0.3350
_exptl_transmission_factor_max   0.7531
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    7.379
_shelx_estimated_absorpt_T_min   0.320
_shelx_estimated_absorpt_T_max   0.320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3350
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed tube'
_diffrn_measurement_device_type  'Bruker D8 Photon 100 CMOS'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17925
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         4.035
_diffrn_reflns_theta_max         68.429
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             4398
_reflns_number_gt                4161
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX II, Bruker'
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'SHELXTL, Bruker'
_computing_publication_material  'SHELXTL, Bruker'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+3.4268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4398
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0420
_refine_ls_wR_factor_ref         0.1092
_refine_ls_wR_factor_gt          0.1070
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.037
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.50607(4) 0.83833(3) 0.19461(2) 0.01620(13) Uani 1 1 d . . . . .
Cl1 Cl 0.54335(6) 0.70642(4) 0.26691(4) 0.02457(17) Uani 1 1 d . . . . .
P1 P 0.43988(6) 0.98431(4) 0.20902(3) 0.01455(16) Uani 1 1 d . . . . .
N1 N 0.3779(2) 1.21837(16) 0.19264(12) 0.0215(5) Uani 1 1 d . . . . .
N2 N 0.3319(2) 1.01739(15) 0.12899(11) 0.0170(4) Uani 1 1 d . . . . .
N3 N 0.5811(2) 1.05543(15) 0.21628(12) 0.0169(4) Uani 1 1 d . . . . .
N4 N 0.3634(2) 1.02911(15) 0.27860(12) 0.0189(5) Uani 1 1 d . . . . .
N5 N 0.3801(2) 0.80717(15) 0.09301(12) 0.0175(4) Uani 1 1 d . . . . .
N6 N 0.6823(2) 0.87468(15) 0.15776(12) 0.0191(5) Uani 1 1 d . . . . .
N7 N 0.1293(3) 0.95172(18) 0.40247(15) 0.0318(6) Uani 1 1 d . . . . .
C1 C 0.2813(3) 1.19430(19) 0.12458(15) 0.0225(6) Uani 1 1 d . . . . .
H1A H 0.3264 1.2039 0.0801 0.027 Uiso 1 1 calc R U . . .
H1B H 0.2023 1.2388 0.1195 0.027 Uiso 1 1 calc R U . . .
C2 C 0.2268(3) 1.09172(18) 0.12290(15) 0.0193(5) Uani 1 1 d . . . . .
H2A H 0.1757 1.0837 0.1652 0.023 Uiso 1 1 calc R U . . .
H2B H 0.1606 1.0822 0.0748 0.023 Uiso 1 1 calc R U . . .
C3 C 0.5222(3) 1.22737(19) 0.18919(15) 0.0210(6) Uani 1 1 d . . . . .
H3A H 0.5721 1.2476 0.2398 0.025 Uiso 1 1 calc R U . . .
H3B H 0.5330 1.2786 0.1526 0.025 Uiso 1 1 calc R U . . .
C4 C 0.5899(3) 1.13700(18) 0.16591(15) 0.0202(5) Uani 1 1 d . . . . .
H4A H 0.5456 1.1195 0.1135 0.024 Uiso 1 1 calc R U . . .
H4B H 0.6881 1.1505 0.1654 0.024 Uiso 1 1 calc R U . . .
C5 C 0.3361(3) 1.20903(19) 0.26545(15) 0.0219(6) Uani 1 1 d . . . . .
H5A H 0.2345 1.2045 0.2569 0.026 Uiso 1 1 calc R U . . .
H5B H 0.3629 1.2679 0.2952 0.026 Uiso 1 1 calc R U . . .
C6 C 0.3963(3) 1.12335(19) 0.31302(14) 0.0198(5) Uani 1 1 d . . . . .
H6A H 0.4976 1.1303 0.3244 0.024 Uiso 1 1 calc R U . . .
H6B H 0.3633 1.1253 0.3621 0.024 Uiso 1 1 calc R U . . .
C7 C 0.3618(3) 0.97575(18) 0.05827(14) 0.0194(5) Uani 1 1 d . . . . .
H7A H 0.4623 0.9789 0.0596 0.023 Uiso 1 1 calc R U . . .
H7B H 0.3166 1.0152 0.0149 0.023 Uiso 1 1 calc R U . . .
C8 C 0.3154(3) 0.87337(18) 0.04411(13) 0.0167(5) Uani 1 1 d . . . . .
C9 C 0.2165(3) 0.8489(2) -0.01830(15) 0.0230(6) Uani 1 1 d . . . . .
H9A H 0.1698 0.8971 -0.0503 0.028 Uiso 1 1 calc R U . . .
C10 C 0.1862(3) 0.7536(2) -0.03365(15) 0.0258(6) Uani 1 1 d . . . . .
H10A H 0.1193 0.7356 -0.0765 0.031 Uiso 1 1 calc R U . . .
C11 C 0.2549(3) 0.6855(2) 0.01432(15) 0.0249(6) Uani 1 1 d . . . . .
H11A H 0.2378 0.6195 0.0045 0.030 Uiso 1 1 calc R U . . .
C12 C 0.3492(3) 0.71475(19) 0.07715(15) 0.0206(5) Uani 1 1 d . . . . .
H12A H 0.3944 0.6674 0.1107 0.025 Uiso 1 1 calc R U . . .
C13 C 0.7108(3) 1.00767(19) 0.24708(15) 0.0194(5) Uani 1 1 d . . . . .
H13A H 0.6973 0.9673 0.2906 0.023 Uiso 1 1 calc R U . . .
H13B H 0.7807 1.0566 0.2666 0.023 Uiso 1 1 calc R U . . .
C14 C 0.7652(3) 0.94611(18) 0.18956(14) 0.0165(5) Uani 1 1 d . . . . .
C15 C 0.8934(3) 0.96268(19) 0.17006(15) 0.0201(5) Uani 1 1 d . . . . .
H15A H 0.9492 1.0138 0.1930 0.024 Uiso 1 1 calc R U . . .
C16 C 0.9394(3) 0.90464(19) 0.11723(15) 0.0228(6) Uani 1 1 d . . . . .
H16A H 1.0273 0.9144 0.1041 0.027 Uiso 1 1 calc R U . . .
C17 C 0.8544(3) 0.83211(19) 0.08406(15) 0.0220(6) Uani 1 1 d . . . . .
H17A H 0.8825 0.7913 0.0473 0.026 Uiso 1 1 calc R U . . .
C18 C 0.7278(3) 0.81991(19) 0.10521(15) 0.0212(5) Uani 1 1 d . . . . .
H18A H 0.6697 0.7704 0.0816 0.025 Uiso 1 1 calc R U . . .
C19 C 0.2395(3) 0.9837(2) 0.29444(15) 0.0239(6) Uani 1 1 d . . . . .
H19A H 0.2195 0.9265 0.2618 0.029 Uiso 1 1 calc R U . . .
H19B H 0.1613 1.0284 0.2810 0.029 Uiso 1 1 calc R U . . .
C20 C 0.2507(3) 0.95395(18) 0.37733(16) 0.0230(6) Uani 1 1 d . . . . .
C21 C 0.3731(3) 0.9316(2) 0.42208(16) 0.0271(6) Uani 1 1 d . . . . .
H21A H 0.4554 0.9325 0.4016 0.032 Uiso 1 1 calc R U . . .
C22 C 0.3771(4) 0.9082(2) 0.49605(18) 0.0340(7) Uani 1 1 d . . . . .
H22A H 0.4622 0.8929 0.5279 0.041 Uiso 1 1 calc R U . . .
C23 C 0.2566(4) 0.9067(2) 0.52462(17) 0.0340(7) Uani 1 1 d . . . . .
H23A H 0.2577 0.8925 0.5767 0.041 Uiso 1 1 calc R U . . .
C24 C 0.1359(4) 0.9260(2) 0.47677(19) 0.0364(8) Uani 1 1 d . . . . .
H24A H 0.0526 0.9214 0.4959 0.044 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N6 2.036(2) . ?
Co1 N5 2.054(2) . ?
Co1 P1 2.1768(7) . ?
Co1 Cl1 2.2470(7) . ?
P1 N2 1.687(2) . ?
P1 N4 1.689(2) . ?
P1 N3 1.700(2) . ?
P1 N1 3.339(2) . ?
N1 C5 1.442(3) . ?
N1 C1 1.443(3) . ?
N1 C3 1.444(3) . ?
N2 C2 1.461(3) . ?
N2 C7 1.471(3) . ?
N3 C13 1.462(3) . ?
N3 C4 1.467(3) . ?
N4 C19 1.453(3) . ?
N4 C6 1.468(3) . ?
N5 C12 1.349(3) . ?
N5 C8 1.353(3) . ?
N6 C14 1.352(3) . ?
N6 C18 1.352(3) . ?
N7 C20 1.356(4) . ?
N7 C24 1.367(4) . ?
C1 C2 1.533(4) . ?
C3 C4 1.525(4) . ?
C5 C6 1.528(4) . ?
C7 C8 1.513(4) . ?
C8 C9 1.386(4) . ?
C9 C10 1.384(4) . ?
C10 C11 1.377(4) . ?
C11 C12 1.385(4) . ?
C13 C14 1.514(3) . ?
C14 C15 1.393(4) . ?
C15 C16 1.384(4) . ?
C16 C17 1.381(4) . ?
C17 C18 1.381(4) . ?
C19 C20 1.524(4) . ?
C20 C21 1.360(4) . ?
C21 C22 1.356(4) . ?
C22 C23 1.379(5) . ?
C23 C24 1.362(5) . ?

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
N6 Co1 N5 100.57(8) . . ?
N6 Co1 P1 95.54(6) . . ?
N5 Co1 P1 99.07(6) . . ?
N6 Co1 Cl1 109.37(6) . . ?
N5 Co1 Cl1 110.09(6) . . ?
P1 Co1 Cl1 136.55(3) . . ?
N2 P1 N4 102.95(11) . . ?
N2 P1 N3 106.70(11) . . ?
N4 P1 N3 101.35(10) . . ?
N2 P1 Co1 108.36(8) . . ?
N4 P1 Co1 128.35(8) . . ?
N3 P1 Co1 107.43(8) . . ?
N2 P1 N1 65.05(8) . . ?
N4 P1 N1 66.44(8) . . ?
N3 P1 N1 64.27(8) . . ?
Co1 P1 N1 165.15(5) . . ?
C5 N1 C1 119.0(2) . . ?
C5 N1 C3 119.6(2) . . ?
C1 N1 C3 119.4(2) . . ?
C5 N1 P1 84.83(14) . . ?
C1 N1 P1 85.82(14) . . ?
C3 N1 P1 85.57(14) . . ?
C2 N2 C7 118.0(2) . . ?
C2 N2 P1 126.19(17) . . ?
C7 N2 P1 115.18(17) . . ?
C13 N3 C4 116.2(2) . . ?
C13 N3 P1 114.32(16) . . ?
C4 N3 P1 123.34(17) . . ?
C19 N4 C6 116.2(2) . . ?
C19 N4 P1 119.11(18) . . ?
C6 N4 P1 123.27(17) . . ?
C12 N5 C8 117.4(2) . . ?
C12 N5 Co1 117.89(17) . . ?
C8 N5 Co1 124.40(17) . . ?
C14 N6 C18 117.3(2) . . ?
C14 N6 Co1 122.55(17) . . ?
C18 N6 Co1 119.71(18) . . ?
C20 N7 C24 116.1(3) . . ?
N1 C1 C2 114.3(2) . . ?
N2 C2 C1 115.1(2) . . ?
N1 C3 C4 115.1(2) . . ?
N3 C4 C3 113.6(2) . . ?
N1 C5 C6 115.3(2) . . ?
N4 C6 C5 116.1(2) . . ?
N2 C7 C8 114.7(2) . . ?
N5 C8 C9 122.1(2) . . ?
N5 C8 C7 116.7(2) . . ?
C9 C8 C7 121.2(2) . . ?
C10 C9 C8 119.6(3) . . ?
C11 C10 C9 118.7(3) . . ?
C10 C11 C12 118.8(3) . . ?
N5 C12 C11 123.2(2) . . ?
N3 C13 C14 113.6(2) . . ?
N6 C14 C15 121.8(2) . . ?
N6 C14 C13 116.4(2) . . ?
C15 C14 C13 121.8(2) . . ?
C16 C15 C14 120.0(2) . . ?
C17 C16 C15 118.4(2) . . ?
C18 C17 C16 118.9(2) . . ?
N6 C18 C17 123.5(3) . . ?
N4 C19 C20 113.3(2) . . ?
N7 C20 C21 123.1(3) . . ?
N7 C20 C19 114.6(3) . . ?
C21 C20 C19 122.3(2) . . ?
C22 C21 C20 119.6(3) . . ?
C21 C22 C23 119.4(3) . . ?
C24 C23 C22 118.7(3) . . ?
C23 C24 N7 123.0(3) . . ?

_refine_diff_density_max         0.561
_refine_diff_density_min         -0.856
_refine_diff_density_rms         0.073


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Pentane'
_chemical_properties_physical    Air-sensitive
####################################################################### 
# 
# 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_jyy160
_database_code_depnum_ccdc_archive 'CCDC 1827014'
_audit_update_record             
;
2018-03-02 deposited with the CCDC.
2018-09-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[PtTPAP(Cl)][PF6]'
_chemical_name_common            '[PtTPAP(Cl)][PF6]'
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C24 H30 Cl F6 N7 P2 Pt'
_chemical_formula_weight         823.03

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.4092(8)
_cell_length_b                   15.4825(12)
_cell_length_c                   19.0637(14)
_cell_angle_alpha                104.4188(9)
_cell_angle_beta                 92.0696(9)
_cell_angle_gamma                94.3920(9)
_cell_volume                     2962.0(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9993
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      28.56

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.238
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.160
_exptl_absorpt_coefficient_mu    5.002
_shelx_estimated_absorpt_T_min   0.382
_shelx_estimated_absorpt_T_max   0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3191
_exptl_absorpt_correction_T_max  0.4315
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   
; 
Reflections not merged 
34963 Corrected reflections written to file jyy160s.hkl 
Estimated minimum and maximum transmission:  0.3191  0.4315 
The ratio (0.7395) of these values is more reliable than their absolute values 
Additional spherical absorption correction applied with mu*r =  0.6000 
Lambda/2 correction factor = 0.00150 
;
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            34958
_diffrn_reflns_av_unetI/netI     0.0351
_diffrn_reflns_av_R_equivalents  0.0248
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.363
_diffrn_reflns_theta_max         28.808
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             14052
_reflns_number_gt                11631
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _reflns_Friedel_fraction is defined as the number of unique 
 Friedel pairs measured divided by the number that would be 
 possible theoretically, ignoring centric projections and 
 systematic absences. 
;

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A colorless crystal of approximate dimensions 0.160 x 0.186 x 0.238 mm 
was mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (30 sec/frame scan time for 
a sphere of diffraction data).  The raw frame data was processed using 
SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  There were no 
systematic absences nor any diffraction symmetry other than the Friedel 
condition.  The centrosymmetric triclinic space group P-1 was assigned and 
later determined to be correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering factors 
for neutral atoms were used throughout the analysis.  Hydrogen atoms were 
included using a riding model.  There were two molecules of the formula-unit 
present (Z = 4).  The platinum atoms were disordered and included using 
multiple components with partial site-occupancy-factors.

Least-squares analysis yielded wR2 = 0.0780 and Goof = 1.036 for 757 variables 
refined against 14052 data (0.74 Å), R1 = 0.0341 for those 11631 data 
with I > 2.0sigma(I).

There were several high residuals present in the final difference-Fourier map.  
It was not possible to determine the nature of the residuals although it was 
probable that diethylether solvent was present.  The SQUEEZE routine in the 
PLATON program package was used to account for the electrons in the solvent 
accessible voids.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0353P)²+6.6469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         14052
_refine_ls_number_parameters     757
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0780
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pt1 Pt 0.96835(4) 0.52798(2) 0.71444(2) 0.01830(7) Uani 0.9 1 d . . P A 1
Pt1B Pt 0.9622(4) 0.5015(2) 0.7238(2) 0.0222(7) Uani 0.1 1 d . . P A 2
Cl1 Cl 0.76987(12) 0.58153(9) 0.67963(7) 0.0368(3) Uani 1 1 d . . . . .
P1 P 1.16421(10) 0.49989(8) 0.74852(6) 0.0214(2) Uani 1 1 d . . . . .
N1 N 1.4320(4) 0.4729(3) 0.7833(2) 0.0358(10) Uani 1 1 d . . . . .
N2 N 1.2367(3) 0.5946(2) 0.8013(2) 0.0258(8) Uani 1 1 d . . . . .
N3 N 1.2428(3) 0.4683(2) 0.67415(19) 0.0244(8) Uani 1 1 d . . . . .
N4 N 1.1650(3) 0.4237(3) 0.7949(2) 0.0274(8) Uani 1 1 d . . . . .
N5 N 0.9437(3) 0.5857(3) 0.82068(19) 0.0246(8) Uani 1 1 d . . . . .
N6 N 0.9804(3) 0.4539(2) 0.61047(19) 0.0248(8) Uani 1 1 d . . . . .
N7 N 0.9536(4) 0.3682(3) 0.8721(2) 0.0434(11) Uani 1 1 d . . . . .
C1 C 1.4639(4) 0.5661(4) 0.8165(3) 0.0407(13) Uani 1 1 d . . . . .
H1A H 1.5529 0.5835 0.8053 0.049 Uiso 1 1 calc R U . . .
H1B H 1.4612 0.5767 0.8698 0.049 Uiso 1 1 calc R U . . .
C2 C 1.3715(4) 0.6241(3) 0.7900(3) 0.0327(11) Uani 1 1 d . . . . .
H2A H 1.3920 0.6875 0.8168 0.039 Uiso 1 1 calc R U . . .
H2B H 1.3816 0.6194 0.7378 0.039 Uiso 1 1 calc R U . . .
C3 C 1.4603(4) 0.4367(4) 0.7086(3) 0.0360(11) Uani 1 1 d . . . . .
H3A H 1.5179 0.3881 0.7054 0.043 Uiso 1 1 calc R U . . .
H3B H 1.5053 0.4842 0.6897 0.043 Uiso 1 1 calc R U . . .
C4 C 1.3359(4) 0.4005(3) 0.6629(3) 0.0291(10) Uani 1 1 d . . . . .
H4A H 1.3547 0.3830 0.6110 0.035 Uiso 1 1 calc R U . . .
H4B H 1.2985 0.3466 0.6764 0.035 Uiso 1 1 calc R U . . .
C5 C 1.3962(5) 0.4148(4) 0.8276(3) 0.0399(13) Uani 1 1 d . . . . .
H5A H 1.4593 0.4258 0.8697 0.048 Uiso 1 1 calc R U . . .
H5B H 1.3983 0.3519 0.7995 0.048 Uiso 1 1 calc R U . . .
C6 C 1.2593(5) 0.4292(4) 0.8552(3) 0.0358(11) Uani 1 1 d . . . . .
H6A H 1.2333 0.3832 0.8811 0.043 Uiso 1 1 calc R U . . .
H6B H 1.2606 0.4887 0.8900 0.043 Uiso 1 1 calc R U . . .
C7 C 1.1565(4) 0.6682(3) 0.8309(2) 0.0246(9) Uani 1 1 d . . . . .
H7A H 1.1299 0.6952 0.7912 0.029 Uiso 1 1 calc R U . . .
H7B H 1.2093 0.7151 0.8678 0.029 Uiso 1 1 calc R U . . .
C8 C 1.0380(4) 0.6395(3) 0.8647(2) 0.0232(9) Uani 1 1 d . . . . .
C9 C 1.0225(5) 0.6693(3) 0.9383(2) 0.0328(11) Uani 1 1 d . . . . .
H9A H 1.0902 0.7056 0.9690 0.039 Uiso 1 1 calc R U . . .
C10 C 0.9092(5) 0.6465(4) 0.9673(3) 0.0397(12) Uani 1 1 d . . . . .
H10A H 0.8979 0.6671 1.0177 0.048 Uiso 1 1 calc R U . . .
C11 C 0.8128(5) 0.5932(4) 0.9217(3) 0.0394(12) Uani 1 1 d . . . . .
H11A H 0.7334 0.5772 0.9402 0.047 Uiso 1 1 calc R U . . .
C12 C 0.8329(4) 0.5633(4) 0.8486(3) 0.0339(11) Uani 1 1 d . . . . .
H12A H 0.7667 0.5260 0.8173 0.041 Uiso 1 1 calc R U . . .
C13 C 1.2069(4) 0.5072(3) 0.6144(2) 0.0263(9) Uani 1 1 d . . . . .
H13A H 1.2788 0.5055 0.5816 0.032 Uiso 1 1 calc R U . . .
H13B H 1.1898 0.5704 0.6339 0.032 Uiso 1 1 calc R U . . .
C14 C 1.0883(4) 0.4550(3) 0.5730(2) 0.0235(9) Uani 1 1 d . . . . .
C15 C 1.0879(5) 0.4082(3) 0.5009(2) 0.0285(10) Uani 1 1 d . . . . .
H15A H 1.1633 0.4115 0.4748 0.034 Uiso 1 1 calc R U . . .
C16 C 0.9787(5) 0.3568(3) 0.4670(3) 0.0334(11) Uani 1 1 d . . . . .
H16A H 0.9775 0.3252 0.4174 0.040 Uiso 1 1 calc R U . . .
C17 C 0.8708(5) 0.3523(3) 0.5066(3) 0.0320(11) Uani 1 1 d . . . . .
H17A H 0.7953 0.3154 0.4851 0.038 Uiso 1 1 calc R U . . .
C18 C 0.8743(4) 0.4020(3) 0.5775(3) 0.0291(10) Uani 1 1 d . . . . .
H18A H 0.7994 0.3997 0.6043 0.035 Uiso 1 1 calc R U . . .
C19 C 1.0821(5) 0.3404(3) 0.7665(3) 0.0340(11) Uani 1 1 d . . . . .
H19A H 1.1271 0.2899 0.7759 0.041 Uiso 1 1 calc R U . . .
H19B H 1.0686 0.3301 0.7133 0.041 Uiso 1 1 calc R U . . .
C20 C 0.9520(5) 0.3404(3) 0.7994(3) 0.0345(11) Uani 1 1 d . . . . .
C21 C 0.8390(5) 0.3112(4) 0.7559(3) 0.0431(13) Uani 1 1 d . . . . .
H21A H 0.8414 0.2936 0.7046 0.052 Uiso 1 1 calc R U . . .
C22 C 0.7222(5) 0.3086(4) 0.7892(4) 0.0527(16) Uani 1 1 d . . . . .
H22A H 0.6435 0.2885 0.7609 0.063 Uiso 1 1 calc R U . . .
C23 C 0.7227(5) 0.3352(4) 0.8629(4) 0.0537(17) Uani 1 1 d . . . . .
H23A H 0.6448 0.3325 0.8870 0.064 Uiso 1 1 calc R U . . .
C24 C 0.8396(5) 0.3663(5) 0.9023(3) 0.0510(16) Uani 1 1 d . . . . .
H24A H 0.8384 0.3874 0.9535 0.061 Uiso 1 1 calc R U . . .
Pt2 Pt 1.01007(4) 0.85998(2) 0.71272(2) 0.01655(7) Uani 0.92 1 d . . P B 1
Pt2B Pt 1.0214(6) 0.8913(3) 0.7164(4) 0.0286(11) Uani 0.08 1 d . . P B 2
Cl2 Cl 1.20899(10) 0.79130(8) 0.69150(6) 0.0287(2) Uani 1 1 d . . . . .
P2 P 0.81562(10) 0.90973(8) 0.73335(6) 0.0204(2) Uani 1 1 d . . . . .
N8 N 0.5652(4) 0.9664(3) 0.7526(2) 0.0346(10) Uani 1 1 d . . . . .
N9 N 0.7498(3) 0.8641(3) 0.7965(2) 0.0278(8) Uani 1 1 d . . . . .
N10 N 0.7292(3) 0.8792(3) 0.65497(19) 0.0248(8) Uani 1 1 d . . . . .
N11 N 0.8295(3) 1.0192(3) 0.76600(19) 0.0245(8) Uani 1 1 d . . . . .
N12 N 1.0435(3) 0.8780(2) 0.82084(19) 0.0246(8) Uani 1 1 d . . . . .
N13 N 0.9941(3) 0.8603(2) 0.60578(18) 0.0221(7) Uani 1 1 d . . . . .
N14 N 1.1214(4) 1.1040(3) 0.6988(2) 0.0341(9) Uani 1 1 d . . . . .
C25 C 0.5281(5) 0.9101(4) 0.7999(3) 0.0442(14) Uani 1 1 d . . . . .
H25A H 0.4358 0.8879 0.7898 0.053 Uiso 1 1 calc R U . . .
H25B H 0.5401 0.9450 0.8512 0.053 Uiso 1 1 calc R U . . .
C26 C 0.6104(4) 0.8317(4) 0.7874(3) 0.0410(13) Uani 1 1 d . . . . .
H26A H 0.5902 0.7956 0.8224 0.049 Uiso 1 1 calc R U . . .
H26B H 0.5907 0.7930 0.7378 0.049 Uiso 1 1 calc R U . . .
C27 C 0.5190(4) 0.9395(4) 0.6772(2) 0.0340(11) Uani 1 1 d . . . . .
H27A H 0.4616 0.9832 0.6663 0.041 Uiso 1 1 calc R U . . .
H27B H 0.4696 0.8800 0.6664 0.041 Uiso 1 1 calc R U . . .
C28 C 0.6368(4) 0.9356(4) 0.6313(2) 0.0299(10) Uani 1 1 d . . . . .
H28A H 0.6098 0.9103 0.5795 0.036 Uiso 1 1 calc R U . . .
H28B H 0.6785 0.9968 0.6370 0.036 Uiso 1 1 calc R U . . .
C29 C 0.6044(5) 1.0588(4) 0.7849(3) 0.0403(13) Uani 1 1 d . . . . .
H29A H 0.5449 1.0836 0.8227 0.048 Uiso 1 1 calc R U . . .
H29B H 0.6023 1.0933 0.7477 0.048 Uiso 1 1 calc R U . . .
C30 C 0.7427(4) 1.0662(3) 0.8192(2) 0.0313(11) Uani 1 1 d . . . . .
H30A H 0.7753 1.1301 0.8365 0.038 Uiso 1 1 calc R U . . .
H30B H 0.7416 1.0398 0.8614 0.038 Uiso 1 1 calc R U . . .
C31 C 0.8291(5) 0.8066(3) 0.8280(2) 0.0303(10) Uani 1 1 d . . . . .
H31A H 0.8483 0.7544 0.7892 0.036 Uiso 1 1 calc R U . . .
H31B H 0.7793 0.7840 0.8640 0.036 Uiso 1 1 calc R U . . .
C32 C 0.9536(4) 0.8554(3) 0.8642(2) 0.0278(10) Uani 1 1 d . . . . .
C33 C 0.9783(5) 0.8751(3) 0.9390(3) 0.0358(11) Uani 1 1 d . . . . .
H33A H 0.9139 0.8607 0.9693 0.043 Uiso 1 1 calc R U . . .
C34 C 1.0974(5) 0.9159(4) 0.9688(3) 0.0411(13) Uani 1 1 d . . . . .
H34A H 1.1159 0.9283 1.0197 0.049 Uiso 1 1 calc R U . . .
C35 C 1.1890(5) 0.9385(3) 0.9249(3) 0.0373(12) Uani 1 1 d . . . . .
H35A H 1.2711 0.9669 0.9447 0.045 Uiso 1 1 calc R U . . .
C36 C 1.1587(4) 0.9188(3) 0.8509(3) 0.0313(10) Uani 1 1 d . . . . .
H36A H 1.2214 0.9347 0.8203 0.038 Uiso 1 1 calc R U . . .
C37 C 0.7700(4) 0.8027(3) 0.6004(2) 0.0275(10) Uani 1 1 d . . . . .
H37A H 0.6981 0.7773 0.5638 0.033 Uiso 1 1 calc R U . . .
H37B H 0.7934 0.7554 0.6240 0.033 Uiso 1 1 calc R U . . .
C38 C 0.8842(4) 0.8331(3) 0.5639(2) 0.0250(9) Uani 1 1 d . . . . .
C39 C 0.8779(5) 0.8351(3) 0.4916(2) 0.0325(11) Uani 1 1 d . . . . .
H39A H 0.8008 0.8140 0.4622 0.039 Uiso 1 1 calc R U . . .
C40 C 0.9858(5) 0.8684(4) 0.4626(3) 0.0369(12) Uani 1 1 d . . . . .
H40A H 0.9825 0.8714 0.4134 0.044 Uiso 1 1 calc R U . . .
C41 C 1.0972(5) 0.8969(3) 0.5056(3) 0.0331(11) Uani 1 1 d . . . . .
H41A H 1.1720 0.9196 0.4866 0.040 Uiso 1 1 calc R U . . .
C42 C 1.0986(4) 0.8919(3) 0.5764(3) 0.0290(10) Uani 1 1 d . . . . .
H42A H 1.1759 0.9115 0.6061 0.035 Uiso 1 1 calc R U . . .
C43 C 0.9015(4) 1.0703(3) 0.7230(2) 0.0265(9) Uani 1 1 d . . . . .
H43A H 0.8570 1.1244 0.7224 0.032 Uiso 1 1 calc R U . . .
H43B H 0.9004 1.0335 0.6724 0.032 Uiso 1 1 calc R U . . .
C44 C 1.0394(4) 1.0986(3) 0.7504(2) 0.0255(9) Uani 1 1 d . . . . .
C45 C 1.0790(5) 1.1197(3) 0.8239(3) 0.0348(11) Uani 1 1 d . . . . .
H45A H 1.0188 1.1145 0.8592 0.042 Uiso 1 1 calc R U . . .
C46 C 1.2069(5) 1.1482(4) 0.8446(3) 0.0412(13) Uani 1 1 d . . . . .
H46A H 1.2359 1.1638 0.8943 0.049 Uiso 1 1 calc R U . . .
C47 C 1.2917(5) 1.1536(4) 0.7915(3) 0.0418(13) Uani 1 1 d . . . . .
H47A H 1.3802 1.1731 0.8040 0.050 Uiso 1 1 calc R U . . .
C48 C 1.2458(5) 1.1301(4) 0.7200(3) 0.0411(13) Uani 1 1 d . . . . .
H48A H 1.3053 1.1326 0.6838 0.049 Uiso 1 1 calc R U . . .
P3 P 0.52110(12) 0.20854(10) 1.00371(7) 0.0339(3) Uani 1 1 d . . . . .
F1 F 0.4756(3) 0.2381(3) 0.93289(18) 0.0607(10) Uani 1 1 d . . . . .
F2 F 0.5679(3) 0.1787(2) 1.07412(15) 0.0434(7) Uani 1 1 d . . . . .
F3 F 0.4281(5) 0.1209(3) 0.9785(2) 0.0975(17) Uani 1 1 d . . . . .
F4 F 0.6363(4) 0.1626(3) 0.9614(2) 0.0880(15) Uani 1 1 d . . . . .
F5 F 0.6146(3) 0.2988(2) 1.02937(17) 0.0564(9) Uani 1 1 d . . . . .
F6 F 0.4104(3) 0.2588(3) 1.0486(2) 0.0723(12) Uani 1 1 d . . . . .
P4 P 0.55686(11) 1.18702(9) 0.58063(7) 0.0294(3) Uani 1 1 d . . . . .
F7 F 0.4355(3) 1.2255(2) 0.54910(18) 0.0527(9) Uani 1 1 d . . . . .
F8 F 0.6123(3) 1.1637(2) 0.50256(16) 0.0505(8) Uani 1 1 d . . . . .
F9 F 0.6327(3) 1.2837(2) 0.59904(18) 0.0503(8) Uani 1 1 d . . . . .
F10 F 0.5007(3) 1.2115(2) 0.65949(17) 0.0529(9) Uani 1 1 d . . . . .
F11 F 0.4804(4) 1.0915(2) 0.5643(2) 0.0710(11) Uani 1 1 d . . . . .
F12 F 0.6788(3) 1.1499(3) 0.61375(18) 0.0622(10) 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
Pt1 N5 2.034(4) . ?
Pt1 N6 2.041(4) . ?
Pt1 P1 2.2245(11) . ?
Pt1 Cl1 2.4153(13) . ?
Pt1B N5 2.003(6) . ?
Pt1B N6 2.122(5) . ?
Pt1B P1 2.142(4) . ?
Pt1B Cl1 2.652(4) . ?
P1 N4 1.642(4) . ?
P1 N3 1.649(4) . ?
P1 N2 1.666(4) . ?
P1 N1 2.927(4) . ?
N1 C5 1.418(7) . ?
N1 C1 1.432(7) . ?
N1 C3 1.445(6) . ?
N2 C7 1.474(5) . ?
N2 C2 1.482(6) . ?
N3 C13 1.464(6) . ?
N3 C4 1.464(5) . ?
N4 C6 1.466(5) . ?
N4 C19 1.467(6) . ?
N5 C12 1.344(6) . ?
N5 C8 1.353(6) . ?
N6 C18 1.350(6) . ?
N6 C14 1.354(5) . ?
N7 C24 1.339(7) . ?
N7 C20 1.343(7) . ?
C1 C2 1.520(7) . ?
C3 C4 1.521(6) . ?
C5 C6 1.550(7) . ?
C7 C8 1.500(6) . ?
C8 C9 1.383(6) . ?
C9 C10 1.378(7) . ?
C10 C11 1.377(8) . ?
C11 C12 1.384(7) . ?
C13 C14 1.503(6) . ?
C14 C15 1.385(6) . ?
C15 C16 1.376(7) . ?
C16 C17 1.382(7) . ?
C17 C18 1.378(6) . ?
C19 C20 1.513(7) . ?
C20 C21 1.392(7) . ?
C21 C22 1.394(8) . ?
C22 C23 1.363(9) . ?
C23 C24 1.392(8) . ?
Pt2 N12 2.024(4) . ?
Pt2 N13 2.041(3) . ?
Pt2 P2 2.2339(11) . ?
Pt2 Cl2 2.4011(12) . ?
Pt2B N13 2.047(7) . ?
Pt2B N12 2.059(7) . ?
Pt2B P2 2.207(6) . ?
Pt2B Cl2 2.569(6) . ?
P2 N11 1.647(4) . ?
P2 N10 1.659(4) . ?
P2 N9 1.682(4) . ?
P2 N8 2.821(4) . ?
N8 C29 1.430(7) . ?
N8 C25 1.446(7) . ?
N8 C27 1.447(6) . ?
N9 C31 1.476(6) . ?
N9 C26 1.488(6) . ?
N10 C37 1.471(6) . ?
N10 C28 1.478(5) . ?
N11 C43 1.461(6) . ?
N11 C30 1.474(5) . ?
N12 C36 1.349(6) . ?
N12 C32 1.354(6) . ?
N13 C38 1.348(5) . ?
N13 C42 1.355(5) . ?
N14 C44 1.340(6) . ?
N14 C48 1.343(6) . ?
C25 C26 1.514(8) . ?
C27 C28 1.528(6) . ?
C29 C30 1.543(6) . ?
C31 C32 1.500(7) . ?
C32 C33 1.392(6) . ?
C33 C34 1.381(7) . ?
C34 C35 1.373(8) . ?
C35 C36 1.385(7) . ?
C37 C38 1.501(6) . ?
C38 C39 1.387(6) . ?
C39 C40 1.389(7) . ?
C40 C41 1.373(7) . ?
C41 C42 1.371(6) . ?
C43 C44 1.504(6) . ?
C44 C45 1.396(6) . ?
C45 C46 1.381(7) . ?
C46 C47 1.381(8) . ?
C47 C48 1.377(8) . ?
P3 F3 1.565(4) . ?
P3 F4 1.584(4) . ?
P3 F6 1.595(4) . ?
P3 F2 1.596(3) . ?
P3 F1 1.597(3) . ?
P3 F5 1.598(4) . ?
P4 F11 1.578(4) . ?
P4 F8 1.583(3) . ?
P4 F9 1.589(3) . ?
P4 F7 1.597(3) . ?
P4 F10 1.600(3) . ?
P4 F12 1.604(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N5 Pt1 N6 171.84(15) . . ?
N5 Pt1 P1 87.62(10) . . ?
N6 Pt1 P1 93.00(10) . . ?
N5 Pt1 Cl1 90.48(10) . . ?
N6 Pt1 Cl1 90.09(11) . . ?
P1 Pt1 Cl1 171.28(5) . . ?
N5 Pt1B N6 160.4(2) . . ?
N5 Pt1B P1 90.8(2) . . ?
N6 Pt1B P1 93.15(19) . . ?
N5 Pt1B Cl1 84.66(17) . . ?
N6 Pt1B Cl1 82.24(15) . . ?
P1 Pt1B Cl1 149.51(15) . . ?
N4 P1 N3 110.10(19) . . ?
N4 P1 N2 107.4(2) . . ?
N3 P1 N2 110.05(19) . . ?
N4 P1 Pt1B 101.99(15) . . ?
N3 P1 Pt1B 111.38(17) . . ?
N2 P1 Pt1B 115.49(17) . . ?
N4 P1 Pt1 114.43(14) . . ?
N3 P1 Pt1 107.03(13) . . ?
N2 P1 Pt1 107.77(13) . . ?
N4 P1 N1 71.14(16) . . ?
N3 P1 N1 68.96(15) . . ?
N2 P1 N1 70.70(15) . . ?
Pt1B P1 N1 172.30(13) . . ?
Pt1 P1 N1 174.29(10) . . ?
C5 N1 C1 119.1(4) . . ?
C5 N1 C3 120.4(4) . . ?
C1 N1 C3 119.5(4) . . ?
C5 N1 P1 93.3(3) . . ?
C1 N1 P1 92.7(3) . . ?
C3 N1 P1 94.3(3) . . ?
C7 N2 C2 114.5(4) . . ?
C7 N2 P1 118.2(3) . . ?
C2 N2 P1 120.3(3) . . ?
C13 N3 C4 119.4(3) . . ?
C13 N3 P1 115.8(3) . . ?
C4 N3 P1 124.6(3) . . ?
C6 N4 C19 119.0(4) . . ?
C6 N4 P1 122.7(3) . . ?
C19 N4 P1 117.5(3) . . ?
C12 N5 C8 119.6(4) . . ?
C12 N5 Pt1B 110.2(3) . . ?
C8 N5 Pt1B 127.4(3) . . ?
C12 N5 Pt1 117.9(3) . . ?
C8 N5 Pt1 122.3(3) . . ?
C18 N6 C14 118.7(4) . . ?
C18 N6 Pt1 117.8(3) . . ?
C14 N6 Pt1 123.4(3) . . ?
C18 N6 Pt1B 111.7(3) . . ?
C14 N6 Pt1B 128.2(3) . . ?
C24 N7 C20 116.8(5) . . ?
N1 C1 C2 111.8(4) . . ?
N2 C2 C1 110.0(4) . . ?
N1 C3 C4 110.0(4) . . ?
N3 C4 C3 110.5(4) . . ?
N1 C5 C6 111.5(4) . . ?
N4 C6 C5 111.0(4) . . ?
N2 C7 C8 113.7(4) . . ?
N5 C8 C9 120.4(4) . . ?
N5 C8 C7 118.0(4) . . ?
C9 C8 C7 121.5(4) . . ?
C10 C9 C8 120.4(5) . . ?
C11 C10 C9 118.7(4) . . ?
C10 C11 C12 119.2(5) . . ?
N5 C12 C11 121.7(5) . . ?
N3 C13 C14 109.5(4) . . ?
N6 C14 C15 120.8(4) . . ?
N6 C14 C13 116.5(4) . . ?
C15 C14 C13 122.7(4) . . ?
C16 C15 C14 120.2(4) . . ?
C15 C16 C17 118.7(4) . . ?
C18 C17 C16 119.0(4) . . ?
N6 C18 C17 122.3(4) . . ?
N4 C19 C20 113.6(4) . . ?
N7 C20 C21 123.1(5) . . ?
N7 C20 C19 116.0(4) . . ?
C21 C20 C19 120.9(5) . . ?
C20 C21 C22 118.6(6) . . ?
C23 C22 C21 118.9(5) . . ?
C22 C23 C24 118.8(5) . . ?
N7 C24 C23 123.8(6) . . ?
N12 Pt2 N13 170.95(15) . . ?
N12 Pt2 P2 89.16(10) . . ?
N13 Pt2 P2 92.61(10) . . ?
N12 Pt2 Cl2 90.00(10) . . ?
N13 Pt2 Cl2 89.16(10) . . ?
P2 Pt2 Cl2 173.90(4) . . ?
N13 Pt2B N12 161.4(3) . . ?
N13 Pt2B P2 93.2(3) . . ?
N12 Pt2B P2 89.0(3) . . ?
N13 Pt2B Cl2 84.5(2) . . ?
N12 Pt2B Cl2 84.7(2) . . ?
P2 Pt2B Cl2 151.36(19) . . ?
N11 P2 N10 111.63(19) . . ?
N11 P2 N9 107.66(19) . . ?
N10 P2 N9 111.94(19) . . ?
N11 P2 Pt2B 98.16(17) . . ?
N10 P2 Pt2B 110.6(2) . . ?
N9 P2 Pt2B 116.0(2) . . ?
N11 P2 Pt2 110.18(13) . . ?
N10 P2 Pt2 107.03(13) . . ?
N9 P2 Pt2 108.36(13) . . ?
N11 P2 N8 72.04(16) . . ?
N10 P2 N8 70.14(15) . . ?
N9 P2 N8 72.38(15) . . ?
Pt2B P2 N8 169.15(15) . . ?
Pt2 P2 N8 177.04(10) . . ?
C29 N8 C25 118.0(4) . . ?
C29 N8 C27 119.1(4) . . ?
C25 N8 C27 119.0(4) . . ?
C29 N8 P2 96.6(3) . . ?
C25 N8 P2 95.6(3) . . ?
C27 N8 P2 97.5(3) . . ?
C31 N9 C26 112.8(4) . . ?
C31 N9 P2 117.2(3) . . ?
C26 N9 P2 119.0(3) . . ?
C37 N10 C28 118.2(3) . . ?
C37 N10 P2 116.6(3) . . ?
C28 N10 P2 123.6(3) . . ?
C43 N11 C30 118.4(4) . . ?
C43 N11 P2 115.7(3) . . ?
C30 N11 P2 122.8(3) . . ?
C36 N12 C32 119.1(4) . . ?
C36 N12 Pt2 117.8(3) . . ?
C32 N12 Pt2 123.0(3) . . ?
C36 N12 Pt2B 109.4(3) . . ?
C32 N12 Pt2B 129.4(3) . . ?
C38 N13 C42 118.8(4) . . ?
C38 N13 Pt2 123.2(3) . . ?
C42 N13 Pt2 117.9(3) . . ?
C38 N13 Pt2B 129.3(3) . . ?
C42 N13 Pt2B 110.1(3) . . ?
C44 N14 C48 117.5(4) . . ?
N8 C25 C26 109.3(4) . . ?
N9 C26 C25 110.4(4) . . ?
N8 C27 C28 107.5(4) . . ?
N10 C28 C27 109.4(4) . . ?
N8 C29 C30 108.5(4) . . ?
N11 C30 C29 110.8(4) . . ?
N9 C31 C32 112.4(4) . . ?
N12 C32 C33 120.7(4) . . ?
N12 C32 C31 117.2(4) . . ?
C33 C32 C31 122.1(4) . . ?
C34 C33 C32 119.4(5) . . ?
C35 C34 C33 120.0(5) . . ?
C34 C35 C36 118.3(5) . . ?
N12 C36 C35 122.5(5) . . ?
N10 C37 C38 109.5(4) . . ?
N13 C38 C39 121.0(4) . . ?
N13 C38 C37 116.4(4) . . ?
C39 C38 C37 122.6(4) . . ?
C38 C39 C40 119.3(4) . . ?
C41 C40 C39 119.4(4) . . ?
C42 C41 C40 118.9(4) . . ?
N13 C42 C41 122.5(4) . . ?
N11 C43 C44 114.1(3) . . ?
N14 C44 C45 122.3(4) . . ?
N14 C44 C43 114.7(4) . . ?
C45 C44 C43 122.9(4) . . ?
C46 C45 C44 119.2(5) . . ?
C47 C46 C45 118.6(5) . . ?
C48 C47 C46 118.9(5) . . ?
N14 C48 C47 123.5(5) . . ?
F3 P3 F4 92.3(3) . . ?
F3 P3 F6 90.5(3) . . ?
F4 P3 F6 177.1(3) . . ?
F3 P3 F2 90.5(2) . . ?
F4 P3 F2 89.98(19) . . ?
F6 P3 F2 89.14(19) . . ?
F3 P3 F1 89.6(2) . . ?
F4 P3 F1 89.4(2) . . ?
F6 P3 F1 91.4(2) . . ?
F2 P3 F1 179.4(2) . . ?
F3 P3 F5 179.3(3) . . ?
F4 P3 F5 88.2(2) . . ?
F6 P3 F5 88.9(2) . . ?
F2 P3 F5 89.97(18) . . ?
F1 P3 F5 89.92(19) . . ?
F11 P4 F8 90.7(2) . . ?
F11 P4 F9 178.6(2) . . ?
F8 P4 F9 90.70(19) . . ?
F11 P4 F7 90.0(2) . . ?
F8 P4 F7 89.99(18) . . ?
F9 P4 F7 90.07(19) . . ?
F11 P4 F10 89.69(19) . . ?
F8 P4 F10 179.5(2) . . ?
F9 P4 F10 88.92(18) . . ?
F7 P4 F10 89.70(19) . . ?
F11 P4 F12 90.6(2) . . ?
F8 P4 F12 90.91(18) . . ?
F9 P4 F12 89.3(2) . . ?
F7 P4 F12 178.9(2) . . ?
F10 P4 F12 89.39(19) . . ?

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
N4 P1 N2 C7 -108.5(3) . . . . ?
N3 P1 N2 C7 131.6(3) . . . . ?
Pt1B P1 N2 C7 4.5(4) . . . . ?
Pt1 P1 N2 C7 15.2(4) . . . . ?
N1 P1 N2 C7 -170.6(4) . . . . ?
N4 P1 N2 C2 102.5(4) . . . . ?
N3 P1 N2 C2 -17.4(4) . . . . ?
Pt1B P1 N2 C2 -144.6(3) . . . . ?
Pt1 P1 N2 C2 -133.8(3) . . . . ?
N1 P1 N2 C2 40.4(3) . . . . ?
N4 P1 N3 C13 155.6(3) . . . . ?
N2 P1 N3 C13 -86.2(3) . . . . ?
Pt1B P1 N3 C13 43.2(3) . . . . ?
Pt1 P1 N3 C13 30.6(3) . . . . ?
N1 P1 N3 C13 -145.1(3) . . . . ?
N4 P1 N3 C4 -19.5(4) . . . . ?
N2 P1 N3 C4 98.7(4) . . . . ?
Pt1B P1 N3 C4 -131.9(3) . . . . ?
Pt1 P1 N3 C4 -144.5(3) . . . . ?
N1 P1 N3 C4 39.8(3) . . . . ?
N3 P1 N4 C6 96.1(4) . . . . ?
N2 P1 N4 C6 -23.8(4) . . . . ?
Pt1B P1 N4 C6 -145.6(4) . . . . ?
Pt1 P1 N4 C6 -143.3(3) . . . . ?
N1 P1 N4 C6 38.0(3) . . . . ?
N3 P1 N4 C19 -73.4(4) . . . . ?
N2 P1 N4 C19 166.8(3) . . . . ?
Pt1B P1 N4 C19 44.9(4) . . . . ?
Pt1 P1 N4 C19 47.2(4) . . . . ?
N1 P1 N4 C19 -131.5(3) . . . . ?
C5 N1 C1 C2 -117.4(5) . . . . ?
C3 N1 C1 C2 74.4(5) . . . . ?
P1 N1 C1 C2 -22.2(4) . . . . ?
C7 N2 C2 C1 136.4(4) . . . . ?
P1 N2 C2 C1 -73.5(5) . . . . ?
N1 C1 C2 N2 54.8(5) . . . . ?
C5 N1 C3 C4 74.4(5) . . . . ?
C1 N1 C3 C4 -117.6(5) . . . . ?
P1 N1 C3 C4 -22.0(4) . . . . ?
C13 N3 C4 C3 112.8(4) . . . . ?
P1 N3 C4 C3 -72.3(5) . . . . ?
N1 C3 C4 N3 52.0(6) . . . . ?
C1 N1 C5 C6 72.9(6) . . . . ?
C3 N1 C5 C6 -119.0(5) . . . . ?
P1 N1 C5 C6 -22.0(4) . . . . ?
C19 N4 C6 C5 100.0(5) . . . . ?
P1 N4 C6 C5 -69.3(5) . . . . ?
N1 C5 C6 N4 52.5(6) . . . . ?
C2 N2 C7 C8 -160.9(4) . . . . ?
P1 N2 C7 C8 48.3(5) . . . . ?
C12 N5 C8 C9 2.0(6) . . . . ?
Pt1B N5 C8 C9 -157.1(3) . . . . ?
Pt1 N5 C8 C9 -172.7(3) . . . . ?
C12 N5 C8 C7 -175.8(4) . . . . ?
Pt1B N5 C8 C7 25.1(5) . . . . ?
Pt1 N5 C8 C7 9.4(5) . . . . ?
N2 C7 C8 N5 -68.2(5) . . . . ?
N2 C7 C8 C9 114.0(5) . . . . ?
N5 C8 C9 C10 -1.9(7) . . . . ?
C7 C8 C9 C10 175.9(4) . . . . ?
C8 C9 C10 C11 0.5(7) . . . . ?
C9 C10 C11 C12 0.8(8) . . . . ?
C8 N5 C12 C11 -0.7(7) . . . . ?
Pt1B N5 C12 C11 161.7(4) . . . . ?
Pt1 N5 C12 C11 174.3(4) . . . . ?
C10 C11 C12 N5 -0.7(8) . . . . ?
C4 N3 C13 C14 92.8(4) . . . . ?
P1 N3 C13 C14 -82.5(4) . . . . ?
C18 N6 C14 C15 4.0(6) . . . . ?
Pt1 N6 C14 C15 -175.4(3) . . . . ?
Pt1B N6 C14 C15 169.3(3) . . . . ?
C18 N6 C14 C13 -174.5(4) . . . . ?
Pt1 N6 C14 C13 6.1(5) . . . . ?
Pt1B N6 C14 C13 -9.2(6) . . . . ?
N3 C13 C14 N6 61.6(5) . . . . ?
N3 C13 C14 C15 -116.8(4) . . . . ?
N6 C14 C15 C16 -2.6(7) . . . . ?
C13 C14 C15 C16 175.8(4) . . . . ?
C14 C15 C16 C17 -0.8(7) . . . . ?
C15 C16 C17 C18 2.6(7) . . . . ?
C14 N6 C18 C17 -2.1(6) . . . . ?
Pt1 N6 C18 C17 177.4(3) . . . . ?
Pt1B N6 C18 C17 -169.7(4) . . . . ?
C16 C17 C18 N6 -1.3(7) . . . . ?
C6 N4 C19 C20 94.8(5) . . . . ?
P1 N4 C19 C20 -95.4(4) . . . . ?
C24 N7 C20 C21 0.6(8) . . . . ?
C24 N7 C20 C19 -178.2(5) . . . . ?
N4 C19 C20 N7 -47.8(6) . . . . ?
N4 C19 C20 C21 133.4(5) . . . . ?
N7 C20 C21 C22 -1.7(8) . . . . ?
C19 C20 C21 C22 177.0(5) . . . . ?
C20 C21 C22 C23 0.5(8) . . . . ?
C21 C22 C23 C24 1.6(9) . . . . ?
C20 N7 C24 C23 1.8(9) . . . . ?
C22 C23 C24 N7 -3.0(9) . . . . ?
N11 P2 N9 C31 -116.3(3) . . . . ?
N10 P2 N9 C31 120.7(3) . . . . ?
Pt2B P2 N9 C31 -7.6(4) . . . . ?
Pt2 P2 N9 C31 2.8(4) . . . . ?
N8 P2 N9 C31 179.8(4) . . . . ?
N11 P2 N9 C26 102.1(4) . . . . ?
N10 P2 N9 C26 -20.9(4) . . . . ?
Pt2B P2 N9 C26 -149.1(4) . . . . ?
Pt2 P2 N9 C26 -138.7(3) . . . . ?
N8 P2 N9 C26 38.3(4) . . . . ?
N11 P2 N10 C37 143.5(3) . . . . ?
N9 P2 N10 C37 -95.7(3) . . . . ?
Pt2B P2 N10 C37 35.3(4) . . . . ?
Pt2 P2 N10 C37 22.8(3) . . . . ?
N8 P2 N10 C37 -156.2(4) . . . . ?
N11 P2 N10 C28 -21.7(4) . . . . ?
N9 P2 N10 C28 99.1(4) . . . . ?
Pt2B P2 N10 C28 -129.9(3) . . . . ?
Pt2 P2 N10 C28 -142.3(3) . . . . ?
N8 P2 N10 C28 38.6(3) . . . . ?
N10 P2 N11 C43 -65.0(3) . . . . ?
N9 P2 N11 C43 171.8(3) . . . . ?
Pt2B P2 N11 C43 51.1(3) . . . . ?
Pt2 P2 N11 C43 53.8(3) . . . . ?
N8 P2 N11 C43 -124.1(3) . . . . ?
N10 P2 N11 C30 95.0(3) . . . . ?
N9 P2 N11 C30 -28.3(4) . . . . ?
Pt2B P2 N11 C30 -149.0(4) . . . . ?
Pt2 P2 N11 C30 -146.3(3) . . . . ?
N8 P2 N11 C30 35.8(3) . . . . ?
C29 N8 C25 C26 -123.5(5) . . . . ?
C27 N8 C25 C26 78.8(5) . . . . ?
P2 N8 C25 C26 -23.0(4) . . . . ?
C31 N9 C26 C25 145.7(4) . . . . ?
P2 N9 C26 C25 -71.2(5) . . . . ?
N8 C25 C26 N9 54.8(5) . . . . ?
C29 N8 C27 C28 78.3(5) . . . . ?
C25 N8 C27 C28 -124.3(5) . . . . ?
P2 N8 C27 C28 -23.6(4) . . . . ?
C37 N10 C28 C27 124.1(4) . . . . ?
P2 N10 C28 C27 -70.9(5) . . . . ?
N8 C27 C28 N10 52.6(5) . . . . ?
C25 N8 C29 C30 76.2(5) . . . . ?
C27 N8 C29 C30 -126.0(4) . . . . ?
P2 N8 C29 C30 -23.6(4) . . . . ?
C43 N11 C30 C29 92.4(5) . . . . ?
P2 N11 C30 C29 -67.0(5) . . . . ?
N8 C29 C30 N11 52.3(5) . . . . ?
C26 N9 C31 C32 -157.1(4) . . . . ?
P2 N9 C31 C32 59.1(5) . . . . ?
C36 N12 C32 C33 1.0(6) . . . . ?
Pt2 N12 C32 C33 -175.3(3) . . . . ?
Pt2B N12 C32 C33 -160.7(4) . . . . ?
C36 N12 C32 C31 -177.5(4) . . . . ?
Pt2 N12 C32 C31 6.2(5) . . . . ?
Pt2B N12 C32 C31 20.8(6) . . . . ?
N9 C31 C32 N12 -69.6(5) . . . . ?
N9 C31 C32 C33 111.9(5) . . . . ?
N12 C32 C33 C34 -1.9(7) . . . . ?
C31 C32 C33 C34 176.6(4) . . . . ?
C32 C33 C34 C35 1.5(7) . . . . ?
C33 C34 C35 C36 -0.4(7) . . . . ?
C32 N12 C36 C35 0.1(7) . . . . ?
Pt2 N12 C36 C35 176.7(4) . . . . ?
Pt2B N12 C36 C35 165.3(4) . . . . ?
C34 C35 C36 N12 -0.5(7) . . . . ?
C28 N10 C37 C38 87.4(4) . . . . ?
P2 N10 C37 C38 -78.6(4) . . . . ?
C42 N13 C38 C39 1.5(6) . . . . ?
Pt2 N13 C38 C39 179.6(3) . . . . ?
Pt2B N13 C38 C39 164.7(4) . . . . ?
C42 N13 C38 C37 -177.3(4) . . . . ?
Pt2 N13 C38 C37 0.8(5) . . . . ?
Pt2B N13 C38 C37 -14.1(6) . . . . ?
N10 C37 C38 N13 66.3(5) . . . . ?
N10 C37 C38 C39 -112.4(5) . . . . ?
N13 C38 C39 C40 -2.0(7) . . . . ?
C37 C38 C39 C40 176.7(4) . . . . ?
C38 C39 C40 C41 1.3(7) . . . . ?
C39 C40 C41 C42 -0.2(7) . . . . ?
C38 N13 C42 C41 -0.4(7) . . . . ?
Pt2 N13 C42 C41 -178.6(4) . . . . ?
Pt2B N13 C42 C41 -166.6(4) . . . . ?
C40 C41 C42 N13 -0.3(7) . . . . ?
C30 N11 C43 C44 100.0(4) . . . . ?
P2 N11 C43 C44 -99.1(4) . . . . ?
C48 N14 C44 C45 0.5(7) . . . . ?
C48 N14 C44 C43 179.1(4) . . . . ?
N11 C43 C44 N14 148.5(4) . . . . ?
N11 C43 C44 C45 -32.9(6) . . . . ?
N14 C44 C45 C46 0.8(7) . . . . ?
C43 C44 C45 C46 -177.7(5) . . . . ?
C44 C45 C46 C47 -0.9(8) . . . . ?
C45 C46 C47 C48 -0.2(8) . . . . ?
C44 N14 C48 C47 -1.7(8) . . . . ?
C46 C47 C48 N14 1.6(8) . . . . ?

_refine_diff_density_max         2.145
_refine_diff_density_min         -1.065
_refine_diff_density_rms         0.129



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Acetonitrile / Diethyl Ether'
