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

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

data_jyy71
_database_code_depnum_ccdc_archive 'CCDC 1448469'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'[Nickle(0)-tricarbonyl-(2,8,9-triisopropyl-2,3,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane)]'
_chemical_name_common            Ni(LIPr)(CO)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C18 H33 N4 Ni O3 P'
_chemical_formula_weight         443.16

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   9.4521(6)
_cell_length_b                   16.0515(11)
_cell_length_c                   14.5677(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8772(8)
_cell_angle_gamma                90.00
_cell_volume                     2205.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9960
_cell_measurement_theta_min      2.49
_cell_measurement_theta_max      28.09

_exptl_crystal_description       irregular
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_absorpt_coefficient_mu    0.977
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.6800
_exptl_absorpt_correction_T_max  0.9455
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            24569
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.89
_diffrn_reflns_theta_max         28.29
_reflns_number_total             5360
_reflns_number_gt                4297
_reflns_threshold_expression     >2sigma(I)

_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    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0382P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5360
_refine_ls_number_parameters     250
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0359
_refine_ls_wR_factor_ref         0.0810
_refine_ls_wR_factor_gt          0.0749
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_restrained_S_all      1.220
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.84878(2) 0.844533(14) 0.912815(14) 0.01692(7) Uani 1 1 d . . .
P1 P 0.81462(5) 0.85926(3) 0.75806(3) 0.01339(10) Uani 1 1 d . . .
O1 O 1.15325(15) 0.86784(9) 0.95965(9) 0.0308(3) Uani 1 1 d . . .
O2 O 0.76208(16) 0.67997(9) 0.97561(10) 0.0320(3) Uani 1 1 d . . .
O3 O 0.67826(17) 0.96624(9) 1.00816(10) 0.0407(4) Uani 1 1 d . . .
N2 N 0.64451(15) 0.84722(9) 0.71596(9) 0.0163(3) Uani 1 1 d . . .
N1 N 0.76114(16) 0.88695(10) 0.53186(10) 0.0228(3) Uani 1 1 d . . .
N3 N 0.86124(14) 0.95379(9) 0.71891(9) 0.0151(3) Uani 1 1 d . . .
N4 N 0.90777(15) 0.79252(8) 0.69577(9) 0.0161(3) Uani 1 1 d . . .
C16 C 1.0348(2) 0.85988(11) 0.94150(12) 0.0214(4) Uani 1 1 d . . .
C3 C 0.52827(19) 0.86832(12) 0.77462(13) 0.0242(4) Uani 1 1 d . . .
H3 H 0.5698 0.9037 0.8262 0.029 Uiso 1 1 calc R . .
C5 C 0.4660(2) 0.79109(15) 0.81758(16) 0.0418(6) Uani 1 1 d . . .
H5A H 0.4213 0.7558 0.7690 0.063 Uiso 1 1 calc R . .
H5B H 0.3950 0.8080 0.8599 0.063 Uiso 1 1 calc R . .
H5C H 0.5418 0.7599 0.8515 0.063 Uiso 1 1 calc R . .
C4 C 0.4100(2) 0.91924(13) 0.72392(14) 0.0309(5) Uani 1 1 d . . .
H4A H 0.4508 0.9687 0.6965 0.046 Uiso 1 1 calc R . .
H4B H 0.3410 0.9365 0.7675 0.046 Uiso 1 1 calc R . .
H4C H 0.3624 0.8851 0.6753 0.046 Uiso 1 1 calc R . .
C2 C 0.60629(19) 0.80311(11) 0.62991(12) 0.0209(4) Uani 1 1 d . . .
H2A H 0.5071 0.7835 0.6309 0.025 Uiso 1 1 calc R . .
H2B H 0.6676 0.7534 0.6266 0.025 Uiso 1 1 calc R . .
C1 C 0.6200(2) 0.85547(11) 0.54298(12) 0.0234(4) Uani 1 1 d . . .
H1A H 0.5902 0.8211 0.4886 0.028 Uiso 1 1 calc R . .
H1B H 0.5539 0.9032 0.5443 0.028 Uiso 1 1 calc R . .
C6 C 0.7908(2) 0.97386(11) 0.55097(11) 0.0228(4) Uani 1 1 d . . .
H6A H 0.7272 1.0082 0.5096 0.027 Uiso 1 1 calc R . .
H6B H 0.8894 0.9858 0.5360 0.027 Uiso 1 1 calc R . .
C7 C 0.77307(19) 1.00078(11) 0.65065(11) 0.0183(4) Uani 1 1 d . . .
H7A H 0.7969 1.0607 0.6569 0.022 Uiso 1 1 calc R . .
H7B H 0.6724 0.9941 0.6639 0.022 Uiso 1 1 calc R . .
C8 C 0.99056(18) 0.99505(11) 0.76034(11) 0.0189(4) Uani 1 1 d . . .
H8 H 1.0489 0.9513 0.7939 0.023 Uiso 1 1 calc R . .
C9 C 0.9556(2) 1.06089(12) 0.83039(13) 0.0281(4) Uani 1 1 d . . .
H9A H 0.9012 1.1059 0.7993 0.042 Uiso 1 1 calc R . .
H9B H 1.0437 1.0834 0.8598 0.042 Uiso 1 1 calc R . .
H9C H 0.8993 1.0357 0.8772 0.042 Uiso 1 1 calc R . .
C10 C 1.0825(2) 1.03404(12) 0.68931(12) 0.0247(4) Uani 1 1 d . . .
H10A H 1.1089 0.9912 0.6456 0.037 Uiso 1 1 calc R . .
H10B H 1.1685 1.0575 0.7207 0.037 Uiso 1 1 calc R . .
H10C H 1.0292 1.0783 0.6562 0.037 Uiso 1 1 calc R . .
C11 C 0.8765(2) 0.82866(12) 0.52642(12) 0.0250(4) Uani 1 1 d . . .
H11A H 0.9338 0.8461 0.4753 0.030 Uiso 1 1 calc R . .
H11B H 0.8358 0.7733 0.5102 0.030 Uiso 1 1 calc R . .
C12 C 0.97600(19) 0.81887(12) 0.61307(12) 0.0217(4) Uani 1 1 d . . .
H12A H 1.0500 0.7776 0.6003 0.026 Uiso 1 1 calc R . .
H12B H 1.0240 0.8728 0.6261 0.026 Uiso 1 1 calc R . .
C13 C 0.94046(19) 0.70781(11) 0.73060(12) 0.0199(4) Uani 1 1 d . . .
H13 H 0.8762 0.6965 0.7809 0.024 Uiso 1 1 calc R . .
C15 C 1.0925(2) 0.70039(13) 0.77238(15) 0.0342(5) Uani 1 1 d . . .
H15A H 1.1586 0.7073 0.7240 0.051 Uiso 1 1 calc R . .
H15B H 1.1062 0.6454 0.8009 0.051 Uiso 1 1 calc R . .
H15C H 1.1101 0.7437 0.8191 0.051 Uiso 1 1 calc R . .
C14 C 0.9118(2) 0.64034(11) 0.65731(14) 0.0270(4) Uani 1 1 d . . .
H14A H 0.8149 0.6463 0.6297 0.041 Uiso 1 1 calc R . .
H14B H 0.9229 0.5852 0.6859 0.041 Uiso 1 1 calc R . .
H14C H 0.9792 0.6463 0.6095 0.041 Uiso 1 1 calc R . .
C17 C 0.79513(19) 0.74346(12) 0.94867(11) 0.0209(4) Uani 1 1 d . . .
C18 C 0.7437(2) 0.92082(12) 0.96921(12) 0.0245(4) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C17 1.7882(19) . ?
Ni1 C16 1.796(2) . ?
Ni1 C18 1.8086(19) . ?
Ni1 P1 2.2680(5) . ?
P1 N4 1.6894(14) . ?
P1 N3 1.6900(14) . ?
P1 N2 1.6927(14) . ?
O1 C16 1.140(2) . ?
O2 C17 1.143(2) . ?
O3 C18 1.133(2) . ?
N2 C2 1.464(2) . ?
N2 C3 1.476(2) . ?
N1 C11 1.443(2) . ?
N1 C1 1.446(2) . ?
N1 C6 1.446(2) . ?
N3 C7 1.463(2) . ?
N3 C8 1.482(2) . ?
N4 C12 1.467(2) . ?
N4 C13 1.477(2) . ?
C3 C5 1.525(3) . ?
C3 C4 1.534(3) . ?
C2 C1 1.533(2) . ?
C6 C7 1.535(2) . ?
C8 C9 1.521(2) . ?
C8 C10 1.530(2) . ?
C11 C12 1.530(3) . ?
C13 C15 1.527(3) . ?
C13 C14 1.532(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C17 Ni1 C16 110.42(8) . . ?
C17 Ni1 C18 107.84(8) . . ?
C16 Ni1 C18 111.12(8) . . ?
C17 Ni1 P1 111.15(6) . . ?
C16 Ni1 P1 106.75(6) . . ?
C18 Ni1 P1 109.59(6) . . ?
N4 P1 N3 103.34(7) . . ?
N4 P1 N2 104.46(7) . . ?
N3 P1 N2 104.07(7) . . ?
N4 P1 Ni1 115.05(5) . . ?
N3 P1 Ni1 113.96(5) . . ?
N2 P1 Ni1 114.59(5) . . ?
C2 N2 C3 117.17(14) . . ?
C2 N2 P1 122.61(12) . . ?
C3 N2 P1 119.34(11) . . ?
C11 N1 C1 119.06(15) . . ?
C11 N1 C6 119.91(16) . . ?
C1 N1 C6 118.95(15) . . ?
C7 N3 C8 117.55(13) . . ?
C7 N3 P1 122.87(11) . . ?
C8 N3 P1 119.37(11) . . ?
C12 N4 C13 117.02(13) . . ?
C12 N4 P1 122.17(11) . . ?
C13 N4 P1 120.26(11) . . ?
O1 C16 Ni1 178.56(16) . . ?
N2 C3 C5 111.96(16) . . ?
N2 C3 C4 112.99(15) . . ?
C5 C3 C4 110.00(16) . . ?
N2 C2 C1 114.37(14) . . ?
N1 C1 C2 114.48(14) . . ?
N1 C6 C7 114.92(14) . . ?
N3 C7 C6 113.84(14) . . ?
N3 C8 C9 111.90(15) . . ?
N3 C8 C10 113.46(14) . . ?
C9 C8 C10 109.20(15) . . ?
N1 C11 C12 116.47(15) . . ?
N4 C12 C11 115.29(15) . . ?
N4 C13 C15 112.23(15) . . ?
N4 C13 C14 112.86(14) . . ?
C15 C13 C14 109.88(15) . . ?
O2 C17 Ni1 176.91(16) . . ?
O3 C18 Ni1 176.71(17) . . ?

_diffrn_measured_fraction_theta_max 0.979
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.067
####################################################################### 
# 
# 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_jyy72
_database_code_depnum_ccdc_archive 'CCDC 1448470'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
'[Nickle(0)-tricarbonyl-(2,8,9-triisobutyl-2,3,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane)]'
_chemical_name_common            Ni(LiBu)(CO)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C21 H39 N4 Ni O3 P'
_chemical_formula_weight         485.24

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

_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                   10.4524(5)
_cell_length_b                   17.9047(8)
_cell_length_c                   13.5993(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.2348(6)
_cell_angle_gamma                90
_cell_volume                     2524.8(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9976
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      28.96

_exptl_crystal_description       irregular
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.287
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.139
_exptl_absorpt_coefficient_mu    0.859
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.890
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.8177
_exptl_absorpt_correction_T_max  0.9423
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_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 SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31264
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.890
_diffrn_reflns_theta_max         29.204
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6479
_reflns_number_gt                5607
_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 colorless crystal of approximate dimensions 0.139 x 0.235 x 0.287 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 (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.  The diffraction symmetry was 2/m and the systematic absences 
were consistent with the monoclinic space group P21/n that was later determined to be correct.

The structure was solved by direct 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 either located from a difference-Fourier map and refined 
(x,y,z and Uiso) or were included using a riding model (mixed refinement).  Carbon atoms 
C(16), C(17) and C(18) were disordered and included using multiple components with partial 
site-occupancy-factors.

At convergence, wR2 = 0.0701 and Goof = 1.029 for 431 variables refined against 6479 data 
(0.73Å), R1 = 0.0272 for those 5607 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)+(0.0363P)²+0.8703P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6479
_refine_ls_number_parameters     431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0272
_refine_ls_wR_factor_ref         0.0701
_refine_ls_wR_factor_gt          0.0665
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_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 0.33002(2) 0.83864(2) 0.36713(2) 0.01419(5) Uani 1 1 d . . . . .
P1 P 0.29209(3) 0.86759(2) 0.20493(2) 0.01139(7) Uani 1 1 d . . . . .
O1 O 0.18190(11) 0.94576(7) 0.47173(8) 0.0319(2) Uani 1 1 d . . . . .
O2 O 0.23226(13) 0.69110(6) 0.41350(10) 0.0429(3) Uani 1 1 d . . . . .
O3 O 0.60951(10) 0.83970(7) 0.42875(8) 0.0327(3) Uani 1 1 d . . . . .
N1 N 0.22815(12) 0.91431(7) -0.04135(8) 0.0244(3) Uani 1 1 d . . . . .
N2 N 0.13490(10) 0.86292(6) 0.15747(8) 0.0141(2) Uani 1 1 d . . . . .
N3 N 0.33651(9) 0.95527(6) 0.17854(7) 0.0133(2) Uani 1 1 d . . . . .
N4 N 0.36879(10) 0.81330(6) 0.12947(8) 0.0156(2) Uani 1 1 d . . . . .
C1 C 0.09929(14) 0.88999(9) -0.02729(10) 0.0243(3) Uani 1 1 d . . . . .
C2 C 0.09129(13) 0.83477(8) 0.05777(10) 0.0192(3) Uani 1 1 d . . . . .
C3 C 0.03855(12) 0.90387(7) 0.20566(10) 0.0162(2) Uani 1 1 d . . . . .
C4 C -0.07949(14) 0.85876(9) 0.22744(12) 0.0255(3) Uani 1 1 d . . . . .
C5 C -0.04137(17) 0.78966(11) 0.28903(16) 0.0397(4) Uani 1 1 d . . . . .
C6 C -0.16699(16) 0.91062(11) 0.27844(15) 0.0380(4) Uani 1 1 d . . . . .
C7 C 0.27190(14) 0.98697(8) -0.00425(10) 0.0238(3) Uani 1 1 d . . . . .
C8 C 0.26092(12) 1.00297(7) 0.10513(10) 0.0167(2) Uani 1 1 d . . . . .
C9 C 0.46656(12) 0.98096(7) 0.21630(9) 0.0157(2) Uani 1 1 d . . . . .
C10 C 0.47538(13) 1.05759(8) 0.26700(11) 0.0221(3) Uani 1 1 d . . . . .
C11 C 0.38852(18) 1.06318(11) 0.34817(15) 0.0398(4) Uani 1 1 d . . . . .
C12 C 0.61533(15) 1.07246(9) 0.30940(12) 0.0280(3) Uani 1 1 d . . . . .
C13 C 0.32423(16) 0.85690(9) -0.05046(10) 0.0264(3) Uani 1 1 d . . . . .
C14 C 0.42081(14) 0.84255(8) 0.04210(10) 0.0209(3) Uani 1 1 d . . . . .
C15 C 0.36639(13) 0.73168(7) 0.14015(11) 0.0181(3) Uani 1 1 d . . . . .
C16 C 0.4977(2) 0.69265(12) 0.1358(2) 0.0210(7) Uani 0.624(5) 1 d . . P A 1
H16 H 0.5213 0.6978 0.0671 0.025 Uiso 0.624(5) 1 calc R U P A 1
C17 C 0.6039(4) 0.7279(2) 0.2081(3) 0.0305(8) Uani 0.624(5) 1 d . . P A 1
H17A H 0.6848 0.7008 0.2055 0.046 Uiso 0.624(5) 1 calc R U P A 1
H17B H 0.5800 0.7254 0.2754 0.046 Uiso 0.624(5) 1 calc R U P A 1
H17C H 0.6151 0.7803 0.1899 0.046 Uiso 0.624(5) 1 calc R U P A 1
C18 C 0.4822(3) 0.60939(17) 0.1580(3) 0.0283(7) Uani 0.624(5) 1 d . . P A 1
H18A H 0.4590 0.6035 0.2252 0.043 Uiso 0.624(5) 1 calc R U P A 1
H18B H 0.5636 0.5834 0.1530 0.043 Uiso 0.624(5) 1 calc R U P A 1
H18C H 0.4141 0.5881 0.1102 0.043 Uiso 0.624(5) 1 calc R U P A 1
C16B C 0.4857(4) 0.6975(2) 0.2026(3) 0.0230(12) Uani 0.376(5) 1 d . . P A 2
H16B H 0.4887 0.7167 0.2719 0.028 Uiso 0.376(5) 1 calc R U P A 2
C17B C 0.6100(6) 0.7189(4) 0.1648(5) 0.0329(14) Uani 0.376(5) 1 d . . P A 2
H17D H 0.6210 0.7732 0.1688 0.049 Uiso 0.376(5) 1 calc R U P A 2
H17E H 0.6075 0.7028 0.0957 0.049 Uiso 0.376(5) 1 calc R U P A 2
H17F H 0.6824 0.6945 0.2053 0.049 Uiso 0.376(5) 1 calc R U P A 2
C18B C 0.4706(6) 0.6117(3) 0.2056(5) 0.0298(12) Uani 0.376(5) 1 d . . P A 2
H18D H 0.5450 0.5900 0.2469 0.045 Uiso 0.376(5) 1 calc R U P A 2
H18E H 0.4657 0.5916 0.1382 0.045 Uiso 0.376(5) 1 calc R U P A 2
H18F H 0.3914 0.5991 0.2337 0.045 Uiso 0.376(5) 1 calc R U P A 2
C19 C 0.24155(13) 0.90546(8) 0.43142(10) 0.0206(3) Uani 1 1 d . . . . .
C20 C 0.27010(14) 0.74793(8) 0.39158(11) 0.0240(3) Uani 1 1 d . . . . .
C21 C 0.50106(14) 0.84091(8) 0.40439(10) 0.0207(3) Uani 1 1 d . . . . .
H1A H 0.0542(16) 0.8631(10) -0.0895(13) 0.026(4) Uiso 1 1 d . . . . .
H1B H 0.0480(15) 0.9338(9) -0.0186(11) 0.019(4) Uiso 1 1 d . . . . .
H2A H 0.0049(16) 0.8196(9) 0.0553(12) 0.020(4) Uiso 1 1 d . . . . .
H2B H 0.1403(15) 0.7900(9) 0.0460(11) 0.018(4) Uiso 1 1 d . . . . .
H3A H 0.0027(15) 0.9468(9) 0.1668(12) 0.019(4) Uiso 1 1 d . . . . .
H3B H 0.0812(14) 0.9248(9) 0.2659(12) 0.016(4) Uiso 1 1 d . . . . .
H4A H -0.1308(16) 0.8408(8) 0.1632(12) 0.020(4) Uiso 1 1 d . . . . .
H5A H 0.013(2) 0.7536(13) 0.2532(17) 0.058(6) Uiso 1 1 d . . . . .
H5B H -0.118(2) 0.7602(12) 0.2957(15) 0.051(6) Uiso 1 1 d . . . . .
H5C H 0.007(2) 0.8084(13) 0.3568(18) 0.061(7) Uiso 1 1 d . . . . .
H6A H -0.193(2) 0.9591(14) 0.2352(18) 0.065(7) Uiso 1 1 d . . . . .
H6B H -0.1192(17) 0.9184(10) 0.3438(14) 0.029(4) Uiso 1 1 d . . . . .
H6C H -0.246(2) 0.8840(12) 0.2924(15) 0.049(6) Uiso 1 1 d . . . . .
H7A H 0.2202(17) 1.0255(10) -0.0409(13) 0.031(5) Uiso 1 1 d . . . . .
H7B H 0.3623(16) 0.9950(9) -0.0181(12) 0.022(4) Uiso 1 1 d . . . . .
H8A H 0.2888(15) 1.0542(9) 0.1179(11) 0.019(4) Uiso 1 1 d . . . . .
H8B H 0.1699(14) 0.9997(8) 0.1160(10) 0.011(3) Uiso 1 1 d . . . . .
H9A H 0.5218(15) 0.9819(9) 0.1617(12) 0.021(4) Uiso 1 1 d . . . . .
H9B H 0.5032(15) 0.9427(9) 0.2640(12) 0.022(4) Uiso 1 1 d . . . . .
H10A H 0.4503(16) 1.0961(9) 0.2162(13) 0.026(4) Uiso 1 1 d . . . . .
H11A H 0.299(2) 1.0504(12) 0.3209(15) 0.049(6) Uiso 1 1 d . . . . .
H11B H 0.3896(19) 1.1159(12) 0.3749(15) 0.043(5) Uiso 1 1 d . . . . .
H11C H 0.417(2) 1.0287(13) 0.4027(17) 0.053(6) Uiso 1 1 d . . . . .
H12A H 0.6735(18) 1.0689(10) 0.2562(14) 0.036(5) Uiso 1 1 d . . . . .
H12B H 0.6436(17) 1.0342(10) 0.3570(14) 0.032(5) Uiso 1 1 d . . . . .
H12C H 0.6262(18) 1.1231(11) 0.3407(14) 0.038(5) Uiso 1 1 d . . . . .
H13A H 0.3758(16) 0.8720(9) -0.1029(13) 0.025(4) Uiso 1 1 d . . . . .
H13B H 0.2803(17) 0.8111(10) -0.0723(13) 0.028(4) Uiso 1 1 d . . . . .
H14A H 0.4834(16) 0.8077(9) 0.0232(12) 0.021(4) Uiso 1 1 d . . . . .
H14B H 0.4684(15) 0.8885(9) 0.0603(11) 0.016(4) Uiso 1 1 d . . . . .
H15A H 0.3199(19) 0.7095(11) 0.0843(15) 0.041(5) Uiso 1 1 d . . . . .
H15B H 0.321(2) 0.7187(12) 0.1882(16) 0.050(6) Uiso 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C20 1.7869(14) . ?
Ni1 C21 1.7961(14) . ?
Ni1 C19 1.8040(14) . ?
Ni1 P1 2.2519(3) . ?
P1 N4 1.6876(11) . ?
P1 N3 1.6885(11) . ?
P1 N2 1.6899(11) . ?
O1 C19 1.1385(17) . ?
O2 C20 1.1447(18) . ?
O3 C21 1.1404(18) . ?
N1 C7 1.449(2) . ?
N1 C1 1.451(2) . ?
N1 C13 1.4532(19) . ?
N2 C2 1.4645(16) . ?
N2 C3 1.4654(16) . ?
N3 C9 1.4654(15) . ?
N3 C8 1.4668(15) . ?
N4 C14 1.4643(17) . ?
N4 C15 1.4691(17) . ?
C1 C2 1.532(2) . ?
C3 C4 1.5344(18) . ?
C4 C5 1.519(2) . ?
C4 C6 1.529(2) . ?
C7 C8 1.5332(19) . ?
C9 C10 1.5330(19) . ?
C10 C11 1.518(2) . ?
C10 C12 1.5267(19) . ?
C13 C14 1.533(2) . ?
C15 C16B 1.544(4) . ?
C15 C16 1.548(2) . ?
C16 C17 1.525(5) . ?
C16 C18 1.534(4) . ?
C16B C17B 1.506(8) . ?
C16B C18B 1.545(6) . ?

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
C20 Ni1 C21 109.14(6) . . ?
C20 Ni1 C19 107.43(7) . . ?
C21 Ni1 C19 113.64(6) . . ?
C20 Ni1 P1 111.64(5) . . ?
C21 Ni1 P1 108.50(4) . . ?
C19 Ni1 P1 106.52(4) . . ?
N4 P1 N3 104.00(5) . . ?
N4 P1 N2 104.64(5) . . ?
N3 P1 N2 104.18(5) . . ?
N4 P1 Ni1 115.12(4) . . ?
N3 P1 Ni1 113.77(4) . . ?
N2 P1 Ni1 113.93(4) . . ?
C7 N1 C1 118.76(12) . . ?
C7 N1 C13 118.28(12) . . ?
C1 N1 C13 117.52(13) . . ?
C2 N2 C3 115.78(10) . . ?
C2 N2 P1 123.02(9) . . ?
C3 N2 P1 119.63(8) . . ?
C9 N3 C8 116.88(10) . . ?
C9 N3 P1 119.03(8) . . ?
C8 N3 P1 123.16(8) . . ?
C14 N4 C15 116.66(11) . . ?
C14 N4 P1 122.74(9) . . ?
C15 N4 P1 119.84(9) . . ?
N1 C1 C2 115.66(11) . . ?
N2 C2 C1 115.90(11) . . ?
N2 C3 C4 115.95(11) . . ?
C5 C4 C6 112.01(15) . . ?
C5 C4 C3 111.95(12) . . ?
C6 C4 C3 108.02(13) . . ?
N1 C7 C8 116.54(11) . . ?
N3 C8 C7 116.86(11) . . ?
N3 C9 C10 116.05(11) . . ?
C11 C10 C12 110.25(13) . . ?
C11 C10 C9 112.24(12) . . ?
C12 C10 C9 109.05(12) . . ?
N1 C13 C14 116.05(12) . . ?
N4 C14 C13 116.93(12) . . ?
N4 C15 C16B 115.23(17) . . ?
N4 C15 C16 114.78(13) . . ?
C17 C16 C18 111.2(2) . . ?
C17 C16 C15 111.4(2) . . ?
C18 C16 C15 108.39(19) . . ?
C17B C16B C15 112.5(4) . . ?
C17B C16B C18B 111.0(4) . . ?
C15 C16B C18B 109.3(3) . . ?
O1 C19 Ni1 177.39(13) . . ?
O2 C20 Ni1 175.61(14) . . ?
O3 C21 Ni1 177.56(13) . . ?

_refine_diff_density_max         0.581
_refine_diff_density_min         -0.234
_refine_diff_density_rms         0.051

####################################################################### 
# 
# 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_jyy74s
_database_code_depnum_ccdc_archive 'CCDC 1448471'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'[Nickle(0)-tricarbonyl-(2,8,9-tribenzyl-2,3,8,9-tetraaza-1-phosphabicyclo[3,3,3]undecane)]'
_chemical_name_common            Ni(LBz)(CO)3
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H33 N4 Ni O3 P'
_chemical_formula_weight         587.28

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   9.7263(8)
_cell_length_b                   23.412(2)
_cell_length_c                   12.5881(11)
_cell_angle_alpha                90.00
_cell_angle_beta                 99.3160(10)
_cell_angle_gamma                90.00
_cell_volume                     2828.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9924
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      29.00

_exptl_crystal_description       irregular
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1232
_exptl_absorpt_coefficient_mu    0.781
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7788
_exptl_absorpt_correction_T_max  0.8748
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70276
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.74
_diffrn_reflns_theta_max         29.23
_reflns_number_total             7270
_reflns_number_gt                6422
_reflns_threshold_expression     >2sigma(I)

_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    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7270
_refine_ls_number_parameters     352
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1393
_refine_ls_wR_factor_gt          0.1283
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_restrained_S_all      1.168
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni -0.18002(2) 0.174315(8) 0.255603(16) 0.01474(10) Uani 1 1 d . . .
P1 P 0.04762(4) 0.170562(16) 0.24461(3) 0.01165(11) Uani 1 1 d . . .
O1 O -0.21788(16) 0.26550(7) 0.40785(11) 0.0370(3) Uani 1 1 d . . .
N1 N 0.38481(15) 0.15990(6) 0.23269(11) 0.0179(3) Uani 1 1 d . . .
C1 C 0.39898(16) 0.13646(7) 0.33996(13) 0.0181(3) Uani 1 1 d . . .
H1A H 0.4311 0.1671 0.3924 0.022 Uiso 1 1 calc R . .
H1B H 0.4719 0.1066 0.3478 0.022 Uiso 1 1 calc R . .
O2 O -0.35698(14) 0.18953(6) 0.04492(11) 0.0278(3) Uani 1 1 d . . .
N2 N 0.14639(13) 0.14985(6) 0.36100(10) 0.0140(3) Uani 1 1 d . . .
C2 C 0.26439(16) 0.11045(7) 0.36847(12) 0.0159(3) Uani 1 1 d . . .
H2A H 0.2369 0.0777 0.3199 0.019 Uiso 1 1 calc R . .
H2B H 0.2844 0.0954 0.4429 0.019 Uiso 1 1 calc R . .
O3 O -0.26849(14) 0.06254(6) 0.32688(11) 0.0318(3) Uani 1 1 d . . .
N3 N 0.08763(13) 0.12318(5) 0.15387(10) 0.0130(3) Uani 1 1 d . . .
C3 C 0.13010(17) 0.17914(6) 0.46032(13) 0.0154(3) Uani 1 1 d . . .
H3A H 0.0670 0.2121 0.4420 0.018 Uiso 1 1 calc R . .
H3B H 0.2220 0.1944 0.4936 0.018 Uiso 1 1 calc R . .
N4 N 0.11963(13) 0.23284(5) 0.21398(10) 0.0137(3) Uani 1 1 d . . .
C4 C 0.07321(16) 0.14268(7) 0.54292(12) 0.0150(3) Uani 1 1 d . . .
C5 C 0.01363(17) 0.08940(7) 0.51832(13) 0.0192(3) Uani 1 1 d . . .
H5 H 0.0091 0.0744 0.4477 0.023 Uiso 1 1 calc R . .
C6 C -0.03951(19) 0.05767(7) 0.59594(14) 0.0238(4) Uani 1 1 d . . .
H6 H -0.0803 0.0214 0.5779 0.029 Uiso 1 1 calc R . .
C7 C -0.03318(19) 0.07884(8) 0.69941(14) 0.0241(4) Uani 1 1 d . . .
H7 H -0.0696 0.0571 0.7523 0.029 Uiso 1 1 calc R . .
C8 C 0.02671(18) 0.13198(8) 0.72551(13) 0.0228(4) Uani 1 1 d . . .
H8 H 0.0316 0.1466 0.7964 0.027 Uiso 1 1 calc R . .
C9 C 0.07928(17) 0.16370(7) 0.64802(13) 0.0180(3) Uani 1 1 d . . .
H9 H 0.1198 0.2000 0.6663 0.022 Uiso 1 1 calc R . .
C10 C 0.34457(16) 0.12321(7) 0.14075(13) 0.0177(3) Uani 1 1 d . . .
H10A H 0.3564 0.0829 0.1644 0.021 Uiso 1 1 calc R . .
H10B H 0.4080 0.1302 0.0880 0.021 Uiso 1 1 calc R . .
C11 C 0.19387(16) 0.13206(7) 0.08479(12) 0.0152(3) Uani 1 1 d . . .
H11A H 0.1846 0.1714 0.0559 0.018 Uiso 1 1 calc R . .
H11B H 0.1750 0.1055 0.0229 0.018 Uiso 1 1 calc R . .
C12 C 0.02748(15) 0.06589(6) 0.15302(12) 0.0140(3) Uani 1 1 d . . .
H12A H 0.0049 0.0578 0.2255 0.017 Uiso 1 1 calc R . .
H12B H 0.0990 0.0379 0.1394 0.017 Uiso 1 1 calc R . .
C13 C -0.10299(15) 0.05635(6) 0.07045(12) 0.0138(3) Uani 1 1 d . . .
C14 C -0.19088(16) 0.01107(7) 0.08579(12) 0.0165(3) Uani 1 1 d . . .
H14 H -0.1683 -0.0128 0.1472 0.020 Uiso 1 1 calc R . .
C15 C -0.31092(17) 0.00045(7) 0.01250(13) 0.0198(3) Uani 1 1 d . . .
H15 H -0.3704 -0.0303 0.0241 0.024 Uiso 1 1 calc R . .
C16 C -0.34383(17) 0.03502(8) -0.07803(14) 0.0209(3) Uani 1 1 d . . .
H16 H -0.4257 0.0278 -0.1285 0.025 Uiso 1 1 calc R . .
C17 C -0.25720(17) 0.07992(8) -0.09450(13) 0.0206(3) Uani 1 1 d . . .
H17 H -0.2794 0.1035 -0.1564 0.025 Uiso 1 1 calc R . .
C18 C -0.13692(16) 0.09061(7) -0.02004(12) 0.0175(3) Uani 1 1 d . . .
H18 H -0.0779 0.1216 -0.0315 0.021 Uiso 1 1 calc R . .
C19 C 0.38069(16) 0.22118(7) 0.21933(13) 0.0172(3) Uani 1 1 d . . .
H19A H 0.3737 0.2300 0.1417 0.021 Uiso 1 1 calc R . .
H19B H 0.4697 0.2373 0.2565 0.021 Uiso 1 1 calc R . .
C20 C 0.26055(15) 0.25093(6) 0.26222(12) 0.0153(3) Uani 1 1 d . . .
H20A H 0.2719 0.2444 0.3409 0.018 Uiso 1 1 calc R . .
H20B H 0.2686 0.2926 0.2508 0.018 Uiso 1 1 calc R . .
C21 C 0.05690(17) 0.26386(7) 0.11659(12) 0.0159(3) Uani 1 1 d . . .
H21A H -0.0354 0.2469 0.0897 0.019 Uiso 1 1 calc R . .
H21B H 0.1161 0.2582 0.0604 0.019 Uiso 1 1 calc R . .
C22 C 0.03848(17) 0.32734(6) 0.13210(13) 0.0152(3) Uani 1 1 d . . .
C23 C -0.06404(17) 0.34764(7) 0.18832(13) 0.0207(3) Uani 1 1 d . . .
H23 H -0.1169 0.3214 0.2228 0.025 Uiso 1 1 calc R . .
C24 C -0.08956(18) 0.40585(8) 0.19430(14) 0.0248(4) Uani 1 1 d . . .
H24 H -0.1602 0.4191 0.2322 0.030 Uiso 1 1 calc R . .
C25 C -0.01252(19) 0.44480(7) 0.14526(14) 0.0239(4) Uani 1 1 d . . .
H25 H -0.0313 0.4845 0.1483 0.029 Uiso 1 1 calc R . .
C26 C 0.09223(19) 0.42525(7) 0.09170(14) 0.0230(4) Uani 1 1 d . . .
H26 H 0.1470 0.4517 0.0594 0.028 Uiso 1 1 calc R . .
C27 C 0.11731(17) 0.36690(7) 0.08514(13) 0.0187(3) Uani 1 1 d . . .
H27 H 0.1891 0.3539 0.0482 0.022 Uiso 1 1 calc R . .
C28 C -0.20298(18) 0.23007(8) 0.34796(14) 0.0224(3) Uani 1 1 d . . .
C29 C -0.28475(17) 0.18443(7) 0.12517(14) 0.0182(3) Uani 1 1 d . . .
C30 C -0.23159(17) 0.10589(7) 0.30090(14) 0.0216(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
Ni1 C28 1.7859(18) . ?
Ni1 C30 1.7987(17) . ?
Ni1 C29 1.8023(17) . ?
Ni1 P1 2.2424(5) . ?
P1 N3 1.6824(13) . ?
P1 N2 1.6879(13) . ?
P1 N4 1.6890(13) . ?
O1 C28 1.146(2) . ?
N1 C10 1.444(2) . ?
N1 C19 1.444(2) . ?
N1 C1 1.443(2) . ?
C1 C2 1.538(2) . ?
O2 C29 1.140(2) . ?
N2 C3 1.4570(19) . ?
N2 C2 1.4635(19) . ?
O3 C30 1.142(2) . ?
N3 C12 1.4627(19) . ?
N3 C11 1.4690(19) . ?
C3 C4 1.517(2) . ?
N4 C20 1.4688(19) . ?
N4 C21 1.4698(19) . ?
C4 C5 1.389(2) . ?
C4 C9 1.404(2) . ?
C5 C6 1.392(2) . ?
C6 C7 1.386(3) . ?
C7 C8 1.390(3) . ?
C8 C9 1.388(2) . ?
C10 C11 1.534(2) . ?
C12 C13 1.521(2) . ?
C13 C18 1.389(2) . ?
C13 C14 1.395(2) . ?
C14 C15 1.388(2) . ?
C15 C16 1.392(2) . ?
C16 C17 1.384(2) . ?
C17 C18 1.398(2) . ?
C19 C20 1.532(2) . ?
C21 C22 1.513(2) . ?
C22 C27 1.393(2) . ?
C22 C23 1.396(2) . ?
C23 C24 1.389(2) . ?
C24 C25 1.387(3) . ?
C25 C26 1.387(3) . ?
C26 C27 1.392(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C28 Ni1 C30 111.96(8) . . ?
C28 Ni1 C29 112.66(8) . . ?
C30 Ni1 C29 105.09(8) . . ?
C28 Ni1 P1 107.31(6) . . ?
C30 Ni1 P1 108.27(5) . . ?
C29 Ni1 P1 111.53(5) . . ?
N3 P1 N2 103.78(6) . . ?
N3 P1 N4 105.32(6) . . ?
N2 P1 N4 104.32(6) . . ?
N3 P1 Ni1 114.01(5) . . ?
N2 P1 Ni1 112.74(5) . . ?
N4 P1 Ni1 115.49(5) . . ?
C10 N1 C19 119.93(13) . . ?
C10 N1 C1 119.75(14) . . ?
C19 N1 C1 118.90(13) . . ?
N1 C1 C2 114.39(13) . . ?
C3 N2 C2 115.76(12) . . ?
C3 N2 P1 118.95(10) . . ?
C2 N2 P1 124.55(10) . . ?
N2 C2 C1 115.07(13) . . ?
C12 N3 C11 116.37(12) . . ?
C12 N3 P1 118.25(10) . . ?
C11 N3 P1 124.81(10) . . ?
N2 C3 C4 115.20(13) . . ?
C20 N4 C21 115.85(12) . . ?
C20 N4 P1 123.24(10) . . ?
C21 N4 P1 119.04(10) . . ?
C5 C4 C9 118.51(15) . . ?
C5 C4 C3 122.52(14) . . ?
C9 C4 C3 118.97(14) . . ?
C4 C5 C6 120.78(15) . . ?
C7 C6 C5 120.26(16) . . ?
C6 C7 C8 119.69(16) . . ?
C9 C8 C7 120.04(16) . . ?
C8 C9 C4 120.72(16) . . ?
N1 C10 C11 113.74(13) . . ?
N3 C11 C10 114.86(12) . . ?
N3 C12 C13 115.34(12) . . ?
C18 C13 C14 118.89(14) . . ?
C18 C13 C12 122.48(14) . . ?
C14 C13 C12 118.63(13) . . ?
C15 C14 C13 120.83(15) . . ?
C14 C15 C16 119.80(15) . . ?
C17 C16 C15 119.97(15) . . ?
C16 C17 C18 119.95(16) . . ?
C13 C18 C17 120.57(15) . . ?
N1 C19 C20 114.77(13) . . ?
N4 C20 C19 115.92(13) . . ?
N4 C21 C22 114.80(12) . . ?
C27 C22 C23 118.42(15) . . ?
C27 C22 C21 120.88(15) . . ?
C23 C22 C21 120.59(14) . . ?
C24 C23 C22 120.65(15) . . ?
C25 C24 C23 120.44(16) . . ?
C24 C25 C26 119.44(16) . . ?
C27 C26 C25 120.13(16) . . ?
C26 C27 C22 120.87(16) . . ?
O1 C28 Ni1 179.42(17) . . ?
O2 C29 Ni1 176.22(15) . . ?
O3 C30 Ni1 177.53(17) . . ?

_diffrn_measured_fraction_theta_max 0.946
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_jyy64s
_database_code_depnum_ccdc_archive 'CCDC 1448472'
_audit_update_record             
;
2016-01-19 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'[Nickle (0) dicarbonyl-(Bis(2,8,9-trimethyl-2,3,8,9-tetraaza-1-phosphabicyclo[3,3,3]))]'
_chemical_name_common            Ni(LMe)2(CO)2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H42 N8 Ni O2 P2'
_chemical_formula_weight         547.27

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   8.5551(5)
_cell_length_b                   19.4034(12)
_cell_length_c                   15.9663(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.7970(10)
_cell_angle_gamma                90.00
_cell_volume                     2562.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9782
_cell_measurement_theta_min      2.48
_cell_measurement_theta_max      29.12

_exptl_crystal_description       rectangular
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_absorpt_coefficient_mu    0.916
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.5853
_exptl_absorpt_correction_T_max  0.7980
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62910
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0082
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         29.20
_reflns_number_total             6562
_reflns_number_gt                6327
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6562
_refine_ls_number_parameters     304
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0232
_refine_ls_wR_factor_ref         0.1122
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.419842(15) 0.715705(7) 0.525127(8) 0.00823(8) Uani 1 1 d . . .
P1 P 0.60556(3) 0.650181(13) 0.613352(16) 0.00757(9) Uani 1 1 d . . .
O1 O 0.59249(12) 0.77956(5) 0.40902(6) 0.0237(2) Uani 1 1 d . . .
N1 N 0.88918(11) 0.53668(5) 0.73481(6) 0.01306(19) Uani 1 1 d . . .
C1 C 0.75826(13) 0.48754(6) 0.70412(7) 0.0140(2) Uani 1 1 d . . .
H1A H 0.7000 0.4817 0.7498 0.017 Uiso 1 1 calc R . .
H1B H 0.8062 0.4424 0.6959 0.017 Uiso 1 1 calc R . .
P2 P 0.30565(3) 0.799019(14) 0.584651(16) 0.00730(8) Uani 1 1 d . . .
O2 O 0.15835(10) 0.61883(5) 0.45256(6) 0.02149(19) Uani 1 1 d . . .
N2 N 0.54060(10) 0.56902(4) 0.62267(6) 0.01094(18) Uani 1 1 d . . .
C2 C 0.63548(13) 0.50680(5) 0.61985(7) 0.0124(2) Uani 1 1 d . . .
H2A H 0.6940 0.5128 0.5742 0.015 Uiso 1 1 calc R . .
H2B H 0.5599 0.4677 0.6023 0.015 Uiso 1 1 calc R . .
N3 N 0.68403(11) 0.67412(5) 0.71741(6) 0.00981(17) Uani 1 1 d . . .
C3 C 0.38962(13) 0.55829(6) 0.64684(8) 0.0151(2) Uani 1 1 d . . .
H3A H 0.4128 0.5415 0.7067 0.023 Uiso 1 1 calc R . .
H3B H 0.3239 0.5242 0.6080 0.023 Uiso 1 1 calc R . .
H3C H 0.3303 0.6019 0.6421 0.023 Uiso 1 1 calc R . .
N4 N 0.77259(10) 0.63747(5) 0.57679(6) 0.01002(18) Uani 1 1 d . . .
C4 C 0.87827(13) 0.58368(5) 0.80404(7) 0.0135(2) Uani 1 1 d . . .
H4A H 0.9703 0.6162 0.8133 0.016 Uiso 1 1 calc R . .
H4B H 0.8918 0.5565 0.8579 0.016 Uiso 1 1 calc R . .
N5 N 0.12391(12) 0.93021(5) 0.67266(6) 0.0159(2) Uani 1 1 d . . .
C5 C 0.72197(13) 0.62598(6) 0.79055(7) 0.0125(2) Uani 1 1 d . . .
H5A H 0.6305 0.5933 0.7834 0.015 Uiso 1 1 calc R . .
H5B H 0.7277 0.6526 0.8442 0.015 Uiso 1 1 calc R . .
N6 N 0.33872(11) 0.79893(5) 0.69345(6) 0.00996(18) Uani 1 1 d . . .
C6 C 0.73237(13) 0.74568(5) 0.73689(7) 0.0125(2) Uani 1 1 d . . .
H6A H 0.8506 0.7489 0.7528 0.019 Uiso 1 1 calc R . .
H6B H 0.6908 0.7619 0.7852 0.019 Uiso 1 1 calc R . .
H6C H 0.6881 0.7743 0.6857 0.019 Uiso 1 1 calc R . .
N7 N 0.35726(11) 0.88007(4) 0.56194(6) 0.01110(18) Uani 1 1 d . . .
C7 C 0.98086(12) 0.55951(6) 0.67504(7) 0.0138(2) Uani 1 1 d . . .
H7A H 0.9675 0.5250 0.6281 0.017 Uiso 1 1 calc R . .
H7B H 1.0968 0.5603 0.7063 0.017 Uiso 1 1 calc R . .
N8 N 0.10140(11) 0.80114(5) 0.55129(6) 0.00954(17) Uani 1 1 d . . .
C8 C 0.93567(12) 0.63060(5) 0.63347(7) 0.0118(2) Uani 1 1 d . . .
H8A H 0.9487 0.6651 0.6804 0.014 Uiso 1 1 calc R . .
H8B H 1.0140 0.6423 0.5995 0.014 Uiso 1 1 calc R . .
C9 C 0.75752(13) 0.62013(6) 0.48632(7) 0.0138(2) Uani 1 1 d . . .
H9A H 0.8036 0.5743 0.4827 0.021 Uiso 1 1 calc R . .
H9B H 0.8158 0.6543 0.4606 0.021 Uiso 1 1 calc R . .
H9C H 0.6431 0.6201 0.4548 0.021 Uiso 1 1 calc R . .
C10 C 0.21933(14) 0.90126(6) 0.75355(7) 0.0162(2) Uani 1 1 d . . .
H10A H 0.1490 0.8705 0.7773 0.019 Uiso 1 1 calc R . .
H10B H 0.2542 0.9394 0.7954 0.019 Uiso 1 1 calc R . .
C11 C 0.36959(13) 0.86052(6) 0.74738(7) 0.0135(2) Uani 1 1 d . . .
H11A H 0.4407 0.8915 0.7244 0.016 Uiso 1 1 calc R . .
H11B H 0.4295 0.8468 0.8066 0.016 Uiso 1 1 calc R . .
C12 C 0.31603(14) 0.73515(6) 0.73734(7) 0.0134(2) Uani 1 1 d . . .
H12A H 0.2788 0.6988 0.6943 0.020 Uiso 1 1 calc R . .
H12B H 0.2352 0.7425 0.7703 0.020 Uiso 1 1 calc R . .
H12C H 0.4188 0.7214 0.7769 0.020 Uiso 1 1 calc R . .
C13 C 0.20549(14) 0.97298(6) 0.62223(8) 0.0171(2) Uani 1 1 d . . .
H13A H 0.3080 0.9897 0.6610 0.021 Uiso 1 1 calc R . .
H13B H 0.1371 1.0138 0.6015 0.021 Uiso 1 1 calc R . .
C14 C 0.24409(13) 0.93778(5) 0.54367(7) 0.0139(2) Uani 1 1 d . . .
H14A H 0.1414 0.9211 0.5051 0.017 Uiso 1 1 calc R . .
H14B H 0.2884 0.9730 0.5112 0.017 Uiso 1 1 calc R . .
C15 C 0.52681(13) 0.89737(6) 0.57187(8) 0.0151(2) Uani 1 1 d . . .
H15A H 0.5634 0.9284 0.6214 0.023 Uiso 1 1 calc R . .
H15B H 0.5392 0.9202 0.5192 0.023 Uiso 1 1 calc R . .
H15C H 0.5918 0.8552 0.5817 0.023 Uiso 1 1 calc R . .
C16 C -0.02241(13) 0.89425(6) 0.62745(8) 0.0160(2) Uani 1 1 d . . .
H16A H -0.0682 0.9182 0.5719 0.019 Uiso 1 1 calc R . .
H16B H -0.1022 0.8982 0.6625 0.019 Uiso 1 1 calc R . .
C17 C -0.00314(12) 0.81744(5) 0.60805(7) 0.0121(2) Uani 1 1 d . . .
H17A H 0.0396 0.7933 0.6638 0.014 Uiso 1 1 calc R . .
H17B H -0.1118 0.7983 0.5816 0.014 Uiso 1 1 calc R . .
C18 C 0.02097(13) 0.79455(6) 0.45966(7) 0.0128(2) Uani 1 1 d . . .
H18A H -0.0200 0.8397 0.4365 0.019 Uiso 1 1 calc R . .
H18B H -0.0694 0.7621 0.4523 0.019 Uiso 1 1 calc R . .
H18C H 0.0981 0.7774 0.4285 0.019 Uiso 1 1 calc R . .
C19 C 0.52243(13) 0.75514(6) 0.45412(7) 0.0141(2) Uani 1 1 d . . .
C20 C 0.26157(13) 0.65719(6) 0.47937(7) 0.0134(2) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 C19 1.7747(11) . ?
Ni1 C20 1.7751(11) . ?
Ni1 P2 2.2238(3) . ?
Ni1 P1 2.2320(3) . ?
P1 N2 1.6892(9) . ?
P1 N3 1.6902(9) . ?
P1 N4 1.6939(9) . ?
O1 C19 1.1500(15) . ?
N1 C7 1.4507(14) . ?
N1 C4 1.4542(14) . ?
N1 C1 1.4572(14) . ?
C1 C2 1.5270(15) . ?
P2 N6 1.6871(9) . ?
P2 N8 1.6921(9) . ?
P2 N7 1.6975(9) . ?
O2 C20 1.1506(14) . ?
N2 C3 1.4544(13) . ?
N2 C2 1.4618(13) . ?
N3 C6 1.4595(13) . ?
N3 C5 1.4657(13) . ?
N4 C9 1.4565(13) . ?
N4 C8 1.4623(12) . ?
C4 C5 1.5365(15) . ?
N5 C13 1.4529(15) . ?
N5 C10 1.4530(15) . ?
N5 C16 1.4538(14) . ?
N6 C11 1.4571(13) . ?
N6 C12 1.4594(13) . ?
N7 C15 1.4575(13) . ?
N7 C14 1.4602(13) . ?
C7 C8 1.5369(15) . ?
N8 C18 1.4547(14) . ?
N8 C17 1.4613(13) . ?
C10 C11 1.5336(15) . ?
C13 C14 1.5365(16) . ?
C16 C17 1.5395(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C19 Ni1 C20 117.55(5) . . ?
C19 Ni1 P2 107.61(4) . . ?
C20 Ni1 P2 105.59(4) . . ?
C19 Ni1 P1 105.09(4) . . ?
C20 Ni1 P1 103.92(4) . . ?
P2 Ni1 P1 117.644(12) . . ?
N2 P1 N3 103.10(5) . . ?
N2 P1 N4 102.71(4) . . ?
N3 P1 N4 102.74(5) . . ?
N2 P1 Ni1 112.92(3) . . ?
N3 P1 Ni1 120.25(3) . . ?
N4 P1 Ni1 113.12(3) . . ?
C7 N1 C4 117.32(9) . . ?
C7 N1 C1 118.48(9) . . ?
C4 N1 C1 118.23(9) . . ?
N1 C1 C2 115.65(9) . . ?
N6 P2 N8 102.25(5) . . ?
N6 P2 N7 103.68(5) . . ?
N8 P2 N7 102.37(4) . . ?
N6 P2 Ni1 117.57(3) . . ?
N8 P2 Ni1 114.47(3) . . ?
N7 P2 Ni1 114.55(3) . . ?
C3 N2 C2 115.33(8) . . ?
C3 N2 P1 119.42(7) . . ?
C2 N2 P1 124.71(7) . . ?
N2 C2 C1 115.94(9) . . ?
C6 N3 C5 116.33(9) . . ?
C6 N3 P1 119.38(7) . . ?
C5 N3 P1 124.03(7) . . ?
C9 N4 C8 114.93(8) . . ?
C9 N4 P1 120.44(7) . . ?
C8 N4 P1 123.75(7) . . ?
N1 C4 C5 116.80(9) . . ?
C13 N5 C10 118.23(9) . . ?
C13 N5 C16 118.26(10) . . ?
C10 N5 C16 118.22(10) . . ?
N3 C5 C4 117.37(9) . . ?
C11 N6 C12 115.97(9) . . ?
C11 N6 P2 124.40(7) . . ?
C12 N6 P2 119.17(7) . . ?
C15 N7 C14 115.84(8) . . ?
C15 N7 P2 119.74(7) . . ?
C14 N7 P2 123.90(7) . . ?
N1 C7 C8 116.07(9) . . ?
C18 N8 C17 115.82(9) . . ?
C18 N8 P2 119.97(7) . . ?
C17 N8 P2 123.81(7) . . ?
N4 C8 C7 116.37(9) . . ?
N5 C10 C11 115.60(9) . . ?
N6 C11 C10 115.62(9) . . ?
N5 C13 C14 115.62(9) . . ?
N7 C14 C13 116.59(9) . . ?
N5 C16 C17 116.21(9) . . ?
N8 C17 C16 116.63(9) . . ?
O1 C19 Ni1 178.13(10) . . ?
O2 C20 Ni1 177.61(11) . . ?

_diffrn_measured_fraction_theta_max 0.945
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.055
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_jyy62a
_database_code_depnum_ccdc_archive 'CCDC 1448474'
_audit_update_record             
;
2016-01-20 deposited with the CCDC.
2016-02-16 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'[Nickle (0) dicarbonyl-(2,8,9-tri(2-pyridinemethyl)-2,3,8,9-tetraaza-1-phosphabicyclo-[3,3,3]undecane)]'
_chemical_name_common            Ni(TPAP)(CO)2
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C26 H30 N7 Ni O2 P'
_chemical_formula_weight         562.25

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

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   12.8799(6)
_cell_length_b                   14.0169(7)
_cell_length_c                   15.4714(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 109.6630(10)
_cell_angle_gamma                90.00
_cell_volume                     2630.3(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9897
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      29.09

_exptl_crystal_description       rectangular
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.11
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.836
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.7276
_exptl_absorpt_correction_T_max  0.9151
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32415
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.79
_diffrn_reflns_theta_max         29.27
_reflns_number_total             6760
_reflns_number_gt                5554
_reflns_threshold_expression     >2sigma(I)

_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    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0395P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6760
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0291
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0753
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.303344(15) 0.631870(13) 0.103635(13) 0.01202(6) Uani 1 1 d . . .
P1 P 0.23762(3) 0.76515(3) 0.02858(2) 0.01026(8) Uani 1 1 d . . .
O1 O 0.30040(9) 0.63286(8) 0.29145(8) 0.0234(3) Uani 1 1 d . . .
N1 N 0.18912(10) 0.97157(9) -0.07644(9) 0.0165(3) Uani 1 1 d . . .
C1 C 0.12250(13) 0.92145(11) -0.15715(10) 0.0192(3) Uani 1 1 d . . .
H1A H 0.1667 0.9101 -0.1975 0.023 Uiso 1 1 calc R . .
H1B H 0.0591 0.9621 -0.1911 0.023 Uiso 1 1 calc R . .
O2 O 0.18940(9) 0.45973(8) 0.01509(8) 0.0219(2) Uani 1 1 d . . .
N2 N 0.16034(9) 0.83741(8) 0.06929(8) 0.0119(2) Uani 1 1 d . . .
C2 C 0.07930(12) 0.82573(11) -0.13571(10) 0.0160(3) Uani 1 1 d . . .
H2A H 0.0298 0.8381 -0.1000 0.019 Uiso 1 1 calc R . .
H2B H 0.0346 0.7956 -0.1943 0.019 Uiso 1 1 calc R . .
N3 N 0.16445(10) 0.75792(9) -0.08449(8) 0.0125(2) Uani 1 1 d . . .
C3 C 0.14135(13) 0.99974(11) -0.00820(10) 0.0172(3) Uani 1 1 d . . .
H3A H 0.0601 0.9959 -0.0360 0.021 Uiso 1 1 calc R . .
H3B H 0.1606 1.0673 0.0081 0.021 Uiso 1 1 calc R . .
N4 N 0.34822(9) 0.83395(9) 0.03599(8) 0.0121(2) Uani 1 1 d . . .
C4 C 0.17724(12) 0.94057(10) 0.08035(10) 0.0150(3) Uani 1 1 d . . .
H4A H 0.2566 0.9524 0.1129 0.018 Uiso 1 1 calc R . .
H4B H 0.1366 0.9641 0.1202 0.018 Uiso 1 1 calc R . .
N5 N -0.05848(11) 0.80363(10) 0.16900(9) 0.0215(3) Uani 1 1 d . . .
C5 C 0.30609(12) 0.98096(10) -0.05839(11) 0.0172(3) Uani 1 1 d . . .
H5A H 0.3381 1.0226 -0.0043 0.021 Uiso 1 1 calc R . .
H5B H 0.3184 1.0119 -0.1116 0.021 Uiso 1 1 calc R . .
N6 N 0.13896(10) 0.53758(9) -0.22140(8) 0.0151(3) Uani 1 1 d . . .
C6 C 0.36523(12) 0.88465(10) -0.04055(10) 0.0149(3) Uani 1 1 d . . .
H6A H 0.3377 0.8449 -0.0966 0.018 Uiso 1 1 calc R . .
H6B H 0.4452 0.8950 -0.0270 0.018 Uiso 1 1 calc R . .
N7 N 0.46226(10) 0.64833(8) 0.10322(8) 0.0126(2) Uani 1 1 d . . .
C7 C 0.05965(11) 0.79627(10) 0.07748(10) 0.0139(3) Uani 1 1 d . . .
H7A H 0.0582 0.7273 0.0633 0.017 Uiso 1 1 calc R . .
H7B H -0.0045 0.8261 0.0306 0.017 Uiso 1 1 calc R . .
C8 C 0.04631(12) 0.80790(10) 0.17036(10) 0.0149(3) Uani 1 1 d . . .
C9 C 0.13516(13) 0.81750(11) 0.25099(11) 0.0183(3) Uani 1 1 d . . .
H9 H 0.2080 0.8225 0.2494 0.022 Uiso 1 1 calc R . .
C10 C 0.11601(15) 0.81968(11) 0.33410(11) 0.0237(4) Uani 1 1 d . . .
H10 H 0.1757 0.8247 0.3903 0.028 Uiso 1 1 calc R . .
C11 C 0.00858(15) 0.81445(12) 0.33351(12) 0.0275(4) Uani 1 1 d . . .
H11 H -0.0073 0.8156 0.3892 0.033 Uiso 1 1 calc R . .
C12 C -0.07483(15) 0.80752(13) 0.25014(12) 0.0290(4) Uani 1 1 d . . .
H12 H -0.1486 0.8054 0.2500 0.035 Uiso 1 1 calc R . .
C13 C 0.19359(11) 0.68399(10) -0.13801(10) 0.0131(3) Uani 1 1 d . . .
H13A H 0.2658 0.6569 -0.1009 0.016 Uiso 1 1 calc R . .
H13B H 0.2028 0.7139 -0.1929 0.016 Uiso 1 1 calc R . .
C14 C 0.11150(11) 0.60303(10) -0.16926(9) 0.0128(3) Uani 1 1 d . . .
C15 C 0.01655(12) 0.59590(11) -0.14594(10) 0.0174(3) Uani 1 1 d . . .
H15 H -0.0002 0.6431 -0.1085 0.021 Uiso 1 1 calc R . .
C16 C -0.05324(13) 0.51905(12) -0.17804(11) 0.0215(3) Uani 1 1 d . . .
H16 H -0.1193 0.5134 -0.1640 0.026 Uiso 1 1 calc R . .
C17 C -0.02548(13) 0.45061(11) -0.23093(11) 0.0213(3) Uani 1 1 d . . .
H17 H -0.0716 0.3969 -0.2536 0.026 Uiso 1 1 calc R . .
C18 C 0.07132(13) 0.46271(11) -0.24982(11) 0.0189(3) Uani 1 1 d . . .
H18 H 0.0911 0.4150 -0.2851 0.023 Uiso 1 1 calc R . .
C19 C 0.44523(11) 0.81999(10) 0.11781(10) 0.0134(3) Uani 1 1 d . . .
H19A H 0.4212 0.8120 0.1718 0.016 Uiso 1 1 calc R . .
H19B H 0.4921 0.8777 0.1280 0.016 Uiso 1 1 calc R . .
C20 C 0.51261(11) 0.73425(10) 0.11021(9) 0.0127(3) Uani 1 1 d . . .
C21 C 0.61990(12) 0.74337(11) 0.10956(10) 0.0162(3) Uani 1 1 d . . .
H21 H 0.6525 0.8048 0.1137 0.019 Uiso 1 1 calc R . .
C22 C 0.67936(12) 0.66270(11) 0.10290(10) 0.0186(3) Uani 1 1 d . . .
H22 H 0.7527 0.6677 0.1024 0.022 Uiso 1 1 calc R . .
C23 C 0.62852(12) 0.57485(11) 0.09708(10) 0.0181(3) Uani 1 1 d . . .
H23 H 0.6668 0.5180 0.0930 0.022 Uiso 1 1 calc R . .
C24 C 0.52113(12) 0.57077(10) 0.09724(10) 0.0153(3) Uani 1 1 d . . .
H24 H 0.4872 0.5100 0.0929 0.018 Uiso 1 1 calc R . .
C25 C 0.30506(12) 0.63448(10) 0.21826(11) 0.0156(3) Uani 1 1 d . . .
C26 C 0.23911(12) 0.52660(10) 0.04687(10) 0.0153(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
Ni1 C25 1.7665(16) . ?
Ni1 C26 1.7731(15) . ?
Ni1 N7 2.0619(12) . ?
Ni1 P1 2.2121(4) . ?
P1 N2 1.6837(12) . ?
P1 N3 1.6880(12) . ?
P1 N4 1.6919(12) . ?
O1 C25 1.1541(18) . ?
N1 C1 1.4380(19) . ?
N1 C5 1.4428(18) . ?
N1 C3 1.4445(18) . ?
C1 C2 1.531(2) . ?
O2 C26 1.1482(17) . ?
N2 C7 1.4633(17) . ?
N2 C4 1.4637(18) . ?
C2 N3 1.4662(18) . ?
N3 C13 1.4524(18) . ?
C3 C4 1.534(2) . ?
N4 C6 1.4595(18) . ?
N4 C19 1.4619(18) . ?
N5 C12 1.342(2) . ?
N5 C8 1.3440(19) . ?
C5 C6 1.5288(19) . ?
N6 C18 1.3401(19) . ?
N6 C14 1.3452(18) . ?
N7 C24 1.3463(18) . ?
N7 C20 1.3549(18) . ?
C7 C8 1.512(2) . ?
C8 C9 1.387(2) . ?
C9 C10 1.389(2) . ?
C10 C11 1.383(2) . ?
C11 C12 1.377(2) . ?
C13 C14 1.515(2) . ?
C14 C15 1.390(2) . ?
C15 C16 1.384(2) . ?
C16 C17 1.384(2) . ?
C17 C18 1.383(2) . ?
C19 C20 1.5099(19) . ?
C20 C21 1.391(2) . ?
C21 C22 1.389(2) . ?
C22 C23 1.383(2) . ?
C23 C24 1.385(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C25 Ni1 C26 111.14(7) . . ?
C25 Ni1 N7 108.89(6) . . ?
C26 Ni1 N7 112.94(6) . . ?
C25 Ni1 P1 112.51(5) . . ?
C26 Ni1 P1 114.23(5) . . ?
N7 Ni1 P1 96.25(3) . . ?
N2 P1 N3 103.28(6) . . ?
N2 P1 N4 102.83(6) . . ?
N3 P1 N4 105.56(6) . . ?
N2 P1 Ni1 118.80(4) . . ?
N3 P1 Ni1 118.35(5) . . ?
N4 P1 Ni1 106.32(4) . . ?
C1 N1 C5 119.45(12) . . ?
C1 N1 C3 119.45(12) . . ?
C5 N1 C3 120.50(13) . . ?
N1 C1 C2 113.22(12) . . ?
C7 N2 C4 118.71(11) . . ?
C7 N2 P1 116.62(9) . . ?
C4 N2 P1 123.69(9) . . ?
N3 C2 C1 115.15(12) . . ?
C13 N3 C2 116.37(12) . . ?
C13 N3 P1 118.20(9) . . ?
C2 N3 P1 125.20(10) . . ?
N1 C3 C4 115.51(12) . . ?
C6 N4 C19 116.73(11) . . ?
C6 N4 P1 125.13(10) . . ?
C19 N4 P1 115.92(9) . . ?
N2 C4 C3 116.20(12) . . ?
C12 N5 C8 117.16(14) . . ?
N1 C5 C6 112.26(12) . . ?
C18 N6 C14 117.24(13) . . ?
N4 C6 C5 112.01(12) . . ?
C24 N7 C20 117.25(12) . . ?
C24 N7 Ni1 119.50(10) . . ?
C20 N7 Ni1 123.24(9) . . ?
N2 C7 C8 115.29(12) . . ?
N5 C8 C9 122.59(14) . . ?
N5 C8 C7 114.51(13) . . ?
C9 C8 C7 122.82(13) . . ?
C8 C9 C10 119.02(15) . . ?
C11 C10 C9 118.81(16) . . ?
C12 C11 C10 118.27(15) . . ?
N5 C12 C11 124.11(16) . . ?
N3 C13 C14 115.46(12) . . ?
N6 C14 C15 122.58(14) . . ?
N6 C14 C13 113.96(12) . . ?
C15 C14 C13 123.47(13) . . ?
C16 C15 C14 119.00(14) . . ?
C15 C16 C17 119.08(14) . . ?
C18 C17 C16 118.07(14) . . ?
N6 C18 C17 124.01(14) . . ?
N4 C19 C20 112.67(11) . . ?
N7 C20 C21 122.08(13) . . ?
N7 C20 C19 116.20(12) . . ?
C21 C20 C19 121.72(13) . . ?
C22 C21 C20 119.97(14) . . ?
C23 C22 C21 117.96(14) . . ?
C22 C23 C24 119.20(14) . . ?
N7 C24 C23 123.54(14) . . ?
O1 C25 Ni1 175.82(13) . . ?
O2 C26 Ni1 172.49(13) . . ?

_diffrn_measured_fraction_theta_max 0.941
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.059
