# 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_iPr2PPrDINi
_database_code_depnum_ccdc_archive 'CCDC 1586336'
_audit_update_record             
;
2017-11-17 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            iPr2PPrDINi
_chemical_formula_moiety         'C22 H46 N2 Ni P2'
_chemical_formula_sum            'C22 H46 N2 Ni P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         459.26

_chemical_melting_point          ?

_space_group_crystal_system      triclinic
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.0477(5)
_cell_length_b                   10.1518(6)
_cell_length_c                   15.4698(9)
_cell_angle_alpha                94.4200(10)
_cell_angle_beta                 100.1970(10)
_cell_angle_gamma                115.7230(10)
_cell_volume                     1240.76(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4465
_cell_measurement_theta_min      2.4274
_cell_measurement_theta_max      25.0714
_cell_measurement_temperature    123.(2)

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear dark red-orange'
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.182
_exptl_crystal_size_min          0.104
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             500

_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.91

_exptl_special_details           
;
;

_diffrn_ambient_temperature      123.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       'ω and φ scans'

_diffrn_detector_area_resol_mean 8.3330

_diffrn_reflns_number            10079
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_theta_min         2.26
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18

_refine_special_details          
;
;

_reflns_number_total             4368
_reflns_number_gt                3867
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1071
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.070
_refine_ls_number_reflns         4368
_refine_ls_number_parameters     254
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0641P)²+0.0916P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.246
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2013.6-2 (Bruker-AXS, 2013)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0.29774(4) 0.24812(3) 0.22771(2) 0.01743(12) Uani d . . . 1 . .
P P1 0.24222(8) 0.05990(7) 0.29393(4) 0.01874(17) Uani d . . . 1 . .
P P2 0.18737(8) 0.38645(7) 0.26710(4) 0.01921(17) Uani d . . . 1 . .
N N1 0.2931(3) 0.1538(2) 0.11312(13) 0.0206(5) Uani d . . . 1 . .
N N2 0.4982(3) 0.4067(2) 0.20723(14) 0.0211(5) Uani d . . . 1 . .
C C1 0.4462(4) 0.1794(3) -0.00902(18) 0.0322(7) Uani d . . . 1 . .
H H1A 0.476 0.0985 -0.0004 0.048 Uiso calc U . R 1 . .
H H1B 0.5373 0.2597 -0.0274 0.048 Uiso calc U . R 1 . .
H H1C 0.3416 0.1424 -0.0553 0.048 Uiso calc U . R 1 . .
C C2 0.4215(3) 0.2372(3) 0.07721(17) 0.0232(6) Uani d . . . 1 . .
C C3 0.5274(3) 0.3826(3) 0.12628(17) 0.0235(6) Uani d . . . 1 . .
C C4 0.6637(4) 0.5004(3) 0.0924(2) 0.0332(7) Uani d . . . 1 . .
H H4A 0.6301 0.5771 0.0776 0.05 Uiso calc U . R 1 . .
H H4B 0.6804 0.4555 0.039 0.05 Uiso calc U . R 1 . .
H H4C 0.7692 0.5452 0.1387 0.05 Uiso calc U . R 1 . .
C C5 0.1944(3) -0.0028(3) 0.07098(17) 0.0266(6) Uani d . . . 1 . .
H H5A 0.273 -0.0449 0.0647 0.032 Uiso calc U . R 1 . .
H H5B 0.1317 -0.0086 0.0103 0.032 Uiso calc U . R 1 . .
C C6 0.0700(3) -0.0973(3) 0.12175(17) 0.0268(6) Uani d . . . 1 . .
H H6A -0.0015 -0.1972 0.0852 0.032 Uiso calc U . R 1 . .
H H6B -0.0047 -0.0523 0.1314 0.032 Uiso calc U . R 1 . .
C C7 0.1560(3) -0.1131(3) 0.21209(18) 0.0276(6) Uani d . . . 1 . .
H H7A 0.2485 -0.1371 0.2047 0.033 Uiso calc U . R 1 . .
H H7B 0.0732 -0.1959 0.2347 0.033 Uiso calc U . R 1 . .
C C8 0.0880(3) 0.0079(3) 0.36599(19) 0.0293(6) Uani d . . . 1 . .
H H8 0.1178 0.0997 0.4086 0.035 Uiso calc U . R 1 . .
C C9 -0.0899(4) -0.0410(3) 0.3089(2) 0.0401(8) Uani d . . . 1 . .
H H9A -0.1291 -0.1374 0.2713 0.06 Uiso calc U . R 1 . .
H H9B -0.0873 0.0327 0.2711 0.06 Uiso calc U . R 1 . .
H H9C -0.1669 -0.0496 0.3478 0.06 Uiso calc U . R 1 . .
C C10 0.0851(5) -0.1116(4) 0.4219(2) 0.0465(9) Uani d . . . 1 . .
H H10A -0.0027 -0.1332 0.4554 0.07 Uiso calc U . R 1 . .
H H10B 0.1951 -0.0755 0.4635 0.07 Uiso calc U . R 1 . .
H H10C 0.0611 -0.2022 0.3823 0.07 Uiso calc U . R 1 . .
C C11 0.4315(3) 0.0599(3) 0.36446(18) 0.0278(6) Uani d . . . 1 . .
H H11 0.3992 -0.0393 0.383 0.033 Uiso calc U . R 1 . .
C C12 0.5662(4) 0.0898(4) 0.3109(2) 0.0400(8) Uani d . . . 1 . .
H H12A 0.5921 0.1835 0.2889 0.06 Uiso calc U . R 1 . .
H H12B 0.524 0.0086 0.2603 0.06 Uiso calc U . R 1 . .
H H12C 0.6686 0.0964 0.3492 0.06 Uiso calc U . R 1 . .
C C13 0.5011(4) 0.1793(4) 0.4471(2) 0.0425(8) Uani d . . . 1 . .
H H13A 0.6055 0.1838 0.4817 0.064 Uiso calc U . R 1 . .
H H13B 0.4179 0.1555 0.4837 0.064 Uiso calc U . R 1 . .
H H13C 0.5249 0.2756 0.4291 0.064 Uiso calc U . R 1 . .
C C14 0.5955(3) 0.5591(3) 0.25686(18) 0.0282(6) Uani d . . . 1 . .
H H14A 0.5983 0.629 0.2152 0.034 Uiso calc U . R 1 . .
H H14B 0.7131 0.5777 0.2807 0.034 Uiso calc U . R 1 . .
C C15 0.5256(3) 0.5912(3) 0.33324(18) 0.0290(6) Uani d . . . 1 . .
H H15A 0.604 0.6918 0.3673 0.035 Uiso calc U . R 1 . .
H H15B 0.5182 0.5191 0.3739 0.035 Uiso calc U . R 1 . .
C C16 0.3511(3) 0.5820(3) 0.30109(18) 0.0272(6) Uani d . . . 1 . .
H H16A 0.3511 0.6348 0.2499 0.033 Uiso calc U . R 1 . .
H H16B 0.3247 0.6314 0.3496 0.033 Uiso calc U . R 1 . .
C C17 0.0776(3) 0.3639(3) 0.36000(17) 0.0242(6) Uani d . . . 1 . .
H H17 -0.0061 0.2568 0.3512 0.029 Uiso calc U . R 1 . .
C C18 -0.0199(4) 0.4548(3) 0.3650(2) 0.0358(7) Uani d . . . 1 . .
H H18A -0.0701 0.4383 0.4168 0.054 Uiso calc U . R 1 . .
H H18B -0.1093 0.4237 0.3105 0.054 Uiso calc U . R 1 . .
H H18C 0.0575 0.5605 0.3709 0.054 Uiso calc U . R 1 . .
C C19 0.2039(4) 0.3989(3) 0.44902(17) 0.0298(6) Uani d . . . 1 . .
H H19A 0.2774 0.5062 0.4644 0.045 Uiso calc U . R 1 . .
H H19B 0.2725 0.3472 0.4439 0.045 Uiso calc U . R 1 . .
H H19C 0.1427 0.3657 0.4958 0.045 Uiso calc U . R 1 . .
C C20 0.0373(4) 0.3967(3) 0.17203(18) 0.0303(7) Uani d . . . 1 . .
H H20 0.0111 0.4795 0.19 0.036 Uiso calc U . R 1 . .
C C21 -0.1259(4) 0.2516(3) 0.1471(2) 0.0379(7) Uani d . . . 1 . .
H H21A -0.2015 0.2561 0.0949 0.057 Uiso calc U . R 1 . .
H H21B -0.1807 0.2363 0.1973 0.057 Uiso calc U . R 1 . .
H H21C -0.1004 0.169 0.1332 0.057 Uiso calc U . R 1 . .
C C22 0.1191(4) 0.4287(4) 0.09272(19) 0.0417(8) Uani d . . . 1 . .
H H22A 0.1538 0.3524 0.0779 0.063 Uiso calc U . R 1 . .
H H22B 0.2182 0.5264 0.1082 0.063 Uiso calc U . R 1 . .
H H22C 0.0377 0.4277 0.0413 0.063 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N2 . 1.931(2) ?
Ni1 N1 . 1.933(2) ?
Ni1 P1 . 2.1455(7) ?
Ni1 P2 . 2.1544(7) ?
P1 C7 . 1.848(3) ?
P1 C11 . 1.861(3) ?
P1 C8 . 1.863(3) ?
P2 C16 . 1.850(3) ?
P2 C20 . 1.859(3) ?
P2 C17 . 1.861(3) ?
N1 C2 . 1.350(3) ?
N1 C5 . 1.467(3) ?
N2 C3 . 1.350(3) ?
N2 C14 . 1.468(3) ?
C1 C2 . 1.508(4) ?
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?
C2 C3 . 1.420(4) ?
C3 C4 . 1.506(4) ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
C5 C6 . 1.515(4) ?
C5 H5A . 0.99 ?
C5 H5B . 0.99 ?
C6 C7 . 1.530(4) ?
C6 H6A . 0.99 ?
C6 H6B . 0.99 ?
C7 H7A . 0.99 ?
C7 H7B . 0.99 ?
C8 C9 . 1.534(4) ?
C8 C10 . 1.537(4) ?
C8 H8 . 1.0 ?
C9 H9A . 0.98 ?
C9 H9B . 0.98 ?
C9 H9C . 0.98 ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
C11 C13 . 1.521(4) ?
C11 C12 . 1.529(4) ?
C11 H11 . 1.0 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?
C14 C15 . 1.512(4) ?
C14 H14A . 0.99 ?
C14 H14B . 0.99 ?
C15 C16 . 1.528(4) ?
C15 H15A . 0.99 ?
C15 H15B . 0.99 ?
C16 H16A . 0.99 ?
C16 H16B . 0.99 ?
C17 C19 . 1.531(4) ?
C17 C18 . 1.536(4) ?
C17 H17 . 1.0 ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?
C19 H19A . 0.98 ?
C19 H19B . 0.98 ?
C19 H19C . 0.98 ?
C20 C21 . 1.523(4) ?
C20 C22 . 1.527(4) ?
C20 H20 . 1.0 ?
C21 H21A . 0.98 ?
C21 H21B . 0.98 ?
C21 H21C . 0.98 ?
C22 H22A . 0.98 ?
C22 H22B . 0.98 ?
C22 H22C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N2 Ni1 N1 . . 82.46(9) ?
N2 Ni1 P1 . . 136.15(6) ?
N1 Ni1 P1 . . 97.54(7) ?
N2 Ni1 P2 . . 96.12(6) ?
N1 Ni1 P2 . . 133.06(6) ?
P1 Ni1 P2 . . 113.80(3) ?
C7 P1 C11 . . 102.27(12) ?
C7 P1 C8 . . 101.69(13) ?
C11 P1 C8 . . 103.44(13) ?
C7 P1 Ni1 . . 110.71(9) ?
C11 P1 Ni1 . . 114.01(9) ?
C8 P1 Ni1 . . 122.31(9) ?
C16 P2 C20 . . 102.47(13) ?
C16 P2 C17 . . 101.08(12) ?
C20 P2 C17 . . 103.87(12) ?
C16 P2 Ni1 . . 110.10(9) ?
C20 P2 Ni1 . . 112.30(9) ?
C17 P2 Ni1 . . 124.45(9) ?
C2 N1 C5 . . 116.1(2) ?
C2 N1 Ni1 . . 113.92(17) ?
C5 N1 Ni1 . . 128.48(17) ?
C3 N2 C14 . . 116.0(2) ?
C3 N2 Ni1 . . 113.90(17) ?
C14 N2 Ni1 . . 128.30(17) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 C3 . . 114.6(2) ?
N1 C2 C1 . . 121.9(2) ?
C3 C2 C1 . . 123.5(2) ?
N2 C3 C2 . . 114.4(2) ?
N2 C3 C4 . . 122.3(2) ?
C2 C3 C4 . . 123.3(2) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
N1 C5 C6 . . 114.2(2) ?
N1 C5 H5A . . 108.7 ?
C6 C5 H5A . . 108.7 ?
N1 C5 H5B . . 108.7 ?
C6 C5 H5B . . 108.7 ?
H5A C5 H5B . . 107.6 ?
C5 C6 C7 . . 113.0(2) ?
C5 C6 H6A . . 109.0 ?
C7 C6 H6A . . 109.0 ?
C5 C6 H6B . . 109.0 ?
C7 C6 H6B . . 109.0 ?
H6A C6 H6B . . 107.8 ?
C6 C7 P1 . . 111.04(18) ?
C6 C7 H7A . . 109.4 ?
P1 C7 H7A . . 109.4 ?
C6 C7 H7B . . 109.4 ?
P1 C7 H7B . . 109.4 ?
H7A C7 H7B . . 108.0 ?
C9 C8 C10 . . 109.3(2) ?
C9 C8 P1 . . 109.6(2) ?
C10 C8 P1 . . 116.0(2) ?
C9 C8 H8 . . 107.2 ?
C10 C8 H8 . . 107.2 ?
P1 C8 H8 . . 107.2 ?
C8 C9 H9A . . 109.5 ?
C8 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C8 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C8 C10 H10A . . 109.5 ?
C8 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
C8 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
C13 C11 C12 . . 109.7(3) ?
C13 C11 P1 . . 109.86(19) ?
C12 C11 P1 . . 109.44(19) ?
C13 C11 H11 . . 109.3 ?
C12 C11 H11 . . 109.3 ?
P1 C11 H11 . . 109.3 ?
C11 C12 H12A . . 109.5 ?
C11 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C11 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C11 C13 H13A . . 109.5 ?
C11 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C11 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?
N2 C14 C15 . . 113.8(2) ?
N2 C14 H14A . . 108.8 ?
C15 C14 H14A . . 108.8 ?
N2 C14 H14B . . 108.8 ?
C15 C14 H14B . . 108.8 ?
H14A C14 H14B . . 107.7 ?
C14 C15 C16 . . 112.2(2) ?
C14 C15 H15A . . 109.2 ?
C16 C15 H15A . . 109.2 ?
C14 C15 H15B . . 109.2 ?
C16 C15 H15B . . 109.2 ?
H15A C15 H15B . . 107.9 ?
C15 C16 P2 . . 110.89(18) ?
C15 C16 H16A . . 109.5 ?
P2 C16 H16A . . 109.5 ?
C15 C16 H16B . . 109.5 ?
P2 C16 H16B . . 109.5 ?
H16A C16 H16B . . 108.0 ?
C19 C17 C18 . . 109.8(2) ?
C19 C17 P2 . . 109.83(18) ?
C18 C17 P2 . . 115.35(19) ?
C19 C17 H17 . . 107.2 ?
C18 C17 H17 . . 107.2 ?
P2 C17 H17 . . 107.2 ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C17 C19 H19A . . 109.5 ?
C17 C19 H19B . . 109.5 ?
H19A C19 H19B . . 109.5 ?
C17 C19 H19C . . 109.5 ?
H19A C19 H19C . . 109.5 ?
H19B C19 H19C . . 109.5 ?
C21 C20 C22 . . 110.6(2) ?
C21 C20 P2 . . 110.15(19) ?
C22 C20 P2 . . 109.2(2) ?
C21 C20 H20 . . 109.0 ?
C22 C20 H20 . . 109.0 ?
P2 C20 H20 . . 109.0 ?
C20 C21 H21A . . 109.5 ?
C20 C21 H21B . . 109.5 ?
H21A C21 H21B . . 109.5 ?
C20 C21 H21C . . 109.5 ?
H21A C21 H21C . . 109.5 ?
H21B C21 H21C . . 109.5 ?
C20 C22 H22A . . 109.5 ?
C20 C22 H22B . . 109.5 ?
H22A C22 H22B . . 109.5 ?
C20 C22 H22C . . 109.5 ?
H22A C22 H22C . . 109.5 ?
H22B C22 H22C . . 109.5 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C5 N1 C2 C3 . . . . -172.3(2) ?
Ni1 N1 C2 C3 . . . . -5.0(3) ?
C5 N1 C2 C1 . . . . 8.8(3) ?
Ni1 N1 C2 C1 . . . . 176.04(18) ?
C14 N2 C3 C2 . . . . -175.1(2) ?
Ni1 N2 C3 C2 . . . . -9.2(3) ?
C14 N2 C3 C4 . . . . 6.0(3) ?
Ni1 N2 C3 C4 . . . . 171.94(19) ?
N1 C2 C3 N2 . . . . 9.4(3) ?
C1 C2 C3 N2 . . . . -171.7(2) ?
N1 C2 C3 C4 . . . . -171.8(2) ?
C1 C2 C3 C4 . . . . 7.1(4) ?
C2 N1 C5 C6 . . . . 170.9(2) ?
Ni1 N1 C5 C6 . . . . 5.9(3) ?
N1 C5 C6 C7 . . . . -66.2(3) ?
C5 C6 C7 P1 . . . . 74.4(3) ?
C11 P1 C7 C6 . . . . -147.85(19) ?
C8 P1 C7 C6 . . . . 105.4(2) ?
Ni1 P1 C7 C6 . . . . -26.0(2) ?
C7 P1 C8 C9 . . . . -57.8(2) ?
C11 P1 C8 C9 . . . . -163.59(19) ?
Ni1 P1 C8 C9 . . . . 66.2(2) ?
C7 P1 C8 C10 . . . . 66.6(3) ?
C11 P1 C8 C10 . . . . -39.2(3) ?
Ni1 P1 C8 C10 . . . . -169.4(2) ?
C7 P1 C11 C13 . . . . -169.1(2) ?
C8 P1 C11 C13 . . . . -63.7(2) ?
Ni1 P1 C11 C13 . . . . 71.4(2) ?
C7 P1 C11 C12 . . . . 70.4(2) ?
C8 P1 C11 C12 . . . . 175.8(2) ?
Ni1 P1 C11 C12 . . . . -49.1(2) ?
C3 N2 C14 C15 . . . . 163.6(2) ?
Ni1 N2 C14 C15 . . . . 0.1(3) ?
N2 C14 C15 C16 . . . . -64.9(3) ?
C14 C15 C16 P2 . . . . 75.7(2) ?
C20 P2 C16 C15 . . . . -145.11(19) ?
C17 P2 C16 C15 . . . . 107.8(2) ?
Ni1 P2 C16 C15 . . . . -25.5(2) ?
C16 P2 C17 C19 . . . . -57.6(2) ?
C20 P2 C17 C19 . . . . -163.55(18) ?
Ni1 P2 C17 C19 . . . . 66.4(2) ?
C16 P2 C17 C18 . . . . 67.1(2) ?
C20 P2 C17 C18 . . . . -38.9(2) ?
Ni1 P2 C17 C18 . . . . -168.89(16) ?
C16 P2 C20 C21 . . . . -168.1(2) ?
C17 P2 C20 C21 . . . . -63.2(2) ?
Ni1 P2 C20 C21 . . . . 73.8(2) ?
C16 P2 C20 C22 . . . . 70.3(2) ?
C17 P2 C20 C22 . . . . 175.2(2) ?
Ni1 P2 C20 C22 . . . . -47.8(2) ?

####################################################################### 
# 
# 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_tBu2PPrDINi
_database_code_depnum_ccdc_archive 'CCDC 1586337'
_audit_update_record             
;
2017-11-17 deposited with the CCDC.
2018-06-14 downloaded from the CCDC.
;
_chemical_name_systematic        ?
_chemical_name_common            tBu2PPrDINi
_chemical_formula_moiety         'C26 H54 N2 Ni P2'
_chemical_formula_sum            'C26 H54 N2 Ni P2'
_chemical_formula_iupac          ?
_chemical_formula_weight         515.36

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   13.1585(5)
_cell_length_b                   17.2832(7)
_cell_length_c                   12.2496(5)
_cell_angle_alpha                90
_cell_angle_beta                 91.5308(6)
_cell_angle_gamma                90
_cell_volume                     2784.82(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5176
_cell_measurement_theta_min      2.3568
_cell_measurement_theta_max      25.0365
_cell_measurement_temperature    123.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.137
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1128

_exptl_absorpt_coefficient_mu    0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_T_max  0.90

_exptl_special_details           
;
;

_diffrn_ambient_temperature      123.(2)

_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'sealed tube'

_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  graphite

_diffrn_measurement_device_type  'Bruker Smart APEX'
_diffrn_measurement_method       'ω and φ scans'

_diffrn_detector_area_resol_mean 8.3330

_diffrn_reflns_number            11141
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    ?
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14

_refine_special_details          
;
;

_reflns_number_total             2458
_reflns_number_gt                2251
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0396
_refine_ls_R_factor_gt           0.0370
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.0957
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_number_reflns         2458
_refine_ls_number_parameters     148
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0602P)²+1.1440P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.027
_refine_diff_density_min         -0.193
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'

_computing_data_collection       'Bruker Instrument Service v2010.9.0.0'
_computing_cell_refinement       'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XShell ver. 6.3.1 (Bruker AXS, 2004)'
_computing_publication_material  'Bruker APEX2 v2013.6-2 (Bruker-AXS, 2013)'

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni1 0 0.32176(2) 0.25 0.01481(15) Uani d T P S 1 . .
P P1 0.14724(4) 0.37481(3) 0.20496(4) 0.01455(16) Uani d . . . 1 . .
N N1 0.01105(12) 0.23530(10) 0.14768(13) 0.0176(4) Uani d . . . 1 . .
C C1 0.03122(17) 0.09259(13) 0.1285(2) 0.0283(5) Uani d . . . 1 . .
H H1A -0.015 0.0904 0.0645 0.042 Uiso calc U . R 1 . .
H H1B 0.0206 0.047 0.1744 0.042 Uiso calc U . R 1 . .
H H1C 0.1017 0.0934 0.1046 0.042 Uiso calc U . R 1 . .
C C2 0.01017(15) 0.16490(12) 0.19323(18) 0.0202(5) Uani d . . . 1 . .
C C3 0.03962(16) 0.23986(12) 0.03283(16) 0.0219(5) Uani d . . . 1 . .
H H3A -0.0189 0.2238 -0.0143 0.026 Uiso calc U . R 1 . .
H H3B 0.0962 0.2034 0.0202 0.026 Uiso calc U . R 1 . .
C C4 0.07203(16) 0.32063(12) 0.00076(17) 0.0205(5) Uani d . . . 1 . .
H H4A 0.0168 0.3574 0.0171 0.025 Uiso calc U . R 1 . .
H H4B 0.0825 0.3221 -0.0789 0.025 Uiso calc U . R 1 . .
C C5 0.16976(15) 0.34658(12) 0.06043(16) 0.0196(4) Uani d . . . 1 . .
H H5A 0.1989 0.3912 0.0213 0.023 Uiso calc U . R 1 . .
H H5B 0.2199 0.3039 0.0595 0.023 Uiso calc U . R 1 . .
C C6 0.25403(16) 0.32402(11) 0.28563(17) 0.0186(5) Uani d . . . 1 . .
C C7 0.24324(16) 0.23676(12) 0.26546(19) 0.0250(5) Uani d . . . 1 . .
H H7A 0.2953 0.209 0.3087 0.038 Uiso calc U . R 1 . .
H H7B 0.2519 0.2258 0.1878 0.038 Uiso calc U . R 1 . .
H H7C 0.1757 0.2197 0.287 0.038 Uiso calc U . R 1 . .
C C8 0.23880(17) 0.33774(13) 0.40783(17) 0.0256(5) Uani d . . . 1 . .
H H8A 0.2891 0.3078 0.4504 0.038 Uiso calc U . R 1 . .
H H8B 0.1702 0.3213 0.4269 0.038 Uiso calc U . R 1 . .
H H8C 0.2473 0.3929 0.4242 0.038 Uiso calc U . R 1 . .
C C9 0.36245(16) 0.34750(14) 0.25729(19) 0.0261(5) Uani d . . . 1 . .
H H9A 0.3764 0.3998 0.2848 0.039 Uiso calc U . R 1 . .
H H9B 0.3694 0.3467 0.1778 0.039 Uiso calc U . R 1 . .
H H9C 0.4109 0.3111 0.2911 0.039 Uiso calc U . R 1 . .
C C10 0.18061(15) 0.48213(11) 0.19849(16) 0.0174(4) Uani d . . . 1 . .
C C11 0.18631(17) 0.51617(12) 0.31389(16) 0.0233(5) Uani d . . . 1 . .
H H11A 0.1793 0.5726 0.3099 0.035 Uiso calc U . R 1 . .
H H11B 0.252 0.503 0.3487 0.035 Uiso calc U . R 1 . .
H H11C 0.1313 0.4947 0.357 0.035 Uiso calc U . R 1 . .
C C12 0.27865(16) 0.50511(13) 0.14076(17) 0.0236(5) Uani d . . . 1 . .
H H12A 0.276 0.4856 0.0656 0.035 Uiso calc U . R 1 . .
H H12B 0.3375 0.4827 0.18 0.035 Uiso calc U . R 1 . .
H H12C 0.2849 0.5616 0.1399 0.035 Uiso calc U . R 1 . .
C C13 0.09183(16) 0.51956(13) 0.13366(17) 0.0227(5) Uani d . . . 1 . .
H H13A 0.0275 0.5055 0.1669 0.034 Uiso calc U . R 1 . .
H H13B 0.0917 0.5011 0.058 0.034 Uiso calc U . R 1 . .
H H13C 0.0997 0.5759 0.1347 0.034 Uiso calc U . R 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 N1 . 1.9582(17) ?
Ni1 N1 2 1.9582(17) ?
Ni1 P1 2 2.2261(5) ?
Ni1 P1 . 2.2262(5) ?
P1 C5 . 1.868(2) ?
P1 C10 . 1.908(2) ?
P1 C6 . 1.910(2) ?
N1 C2 . 1.339(3) ?
N1 C3 . 1.468(3) ?
C1 C2 . 1.509(3) ?
C1 H1A . 0.98 ?
C1 H1B . 0.98 ?
C1 H1C . 0.98 ?
C2 C2 2 1.423(4) ?
C3 C4 . 1.515(3) ?
C3 H3A . 0.99 ?
C3 H3B . 0.99 ?
C4 C5 . 1.529(3) ?
C4 H4A . 0.99 ?
C4 H4B . 0.99 ?
C5 H5A . 0.99 ?
C5 H5B . 0.99 ?
C6 C9 . 1.532(3) ?
C6 C8 . 1.534(3) ?
C6 C7 . 1.534(3) ?
C7 H7A . 0.98 ?
C7 H7B . 0.98 ?
C7 H7C . 0.98 ?
C8 H8A . 0.98 ?
C8 H8B . 0.98 ?
C8 H8C . 0.98 ?
C9 H9A . 0.98 ?
C9 H9B . 0.98 ?
C9 H9C . 0.98 ?
C10 C11 . 1.531(3) ?
C10 C13 . 1.538(3) ?
C10 C12 . 1.540(3) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 H12A . 0.98 ?
C12 H12B . 0.98 ?
C12 H12C . 0.98 ?
C13 H13A . 0.98 ?
C13 H13B . 0.98 ?
C13 H13C . 0.98 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 . 2 80.53(10) ?
N1 Ni1 P1 . 2 123.57(5) ?
N1 Ni1 P1 2 2 94.34(5) ?
N1 Ni1 P1 . . 94.34(5) ?
N1 Ni1 P1 2 . 123.57(5) ?
P1 Ni1 P1 2 . 131.35(3) ?
C5 P1 C10 . . 99.91(9) ?
C5 P1 C6 . . 103.72(9) ?
C10 P1 C6 . . 107.53(9) ?
C5 P1 Ni1 . . 106.77(7) ?
C10 P1 Ni1 . . 127.84(6) ?
C6 P1 Ni1 . . 108.40(7) ?
C2 N1 C3 . . 116.97(16) ?
C2 N1 Ni1 . . 115.16(14) ?
C3 N1 Ni1 . . 126.71(13) ?
C2 C1 H1A . . 109.5 ?
C2 C1 H1B . . 109.5 ?
H1A C1 H1B . . 109.5 ?
C2 C1 H1C . . 109.5 ?
H1A C1 H1C . . 109.5 ?
H1B C1 H1C . . 109.5 ?
N1 C2 C2 . 2 114.28(11) ?
N1 C2 C1 . . 122.00(19) ?
C2 C2 C1 2 . 123.71(12) ?
N1 C3 C4 . . 112.28(16) ?
N1 C3 H3A . . 109.1 ?
C4 C3 H3A . . 109.1 ?
N1 C3 H3B . . 109.1 ?
C4 C3 H3B . . 109.1 ?
H3A C3 H3B . . 107.9 ?
C3 C4 C5 . . 112.66(18) ?
C3 C4 H4A . . 109.1 ?
C5 C4 H4A . . 109.1 ?
C3 C4 H4B . . 109.1 ?
C5 C4 H4B . . 109.1 ?
H4A C4 H4B . . 107.8 ?
C4 C5 P1 . . 112.15(14) ?
C4 C5 H5A . . 109.2 ?
P1 C5 H5A . . 109.2 ?
C4 C5 H5B . . 109.2 ?
P1 C5 H5B . . 109.2 ?
H5A C5 H5B . . 107.9 ?
C9 C6 C8 . . 109.08(18) ?
C9 C6 C7 . . 107.86(17) ?
C8 C6 C7 . . 107.16(17) ?
C9 C6 P1 . . 115.97(14) ?
C8 C6 P1 . . 108.68(14) ?
C7 C6 P1 . . 107.75(14) ?
C6 C7 H7A . . 109.5 ?
C6 C7 H7B . . 109.5 ?
H7A C7 H7B . . 109.5 ?
C6 C7 H7C . . 109.5 ?
H7A C7 H7C . . 109.5 ?
H7B C7 H7C . . 109.5 ?
C6 C8 H8A . . 109.5 ?
C6 C8 H8B . . 109.5 ?
H8A C8 H8B . . 109.5 ?
C6 C8 H8C . . 109.5 ?
H8A C8 H8C . . 109.5 ?
H8B C8 H8C . . 109.5 ?
C6 C9 H9A . . 109.5 ?
C6 C9 H9B . . 109.5 ?
H9A C9 H9B . . 109.5 ?
C6 C9 H9C . . 109.5 ?
H9A C9 H9C . . 109.5 ?
H9B C9 H9C . . 109.5 ?
C11 C10 C13 . . 109.44(17) ?
C11 C10 C12 . . 107.69(17) ?
C13 C10 C12 . . 106.78(16) ?
C11 C10 P1 . . 109.93(14) ?
C13 C10 P1 . . 104.94(13) ?
C12 C10 P1 . . 117.80(14) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C10 C12 H12A . . 109.5 ?
C10 C12 H12B . . 109.5 ?
H12A C12 H12B . . 109.5 ?
C10 C12 H12C . . 109.5 ?
H12A C12 H12C . . 109.5 ?
H12B C12 H12C . . 109.5 ?
C10 C13 H13A . . 109.5 ?
C10 C13 H13B . . 109.5 ?
H13A C13 H13B . . 109.5 ?
C10 C13 H13C . . 109.5 ?
H13A C13 H13C . . 109.5 ?
H13B C13 H13C . . 109.5 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C3 N1 C2 C2 . . . 2 175.2(2) ?
Ni1 N1 C2 C2 . . . 2 6.7(3) ?
C3 N1 C2 C1 . . . . -3.6(3) ?
Ni1 N1 C2 C1 . . . . -172.12(15) ?
C2 N1 C3 C4 . . . . -160.94(18) ?
Ni1 N1 C3 C4 . . . . 6.1(2) ?
N1 C3 C4 C5 . . . . 65.5(2) ?
C3 C4 C5 P1 . . . . -76.24(19) ?
C10 P1 C5 C4 . . . . -115.43(15) ?
C6 P1 C5 C4 . . . . 133.63(15) ?
Ni1 P1 C5 C4 . . . . 19.23(16) ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C7 H7C N1 2 0.98 2.62 3.538(3) 156.5 ?


# start Validation Reply Form
_vrf_PLAT094_tBu2PPrDINi         
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PROBLEM: Ratio of Maximum / Minimum Residual Density ....       5.32 Report
RESPONSE: Maximum residual density within 1.0 Angstrom of P1.
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# end Validation Reply Form





