#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:45:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179862 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/58/7015832.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7015832
loop_
_publ_author_name
'Cariou, Renan'
'Dahcheh, Fatme'
'Graham, Todd W.'
'Stephan, Douglas W.'
_publ_section_title
;
 Mononuclear and dinuclear palladium and nickel complexes of
 phosphinimine-based tridentate ligands.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4918
_journal_page_last               4925
_journal_paper_doi               10.1039/c1dt10131e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C59 H50 Cl3 N3 Ni2 P2'
_chemical_formula_weight         1086.73
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 133.969(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   33.823(3)
_cell_length_b                   8.9261(9)
_cell_length_c                   23.968(2)
_cell_measurement_temperature    150(2)
_cell_volume                     5207.9(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0901
_diffrn_reflns_av_sigmaI/netI    0.1340
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21713
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  0.9526
_exptl_absorpt_correction_T_min  0.9083
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.871
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         5929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.1676
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1305P)²+1.3647P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1653
_refine_ls_wR_factor_ref         0.2239
_reflns_number_gt                2836
_reflns_number_total             5929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10131e.txt
_cod_data_source_block           '[N(N=PPh3)2NiCl2]'
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7015832
loop_
_symmetry_equiv_pos_as_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'
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 0.05672(3) 0.47369(8) 0.79546(4) 0.0375(3) Uani 1 1 d . . .
Cl1 Cl 0.0000 0.6775(2) 0.7500 0.0508(6) Uani 1 2 d S . .
Cl2 Cl 0.08993(7) 0.4961(2) 0.74290(10) 0.0555(5) Uani 1 1 d . . .
N1 N 0.08114(18) 0.4116(5) 0.8950(2) 0.0318(10) Uani 1 1 d . . .
N2 N 0.0000 0.3119(7) 0.7500 0.0336(15) Uani 1 2 d S . .
P1 P 0.12589(6) 0.50303(15) 0.97414(8) 0.0303(4) Uani 1 1 d . . .
C1 C 0.1902(2) 0.4039(7) 1.0433(3) 0.0351(13) Uani 1 1 d . . .
C2 C 0.2358(2) 0.4651(8) 1.1122(4) 0.0455(16) Uani 1 1 d . . .
H2A H 0.2339 0.5619 1.1266 0.055 Uiso 1 1 calc R . .
C3 C 0.2847(3) 0.3865(9) 1.1610(4) 0.0572(19) Uani 1 1 d . . .
H3A H 0.3160 0.4297 1.2091 0.069 Uiso 1 1 calc R . .
C4 C 0.2889(3) 0.2478(10) 1.1415(5) 0.065(2) Uani 1 1 d . . .
H4A H 0.3229 0.1956 1.1752 0.078 Uiso 1 1 calc R . .
C5 C 0.2433(3) 0.1846(9) 1.0724(5) 0.065(2) Uani 1 1 d . . .
H5A H 0.2456 0.0875 1.0586 0.078 Uiso 1 1 calc R . .
C6 C 0.1939(3) 0.2628(7) 1.0227(4) 0.0466(16) Uani 1 1 d . . .
H6A H 0.1626 0.2196 0.9747 0.056 Uiso 1 1 calc R . .
C7 C 0.1407(2) 0.6680(6) 0.9491(3) 0.0320(13) Uani 1 1 d . . .
C8 C 0.1159(2) 0.8042(6) 0.9370(4) 0.0430(15) Uani 1 1 d . . .
H8A H 0.0938 0.8138 0.9479 0.052 Uiso 1 1 calc R . .
C9 C 0.1229(3) 0.9247(7) 0.9093(4) 0.0542(18) Uani 1 1 d . . .
H9A H 0.1048 1.0164 0.8996 0.065 Uiso 1 1 calc R . .
C10 C 0.1558(3) 0.9144(7) 0.8956(4) 0.0498(17) Uani 1 1 d . . .
H10F H 0.1615 0.9995 0.8781 0.060 Uiso 1 1 calc R . .
C11 C 0.1807(3) 0.7803(7) 0.9072(4) 0.0496(16) Uani 1 1 d . . .
H11A H 0.2033 0.7725 0.8973 0.060 Uiso 1 1 calc R . .
C12 C 0.1728(3) 0.6580(7) 0.9331(4) 0.0464(16) Uani 1 1 d . . .
H12A H 0.1896 0.5653 0.9402 0.056 Uiso 1 1 calc R . .
C13 C 0.1005(2) 0.5611(6) 1.0163(3) 0.0307(12) Uani 1 1 d . . .
C14 C 0.1326(2) 0.5636(7) 1.0963(3) 0.0423(15) Uani 1 1 d . . .
H14A H 0.1695 0.5290 1.1313 0.051 Uiso 1 1 calc R . .
C15 C 0.1108(3) 0.6160(8) 1.1241(4) 0.0527(18) Uani 1 1 d . . .
H15A H 0.1328 0.6185 1.1784 0.063 Uiso 1 1 calc R . .
C16 C 0.0570(3) 0.6650(7) 1.0737(4) 0.0468(16) Uani 1 1 d . . .
H16A H 0.0424 0.7009 1.0936 0.056 Uiso 1 1 calc R . .
C17 C 0.0246(3) 0.6624(7) 0.9951(4) 0.0442(15) Uani 1 1 d . . .
H17A H -0.0123 0.6972 0.9605 0.053 Uiso 1 1 calc R . .
C18 C 0.0465(2) 0.6075(7) 0.9664(4) 0.0398(14) Uani 1 1 d . . .
H18A H 0.0239 0.6022 0.9120 0.048 Uiso 1 1 calc R . .
C19 C 0.0521(2) 0.2844(6) 0.8863(3) 0.0317(13) Uani 1 1 d . . .
C20 C 0.0623(2) 0.2097(6) 0.9464(3) 0.0360(13) Uani 1 1 d . . .
H20A H 0.0894 0.2471 0.9978 0.043 Uiso 1 1 calc R . .
C21 C 0.0330(3) 0.0814(7) 0.9318(4) 0.0421(15) Uani 1 1 d . . .
H21A H 0.0398 0.0326 0.9730 0.051 Uiso 1 1 calc R . .
C22 C -0.0053(3) 0.0258(7) 0.8586(4) 0.0448(15) Uani 1 1 d . . .
H22A H -0.0241 -0.0641 0.8492 0.054 Uiso 1 1 calc R . .
C23 C -0.0171(3) 0.0989(6) 0.7973(4) 0.0411(14) Uani 1 1 d . . .
H23A H -0.0445 0.0598 0.7463 0.049 Uiso 1 1 calc R . .
C24 C 0.0107(2) 0.2287(6) 0.8100(3) 0.0353(13) Uani 1 1 d . . .
C101 C -0.3791(3) 0.5785(11) 0.1493(5) 0.075(2) Uani 1 1 d . . .
H10G H -0.4124 0.5252 0.1225 0.090 Uiso 1 1 calc R . .
C102 C -0.3661(3) 0.6987(9) 0.1956(5) 0.071(2) Uani 1 1 d . . .
H10D H -0.3910 0.7291 0.1995 0.085 Uiso 1 1 calc R . .
C103 C -0.3185(4) 0.7738(10) 0.2355(5) 0.082(3) Uani 1 1 d . . .
H10E H -0.3097 0.8551 0.2681 0.098 Uiso 1 1 calc R . .
C104 C -0.2826(4) 0.7321(11) 0.2286(6) 0.088(3) Uani 1 1 d . . .
H10A H -0.2492 0.7854 0.2560 0.105 Uiso 1 1 calc R . .
C105 C -0.2951(4) 0.6150(13) 0.1825(5) 0.080(3) Uani 1 1 d . . .
H10C H -0.2704 0.5868 0.1779 0.096 Uiso 1 1 calc R . .
C106 C -0.3439(4) 0.5358(11) 0.1419(5) 0.080(3) Uani 1 1 d . . .
H10B H -0.3526 0.4537 0.1097 0.096 Uiso 1 1 calc R . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
N1 Ni1 N2 83.99(14) . . ?
N1 Ni1 Cl2 139.48(14) . . ?
N2 Ni1 Cl2 115.35(7) . . ?
N1 Ni1 Cl1 107.74(13) . . ?
N2 Ni1 Cl1 98.23(13) . . ?
Cl2 Ni1 Cl1 104.27(6) . . ?
N1 Ni1 Ni1 97.88(13) . 2_556 ?
N2 Ni1 Ni1 45.86(12) . 2_556 ?
Cl2 Ni1 Ni1 121.43(6) . 2_556 ?
Cl1 Ni1 Ni1 52.38(4) . 2_556 ?
Ni1 Cl1 Ni1 75.25(7) 2_556 . ?
C19 N1 P1 124.7(4) . . ?
C19 N1 Ni1 112.3(3) . . ?
P1 N1 Ni1 122.9(3) . . ?
C24 N2 C24 117.2(6) 2_556 . ?
C24 N2 Ni1 110.4(3) 2_556 2_556 ?
C24 N2 Ni1 113.5(2) . 2_556 ?
C24 N2 Ni1 113.5(2) 2_556 . ?
C24 N2 Ni1 110.4(3) . . ?
Ni1 N2 Ni1 88.3(2) 2_556 . ?
N1 P1 C7 106.1(2) . . ?
N1 P1 C13 112.7(2) . . ?
C7 P1 C13 107.8(3) . . ?
N1 P1 C1 112.5(3) . . ?
C7 P1 C1 105.8(3) . . ?
C13 P1 C1 111.6(2) . . ?
C2 C1 C6 119.2(6) . . ?
C2 C1 P1 122.9(5) . . ?
C6 C1 P1 117.8(5) . . ?
C1 C2 C3 120.2(7) . . ?
C4 C3 C2 121.2(7) . . ?
C3 C4 C5 119.2(6) . . ?
C4 C5 C6 120.1(7) . . ?
C1 C6 C5 120.1(6) . . ?
C12 C7 C8 118.4(5) . . ?
C12 C7 P1 119.7(4) . . ?
C8 C7 P1 121.5(4) . . ?
C9 C8 C7 120.4(6) . . ?
C10 C9 C8 120.6(6) . . ?
C9 C10 C11 119.8(6) . . ?
C12 C11 C10 120.0(6) . . ?
C11 C12 C7 120.7(6) . . ?
C18 C13 C14 119.0(5) . . ?
C18 C13 P1 117.4(4) . . ?
C14 C13 P1 123.6(4) . . ?
C15 C14 C13 120.0(5) . . ?
C14 C15 C16 120.5(6) . . ?
C17 C16 C15 120.6(6) . . ?
C16 C17 C18 119.2(6) . . ?
C13 C18 C17 120.7(6) . . ?
C20 C19 C24 118.6(5) . . ?
C20 C19 N1 125.6(5) . . ?
C24 C19 N1 115.8(5) . . ?
C21 C20 C19 120.8(6) . . ?
C22 C21 C20 119.9(5) . . ?
C21 C22 C23 120.7(6) . . ?
C24 C23 C22 120.5(6) . . ?
C23 C24 C19 119.4(5) . . ?
C23 C24 N2 123.8(5) . . ?
C19 C24 N2 116.8(5) . . ?
C106 C101 C102 120.0(9) . . ?
C103 C102 C101 121.0(8) . . ?
C102 C103 C104 119.7(9) . . ?
C105 C104 C103 119.9(9) . . ?
C104 C105 C106 120.7(9) . . ?
C101 C106 C105 118.7(9) . . ?
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 N1 1.986(4) . ?
Ni1 N2 2.013(5) . ?
Ni1 Cl2 2.2029(17) . ?
Ni1 Cl1 2.2964(18) . ?
Ni1 Ni1 2.8037(15) 2_556 ?
Cl1 Ni1 2.2963(18) 2_556 ?
N1 C19 1.419(7) . ?
N1 P1 1.603(5) . ?
N2 C24 1.425(6) 2_556 ?
N2 C24 1.425(6) . ?
N2 Ni1 2.013(4) 2_556 ?
P1 C7 1.788(6) . ?
P1 C13 1.799(5) . ?
P1 C1 1.805(6) . ?
C1 C2 1.367(8) . ?
C1 C6 1.389(8) . ?
C2 C3 1.383(9) . ?
C3 C4 1.365(11) . ?
C4 C5 1.377(11) . ?
C5 C6 1.392(9) . ?
C7 C12 1.383(8) . ?
C7 C8 1.388(8) . ?
C8 C9 1.369(9) . ?
C9 C10 1.363(9) . ?
C10 C11 1.377(9) . ?
C11 C12 1.371(8) . ?
C13 C18 1.380(7) . ?
C13 C14 1.400(7) . ?
C14 C15 1.377(8) . ?
C15 C16 1.380(9) . ?
C16 C17 1.372(9) . ?
C17 C18 1.404(8) . ?
C19 C20 1.396(7) . ?
C19 C24 1.413(8) . ?
C20 C21 1.390(8) . ?
C21 C22 1.360(9) . ?
C22 C23 1.387(8) . ?
C23 C24 1.386(8) . ?
C101 C106 1.374(11) . ?
C101 C102 1.379(11) . ?
C102 C103 1.347(11) . ?
C103 C104 1.389(12) . ?
C104 C105 1.356(13) . ?
C105 C106 1.392(12) . ?
