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#$Date: 2016-03-25 13:45:44 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179862 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/58/7015830.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_7015830
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            'C40 H38 Cl F6 N3 Ni P3'
_chemical_formula_weight         861.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           31
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac -2'
_symmetry_space_group_name_H-M   'P m n 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   21.7288(9)
_cell_length_b                   7.6413(3)
_cell_length_c                   11.6265(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1930.42(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0309
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            54670
_diffrn_reflns_theta_full        33.56
_diffrn_reflns_theta_max         33.56
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.759
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6626
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             886
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.249
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7697
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0664P)²+0.5035P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                6879
_reflns_number_total             7697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10131e.txt
_cod_data_source_block           t1
_cod_original_sg_symbol_H-M      Pmn2(1)
_cod_database_code               7015830
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'
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 0.0000 0.38746(4) 0.37948(3) 0.02000(8) Uani 1 2 d S . .
P2 P 0.5000 0.42139(14) 0.45927(10) 0.0408(2) Uani 1 2 d S . .
P1 P 0.140166(19) 0.27238(5) 0.41221(5) 0.01731(8) Uani 1 1 d . . .
F1 F 0.5000 0.2123(6) 0.4502(5) 0.1035(14) Uani 1 2 d S . .
F2 F 0.44909(11) 0.4213(5) 0.3617(3) 0.0995(10) Uani 1 1 d . . .
F3 F 0.44939(12) 0.4134(5) 0.5557(2) 0.1071(12) Uani 1 1 d . . .
F4 F 0.5000 0.6217(5) 0.4628(5) 0.144(3) Uani 1 2 d S . .
N1 N 0.0000 0.6179(3) 0.3131(3) 0.0314(6) Uani 1 2 d S . .
N2 N 0.08797(6) 0.41612(17) 0.38607(16) 0.0206(3) Uani 1 1 d . . .
Cl1 Cl 0.0000 0.10770(7) 0.40931(6) 0.02197(12) Uani 1 2 d S . .
C2 C 0.21236(8) 0.3878(2) 0.43375(16) 0.0202(3) Uani 1 1 d . . .
C5 C 0.12410(8) 0.1572(3) 0.54380(16) 0.0205(3) Uani 1 1 d . . .
C7 C 0.05778(10) 0.7075(3) 0.3413(2) 0.0337(5) Uani 1 1 d . . .
H7A H 0.0577 0.7461 0.4208 0.040 Uiso 1 1 calc R . .
H7B H 0.0637 0.8084 0.2919 0.040 Uiso 1 1 calc R . .
C8 C 0.11387(11) 0.1217(3) 0.20312(18) 0.0267(4) Uani 1 1 d . . .
H8A H 0.0809 0.1994 0.2016 0.032 Uiso 1 1 calc R . .
C9 C 0.15428(9) 0.1197(2) 0.29683(17) 0.0221(3) Uani 1 1 d . . .
C10 C 0.10719(9) 0.5754(3) 0.3218(2) 0.0307(4) Uani 1 1 d . . .
H10A H 0.1113 0.5499 0.2404 0.037 Uiso 1 1 calc R . .
H10B H 0.1463 0.6183 0.3503 0.037 Uiso 1 1 calc R . .
C10B C 0.12351(13) 0.0052(3) 0.1112(2) 0.0388(5) Uani 1 1 d . . .
H10C H 0.0966 0.0051 0.0490 0.047 Uiso 1 1 calc R . .
C11 C 0.14073(10) -0.0174(3) 0.55911(19) 0.0279(4) Uani 1 1 d . . .
H11A H 0.1602 -0.0780 0.5000 0.033 Uiso 1 1 calc R . .
C12 C 0.12825(14) -0.1006(3) 0.6625(2) 0.0411(6) Uani 1 1 d . . .
H12A H 0.1391 -0.2174 0.6724 0.049 Uiso 1 1 calc R . .
C13 C 0.31711(10) 0.5967(3) 0.4595(2) 0.0340(5) Uani 1 1 d . . .
H13A H 0.3521 0.6654 0.4687 0.041 Uiso 1 1 calc R . .
C14 C 0.25988(11) 0.3845(3) 0.35335(19) 0.0342(5) Uani 1 1 d . . .
H14A H 0.2569 0.3112 0.2898 0.041 Uiso 1 1 calc R . .
C15 C 0.20422(10) 0.0028(3) 0.2967(2) 0.0306(4) Uani 1 1 d . . .
H15A H 0.2314 0.0010 0.3586 0.037 Uiso 1 1 calc R . .
C17 C 0.17242(15) -0.1084(3) 0.1129(3) 0.0466(7) Uani 1 1 d . . .
H17A H 0.1783 -0.1852 0.0518 0.056 Uiso 1 1 calc R . .
C19 C 0.21318(13) -0.1102(3) 0.2045(3) 0.0417(6) Uani 1 1 d . . .
H19A H 0.2465 -0.1867 0.2043 0.050 Uiso 1 1 calc R . .
C21 C 0.08344(12) 0.1628(4) 0.7369(2) 0.0378(5) Uani 1 1 d . . .
H21A H 0.0644 0.2234 0.7965 0.045 Uiso 1 1 calc R . .
C22 C 0.09961(14) -0.0102(4) 0.7517(2) 0.0451(6) Uani 1 1 d . . .
H22A H 0.0914 -0.0663 0.8210 0.054 Uiso 1 1 calc R . .
C23 C 0.31132(10) 0.4883(4) 0.3665(2) 0.0391(5) Uani 1 1 d . . .
H23A H 0.3424 0.4845 0.3116 0.047 Uiso 1 1 calc R . .
C25 C 0.09548(10) 0.2472(3) 0.63348(18) 0.0281(4) Uani 1 1 d . . .
H25A H 0.0845 0.3639 0.6240 0.034 Uiso 1 1 calc R . .
C26 C 0.21914(11) 0.4947(4) 0.5282(2) 0.0459(7) Uani 1 1 d . . .
H26A H 0.1891 0.4946 0.5853 0.055 Uiso 1 1 calc R . .
C27 C 0.27021(14) 0.6025(5) 0.5395(3) 0.0601(11) Uani 1 1 d . . .
H27A H 0.2728 0.6793 0.6014 0.072 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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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 84.94(4) . . ?
N1 Ni1 N2 84.94(4) . 4 ?
N2 Ni1 N2 166.16(8) . 4 ?
N1 Ni1 Cl1 165.54(10) . . ?
N2 Ni1 Cl1 96.08(4) . . ?
N2 Ni1 Cl1 96.08(4) 4 . ?
F4 P2 F3 91.1(2) . . ?
F4 P2 F3 91.1(2) . 4_655 ?
F3 P2 F3 88.8(2) . 4_655 ?
F4 P2 F2 91.1(2) . 4_655 ?
F3 P2 F2 177.8(2) . 4_655 ?
F3 P2 F2 91.26(16) 4_655 4_655 ?
F4 P2 F2 91.1(2) . . ?
F3 P2 F2 91.26(16) . . ?
F3 P2 F2 177.8(2) 4_655 . ?
F2 P2 F2 88.6(2) 4_655 . ?
F4 P2 F1 177.7(3) . . ?
F3 P2 F1 90.5(2) . . ?
F3 P2 F1 90.5(2) 4_655 . ?
F2 P2 F1 87.28(19) 4_655 . ?
F2 P2 F1 87.28(19) . . ?
N2 P1 C5 110.99(9) . . ?
N2 P1 C9 114.90(9) . . ?
C5 P1 C9 110.41(9) . . ?
N2 P1 C2 107.67(7) . . ?
C5 P1 C2 106.72(8) . . ?
C9 P1 C2 105.64(8) . . ?
C7 N1 C7 117.7(3) 4 . ?
C7 N1 Ni1 109.74(14) 4 . ?
C7 N1 Ni1 109.74(14) . . ?
C10 N2 P1 117.12(12) . . ?
C10 N2 Ni1 110.58(11) . . ?
P1 N2 Ni1 129.06(8) . . ?
C26 C2 C14 117.82(17) . . ?
C26 C2 P1 119.36(14) . . ?
C14 C2 P1 122.60(14) . . ?
C11 C5 C25 119.47(19) . . ?
C11 C5 P1 121.79(15) . . ?
C25 C5 P1 118.73(15) . . ?
N1 C7 C10 105.45(18) . . ?
C9 C8 C10B 119.4(2) . . ?
C8 C9 C15 119.40(19) . . ?
C8 C9 P1 117.73(15) . . ?
C15 C9 P1 122.87(17) . . ?
N2 C10 C7 105.97(16) . . ?
C17 C10B C8 120.3(3) . . ?
C12 C11 C5 119.9(2) . . ?
C11 C12 C22 120.3(2) . . ?
C23 C13 C27 119.0(2) . . ?
C23 C14 C2 121.1(2) . . ?
C19 C15 C9 120.2(2) . . ?
C10B C17 C19 120.8(2) . . ?
C17 C19 C15 119.8(2) . . ?
C22 C21 C25 120.3(2) . . ?
C21 C22 C12 119.8(2) . . ?
C13 C23 C14 120.7(2) . . ?
C21 C25 C5 120.1(2) . . ?
C2 C26 C27 120.9(2) . . ?
C13 C27 C26 120.5(2) . . ?
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 1.922(2) . ?
Ni1 N2 1.9256(13) . ?
Ni1 N2 1.9256(13) 4 ?
Ni1 Cl1 2.1657(6) . ?
P2 F4 1.531(4) . ?
P2 F3 1.571(3) . ?
P2 F3 1.571(3) 4_655 ?
P2 F2 1.584(3) 4_655 ?
P2 F2 1.584(3) . ?
P2 F1 1.601(5) . ?
P1 N2 1.6078(14) . ?
P1 C5 1.7993(19) . ?
P1 C9 1.8042(19) . ?
P1 C2 1.8169(17) . ?
N1 C7 1.467(3) 4 ?
N1 C7 1.467(3) . ?
N2 C10 1.488(2) . ?
C2 C26 1.377(3) . ?
C2 C14 1.393(3) . ?
C5 C11 1.393(3) . ?
C5 C25 1.395(3) . ?
C7 C10 1.491(3) . ?
C8 C9 1.399(3) . ?
C8 C10B 1.407(3) . ?
C9 C15 1.405(3) . ?
C10B C17 1.372(4) . ?
C11 C12 1.387(3) . ?
C12 C22 1.393(4) . ?
C13 C23 1.368(3) . ?
C13 C27 1.380(4) . ?
C14 C23 1.379(3) . ?
C15 C19 1.390(3) . ?
C17 C19 1.385(5) . ?
C21 C22 1.379(4) . ?
C21 C25 1.389(3) . ?
C26 C27 1.388(3) . ?
