#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:08:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179881 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/77/7017706.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_7017706
loop_
_publ_author_name
'Zhang, Shuanming'
'Pattacini, Roberto'
'Jie, Suyun'
'Braunstein, Pierre'
_publ_section_title
;
 A phosphino-oxazoline ligand as a P,N-bridge in palladium/cobalt or
 P,N-chelate in nickel complexes: catalytic ethylene oligomerization.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              379
_journal_page_last               386
_journal_paper_doi               10.1039/c1dt11352f
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C32 H32 Cl2 N2 Ni O2 P2'
_chemical_formula_sum            'C32 H32 Cl2 N2 Ni O2 P2'
_chemical_formula_weight         668.15
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.2701(2)
_cell_length_b                   15.3634(7)
_cell_length_c                   24.168(1)
_cell_measurement_reflns_used    3456
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3070.7(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0715
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            6317
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.69
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.943
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         3502
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0440
_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)+(0.0790P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1487
_reflns_number_gt                2203
_reflns_number_total             3502
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt11352f.txt
_cod_data_source_block           compound2
_cod_database_code               7017706
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
Ni1 Ni 1.0000 0.0000 0.0000 0.02097(19) Uani 1 2 d S
P1 P 0.93271(10) 0.09400(6) 0.08254(4) 0.0251(2) Uani 1 1 d .
Cl1 Cl 1.12531(9) 0.12707(5) -0.03918(4) 0.0280(2) Uani 1 1 d .
N1 N 0.7795(3) 0.05029(18) -0.02219(12) 0.0235(6) Uani 1 1 d .
O1 O 0.5785(3) 0.14715(15) -0.01775(11) 0.0319(6) Uani 1 1 d .
C1 C 0.6628(4) 0.0189(2) -0.06331(17) 0.0338(9) Uani 1 1 d .
H1A H 0.6186 -0.0372 -0.0526 0.041 Uiso 1 1 calc R
H1B H 0.7125 0.0136 -0.0995 0.041 Uiso 1 1 calc R
C2 C 0.5319(4) 0.0890(2) -0.06332(18) 0.0358(9) Uani 1 1 d .
H2A H 0.5301 0.1201 -0.0983 0.043 Uiso 1 1 calc R
H2B H 0.4260 0.0638 -0.0568 0.043 Uiso 1 1 calc R
C3 C 0.7245(4) 0.1193(2) -0.00082(13) 0.0227(7) Uani 1 1 d .
C4 C 0.8110(4) 0.1715(2) 0.04190(14) 0.0267(8) Uani 1 1 d .
H4A H 0.7342 0.2014 0.0656 0.032 Uiso 1 1 calc R
H4B H 0.8802 0.2145 0.0245 0.032 Uiso 1 1 calc R
C5 C 1.0680(4) 0.1638(2) 0.12360(15) 0.0280(8) Uani 1 1 d .
C6 C 1.0480(5) 0.1766(3) 0.17990(17) 0.0458(11) Uani 1 1 d .
H6 H 0.9614 0.1509 0.1982 0.055 Uiso 1 1 calc R
C7 C 1.1579(5) 0.2279(3) 0.20914(17) 0.0574(13) Uani 1 1 d .
H7 H 1.1454 0.2354 0.2471 0.069 Uiso 1 1 calc R
C8 C 1.2847(5) 0.2674(3) 0.18207(18) 0.0483(11) Uani 1 1 d .
H8 H 1.3560 0.3027 0.2016 0.058 Uiso 1 1 calc R
C9 C 1.3066(4) 0.2548(2) 0.12584(15) 0.0359(9) Uani 1 1 d .
H9 H 1.3922 0.2814 0.1075 0.043 Uiso 1 1 calc R
C10 C 1.1996(4) 0.2022(2) 0.09725(15) 0.0307(8) Uani 1 1 d .
H10 H 1.2159 0.1923 0.0597 0.037 Uiso 1 1 calc R
C11 C 0.7887(4) 0.0511(2) 0.13306(14) 0.0285(8) Uani 1 1 d .
C12 C 0.8278(5) -0.0274(3) 0.15792(16) 0.0416(10) Uani 1 1 d .
H12 H 0.9254 -0.0543 0.1495 0.050 Uiso 1 1 calc R
C13 C 0.7221(6) -0.0663(3) 0.19534(18) 0.0555(12) Uani 1 1 d .
H13 H 0.7494 -0.1189 0.2118 0.067 Uiso 1 1 calc R
C14 C 0.5778(6) -0.0270(4) 0.20792(18) 0.0561(13) Uani 1 1 d .
H14 H 0.5077 -0.0529 0.2331 0.067 Uiso 1 1 calc R
C15 C 0.5369(5) 0.0500(4) 0.18356(19) 0.0541(13) Uani 1 1 d .
H15 H 0.4385 0.0760 0.1919 0.065 Uiso 1 1 calc R
C16 C 0.6418(4) 0.0899(3) 0.14614(17) 0.0432(10) Uani 1 1 d .
H16 H 0.6133 0.1425 0.1299 0.052 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
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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'
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
N1 Ni1 N1 180.0(2) 5_755 .
N1 Ni1 Cl1 88.53(8) 5_755 5_755
N1 Ni1 Cl1 91.47(8) . 5_755
N1 Ni1 Cl1 91.47(8) 5_755 .
N1 Ni1 Cl1 88.53(8) . .
Cl1 Ni1 Cl1 180.00(5) 5_755 .
N1 Ni1 P1 78.18(8) 5_755 5_755
N1 Ni1 P1 101.82(8) . 5_755
Cl1 Ni1 P1 86.66(3) 5_755 5_755
Cl1 Ni1 P1 93.34(3) . 5_755
N1 Ni1 P1 101.82(8) 5_755 .
N1 Ni1 P1 78.18(8) . .
Cl1 Ni1 P1 93.34(3) 5_755 .
Cl1 Ni1 P1 86.66(3) . .
P1 Ni1 P1 180.00(6) 5_755 .
C11 P1 C5 104.25(16) . .
C11 P1 C4 103.48(16) . .
C5 P1 C4 104.04(16) . .
C11 P1 Ni1 117.71(12) . .
C5 P1 Ni1 128.71(12) . .
C4 P1 Ni1 93.96(11) . .
C3 N1 C1 108.4(3) . .
C3 N1 Ni1 121.9(2) . .
C1 N1 Ni1 129.6(2) . .
C3 O1 C2 105.7(2) . .
N1 C1 C2 103.5(3) . .
N1 C1 H1A 111.1 . .
C2 C1 H1A 111.1 . .
N1 C1 H1B 111.1 . .
C2 C1 H1B 111.1 . .
H1A C1 H1B 109.0 . .
O1 C2 C1 104.0(3) . .
O1 C2 H2A 110.9 . .
C1 C2 H2A 110.9 . .
O1 C2 H2B 110.9 . .
C1 C2 H2B 110.9 . .
H2A C2 H2B 109.0 . .
N1 C3 O1 117.7(3) . .
N1 C3 C4 124.2(3) . .
O1 C3 C4 118.1(3) . .
C3 C4 P1 106.5(2) . .
C3 C4 H4A 110.4 . .
P1 C4 H4A 110.4 . .
C3 C4 H4B 110.4 . .
P1 C4 H4B 110.4 . .
H4A C4 H4B 108.6 . .
C6 C5 C10 118.9(3) . .
C6 C5 P1 122.6(3) . .
C10 C5 P1 118.4(3) . .
C5 C6 C7 120.0(4) . .
C5 C6 H6 120.0 . .
C7 C6 H6 120.0 . .
C8 C7 C6 120.3(4) . .
C8 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
C7 C8 C9 120.2(4) . .
C7 C8 H8 119.9 . .
C9 C8 H8 119.9 . .
C10 C9 C8 119.3(4) . .
C10 C9 H9 120.4 . .
C8 C9 H9 120.4 . .
C9 C10 C5 121.3(3) . .
C9 C10 H10 119.4 . .
C5 C10 H10 119.4 . .
C12 C11 C16 118.5(3) . .
C12 C11 P1 116.8(3) . .
C16 C11 P1 124.5(3) . .
C11 C12 C13 120.6(4) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C14 C13 C12 120.1(4) . .
C14 C13 H13 120.0 . .
C12 C13 H13 120.0 . .
C15 C14 C13 120.1(4) . .
C15 C14 H14 119.9 . .
C13 C14 H14 119.9 . .
C14 C15 C16 120.5(4) . .
C14 C15 H15 119.8 . .
C16 C15 H15 119.8 . .
C11 C16 C15 120.2(4) . .
C11 C16 H16 119.9 . .
C15 C16 H16 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.052(2) 5_755
Ni1 N1 2.052(2) .
Ni1 Cl1 2.4045(8) 5_755
Ni1 Cl1 2.4045(8) .
Ni1 P1 2.5249(9) 5_755
Ni1 P1 2.5249(9) .
P1 C11 1.828(3) .
P1 C5 1.841(3) .
P1 C4 1.843(3) .
N1 C3 1.264(4) .
N1 C1 1.467(4) .
O1 C3 1.345(4) .
O1 C2 1.469(4) .
C1 C2 1.528(5) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.490(5) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.384(5) .
C5 C10 1.392(5) .
C6 C7 1.395(5) .
C6 H6 0.9300 .
C7 C8 1.378(6) .
C7 H7 0.9300 .
C8 C9 1.385(5) .
C8 H8 0.9300 .
C9 C10 1.383(5) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.385(5) .
C11 C16 1.390(5) .
C12 C13 1.392(5) .
C12 H12 0.9300 .
C13 C14 1.371(6) .
C13 H13 0.9300 .
C14 C15 1.363(7) .
C14 H14 0.9300 .
C15 C16 1.395(6) .
C15 H15 0.9300 .
C16 H16 0.9300 .
