#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/32/7013277.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_7013277
loop_
_publ_author_name
'Masuda, Jason D.'
'Wei, Pingrong'
'Stephan, Douglas W.'
_publ_section_title
;
 Nickel and palladium phosphinimine-imine ligand complexes
;
_journal_issue                   18
_journal_name_full               'Dalton Transactions'
_journal_page_first              3500
_journal_paper_doi               10.1039/b306110h
_journal_year                    2003
_chemical_formula_sum            'C43 H55 Li N2 O P'
_chemical_formula_weight         653.80
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 98.359(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.687(7)
_cell_length_b                   19.406(12)
_cell_length_c                   19.757(12)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.0
_cell_measurement_theta_min      2.0
_cell_volume                     4054(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0850
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17063
_diffrn_reflns_theta_full        23.33
_diffrn_reflns_theta_max         23.33
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_T_max  0.488950
_exptl_absorpt_correction_T_min  0.310565
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.225
_refine_diff_density_min         -0.232
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         5785
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0471P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1085
_refine_ls_wR_factor_ref         0.1176
_reflns_number_gt                2723
_reflns_number_total             5785
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b306110h.txt
_cod_data_source_block
'[Li(THF)][(C6H3i-Pr2)NC(Me)CHPPh2(NC6H3i-Pr2)]'
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7013277
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'
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
Li1 Li 1.0072(5) 0.7874(3) 0.8071(3) 0.0683(15) Uani 1 1 d . . .
P1 P 0.95615(8) 0.92533(4) 0.86533(4) 0.0550(3) Uani 1 1 d . . .
N1 N 0.9562(2) 0.88240(11) 0.79640(12) 0.0497(6) Uani 1 1 d . . .
N2 N 1.0522(2) 0.76863(13) 0.90268(12) 0.0496(6) Uani 1 1 d . . .
O1 O 0.9998(3) 0.72219(13) 0.73532(13) 0.1097(9) Uani 1 1 d . . .
C1 C 0.9567(3) 0.90948(14) 0.72944(16) 0.0513(8) Uani 1 1 d . . .
C2 C 0.8433(3) 0.91370(15) 0.68268(17) 0.0597(9) Uani 1 1 d . . .
C3 C 0.8493(4) 0.93470(19) 0.6162(2) 0.0933(12) Uani 1 1 d . . .
H3A H 0.7748 0.9383 0.5856 0.112 Uiso 1 1 calc R . .
C4 C 0.9612(5) 0.9503(2) 0.5943(2) 0.1104(15) Uani 1 1 d . . .
H4A H 0.9628 0.9639 0.5492 0.133 Uiso 1 1 calc R . .
C5 C 1.0708(4) 0.94576(19) 0.6391(2) 0.0926(12) Uani 1 1 d . . .
H5A H 1.1470 0.9565 0.6242 0.111 Uiso 1 1 calc R . .
C6 C 1.0711(3) 0.92545(16) 0.70657(17) 0.0616(9) Uani 1 1 d . . .
C7 C 1.2740(3) 0.9863(2) 0.7567(2) 0.1145(14) Uani 1 1 d . . .
H7A H 1.2238 1.0234 0.7704 0.172 Uiso 1 1 calc R . .
H7B H 1.2969 0.9961 0.7125 0.172 Uiso 1 1 calc R . .
H7C H 1.3491 0.9813 0.7894 0.172 Uiso 1 1 calc R . .
C8 C 1.2760(4) 0.8587(2) 0.7332(2) 0.1286(16) Uani 1 1 d . . .
H8A H 1.2273 0.8172 0.7330 0.193 Uiso 1 1 calc R . .
H8B H 1.3517 0.8544 0.7657 0.193 Uiso 1 1 calc R . .
H8C H 1.2982 0.8665 0.6885 0.193 Uiso 1 1 calc R . .
C9 C 1.1979(3) 0.9196(2) 0.75320(18) 0.0824(11) Uani 1 1 d . . .
H9A H 1.1792 0.9103 0.7995 0.099 Uiso 1 1 calc R . .
C10 C 0.7175(3) 0.89591(19) 0.70480(18) 0.0795(11) Uani 1 1 d . . .
H10A H 0.7329 0.8908 0.7547 0.095 Uiso 1 1 calc R . .
C11 C 0.6185(4) 0.9514(3) 0.6893(4) 0.229(4) Uani 1 1 d . . .
H11A H 0.5419 0.9371 0.7052 0.343 Uiso 1 1 calc R . .
H11B H 0.6023 0.9592 0.6408 0.343 Uiso 1 1 calc R . .
H11C H 0.6484 0.9933 0.7120 0.343 Uiso 1 1 calc R . .
C12 C 0.6651(5) 0.8294(3) 0.6769(3) 0.211(3) Uani 1 1 d . . .
H12A H 0.7276 0.7940 0.6871 0.316 Uiso 1 1 calc R . .
H12B H 0.6423 0.8332 0.6282 0.316 Uiso 1 1 calc R . .
H12C H 0.5916 0.8180 0.6973 0.316 Uiso 1 1 calc R . .
C13 C 1.0044(3) 1.01444(15) 0.85926(17) 0.0576(9) Uani 1 1 d . . .
C14 C 0.9434(3) 1.05723(18) 0.80855(17) 0.0713(10) Uani 1 1 d . . .
H14A H 0.8758 1.0400 0.7783 0.086 Uiso 1 1 calc R . .
C15 C 0.9808(4) 1.1249(2) 0.8019(2) 0.0916(13) Uani 1 1 d . . .
H15A H 0.9384 1.1526 0.7675 0.110 Uiso 1 1 calc R . .
C16 C 1.0801(5) 1.1508(2) 0.8459(3) 0.0990(14) Uani 1 1 d . . .
H16A H 1.1054 1.1962 0.8414 0.119 Uiso 1 1 calc R . .
C17 C 1.1427(4) 1.1101(2) 0.8967(2) 0.0977(13) Uani 1 1 d . . .
H17A H 1.2093 1.1282 0.9270 0.117 Uiso 1 1 calc R . .
C18 C 1.1064(4) 1.04128(19) 0.90285(18) 0.0787(10) Uani 1 1 d . . .
H18A H 1.1509 1.0134 0.9364 0.094 Uiso 1 1 calc R . .
C19 C 0.7961(3) 0.93295(19) 0.88738(15) 0.0619(9) Uani 1 1 d . . .
C20 C 0.7479(4) 0.9913(2) 0.91356(17) 0.0838(11) Uani 1 1 d . . .
H20A H 0.7958 1.0315 0.9180 0.101 Uiso 1 1 calc R . .
C21 C 0.6274(5) 0.9909(3) 0.9336(2) 0.1137(16) Uani 1 1 d . . .
H21A H 0.5959 1.0304 0.9517 0.136 Uiso 1 1 calc R . .
C22 C 0.5568(5) 0.9321(4) 0.9263(3) 0.1283(19) Uani 1 1 d . . .
H22A H 0.4761 0.9320 0.9386 0.154 Uiso 1 1 calc R . .
C23 C 0.6032(5) 0.8738(3) 0.9011(2) 0.1222(16) Uani 1 1 d . . .
H23A H 0.5547 0.8338 0.8968 0.147 Uiso 1 1 calc R . .
C24 C 0.7222(4) 0.8740(2) 0.88215(19) 0.0943(13) Uani 1 1 d . . .
H24A H 0.7536 0.8337 0.8655 0.113 Uiso 1 1 calc R . .
C25 C 1.0778(3) 0.69848(15) 0.92149(14) 0.0498(8) Uani 1 1 d . . .
C26 C 0.9791(3) 0.65554(17) 0.93609(15) 0.0594(9) Uani 1 1 d . . .
C27 C 1.0002(3) 0.58513(18) 0.94424(17) 0.0735(10) Uani 1 1 d . . .
H27A H 0.9350 0.5566 0.9537 0.088 Uiso 1 1 calc R . .
C28 C 1.1173(4) 0.55694(17) 0.93839(16) 0.0727(10) Uani 1 1 d . . .
H28A H 1.1302 0.5097 0.9430 0.087 Uiso 1 1 calc R . .
C29 C 1.2127(3) 0.59869(18) 0.92588(16) 0.0641(9) Uani 1 1 d . . .
H29A H 1.2915 0.5795 0.9229 0.077 Uiso 1 1 calc R . .
C30 C 1.1969(3) 0.66909(16) 0.91733(14) 0.0532(8) Uani 1 1 d . . .
C31 C 1.3092(3) 0.71327(16) 0.90447(17) 0.0673(9) Uani 1 1 d . . .
H31A H 1.2814 0.7614 0.9006 0.081 Uiso 1 1 calc R . .
C32 C 1.4165(3) 0.7078(2) 0.9641(2) 0.1113(14) Uani 1 1 d . . .
H32A H 1.3867 0.7220 1.0055 0.167 Uiso 1 1 calc R . .
H32B H 1.4851 0.7371 0.9557 0.167 Uiso 1 1 calc R . .
H32C H 1.4453 0.6610 0.9687 0.167 Uiso 1 1 calc R . .
C33 C 1.3573(3) 0.6934(2) 0.83827(19) 0.1106(14) Uani 1 1 d . . .
H33A H 1.2901 0.6981 0.8006 0.166 Uiso 1 1 calc R . .
H33B H 1.3861 0.6465 0.8412 0.166 Uiso 1 1 calc R . .
H33C H 1.4261 0.7232 0.8312 0.166 Uiso 1 1 calc R . .
C34 C 0.8491(3) 0.68537(18) 0.9422(2) 0.0814(11) Uani 1 1 d . . .
H34A H 0.8575 0.7357 0.9423 0.098 Uiso 1 1 calc R . .
C35 C 0.8034(4) 0.6653(3) 1.0091(2) 0.163(2) Uani 1 1 d . . .
H35A H 0.7226 0.6861 1.0112 0.244 Uiso 1 1 calc R . .
H35B H 0.8632 0.6810 1.0470 0.244 Uiso 1 1 calc R . .
H35C H 0.7957 0.6161 1.0113 0.244 Uiso 1 1 calc R . .
C36 C 0.7540(4) 0.6666(3) 0.8813(3) 0.157(2) Uani 1 1 d . . .
H36A H 0.7842 0.6814 0.8402 0.235 Uiso 1 1 calc R . .
H36B H 0.6750 0.6890 0.8848 0.235 Uiso 1 1 calc R . .
H36C H 0.7420 0.6176 0.8800 0.235 Uiso 1 1 calc R . .
C37 C 1.0429(3) 0.88735(16) 0.93608(15) 0.0633(9) Uani 1 1 d . . .
H37A H 1.0757 0.9177 0.9706 0.076 Uiso 1 1 calc R . .
C38 C 1.0714(3) 0.81782(17) 0.94923(16) 0.0532(8) Uani 1 1 d . . .
C39 C 1.1248(3) 0.80007(16) 1.02322(15) 0.0813(11) Uani 1 1 d . . .
H39A H 1.1413 0.7515 1.0269 0.122 Uiso 1 1 calc R . .
H39B H 1.0646 0.8126 1.0527 0.122 Uiso 1 1 calc R . .
H39C H 1.2021 0.8250 1.0364 0.122 Uiso 1 1 calc R . .
C40 C 0.9886(5) 0.7347(3) 0.6633(2) 0.153(2) Uani 1 1 d . . .
H40A H 0.9103 0.7590 0.6478 0.183 Uiso 1 1 calc R . .
H40B H 1.0584 0.7632 0.6535 0.183 Uiso 1 1 calc R . .
C41 C 0.9896(7) 0.6739(3) 0.6300(3) 0.214(3) Uani 1 1 d . . .
H41A H 1.0620 0.6710 0.6056 0.256 Uiso 1 1 calc R . .
H41B H 0.9129 0.6680 0.5977 0.256 Uiso 1 1 calc R . .
C42 C 0.9978(9) 0.6225(3) 0.6841(4) 0.317(6) Uani 1 1 d . . .
H42A H 0.9251 0.5921 0.6754 0.380 Uiso 1 1 calc R . .
H42B H 1.0730 0.5948 0.6831 0.380 Uiso 1 1 calc R . .
C43 C 1.0018(5) 0.6491(2) 0.7444(3) 0.143(2) Uani 1 1 d . . .
H43A H 1.0054 0.6253 0.7855 0.172 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'
Li Li -0.0003 0.0001 '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'
O O 0.0106 0.0060 '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
O1 Li1 N2 126.1(3) . . ?
O1 Li1 N1 125.2(3) . . ?
N2 Li1 N1 108.5(3) . . ?
O1 Li1 P1 153.5(3) . . ?
N2 Li1 P1 79.93(18) . . ?
N1 Li1 P1 28.59(11) . . ?
N1 P1 C37 113.64(14) . . ?
N1 P1 C13 113.94(13) . . ?
C37 P1 C13 109.64(17) . . ?
N1 P1 C19 111.19(14) . . ?
C37 P1 C19 104.61(15) . . ?
C13 P1 C19 102.91(16) . . ?
N1 P1 Li1 35.24(13) . . ?
C37 P1 Li1 79.80(15) . . ?
C13 P1 Li1 139.24(14) . . ?
C19 P1 Li1 113.08(16) . . ?
C1 N1 P1 126.89(19) . . ?
C1 N1 Li1 114.6(2) . . ?
P1 N1 Li1 116.2(2) . . ?
C38 N2 C25 120.2(2) . . ?
C38 N2 Li1 122.7(3) . . ?
C25 N2 Li1 116.7(2) . . ?
C40 O1 C43 106.9(3) . . ?
C40 O1 Li1 128.3(3) . . ?
C43 O1 Li1 124.8(3) . . ?
C6 C1 C2 118.8(3) . . ?
C6 C1 N1 120.2(3) . . ?
C2 C1 N1 120.6(3) . . ?
C3 C2 C1 118.8(3) . . ?
C3 C2 C10 120.5(3) . . ?
C1 C2 C10 120.7(3) . . ?
C4 C3 C2 122.1(4) . . ?
C5 C4 C3 119.2(4) . . ?
C4 C5 C6 121.6(4) . . ?
C5 C6 C1 119.5(3) . . ?
C5 C6 C9 118.5(3) . . ?
C1 C6 C9 121.9(3) . . ?
C6 C9 C7 112.6(3) . . ?
C6 C9 C8 111.8(3) . . ?
C7 C9 C8 111.0(3) . . ?
C12 C10 C2 113.3(3) . . ?
C12 C10 C11 109.3(4) . . ?
C2 C10 C11 113.8(3) . . ?
C18 C13 C14 117.8(3) . . ?
C18 C13 P1 121.5(3) . . ?
C14 C13 P1 120.6(3) . . ?
C15 C14 C13 121.6(4) . . ?
C16 C15 C14 119.8(4) . . ?
C15 C16 C17 120.3(4) . . ?
C16 C17 C18 120.1(4) . . ?
C13 C18 C17 120.4(4) . . ?
C20 C19 C24 117.8(3) . . ?
C20 C19 P1 124.7(3) . . ?
C24 C19 P1 117.2(3) . . ?
C19 C20 C21 120.7(4) . . ?
C22 C21 C20 119.5(4) . . ?
C23 C22 C21 120.7(5) . . ?
C22 C23 C24 119.8(5) . . ?
C23 C24 C19 121.4(4) . . ?
C30 C25 C26 118.9(3) . . ?
C30 C25 N2 120.8(3) . . ?
C26 C25 N2 119.8(3) . . ?
C27 C26 C25 119.5(3) . . ?
C27 C26 C34 119.9(3) . . ?
C25 C26 C34 120.7(3) . . ?
C28 C27 C26 120.8(3) . . ?
C29 C28 C27 119.5(3) . . ?
C28 C29 C30 122.1(3) . . ?
C29 C30 C25 119.2(3) . . ?
C29 C30 C31 119.3(3) . . ?
C25 C30 C31 121.5(3) . . ?
C33 C31 C32 109.6(3) . . ?
C33 C31 C30 111.9(3) . . ?
C32 C31 C30 110.7(3) . . ?
C36 C34 C35 111.6(3) . . ?
C36 C34 C26 111.3(3) . . ?
C35 C34 C26 112.4(3) . . ?
C38 C37 P1 129.7(2) . . ?
N2 C38 C37 124.1(3) . . ?
N2 C38 C39 120.1(3) . . ?
C37 C38 C39 115.8(3) . . ?
C41 C40 O1 109.3(4) . . ?
C40 C41 C42 104.1(5) . . ?
C43 C42 C41 113.2(5) . . ?
C42 C43 O1 106.4(5) . . ?
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
Li1 O1 1.894(6) . ?
Li1 N2 1.914(6) . ?
Li1 N1 1.925(6) . ?
Li1 P1 2.995(5) . ?
P1 N1 1.597(2) . ?
P1 C37 1.727(3) . ?
P1 C13 1.813(3) . ?
P1 C19 1.831(3) . ?
N1 C1 1.424(3) . ?
N2 C38 1.321(3) . ?
N2 C25 1.427(3) . ?
O1 C40 1.431(4) . ?
O1 C43 1.430(4) . ?
C1 C6 1.399(4) . ?
C1 C2 1.416(4) . ?
C2 C3 1.385(4) . ?
C2 C10 1.513(4) . ?
C3 C4 1.364(5) . ?
C4 C5 1.365(5) . ?
C5 C6 1.389(4) . ?
C6 C9 1.528(4) . ?
C7 C9 1.525(4) . ?
C8 C9 1.530(4) . ?
C10 C12 1.480(5) . ?
C10 C11 1.509(5) . ?
C13 C18 1.389(4) . ?
C13 C14 1.389(4) . ?
C14 C15 1.384(5) . ?
C15 C16 1.367(5) . ?
C16 C17 1.373(5) . ?
C17 C18 1.401(5) . ?
C19 C20 1.376(4) . ?
C19 C24 1.386(4) . ?
C20 C21 1.401(5) . ?
C21 C22 1.364(6) . ?
C22 C23 1.359(6) . ?
C23 C24 1.377(5) . ?
C25 C30 1.408(4) . ?
C25 C26 1.407(4) . ?
C26 C27 1.391(4) . ?
C26 C34 1.525(4) . ?
C27 C28 1.386(4) . ?
C28 C29 1.353(4) . ?
C29 C30 1.384(4) . ?
C30 C31 1.526(4) . ?
C31 C33 1.523(4) . ?
C31 C32 1.523(4) . ?
C34 C36 1.502(5) . ?
C34 C35 1.525(5) . ?
C37 C38 1.399(4) . ?
C38 C39 1.529(4) . ?
C40 C41 1.351(5) . ?
C41 C42 1.457(7) . ?
C42 C43 1.292(6) . ?
