#------------------------------------------------------------------------------
#$Date: 2025-08-20 22:19:29 +0300 (Wed, 20 Aug 2025) $
#$Revision: 301836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/30/82/4308279.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_4308279
loop_
_publ_author_name
'Nicoleta Muresan'
'Krzysztof Chlopek'
'Thomas Weyhermüller'
'Frank Neese'
'Karl Wieghardt'
_publ_section_title
;
Bis(α-diimine)nickel Complexes: Molecular and Electronic Structure of
Three Members of the Electron-Transfer Series [Ni(L)2]z (z= 0, 1+, 2+) (L =
2-Phenyl-1,4-bis(isopropyl)-1,4-diazabutadiene). A Combined Experimental
and Theoretical Study
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5327
_journal_page_last               5337
_journal_paper_doi               10.1021/ic700407m
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         '[C28 H40 N4 Ni ]+, (P F6)-'
_chemical_formula_sum            'C28 H40 F6 N4 Ni P'
_chemical_formula_weight         636.32
_space_group_IT_number           152
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 31 2"'
_symmetry_space_group_name_H-M   'P 31 2 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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.1845(3)
_cell_length_b                   9.1845(3)
_cell_length_c                   30.6806(12)
_cell_measurement_temperature    100(2)
_cell_volume                     2241.33(14)
_computing_cell_refinement       'Bruker AXS Collect Software'
_computing_data_collection       'Bruker AXS Collect Software'
_computing_data_reduction        'Bruker AXS Collect Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method
'820 images at 0.5 deg. stepwise rotation in omega and phi, 82 sec./frame'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode, 50 kV, 80 mA'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            25078
_diffrn_reflns_theta_full        32.50
_diffrn_reflns_theta_max         32.50
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.3455
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             999
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.699
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.495(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         5405
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+2.1623P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1197
_refine_ls_wR_factor_ref         0.1250
_reflns_number_gt                4818
_reflns_number_total             5405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic700407m-file002_2.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' according
to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed
to 'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4308279
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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 0.14375(4) 0.14375(4) 0.0000 0.01664(10) Uani 1 2 d S . .
N1 N -0.0647(3) 0.1254(3) 0.02479(7) 0.0183(4) Uani 1 1 d . . .
C2 C -0.0487(3) 0.1654(3) 0.06603(7) 0.0162(4) Uani 1 1 d . . .
C3 C 0.1222(3) 0.2362(3) 0.08299(8) 0.0171(4) Uani 1 1 d . . .
H3 H 0.1459 0.2616 0.1131 0.021 Uiso 1 1 calc R . .
N4 N 0.2399(2) 0.2629(2) 0.05554(7) 0.0169(4) Uani 1 1 d . . .
C5 C 0.4147(3) 0.3457(3) 0.07270(8) 0.0198(4) Uani 1 1 d . . .
H5 H 0.4110 0.3164 0.1042 0.024 Uiso 1 1 calc R . .
C6 C 0.4911(3) 0.5354(3) 0.06855(9) 0.0234(5) Uani 1 1 d . . .
H6A H 0.4970 0.5656 0.0377 0.035 Uiso 1 1 calc R . .
H6B H 0.6045 0.5919 0.0810 0.035 Uiso 1 1 calc R . .
H6C H 0.4209 0.5706 0.0842 0.035 Uiso 1 1 calc R . .
C7 C 0.5171(3) 0.2834(3) 0.04815(9) 0.0240(5) Uani 1 1 d . . .
H7A H 0.4704 0.1631 0.0537 0.036 Uiso 1 1 calc R . .
H7B H 0.6341 0.3451 0.0581 0.036 Uiso 1 1 calc R . .
H7C H 0.5129 0.3020 0.0168 0.036 Uiso 1 1 calc R . .
C8 C -0.2182(3) 0.0879(4) 0.00025(8) 0.0231(4) Uani 1 1 d . . .
H8 H -0.3046 0.0818 0.0212 0.028 Uiso 1 1 calc R . .
C9 C -0.1751(4) 0.2303(4) -0.03208(11) 0.0317(6) Uani 1 1 d . . .
H9A H -0.1231 0.3379 -0.0165 0.048 Uiso 1 1 calc R . .
H9B H -0.2781 0.2123 -0.0465 0.048 Uiso 1 1 calc R . .
H9C H -0.0966 0.2321 -0.0540 0.048 Uiso 1 1 calc R . .
C10 C -0.2893(4) -0.0782(4) -0.02364(9) 0.0312(6) Uani 1 1 d . . .
H10A H -0.2014 -0.0779 -0.0418 0.047 Uiso 1 1 calc R . .
H10B H -0.3831 -0.0940 -0.0421 0.047 Uiso 1 1 calc R . .
H10C H -0.3292 -0.1701 -0.0024 0.047 Uiso 1 1 calc R . .
C11 C -0.1836(3) 0.1491(3) 0.09566(8) 0.0180(4) Uani 1 1 d . . .
C12 C -0.3353(3) -0.0005(3) 0.09941(9) 0.0234(5) Uani 1 1 d . . .
H12 H -0.3524 -0.0960 0.0832 0.028 Uiso 1 1 calc R . .
C13 C -0.4626(3) -0.0130(4) 0.12648(10) 0.0274(6) Uani 1 1 d . . .
H13 H -0.5663 -0.1157 0.1285 0.033 Uiso 1 1 calc R . .
C14 C -0.4369(4) 0.1260(4) 0.15058(9) 0.0287(6) Uani 1 1 d . . .
H14 H -0.5241 0.1190 0.1687 0.034 Uiso 1 1 calc R . .
C15 C -0.2833(4) 0.2757(4) 0.14829(9) 0.0284(5) Uani 1 1 d . . .
H15 H -0.2648 0.3696 0.1654 0.034 Uiso 1 1 calc R . .
C16 C -0.1572(3) 0.2871(4) 0.12097(8) 0.0223(5) Uani 1 1 d . . .
H16 H -0.0526 0.3891 0.1195 0.027 Uiso 1 1 calc R . .
P20 P 0.0000 0.80736(14) 0.1667 0.0370(3) Uani 1 2 d SD . .
F21 F 0.0628(11) 0.9553(8) 0.1326(2) 0.136(3) Uani 0.687(7) 1 d PD A 1
F22 F -0.1728(4) 0.6994(7) 0.14006(14) 0.0605(12) Uani 0.687(7) 1 d PD A 1
F23 F 0.0783(9) 0.7211(11) 0.1359(3) 0.0622(17) Uani 0.687(7) 1 d PD A 1
F21X F 0.1393(14) 0.9679(18) 0.1406(5) 0.136(3) Uani 0.313(7) 1 d PD A 2
F22X F -0.1352(10) 0.7942(16) 0.1317(3) 0.0605(12) Uani 0.313(7) 1 d PD A 2
F23X F 0.041(3) 0.693(3) 0.1352(6) 0.0622(17) Uani 0.313(7) 1 d PD A 2
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'
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
N4 Ni1 N4 120.03(12) . 4 ?
N4 Ni1 N1 82.07(8) . . ?
N4 Ni1 N1 131.44(8) 4 . ?
N4 Ni1 N1 131.44(8) . 4 ?
N4 Ni1 N1 82.07(8) 4 4 ?
N1 Ni1 N1 116.77(12) . 4 ?
C2 N1 C8 121.3(2) . . ?
C2 N1 Ni1 112.28(17) . . ?
C8 N1 Ni1 126.22(16) . . ?
N1 C2 C3 114.5(2) . . ?
N1 C2 C11 126.5(2) . . ?
C3 C2 C11 118.9(2) . . ?
N4 C3 C2 117.5(2) . . ?
C3 N4 C5 116.9(2) . . ?
C3 N4 Ni1 110.85(16) . . ?
C5 N4 Ni1 131.07(16) . . ?
N4 C5 C7 110.2(2) . . ?
N4 C5 C6 108.5(2) . . ?
C7 C5 C6 111.7(2) . . ?
N1 C8 C10 111.2(2) . . ?
N1 C8 C9 108.8(2) . . ?
C10 C8 C9 110.2(2) . . ?
C12 C11 C16 118.9(2) . . ?
C12 C11 C2 121.7(2) . . ?
C16 C11 C2 119.4(2) . . ?
C11 C12 C13 121.1(3) . . ?
C14 C13 C12 119.5(3) . . ?
C13 C14 C15 120.1(3) . . ?
C16 C15 C14 119.9(3) . . ?
C15 C16 C11 120.3(3) . . ?
F21 P20 F21 94.5(8) 6 . ?
F21 P20 F22X 63.7(4) 6 6 ?
F21 P20 F22X 91.1(5) . 6 ?
F21 P20 F22X 91.1(5) 6 . ?
F21 P20 F22X 63.7(4) . . ?
F22X P20 F22X 143.6(9) 6 . ?
F21 P20 F21X 25.3(6) 6 6 ?
F21 P20 F21X 101.3(7) . 6 ?
F22X P20 F21X 88.1(4) 6 6 ?
F22X P20 F21X 73.0(7) . 6 ?
F21 P20 F21X 101.3(7) 6 . ?
F21 P20 F21X 25.3(6) . . ?
F22X P20 F21X 72.9(7) 6 . ?
F22X P20 F21X 88.1(4) . . ?
F21X P20 F21X 117.1(18) 6 . ?
F21 P20 F23X 93.4(13) 6 6 ?
F21 P20 F23X 171.0(8) . 6 ?
F22X P20 F23X 88.5(4) 6 6 ?
F22X P20 F23X 120.5(8) . 6 ?
F21X P20 F23X 87.7(4) 6 6 ?
F21X P20 F23X 147.7(13) . 6 ?
F21 P20 F23X 171.0(8) 6 . ?
F21 P20 F23X 93.4(13) . . ?
F22X P20 F23X 120.5(8) 6 . ?
F22X P20 F23X 88.5(4) . . ?
F21X P20 F23X 147.7(13) 6 . ?
F21X P20 F23X 87.7(4) . . ?
F23X P20 F23X 79.0(18) 6 . ?
F21 P20 F22 91.0(2) 6 6 ?
F21 P20 F22 98.6(4) . 6 ?
F22X P20 F22 28.9(4) 6 6 ?
F22X P20 F22 162.2(5) . 6 ?
F21X P20 F22 113.7(4) 6 6 ?
F21X P20 F22 74.1(5) . 6 ?
F23X P20 F22 77.0(7) 6 6 ?
F23X P20 F22 92.0(6) . 6 ?
F21 P20 F22 98.6(4) 6 . ?
F21 P20 F22 91.0(2) . . ?
F22X P20 F22 162.2(5) 6 . ?
F22X P20 F22 28.9(4) . . ?
F21X P20 F22 74.1(5) 6 . ?
F21X P20 F22 113.7(4) . . ?
F23X P20 F22 92.0(6) 6 . ?
F23X P20 F22 77.0(7) . . ?
F22 P20 F22 165.9(4) 6 . ?
F21 P20 F23 88.6(3) 6 6 ?
F21 P20 F23 173.7(4) . 6 ?
F22X P20 F23 95.1(6) 6 6 ?
F22X P20 F23 110.9(5) . 6 ?
F21X P20 F23 79.3(12) 6 6 ?
F21X P20 F23 158.6(6) . 6 ?
F23X P20 F23 10.9(10) 6 6 ?
F23X P20 F23 83.1(6) . 6 ?
F22 P20 F23 86.9(2) 6 6 ?
F22 P20 F23 83.1(3) . 6 ?
F21 P20 F23 173.7(4) 6 . ?
F21 P20 F23 88.6(3) . . ?
F22X P20 F23 110.9(5) 6 . ?
F22X P20 F23 95.1(6) . . ?
F21X P20 F23 158.6(6) 6 . ?
F21X P20 F23 79.2(12) . . ?
F23X P20 F23 83.2(6) 6 . ?
F23X P20 F23 10.9(10) . . ?
F22 P20 F23 83.1(3) 6 . ?
F22 P20 F23 86.9(2) . . ?
F23 P20 F23 89.0(8) 6 . ?
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 N4 1.979(2) . ?
Ni1 N4 1.979(2) 4 ?
Ni1 N1 1.987(2) . ?
Ni1 N1 1.987(2) 4 ?
N1 C2 1.305(3) . ?
N1 C8 1.479(3) . ?
C2 C3 1.461(3) . ?
C2 C11 1.483(3) . ?
C3 N4 1.294(3) . ?
N4 C5 1.487(3) . ?
C5 C7 1.522(4) . ?
C5 C6 1.524(4) . ?
C8 C10 1.515(4) . ?
C8 C9 1.528(4) . ?
C11 C12 1.388(4) . ?
C11 C16 1.400(4) . ?
C12 C13 1.391(4) . ?
C13 C14 1.389(5) . ?
C14 C15 1.395(4) . ?
C15 C16 1.390(4) . ?
P20 F21 1.576(3) 6 ?
P20 F21 1.576(3) . ?
P20 F22X 1.600(4) 6 ?
P20 F22X 1.600(4) . ?
P20 F21X 1.601(4) 6 ?
P20 F21X 1.601(4) . ?
P20 F23X 1.604(4) 6 ?
P20 F23X 1.604(4) . ?
P20 F22 1.611(3) 6 ?
P20 F22 1.611(3) . ?
P20 F23 1.614(3) 6 ?
P20 F23 1.614(3) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139129201
