#------------------------------------------------------------------------------
#$Date: 2023-12-22 17:07:40 +0200 (Fri, 22 Dec 2023) $
#$Revision: 288505 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/03/09/7030912.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_7030912
loop_
_publ_author_name
'Swarts, Andrew J.'
'Mapolie, Selwyn F.'
_publ_section_title
;
 The synthesis and application of novel Ni(ii) N-alkyl dipyridylaldiminato
 complexes as selective ethylene oligomerisation catalysts.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9892
_journal_page_last               9900
_journal_paper_doi               10.1039/c4dt00537f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         '2(C13 H16 N3), Cl4 Ni, H2 O'
_chemical_formula_sum            'C26 H34 Cl4 N6 Ni O'
_chemical_formula_weight         647.10
_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                 123.276(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.751(4)
_cell_length_b                   11.949(2)
_cell_length_c                   13.415(2)
_cell_measurement_reflns_used    2911
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.24
_cell_volume                     2914.9(8)
_computing_cell_refinement       'SAINT (Bruker 2002)'
_computing_data_collection       'SAINT (Bruker 2002)'
_computing_data_reduction        'SAINT (Bruker 2002)'
_computing_molecular_graphics    'X-Seed (Atwood & Barbour, 2003)'
_computing_publication_material  'X-Seed (Atwood & Barbour, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8948
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.064
_exptl_absorpt_correction_T_max  0.8983
_exptl_absorpt_correction_T_min  0.8028
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0310
_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)+(0.0299P)²+1.7343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                2794
_reflns_number_total             3379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00537f2.cif
_cod_data_source_block           c:\1e-A.cif
_cod_depositor_comments
;Adding full bibliography for 7030911--7030912.cif.

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_cell_volume        2915.0(8)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7030912
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
Ni1 Ni 0.0000 0.24608(3) 0.2500 0.01559(10) Uani 1 2 d S
N1 N 0.29263(8) -0.01440(13) 0.37997(13) 0.0159(3) Uani 1 1 d .
N2 N 0.18408(8) -0.11870(13) 0.30104(14) 0.0203(3) Uani 1 1 d .
C3 C 0.33448(10) 0.07927(15) 0.41832(16) 0.0174(4) Uani 1 1 d .
C4 C 0.21980(10) -0.01669(16) 0.33545(15) 0.0185(4) Uani 1 1 d .
N5 N 0.29204(8) -0.22533(12) 0.38885(13) 0.0163(3) Uani 1 1 d .
C6 C 0.33019(10) -0.32150(15) 0.43282(16) 0.0173(4) Uani 1 1 d .
C7 C 0.22021(11) -0.41729(17) 0.38135(17) 0.0238(4) Uani 1 1 d .
H7 H 0.1954 -0.4841 0.3778 0.029 Uiso 1 1 calc R
C8 C 0.18512(11) 0.08441(17) 0.32788(17) 0.0228(4) Uani 1 1 d .
H8 H 0.1340 0.0865 0.2970 0.027 Uiso 1 1 calc R
C9 C 0.21984(10) -0.22275(16) 0.34388(16) 0.0187(4) Uani 1 1 d .
C10 C 0.29534(11) -0.42022(16) 0.42841(16) 0.0213(4) Uani 1 1 d .
H10 H 0.3221 -0.4883 0.4568 0.026 Uiso 1 1 calc R
C11 C 0.18145(10) -0.31848(17) 0.33989(17) 0.0223(4) Uani 1 1 d .
H11 H 0.1305 -0.3154 0.3096 0.027 Uiso 1 1 calc R
C12 C 0.41392(10) 0.06426(16) 0.46500(17) 0.0204(4) Uani 1 1 d .
H12A H 0.4372 0.0186 0.5375 0.031 Uiso 1 1 calc R
H12B H 0.4380 0.1376 0.4834 0.031 Uiso 1 1 calc R
H12C H 0.4188 0.0267 0.4047 0.031 Uiso 1 1 calc R
C13 C 0.22639(11) 0.18041(17) 0.36597(17) 0.0242(4) Uani 1 1 d .
H13 H 0.2033 0.2494 0.3613 0.029 Uiso 1 1 calc R
C14 C 0.41106(10) -0.31381(16) 0.48535(18) 0.0221(4) Uani 1 1 d .
H14A H 0.4193 -0.2874 0.4245 0.033 Uiso 1 1 calc R
H14B H 0.4335 -0.3878 0.5136 0.033 Uiso 1 1 calc R
H14C H 0.4333 -0.2612 0.5524 0.033 Uiso 1 1 calc R
C15 C 0.30144(11) 0.17932(16) 0.41139(16) 0.0215(4) Uani 1 1 d .
H15 H 0.3292 0.2467 0.4371 0.026 Uiso 1 1 calc R
C17 C 0.10281(10) -0.11700(19) 0.23067(18) 0.0286(5) Uani 1 1 d .
H17A H 0.0858 -0.1131 0.2847 0.043 Uiso 1 1 calc R
H17B H 0.0838 -0.1853 0.1825 0.043 Uiso 1 1 calc R
H17C H 0.0850 -0.0515 0.1781 0.043 Uiso 1 1 calc R
Cl3 Cl 0.08167(2) 0.36833(4) 0.25443(4) 0.01878(11) Uani 1 1 d .
Cl2 Cl 0.04505(3) 0.12624(4) 0.40501(4) 0.02293(12) Uani 1 1 d .
O3 O 0.0000 0.59785(19) 0.2500 0.0384(6) Uani 1 2 d S
H6 H 0.0311(17) 0.542(3) 0.245(3) 0.095(12) Uiso 1 1 d .
H1 H 0.3121(13) -0.080(2) 0.387(2) 0.040(7) Uiso 1 1 d .
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl2 Ni1 Cl2 101.29(3) 2 .
Cl2 Ni1 Cl3 111.668(18) 2 .
Cl2 Ni1 Cl3 116.424(18) . .
Cl2 Ni1 Cl3 116.423(18) 2 2
Cl2 Ni1 Cl3 111.668(18) . 2
Cl3 Ni1 Cl3 100.12(3) . 2
C4 N1 C3 124.41(16) . .
C4 N1 H1 114.2(16) . .
C3 N1 H1 121.2(16) . .
C4 N2 C9 123.92(15) . .
C4 N2 C17 117.22(16) . .
C9 N2 C17 118.11(16) . .
N1 C3 C15 118.48(17) . .
N1 C3 C12 116.29(15) . .
C15 C3 C12 125.23(17) . .
N1 C4 N2 118.24(16) . .
N1 C4 C8 117.99(17) . .
N2 C4 C8 123.77(17) . .
C9 N5 C6 120.32(16) . .
N5 C6 C10 121.03(17) . .
N5 C6 C14 115.83(16) . .
C10 C6 C14 123.14(17) . .
C11 C7 C10 120.69(18) . .
C11 C7 H7 119.7 . .
C10 C7 H7 119.7 . .
C13 C8 C4 118.62(18) . .
C13 C8 H8 120.7 . .
C4 C8 H8 120.7 . .
N5 C9 C11 121.75(17) . .
N5 C9 N2 116.88(16) . .
C11 C9 N2 121.36(17) . .
C6 C10 C7 118.46(18) . .
C6 C10 H10 120.8 . .
C7 C10 H10 120.8 . .
C7 C11 C9 117.68(18) . .
C7 C11 H11 121.2 . .
C9 C11 H11 121.2 . .
C3 C12 H12A 109.5 . .
C3 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C3 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C8 C13 C15 121.67(18) . .
C8 C13 H13 119.2 . .
C15 C13 H13 119.2 . .
C6 C14 H14A 109.5 . .
C6 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C6 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C3 C15 C13 118.82(18) . .
C3 C15 H15 120.6 . .
C13 C15 H15 120.6 . .
N2 C17 H17A 109.5 . .
N2 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
N2 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 Cl2 2.2581(6) 2
Ni1 Cl2 2.2581(6) .
Ni1 Cl3 2.2753(5) .
Ni1 Cl3 2.2753(5) 2
N1 C4 1.352(2) .
N1 C3 1.354(2) .
N1 H1 0.87(2) .
N2 C4 1.382(2) .
N2 C9 1.411(2) .
N2 C17 1.478(2) .
C3 C15 1.372(3) .
C3 C12 1.491(3) .
C4 C8 1.398(3) .
N5 C9 1.338(2) .
N5 C6 1.349(2) .
C6 C10 1.386(3) .
C6 C14 1.496(2) .
C7 C11 1.378(3) .
C7 C10 1.392(3) .
C7 H7 0.9500 .
C8 C13 1.371(3) .
C8 H8 0.9500 .
C9 C11 1.400(3) .
C10 H10 0.9500 .
C11 H11 0.9500 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C15 1.395(3) .
C13 H13 0.9500 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
C15 H15 0.9500 .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O3 H6 0.98(3) .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C4 N1 C3 C15 -0.4(3)
C4 N1 C3 C12 179.70(16)
C3 N1 C4 N2 -179.16(16)
C3 N1 C4 C8 0.3(3)
C9 N2 C4 N1 22.3(3)
C17 N2 C4 N1 -167.88(16)
C9 N2 C4 C8 -157.16(18)
C17 N2 C4 C8 12.7(3)
C9 N5 C6 C10 2.5(3)
C9 N5 C6 C14 -177.59(16)
N1 C4 C8 C13 -0.1(3)
N2 C4 C8 C13 179.28(17)
C6 N5 C9 C11 -0.5(3)
C6 N5 C9 N2 179.22(16)
C4 N2 C9 N5 -21.6(3)
C17 N2 C9 N5 168.65(16)
C4 N2 C9 C11 158.12(17)
C17 N2 C9 C11 -11.7(3)
N5 C6 C10 C7 -2.3(3)
C14 C6 C10 C7 177.77(17)
C11 C7 C10 C6 0.2(3)
C10 C7 C11 C9 1.7(3)
N5 C9 C11 C7 -1.6(3)
N2 C9 C11 C7 178.71(17)
C4 C8 C13 C15 0.1(3)
N1 C3 C15 C13 0.4(3)
C12 C3 C15 C13 -179.74(17)
C8 C13 C15 C3 -0.3(3)
