#------------------------------------------------------------------------------
#$Date: 2023-05-14 10:24:15 +0300 (Sun, 14 May 2023) $
#$Revision: 283750 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/02/63/7026326.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_7026326
loop_
_publ_author_name
'Knight, James C.'
'Amoroso, Angelo J.'
'Edwards, Peter G.'
'Prabaharan, Ravi'
'Singh, Neha'
_publ_section_title
;
 The co-ordination chemistry of bis(2,2'-bipyrid-6'-yl)ketone with first
 row transition metals: the reversible interconversion of a mononuclear
 complex and a dinuclear hemiketal containing species.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8925
_journal_page_last               8936
_journal_paper_doi               10.1039/c0dt00344a
_journal_volume                  39
_journal_year                    2010
_chemical_compound_source        'synthesised by authors'
_chemical_formula_moiety         'C21 H18 N4 Ni O3, 2(Cl O4)'
_chemical_formula_sum            'C21 H18 Cl2 N4 Ni O11'
_chemical_formula_weight         632.00
_chemical_name_common            aja0607
_chemical_name_systematic        'bisbipyketone nickel'
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      56
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_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            4
_cell_length_a                   9.802(2)
_cell_length_b                   12.453(3)
_cell_length_c                   19.760(4)
_cell_measurement_reflns_used    8144
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     2412.0(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Dirdiff-99 (Beurskens, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.0745
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            10140
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.097
_exptl_absorpt_correction_T_max  0.8982
_exptl_absorpt_correction_T_min  0.7711
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.740
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_recrystallization_method
'slow diffusion of ether in acetonitrile'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2755
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0465
_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)+(0.0399P)²+1.3889P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0971
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                2028
_reflns_number_total             2755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00344a.txt
_cod_data_source_block           pccn
_cod_database_code               7026326
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'x+1/2, -y, -z+1/2'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'-x-1/2, y, z-1/2'
'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 0.2500 0.7500 0.01192(2) 0.01586(15) Uani 1 2 d S
Cl1 Cl -0.02437(7) 0.99844(6) 0.15479(3) 0.02365(19) Uani 1 1 d .
O1 O 0.1447(2) 0.89770(17) 0.00770(9) 0.0237(5) Uani 1 1 d .
N1 N 0.3875(2) 0.79921(18) 0.08306(11) 0.0193(5) Uani 1 1 d .
C1 C 0.2500 0.7500 0.1850(2) 0.0265(9) Uani 1 2 d S
O2 O 0.2500 0.7500 0.24633(14) 0.0404(9) Uani 1 2 d S
N2 N 0.3915(2) 0.82292(18) -0.05036(11) 0.0206(5) Uani 1 1 d .
C2 C 0.3784(3) 0.7878(2) 0.15060(14) 0.0237(6) Uani 1 1 d .
O3 O 0.1056(2) 0.96793(19) 0.18086(11) 0.0383(6) Uani 1 1 d .
C3 C 0.4887(3) 0.8113(3) 0.19326(15) 0.0318(8) Uani 1 1 d .
H3 H 0.4804 0.8035 0.2409 0.038 Uiso 1 1 calc R
O4 O -0.0176(3) 1.10366(19) 0.12646(12) 0.0467(7) Uani 1 1 d .
C4 C 0.6089(3) 0.8457(3) 0.16507(17) 0.0372(8) Uani 1 1 d .
H4 H 0.6848 0.8620 0.1931 0.045 Uiso 1 1 calc R
O5 O -0.1259(2) 0.9940(2) 0.20638(11) 0.0399(6) Uani 1 1 d .
C5 C 0.6188(3) 0.8565(3) 0.09669(17) 0.0325(8) Uani 1 1 d .
H5 H 0.7021 0.8792 0.0767 0.039 Uiso 1 1 calc R
O6 O -0.0627(2) 0.92382(19) 0.10126(10) 0.0373(6) Uani 1 1 d .
C6 C 0.5065(3) 0.8340(2) 0.05639(15) 0.0237(7) Uani 1 1 d .
C7 C 0.5079(3) 0.8492(2) -0.01788(15) 0.0227(6) Uani 1 1 d .
C8 C 0.6176(3) 0.8927(3) -0.05323(18) 0.0361(8) Uani 1 1 d .
H8 H 0.6996 0.9106 -0.0302 0.043 Uiso 1 1 calc R
C9 C 0.6058(4) 0.9096(3) -0.12276(18) 0.0411(9) Uani 1 1 d .
H9 H 0.6808 0.9366 -0.1480 0.049 Uiso 1 1 calc R
C10 C 0.4851(4) 0.8869(3) -0.15403(16) 0.0357(8) Uani 1 1 d .
H10 H 0.4739 0.9005 -0.2010 0.043 Uiso 1 1 calc R
C11 C 0.3807(3) 0.8444(2) -0.11694(14) 0.0276(7) Uani 1 1 d .
H11 H 0.2968 0.8293 -0.1391 0.033 Uiso 1 1 calc R
H1 H 0.0682 0.9017 0.0371 0.073(14) Uiso 1 1 d R
H2 H 0.1126 0.9034 -0.0376 0.085(15) Uiso 1 1 d 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'
O O 0.0106 0.0060 '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'
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 92.97(13) . 2_565
N1 Ni1 N2 170.37(9) . 2_565
N1 Ni1 N2 80.51(9) 2_565 2_565
N1 Ni1 N2 80.51(9) . .
N1 Ni1 N2 170.37(9) 2_565 .
N2 Ni1 N2 106.81(13) 2_565 .
N1 Ni1 O1 88.05(8) . 2_565
N1 Ni1 O1 95.07(8) 2_565 2_565
N2 Ni1 O1 85.50(9) 2_565 2_565
N2 Ni1 O1 91.80(9) . 2_565
N1 Ni1 O1 95.07(8) . .
N1 Ni1 O1 88.05(8) 2_565 .
N2 Ni1 O1 91.80(9) 2_565 .
N2 Ni1 O1 85.50(9) . .
O1 Ni1 O1 175.47(10) 2_565 .
O5 Cl1 O3 110.81(14) . .
O5 Cl1 O4 110.39(15) . .
O3 Cl1 O4 110.17(15) . .
O5 Cl1 O6 108.35(14) . .
O3 Cl1 O6 108.81(14) . .
O4 Cl1 O6 108.24(14) . .
Ni1 O1 H1 114.0 . .
Ni1 O1 H2 105.3 . .
H1 O1 H2 108.1 . .
C2 N1 C6 118.6(2) . .
C2 N1 Ni1 127.42(19) . .
C6 N1 Ni1 113.42(18) . .
O2 C1 C2 116.81(17) . 2_565
O2 C1 C2 116.81(17) . .
C2 C1 C2 126.4(3) 2_565 .
C11 N2 C7 118.8(2) . .
C11 N2 Ni1 128.1(2) . .
C7 N2 Ni1 113.03(18) . .
N1 C2 C3 121.6(3) . .
N1 C2 C1 122.4(3) . .
C3 C2 C1 116.0(3) . .
C4 C3 C2 118.9(3) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C5 C4 C3 119.7(3) . .
C5 C4 H4 120.1 . .
C3 C4 H4 120.1 . .
C4 C5 C6 119.5(3) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
N1 C6 C5 121.7(3) . .
N1 C6 C7 115.8(2) . .
C5 C6 C7 122.4(3) . .
N2 C7 C8 120.6(3) . .
N2 C7 C6 115.6(2) . .
C8 C7 C6 123.7(3) . .
C7 C8 C9 119.3(3) . .
C7 C8 H8 120.4 . .
C9 C8 H8 120.4 . .
C10 C9 C8 119.1(3) . .
C10 C9 H9 120.4 . .
C8 C9 H9 120.4 . .
C9 C10 C11 119.1(3) . .
C9 C10 H10 120.4 . .
C11 C10 H10 120.4 . .
N2 C11 C10 122.9(3) . .
N2 C11 H11 118.6 . .
C10 C11 H11 118.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N1 2.042(2) .
Ni1 N1 2.042(2) 2_565
Ni1 N2 2.064(2) 2_565
Ni1 N2 2.064(2) .
Ni1 O1 2.111(2) 2_565
Ni1 O1 2.111(2) .
Cl1 O5 1.425(2) .
Cl1 O3 1.426(2) .
Cl1 O4 1.426(2) .
Cl1 O6 1.457(2) .
O1 H1 0.9499 .
O1 H2 0.9516 .
N1 C2 1.345(3) .
N1 C6 1.351(4) .
C1 O2 1.212(5) .
C1 C2 1.506(3) 2_565
C1 C2 1.506(3) .
N2 C11 1.347(3) .
N2 C7 1.350(4) .
C2 C3 1.402(4) .
C3 C4 1.372(5) .
C3 H3 0.9500 .
C4 C5 1.361(5) .
C4 H4 0.9500 .
C5 C6 1.387(4) .
C5 H5 0.9500 .
C6 C7 1.480(4) .
C7 C8 1.391(4) .
C8 C9 1.395(5) .
C8 H8 0.9500 .
C9 C10 1.364(5) .
C9 H9 0.9500 .
C10 C11 1.366(4) .
C10 H10 0.9500 .
C11 H11 0.9500 .
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
_geom_torsion_site_symmetry_1
N1 Ni1 N1 C2 4.93(19) 2_565
O1 Ni1 N1 C2 -90.0(2) 2_565
O1 Ni1 N1 C2 93.2(2) .
N1 Ni1 N1 C6 175.9(2) 2_565
N2 Ni1 N1 C6 -11.2(2) .
O1 Ni1 N1 C6 80.9(2) 2_565
O1 Ni1 N1 C6 -95.8(2) .
N1 Ni1 N2 C11 -171.0(2) .
N2 Ni1 N2 C11 15.4(2) 2_565
O1 Ni1 N2 C11 101.2(2) 2_565
O1 Ni1 N2 C11 -75.1(2) .
N1 Ni1 N2 C7 10.00(19) .
N2 Ni1 N2 C7 -163.6(2) 2_565
O1 Ni1 N2 C7 -77.7(2) 2_565
O1 Ni1 N2 C7 105.9(2) .
C6 N1 C2 C3 0.1(4) .
Ni1 N1 C2 C3 170.7(2) .
C6 N1 C2 C1 179.8(2) .
Ni1 N1 C2 C1 -9.7(4) .
O2 C1 C2 N1 -174.89(19) .
C2 C1 C2 N1 5.11(19) 2_565
O2 C1 C2 C3 4.8(3) .
C2 C1 C2 C3 -175.2(3) 2_565
N1 C2 C3 C4 -0.6(4) .
C1 C2 C3 C4 179.7(3) .
C2 C3 C4 C5 0.0(5) .
C3 C4 C5 C6 1.0(5) .
C2 N1 C6 C5 1.0(4) .
Ni1 N1 C6 C5 -170.9(2) .
C2 N1 C6 C7 -177.5(2) .
Ni1 N1 C6 C7 10.7(3) .
C4 C5 C6 N1 -1.5(5) .
C4 C5 C6 C7 176.8(3) .
C11 N2 C7 C8 -3.3(4) .
Ni1 N2 C7 C8 175.8(2) .
C11 N2 C7 C6 173.6(2) .
Ni1 N2 C7 C6 -7.3(3) .
N1 C6 C7 N2 -2.2(4) .
C5 C6 C7 N2 179.4(3) .
N1 C6 C7 C8 174.6(3) .
C5 C6 C7 C8 -3.8(5) .
N2 C7 C8 C9 0.4(5) .
C6 C7 C8 C9 -176.2(3) .
C7 C8 C9 C10 2.5(5) .
C8 C9 C10 C11 -2.5(5) .
C7 N2 C11 C10 3.3(4) .
Ni1 N2 C11 C10 -175.6(2) .
C9 C10 C11 N2 -0.4(5) .
loop_
_cod_changelog_entry_id
_cod_changelog_entry_author
_cod_changelog_entry_date
_cod_changelog_entry_text
1 'Saulius Gra\<zulis' 2023-05-14T10:16:00+03:00
;Changing '_diffrn_radiation_probe' value from 'electron' to 'x-ray',
since all other radiation parameters (radiation source, wavelength, rad. type,
monochromator) specify a sealed X-ray tube, and the scattering factors
are given for X-rays.
;
