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#$Date: 2016-03-25 16:25:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179969 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/63/7026328.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_7026328
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_formula_moiety         'C21 H18 N4 O3 Zn, 2(Cl O4)'
_chemical_formula_sum            'C21 H18 Cl2 N4 O11 Zn'
_chemical_formula_weight         638.66
_chemical_name_common            aja0723
_chemical_name_systematic
;
?
;
_space_group_IT_number           56
_symmetry_cell_setting           orthorhombic
_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                   9.8506(3)
_cell_length_b                   12.4696(4)
_cell_length_c                   19.7856(6)
_cell_measurement_reflns_used    8577
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     2430.33(13)
_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    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0473
_diffrn_reflns_av_sigmaI/netI    0.0491
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8971
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.301
_exptl_absorpt_correction_T_max  0.552
_exptl_absorpt_correction_T_min  0.524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav (Blessing, 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.745
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.329
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2758
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0545
_refine_ls_R_factor_gt           0.0394
_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)+(0.0356P)²+2.6986P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0895
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                2229
_reflns_number_total             2758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00344a.txt
_cod_data_source_block           aja0722
_cod_original_sg_symbol_H-M      Pccn
_cod_database_code               7026328
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
C1 C 0.7500 0.2500 0.1880(2) 0.0216(8) Uani 1 2 d S
C2 C 0.6204(3) 0.2872(2) 0.15395(13) 0.0192(5) Uani 1 1 d .
C3 C 0.5123(3) 0.3094(2) 0.19696(15) 0.0267(6) Uani 1 1 d .
H3 H 0.5217 0.3009 0.2444 0.032 Uiso 1 1 calc R
C4 C 0.3911(3) 0.3440(2) 0.16940(17) 0.0328(7) Uani 1 1 d .
H4 H 0.3157 0.3593 0.1977 0.039 Uiso 1 1 calc R
C5 C 0.3811(3) 0.3561(2) 0.10024(16) 0.0284(7) Uani 1 1 d .
H5 H 0.2982 0.3793 0.0805 0.034 Uiso 1 1 calc R
C6 C 0.4925(2) 0.3342(2) 0.05979(14) 0.0199(6) Uani 1 1 d .
C7 C 0.4900(3) 0.3505(2) -0.01498(14) 0.0197(6) Uani 1 1 d .
C8 C 0.3782(3) 0.3927(2) -0.04872(17) 0.0326(7) Uani 1 1 d .
H8 H 0.2972 0.4091 -0.0248 0.039 Uiso 1 1 calc R
C9 C 0.3871(4) 0.4105(2) -0.11805(17) 0.0393(8) Uani 1 1 d .
H9 H 0.3113 0.4379 -0.1423 0.047 Uiso 1 1 calc R
C10 C 0.5058(3) 0.3882(2) -0.15098(16) 0.0352(8) Uani 1 1 d .
H10 H 0.5146 0.4017 -0.1980 0.042 Uiso 1 1 calc R
C11 C 0.6128(3) 0.3458(2) -0.11453(14) 0.0249(6) Uani 1 1 d .
H11 H 0.6952 0.3301 -0.1374 0.030 Uiso 1 1 calc R
N1 N 0.6110(2) 0.29901(16) 0.08664(11) 0.0159(4) Uani 1 1 d .
N2 N 0.6046(2) 0.32584(16) -0.04829(11) 0.0185(5) Uani 1 1 d .
O1 O 0.7500 0.2500 0.24951(14) 0.0343(7) Uani 1 2 d S
O2 O 0.63929(19) 0.09754(15) 0.00689(9) 0.0229(4) Uani 1 1 d .
H2A H 0.5905 0.0963 -0.0344 0.027 Uiso 1 1 d .
H2B H 0.5681 0.0940 0.0369 0.027 Uiso 1 1 d .
O3 O 0.4370(2) 0.07742(17) 0.10332(10) 0.0322(5) Uani 1 1 d .
O4 O 0.3718(2) 0.00601(18) 0.20809(10) 0.0355(5) Uani 1 1 d .
O5 O 0.6025(2) 0.03187(17) 0.18397(11) 0.0348(5) Uani 1 1 d .
O6 O 0.4809(3) -0.10345(16) 0.12834(11) 0.0402(6) Uani 1 1 d .
Cl1 Cl 0.47353(7) 0.00230(5) 0.15695(3) 0.02093(16) Uani 1 1 d .
Zn1 Zn 0.7500 0.2500 0.01177(2) 0.01521(13) Uani 1 2 d S
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'
Zn Zn 0.2839 1.4301 '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
O1 C1 C2 116.39(17) . .
O1 C1 C2 116.39(17) . 2_655
C2 C1 C2 127.2(3) . 2_655
N1 C2 C3 122.2(3) . .
N1 C2 C1 122.2(2) . .
C3 C2 C1 115.7(3) . .
C4 C3 C2 118.8(3) . .
C4 C3 H3 120.6 . .
C2 C3 H3 120.6 . .
C5 C4 C3 119.2(3) . .
C5 C4 H4 120.4 . .
C3 C4 H4 120.4 . .
C4 C5 C6 119.6(3) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
N1 C6 C5 121.3(3) . .
N1 C6 C7 116.5(2) . .
C5 C6 C7 122.2(2) . .
N2 C7 C8 121.1(3) . .
N2 C7 C6 116.1(2) . .
C8 C7 C6 122.7(2) . .
C7 C8 C9 118.9(3) . .
C7 C8 H8 120.5 . .
C9 C8 H8 120.5 . .
C10 C9 C8 119.4(3) . .
C10 C9 H9 120.3 . .
C8 C9 H9 120.3 . .
C9 C10 C11 118.8(3) . .
C9 C10 H10 120.6 . .
C11 C10 H10 120.6 . .
N2 C11 C10 122.5(3) . .
N2 C11 H11 118.8 . .
C10 C11 H11 118.8 . .
C2 N1 C6 118.9(2) . .
C2 N1 Zn1 128.36(17) . .
C6 N1 Zn1 112.20(17) . .
C11 N2 C7 119.3(2) . .
C11 N2 Zn1 126.95(18) . .
C7 N2 Zn1 113.66(17) . .
Zn1 O2 H2A 107.7 . .
Zn1 O2 H2B 113.1 . .
H2A O2 H2B 99.7 . .
O4 Cl1 O5 110.58(13) . .
O4 Cl1 O6 110.20(14) . .
O5 Cl1 O6 109.86(14) . .
O4 Cl1 O3 108.77(13) . .
O5 Cl1 O3 109.03(13) . .
O6 Cl1 O3 108.36(13) . .
N2 Zn1 N2 110.60(12) . 2_655
N2 Zn1 N1 167.72(8) . 2_655
N2 Zn1 N1 79.81(8) 2_655 2_655
N2 Zn1 N1 79.81(8) . .
N2 Zn1 N1 167.72(8) 2_655 .
N1 Zn1 N1 90.69(12) 2_655 .
N2 Zn1 O2 85.60(8) . 2_655
N2 Zn1 O2 91.52(8) 2_655 2_655
N1 Zn1 O2 87.67(7) 2_655 2_655
N1 Zn1 O2 95.89(7) . 2_655
N2 Zn1 O2 91.52(8) . .
N2 Zn1 O2 85.60(8) 2_655 .
N1 Zn1 O2 95.89(7) 2_655 .
N1 Zn1 O2 87.67(7) . .
O2 Zn1 O2 174.95(10) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O1 1.216(4) .
C1 C2 1.517(3) .
C1 C2 1.517(3) 2_655
C2 N1 1.343(3) .
C2 C3 1.391(4) .
C3 C4 1.381(4) .
C3 H3 0.9500 .
C4 C5 1.380(4) .
C4 H4 0.9500 .
C5 C6 1.385(4) .
C5 H5 0.9500 .
C6 N1 1.356(3) .
C6 C7 1.494(4) .
C7 N2 1.344(3) .
C7 C8 1.391(4) .
C8 C9 1.392(5) .
C8 H8 0.9500 .
C9 C10 1.367(5) .
C9 H9 0.9500 .
C10 C11 1.383(4) .
C10 H10 0.9500 .
C11 N2 1.336(3) .
C11 H11 0.9500 .
N1 Zn1 2.108(2) .
N2 Zn1 2.087(2) .
O2 Zn1 2.1938(18) .
O2 H2A 0.9479 .
O2 H2B 0.9200 .
O3 Cl1 1.460(2) .
O4 Cl1 1.425(2) .
O5 Cl1 1.427(2) .
O6 Cl1 1.437(2) .
Zn1 N2 2.087(2) 2_655
Zn1 N1 2.108(2) 2_655
Zn1 O2 2.1938(18) 2_655
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
_geom_torsion_site_symmetry_4
O1 C1 C2 N1 174.62(17) . .
C2 C1 C2 N1 -5.38(17) 2_655 .
O1 C1 C2 C3 -4.7(2) . .
C2 C1 C2 C3 175.3(2) 2_655 .
N1 C2 C3 C4 0.4(4) . .
C1 C2 C3 C4 179.8(2) . .
C2 C3 C4 C5 -0.3(4) . .
C3 C4 C5 C6 -0.5(4) . .
C4 C5 C6 N1 1.3(4) . .
C4 C5 C6 C7 -177.1(2) . .
N1 C6 C7 N2 1.7(3) . .
C5 C6 C7 N2 -179.8(2) . .
N1 C6 C7 C8 -175.8(2) . .
C5 C6 C7 C8 2.7(4) . .
N2 C7 C8 C9 -0.8(4) . .
C6 C7 C8 C9 176.7(3) . .
C7 C8 C9 C10 -1.3(4) . .
C8 C9 C10 C11 1.7(5) . .
C9 C10 C11 N2 -0.1(4) . .
C3 C2 N1 C6 0.3(4) . .
C1 C2 N1 C6 -179.0(2) . .
C3 C2 N1 Zn1 -170.47(19) . .
C1 C2 N1 Zn1 10.2(3) . .
C5 C6 N1 C2 -1.2(4) . .
C7 C6 N1 C2 177.3(2) . .
C5 C6 N1 Zn1 171.0(2) . .
C7 C6 N1 Zn1 -10.5(3) . .
C10 C11 N2 C7 -1.9(4) . .
C10 C11 N2 Zn1 174.2(2) . .
C8 C7 N2 C11 2.4(4) . .
C6 C7 N2 C11 -175.2(2) . .
C8 C7 N2 Zn1 -174.3(2) . .
C6 C7 N2 Zn1 8.1(3) . .
C11 N2 Zn1 N2 -13.62(18) . 2_655
C7 N2 Zn1 N2 162.7(2) . 2_655
C11 N2 Zn1 N1 133.3(4) . 2_655
C7 N2 Zn1 N1 -50.4(5) . 2_655
C11 N2 Zn1 N1 173.1(2) . .
C7 N2 Zn1 N1 -10.53(17) . .
C11 N2 Zn1 O2 76.4(2) . 2_655
C7 N2 Zn1 O2 -107.32(18) . 2_655
C11 N2 Zn1 O2 -99.5(2) . .
C7 N2 Zn1 O2 76.83(18) . .
C2 N1 Zn1 N2 -177.4(2) . .
C6 N1 Zn1 N2 11.28(17) . .
C2 N1 Zn1 N2 33.8(5) . 2_655
C6 N1 Zn1 N2 -137.5(4) . 2_655
C2 N1 Zn1 N1 -5.26(16) . 2_655
C6 N1 Zn1 N1 -176.6(2) . 2_655
C2 N1 Zn1 O2 -93.0(2) . 2_655
C6 N1 Zn1 O2 95.72(17) . 2_655
C2 N1 Zn1 O2 90.6(2) . .
C6 N1 Zn1 O2 -80.69(17) . .
