#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:31:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179794 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/90/7009006.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_7009006
loop_
_publ_author_name
'Erxleben, Andrea'
'Hermann, Jolante'
_publ_section_title
;
 Di- and poly-nuclear zinc(II) Schiff base complexes: synthesis,
 structural studies and reaction with an α-amino acid ester
;
_journal_issue                   4
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              569
_journal_paper_doi               10.1039/a907839h
_journal_year                    2000
_chemical_formula_sum            'C13 H18 N2 O8 Zn'
_chemical_formula_weight         395.66
_chemical_name_systematic        ?
_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   'Fourier-difference map '
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 108.13(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.290(4)
_cell_length_b                   8.514(2)
_cell_length_c                   19.488(4)
_cell_measurement_reflns_used    5372
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.58
_cell_measurement_theta_min      4.79
_cell_volume                     3199.4(13)
_computing_cell_refinement       'Denzo, Scalepack (Otwinowski, Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius BV, The Netherlands) '
_computing_data_reduction        'Denzo, Scalepack (Otwinowski, Minor,1997)'
_computing_molecular_graphics    'Siemens SHELXTL PLUS '
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       ' Nonius KappaCCD '
_diffrn_measurement_method       ' profile fitted '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.074
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            5372
_diffrn_reflns_theta_max         25.58
_diffrn_reflns_theta_min         4.79
_exptl_absorpt_coefficient_mu    1.580
_exptl_absorpt_correction_T_max  0.7428
_exptl_absorpt_correction_T_min  0.6934
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_description       cube
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.940
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment    isotropically
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         2909
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_obs          0.0430
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0522P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1189
_refine_ls_wR_factor_obs         0.0880
_reflns_number_observed          1864
_reflns_number_total             2920
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907839h.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3199.4(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7009006
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Zn1 Zn 0.30503(2) 0.13543(5) 0.35230(2) 0.0384(2) Uani 1 d . .
N1 N 0.4174(2) -0.1636(4) 0.5365(2) 0.0487(9) Uani 1 d . .
H1 H 0.4151(23) -0.0966(48) 0.5045(24) 0.058 Uiso 1 d . .
N2 N 0.2103(2) 0.1975(3) 0.3589(2) 0.0376(7) Uani 1 d . .
O1 O 0.32175(14) 0.0131(3) 0.44616(15) 0.0490(7) Uani 1 d . .
O2 O 0.60202(14) -0.2321(3) 0.6116(2) 0.0506(7) Uani 1 d . .
O3 O 0.5431(2) -0.0075(4) 0.5839(2) 0.0779(11) Uani 1 d . .
O4 O 0.1840(2) 0.4850(3) 0.2195(2) 0.0531(8) Uani 1 d . .
O5 O 0.27326(14) 0.3250(3) 0.27049(14) 0.0461(7) Uani 1 d . .
C1 C 0.2819(2) -0.0079(4) 0.4856(2) 0.0373(9) Uani 1 d . .
C2 C 0.3055(2) -0.1037(4) 0.5491(2) 0.0398(9) Uani 1 d . .
C3 C 0.2619(2) -0.1358(5) 0.5910(2) 0.0422(9) Uani 1 d . .
H3 H 0.2785(21) -0.1894(45) 0.6303(23) 0.051 Uiso 1 d . .
C4 C 0.1960(2) -0.0717(4) 0.5749(2) 0.0395(9) Uani 1 d . .
C5 C 0.1748(2) 0.0248(5) 0.5150(2) 0.0394(10) Uani 1 d . .
H5 H 0.1384(22) 0.0559(49) 0.5050(23) 0.047 Uiso 1 d . .
C6 C 0.2145(2) 0.0577(4) 0.4694(2) 0.0370(9) Uani 1 d . .
C7 C 0.1488(3) -0.1121(6) 0.6186(3) 0.0503(11) Uani 1 d . .
H7A H 0.1415(22) -0.2155(53) 0.6173(23) 0.060 Uiso 1 d . .
H7B H 0.1143(23) -0.0407(51) 0.6072(23) 0.060 Uiso 1 d . .
H7C H 0.1722(23) -0.0865(48) 0.6674(26) 0.060 Uiso 1 d . .
C8 C 0.3715(2) -0.1786(5) 0.5689(2) 0.0464(10) Uani 1 d . .
H8 H 0.3878(21) -0.2428(43) 0.6177(23) 0.056 Uiso 1 d . .
C9 C 0.4831(2) -0.2532(5) 0.5573(3) 0.0614(13) Uani 1 d . .
H9A H 0.4804(23) -0.3499(50) 0.5937(25) 0.074 Uiso 1 d . .
H9B H 0.4888(23) -0.3114(56) 0.5119(26) 0.074 Uiso 1 d . .
C10 C 0.5474(2) -0.1528(5) 0.5869(2) 0.0491(10) Uani 1 d . .
C11 C 0.1847(2) 0.1602(5) 0.4091(2) 0.0398(10) Uani 1 d . .
H11 H 0.1483(21) 0.1819(47) 0.4078(22) 0.048 Uiso 1 d . .
C12 C 0.1695(2) 0.2996(5) 0.3018(2) 0.0411(10) Uani 1 d . .
H12A H 0.1373(22) 0.2384(46) 0.2686(23) 0.049 Uiso 1 d . .
H12B H 0.1458(20) 0.3799(43) 0.3197(21) 0.049 Uiso 1 d . .
C13 C 0.2140(2) 0.3765(5) 0.2614(2) 0.0387(9) Uani 1 d . .
O1W O 0.1046(2) -0.1354(5) 0.2721(2) 0.1013(13) Uani 1 d . .
O2W O 0.5000 -0.4191(9) 0.2500 0.136(2) Uiso 1 d S .
O3W O 0.5168(16) -0.2231(34) 0.3619(18) 0.139(10) Uiso 0.25 d P .
O4W O 0.5000 0.0960(15) 0.2500 0.104(4) Uiso 0.50 d SP .
O5W O 0.5229(8) -0.2875(19) 0.3995(9) 0.078(4) Uiso 0.25 d P .
O6W O 0.4532(10) 0.0869(24) 0.2472(10) 0.112(6) Uiso 0.25 d P .
O7W O 0.5066(12) -0.1598(26) 0.3231(12) 0.095(8) Uiso 0.25 d P .
O8W O 0.5278(10) -0.1539(24) 0.3490(12) 0.071(5) Uiso 0.25 d P .
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'
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
_geom_angle_publ_flag
O4 Zn1 O2 102.64(12) 4_545 5_656 ?
O4 Zn1 N2 122.25(13) 4_545 . ?
O2 Zn1 N2 133.22(12) 5_656 . ?
O4 Zn1 O1 106.41(12) 4_545 . ?
O2 Zn1 O1 91.10(12) 5_656 . ?
N2 Zn1 O1 88.46(11) . . ?
O4 Zn1 O5 91.97(11) 4_545 . ?
O2 Zn1 O5 89.12(11) 5_656 . ?
N2 Zn1 O5 77.72(11) . . ?
O1 Zn1 O5 161.09(10) . . ?
C8 N1 C9 123.0(4) . . ?
C8 N1 H1 123.6(31) . . ?
C9 N1 H1 113.2(31) . . ?
C11 N2 C12 117.7(3) . . ?
C11 N2 Zn1 126.7(3) . . ?
C12 N2 Zn1 115.5(2) . . ?
C1 O1 Zn1 130.2(2) . . ?
C10 O2 Zn1 122.8(3) . 5_656 ?
C13 O4 Zn1 143.5(3) . 4 ?
C13 O5 Zn1 114.3(2) . . ?
O1 C1 C6 123.5(3) . . ?
O1 C1 C2 119.4(3) . . ?
C6 C1 C2 117.1(3) . . ?
C3 C2 C8 117.7(4) . . ?
C3 C2 C1 120.7(4) . . ?
C8 C2 C1 121.5(4) . . ?
C4 C3 C2 122.0(4) . . ?
C4 C3 H3 119.3(28) . . ?
C2 C3 H3 118.5(28) . . ?
C5 C4 C3 116.8(3) . . ?
C5 C4 C7 121.8(4) . . ?
C3 C4 C7 121.4(4) . . ?
C4 C5 C6 124.3(4) . . ?
C4 C5 H5 116.9(34) . . ?
C6 C5 H5 118.5(34) . . ?
C5 C6 C1 119.0(3) . . ?
C5 C6 C11 117.4(3) . . ?
C1 C6 C11 123.5(3) . . ?
C4 C7 H7A 109.7(28) . . ?
C4 C7 H7B 106.7(27) . . ?
H7A C7 H7B 123.4(42) . . ?
C4 C7 H7C 107.9(26) . . ?
H7A C7 H7C 106.5(38) . . ?
H7B C7 H7C 101.6(37) . . ?
N1 C8 C2 126.0(4) . . ?
N1 C8 H8 115.0(22) . . ?
C2 C8 H8 118.6(22) . . ?
N1 C9 C10 114.1(4) . . ?
N1 C9 H9A 109.9(24) . . ?
C10 C9 H9A 112.7(24) . . ?
N1 C9 H9B 109.8(26) . . ?
C10 C9 H9B 106.3(25) . . ?
H9A C9 H9B 103.4(35) . . ?
O3 C10 O2 126.5(4) . . ?
O3 C10 C9 120.3(4) . . ?
O2 C10 C9 113.2(4) . . ?
N2 C11 C6 127.4(4) . . ?
N2 C11 H11 122.6(33) . . ?
C6 C11 H11 109.5(32) . . ?
N2 C12 C13 111.5(3) . . ?
N2 C12 H12A 108.0(25) . . ?
C13 C12 H12A 106.6(25) . . ?
N2 C12 H12B 112.2(23) . . ?
C13 C12 H12B 109.1(23) . . ?
H12A C12 H12B 109.2(35) . . ?
O5 C13 O4 127.2(4) . . ?
O5 C13 C12 118.7(4) . . ?
O4 C13 C12 114.0(3) . . ?
O8W O3W O5W 146.1(62) . . ?
O8W O3W O7W 38.0(26) . . ?
O5W O3W O7W 175.1(52) . . ?
O6W O4W O6W 170.5(35) 2_655 . ?
O3W O5W O8W 14.9(27) . . ?
O3W O5W O7W 2.5(26) . . ?
O8W O5W O7W 17.0(10) . . ?
O8W O7W O3W 51.5(31) . . ?
O8W O7W O5W 53.5(38) . . ?
O3W O7W O5W 2.5(26) . . ?
O7W O8W O3W 90.5(42) . . ?
O7W O8W O5W 109.5(44) . . ?
O3W O8W O5W 19.0(36) . . ?
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
Zn1 O4 1.960(3) 4_545 ?
Zn1 O2 1.976(3) 5_656 ?
Zn1 N2 2.036(3) . ?
Zn1 O1 2.040(3) . ?
Zn1 O5 2.219(3) . ?
N1 C8 1.284(5) . ?
N1 C9 1.478(5) . ?
N1 H1 0.84(4) . ?
N2 C11 1.282(5) . ?
N2 C12 1.451(5) . ?
O1 C1 1.290(4) . ?
O2 C10 1.258(5) . ?
O2 Zn1 1.976(3) 5_656 ?
O3 C10 1.240(5) . ?
O4 C13 1.257(4) . ?
O4 Zn1 1.960(3) 4 ?
O5 C13 1.239(4) . ?
C1 C6 1.419(5) . ?
C1 C2 1.434(5) . ?
C2 C3 1.405(5) . ?
C2 C8 1.424(6) . ?
C3 C4 1.387(5) . ?
C3 H3 0.86(4) . ?
C4 C5 1.382(6) . ?
C4 C7 1.506(5) . ?
C5 C6 1.403(5) . ?
C5 H5 0.75(4) . ?
C6 C11 1.437(6) . ?
C7 H7A 0.89(4) . ?
C7 H7B 0.90(4) . ?
C7 H7C 0.95(5) . ?
C8 H8 1.06(4) . ?
C9 C10 1.516(6) . ?
C9 H9A 1.10(5) . ?
C9 H9B 1.05(5) . ?
C11 H11 0.75(4) . ?
C12 C13 1.518(5) . ?
C12 H12A 0.92(4) . ?
C12 H12B 0.96(4) . ?
O3W O8W 0.70(3) . ?
O3W O5W 0.89(3) . ?
O3W O7W 0.90(3) . ?
O4W O6W 0.94(2) 2_655 ?
O4W O6W 0.94(2) . ?
O5W O8W 1.53(3) . ?
O5W O7W 1.79(3) . ?
O7W O8W 0.55(3) . ?
