#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:31:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179794 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/90/7009004.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_7009004
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_structural     '[Zn2(C17H27N4O)(CH3CO2)2]ClO4'
_chemical_formula_sum            'C21 H33 Cl N4 O9 Zn2'
_chemical_formula_weight         651.70
_chemical_name_systematic        ?
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                99.370(10)
_cell_angle_beta                 94.00(3)
_cell_angle_gamma                104.04(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7170(10)
_cell_length_b                   11.2850(10)
_cell_length_c                   15.0570(10)
_cell_measurement_reflns_used    4573
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      4.56
_cell_volume                     1408.5(3)
_computing_cell_refinement
'Denzo, Scalepack (Z. Otwinowski, W. Minor, 1997)'
_computing_data_collection       'KappaCCD (Nonius BV, The Netherlands)'
_computing_data_reduction
'Denzo, Scalepack (Z. Otwinowski, W. 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  0.045
_diffrn_reflns_av_sigmaI/netI    0.0738
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4573
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         4.56
_exptl_absorpt_coefficient_mu    1.850
_exptl_absorpt_correction_T_max  0.655
_exptl_absorpt_correction_T_min  0.607
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       cube
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.755
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_hydrogen_treatment    'U(iso) = 1.2 x U(C(bonded)) '
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         4562
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.176
_refine_ls_restrained_S_obs      1.160
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_obs          0.0480
_refine_ls_shift/esd_max         -0.154
_refine_ls_shift/esd_mean        0.016
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0805P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1581
_refine_ls_wR_factor_obs         0.1276
_reflns_number_observed          3164
_reflns_number_total             4573
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            a907839h.txt
_cod_data_source_block           1a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0805P)^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^)+(0.0805P)^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        1408.5(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7009004
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.12606(4) 0.39327(3) 0.17658(2) 0.04780(11) Uani 1 d . .
Zn2 Zn 0.10648(4) 0.63963(3) 0.31431(2) 0.04678(10) Uani 1 d . .
Cl1 Cl 0.3070(2) 0.90299(14) 0.74354(10) 0.1052(4) Uani 1 d D .
C1 C 0.2279(3) 0.4299(3) 0.3826(2) 0.0476(9) Uani 1 d . .
C2 C 0.2928(3) 0.3255(3) 0.3676(2) 0.0487(9) Uani 1 d . .
C3 C 0.3619(4) 0.2876(3) 0.4421(2) 0.0577(10) Uani 1 d . .
H3 H 0.4058(4) 0.2201(3) 0.4308(2) 0.069 Uiso 1 calc R .
C4 C 0.3677(4) 0.3449(4) 0.5299(2) 0.0597(10) Uani 1 d . .
C5 C 0.3058(4) 0.4452(4) 0.5438(2) 0.0595(10) Uani 1 d . .
H5 H 0.3101(4) 0.4861(4) 0.6032(2) 0.071 Uiso 1 calc R .
C6 C 0.2358(4) 0.4911(3) 0.4744(2) 0.0520(9) Uani 1 d . .
C7 C 0.4443(4) 0.3003(4) 0.6084(3) 0.0871(13) Uani 1 d . .
H7A H 0.4812(4) 0.2291(4) 0.5850(3) 0.105 Uiso 1 calc R .
H7B H 0.3671(4) 0.2780(4) 0.6493(3) 0.105 Uiso 1 calc R .
H7C H 0.5325(4) 0.3657(4) 0.6399(3) 0.105 Uiso 1 calc R .
C8 C 0.2895(4) 0.2486(3) 0.2810(3) 0.0583(10) Uani 1 d . .
H8 H 0.3402(4) 0.1849(3) 0.2807(3) 0.070 Uiso 1 calc R .
C9 C 0.2250(5) 0.1616(4) 0.1260(3) 0.0834(13) Uani 1 d . .
H9A H 0.1358(5) 0.0900(4) 0.1237(3) 0.100 Uiso 1 calc R .
H9B H 0.3225(5) 0.1350(4) 0.1310(3) 0.100 Uiso 1 calc R .
C10 C 0.2121(5) 0.2149(4) 0.0411(3) 0.0781(13) Uani 1 d . .
H10A H 0.3108(5) 0.2756(4) 0.0382(3) 0.094 Uiso 1 calc R .
H10B H 0.1949(5) 0.1491(4) -0.0116(3) 0.094 Uiso 1 calc R .
C11 C 0.0930(6) 0.3482(5) -0.0319(4) 0.107(2) Uiso 1 d . .
H11A H 0.1952(6) 0.4073(5) -0.0225(4) 0.129 Uiso 1 calc R .
H11B H 0.0107(6) 0.3914(5) -0.0307(4) 0.129 Uiso 1 calc R .
H11C H 0.0815(6) 0.2942(5) -0.0896(4) 0.129 Uiso 1 calc R .
C12 C -0.0738(5) 0.1859(5) 0.0246(3) 0.100(2) Uani 1 d . .
H12A H -0.1556(5) 0.2295(5) 0.0246(3) 0.119 Uiso 1 calc R .
H12B H -0.0845(5) 0.1376(5) 0.0718(3) 0.119 Uiso 1 calc R .
H12C H -0.0838(5) 0.1318(5) -0.0329(3) 0.119 Uiso 1 calc R .
C13 C 0.1814(4) 0.5996(3) 0.5020(2) 0.0563(10) Uani 1 d . .
H13 H 0.1840(4) 0.6255(3) 0.5641(2) 0.068 Uiso 1 calc R .
C14 C 0.0828(5) 0.7777(4) 0.4949(3) 0.0745(12) Uani 1 d . .
H14A H 0.0081(5) 0.7551(4) 0.5379(3) 0.089 Uiso 1 calc R .
H14B H 0.1761(5) 0.8385(4) 0.5278(3) 0.089 Uiso 1 calc R .
C15 C 0.0093(5) 0.8327(4) 0.4265(3) 0.0915(15) Uani 1 d . .
H15A H -0.1000(5) 0.7847(4) 0.4081(3) 0.110 Uiso 1 calc R .
H15B H 0.0079(5) 0.9168(4) 0.4528(3) 0.110 Uiso 1 calc R .
C16 C 0.2557(6) 0.9202(6) 0.3707(4) 0.120(2) Uiso 1 d . .
H16A H 0.3118(6) 0.9212(6) 0.3181(4) 0.144 Uiso 1 calc R .
H16B H 0.3132(6) 0.8929(6) 0.4166(4) 0.144 Uiso 1 calc R .
H16C H 0.2461(6) 1.0024(6) 0.3933(4) 0.144 Uiso 1 calc R .
C17 C 0.0096(6) 0.8740(6) 0.2729(4) 0.121(2) Uiso 1 d . .
H17A H -0.0943(6) 0.8177(6) 0.2571(4) 0.145 Uiso 1 calc R .
H17B H 0.0671(6) 0.8728(6) 0.2209(4) 0.145 Uiso 1 calc R .
H17C H -0.0007(6) 0.9566(6) 0.2933(4) 0.145 Uiso 1 calc R .
C18 C 0.3225(4) 0.6385(3) 0.1658(2) 0.0529(9) Uani 1 d . .
C19 C 0.4503(5) 0.7207(4) 0.1259(3) 0.0831(14) Uani 1 d . .
H19A H 0.4615(5) 0.8059(4) 0.1530(3) 0.100 Uiso 1 calc R .
H19B H 0.4223(5) 0.7094(4) 0.0617(3) 0.100 Uiso 1 calc R .
H19C H 0.5491(5) 0.6995(4) 0.1373(3) 0.100 Uiso 1 calc R .
C20 C -0.1707(4) 0.4787(3) 0.2014(2) 0.0538(9) Uani 1 d . .
C21 C -0.3478(4) 0.4356(4) 0.1750(3) 0.0824(14) Uani 1 d . .
H21A H -0.3997(4) 0.4860(4) 0.2137(3) 0.099 Uiso 1 calc R .
H21B H -0.3852(4) 0.3503(4) 0.1812(3) 0.099 Uiso 1 calc R .
H21C H -0.3716(4) 0.4428(4) 0.1132(3) 0.099 Uiso 1 calc R .
N1 N 0.2248(3) 0.2576(3) 0.2041(2) 0.0578(8) Uani 1 d . .
N2 N 0.0803(3) 0.2742(3) 0.0402(2) 0.0599(8) Uani 1 d . .
N3 N 0.1299(3) 0.6650(3) 0.4517(2) 0.0556(8) Uani 1 d . .
N4 N 0.0970(3) 0.8352(3) 0.3464(2) 0.0613(9) Uani 1 d . .
O1 O 0.1648(2) 0.4697(2) 0.31509(14) 0.0479(6) Uani 1 d . .
O2 O 0.2922(3) 0.5241(2) 0.1382(2) 0.0627(7) Uani 1 d . .
O3 O 0.2513(3) 0.6904(2) 0.2248(2) 0.0602(6) Uiso 1 d . .
O4 O -0.0863(3) 0.4220(2) 0.1571(2) 0.0603(7) Uani 1 d . .
O5 O -0.1199(2) 0.5700(2) 0.2657(2) 0.0581(7) Uani 1 d . .
O10 O 0.3273(9) 1.0038(6) 0.6923(5) 0.144(3) Uani 0.60 d PD .
O11 O 0.3846(13) 0.9260(11) 0.8233(7) 0.230(5) Uiso 0.60 d PD .
O12 O 0.1420(6) 0.8527(7) 0.7375(5) 0.135(3) Uani 0.60 d PD .
O13 O 0.3607(8) 0.8079(8) 0.6891(7) 0.224(4) Uani 0.60 d PD .
O20 O 0.2347(11) 0.9792(10) 0.7992(8) 0.163(5) Uani 0.40 d PD .
O21 O 0.2189(17) 0.7889(9) 0.7239(7) 0.168(6) Uani 0.40 d PD .
O22 O 0.4477(9) 0.9144(11) 0.8032(7) 0.183(4) Uani 0.40 d PD .
O23 O 0.3698(13) 0.9492(11) 0.6732(7) 0.152(6) Uani 0.40 d PD .
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
_geom_angle_publ_flag
O4 Zn1 O2 111.38(11) . . ?
O4 Zn1 N1 139.08(11) . . ?
O2 Zn1 N1 108.53(11) . . ?
O4 Zn1 O1 95.41(9) . . ?
O2 Zn1 O1 96.66(9) . . ?
N1 Zn1 O1 88.57(10) . . ?
O4 Zn1 N2 88.62(11) . . ?
O2 Zn1 N2 92.63(11) . . ?
N1 Zn1 N2 80.85(12) . . ?
O1 Zn1 N2 167.73(10) . . ?
O3 Zn2 O5 115.32(10) . . ?
O3 Zn2 N3 133.98(10) . . ?
O5 Zn2 N3 110.00(11) . . ?
O3 Zn2 O1 94.59(10) . . ?
O5 Zn2 O1 97.25(9) . . ?
N3 Zn2 O1 87.17(11) . . ?
O3 Zn2 N4 86.93(11) . . ?
O5 Zn2 N4 96.56(10) . . ?
N3 Zn2 N4 80.35(12) . . ?
O1 Zn2 N4 163.90(10) . . ?
O21 Cl1 O11 111.1(7) . . ?
O21 Cl1 O23 115.4(7) . . ?
O11 Cl1 O23 122.7(7) . . ?
O21 Cl1 O20 111.3(8) . . ?
O11 Cl1 O20 73.5(7) . . ?
O23 Cl1 O20 115.9(7) . . ?
O21 Cl1 O12 47.9(7) . . ?
O11 Cl1 O12 116.4(6) . . ?
O23 Cl1 O12 119.2(6) . . ?
O20 Cl1 O12 68.2(5) . . ?
O21 Cl1 O22 111.9(7) . . ?
O11 Cl1 O22 28.1(6) . . ?
O23 Cl1 O22 101.4(6) . . ?
O20 Cl1 O22 99.3(6) . . ?
O12 Cl1 O22 139.1(6) . . ?
O21 Cl1 O13 59.3(7) . . ?
O11 Cl1 O13 107.5(7) . . ?
O23 Cl1 O13 72.0(7) . . ?
O20 Cl1 O13 170.4(6) . . ?
O12 Cl1 O13 103.5(4) . . ?
O22 Cl1 O13 83.9(5) . . ?
O21 Cl1 O10 131.1(6) . . ?
O11 Cl1 O10 117.7(6) . . ?
O23 Cl1 O10 33.5(6) . . ?
O20 Cl1 O10 82.5(6) . . ?
O12 Cl1 O10 105.3(5) . . ?
O22 Cl1 O10 111.5(6) . . ?
O13 Cl1 O10 104.9(5) . . ?
O1 C1 C2 121.6(3) . . ?
O1 C1 C6 121.3(3) . . ?
C2 C1 C6 117.1(3) . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 C8 115.1(3) . . ?
C1 C2 C8 125.4(3) . . ?
C4 C3 C2 123.5(3) . . ?
C5 C4 C3 116.7(3) . . ?
C5 C4 C7 121.8(3) . . ?
C3 C4 C7 121.5(4) . . ?
C4 C5 C6 124.3(3) . . ?
C5 C6 C13 116.2(3) . . ?
C5 C6 C1 118.9(3) . . ?
C13 C6 C1 124.9(3) . . ?
N1 C8 C2 127.5(3) . . ?
N1 C9 C10 108.5(3) . . ?
N2 C10 C9 110.5(3) . . ?
N3 C13 C6 127.6(3) . . ?
C15 C14 N3 111.1(3) . . ?
N4 C15 C14 111.3(4) . . ?
O2 C18 O3 124.4(3) . . ?
O2 C18 C19 118.1(3) . . ?
O3 C18 C19 117.5(3) . . ?
O4 C20 O5 125.4(3) . . ?
O4 C20 C21 117.2(3) . . ?
O5 C20 C21 117.4(3) . . ?
C8 N1 C9 117.7(3) . . ?
C8 N1 Zn1 127.2(2) . . ?
C9 N1 Zn1 115.1(2) . . ?
C12 N2 C10 112.9(3) . . ?
C12 N2 C11 108.5(4) . . ?
C10 N2 C11 108.9(3) . . ?
C12 N2 Zn1 112.8(3) . . ?
C10 N2 Zn1 101.8(2) . . ?
C11 N2 Zn1 111.8(3) . . ?
C13 N3 C14 119.0(3) . . ?
C13 N3 Zn2 128.1(2) . . ?
C14 N3 Zn2 113.0(2) . . ?
C16 N4 C15 110.1(4) . . ?
C16 N4 C17 109.8(4) . . ?
C15 N4 C17 110.8(4) . . ?
C16 N4 Zn2 112.0(3) . . ?
C15 N4 Zn2 100.6(2) . . ?
C17 N4 Zn2 113.3(3) . . ?
C1 O1 Zn1 129.4(2) . . ?
C1 O1 Zn2 129.2(2) . . ?
Zn1 O1 Zn2 100.92(9) . . ?
C18 O2 Zn1 126.9(2) . . ?
C18 O3 Zn2 137.3(2) . . ?
C20 O4 Zn1 136.8(2) . . ?
C20 O5 Zn2 124.6(2) . . ?
O23 O10 Cl1 65.7(9) . . ?
O22 O11 Cl1 87.9(13) . . ?
O22 O11 O20 137.6(17) . . ?
Cl1 O11 O20 56.2(6) . . ?
O21 O12 Cl1 61.3(6) . . ?
O21 O12 O20 111.9(8) . . ?
Cl1 O12 O20 55.6(4) . . ?
O21 O13 Cl1 55.6(5) . . ?
O21 O13 O23 96.5(7) . . ?
Cl1 O13 O23 51.6(5) . . ?
Cl1 O20 O12 56.2(4) . . ?
Cl1 O20 O11 50.3(5) . . ?
O12 O20 O11 92.3(7) . . ?
O12 O21 Cl1 70.7(7) . . ?
O12 O21 O13 129.4(11) . . ?
Cl1 O21 O13 65.1(7) . . ?
O11 O22 Cl1 64.0(11) . . ?
O10 O23 Cl1 80.8(10) . . ?
O10 O23 O13 135.8(13) . . ?
Cl1 O23 O13 56.5(5) . . ?
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 1.966(2) . ?
Zn1 O2 1.991(2) . ?
Zn1 N1 2.013(3) . ?
Zn1 O1 2.093(2) . ?
Zn1 N2 2.216(3) . ?
Zn2 O3 1.969(2) . ?
Zn2 O5 1.976(2) . ?
Zn2 N3 2.031(3) . ?
Zn2 O1 2.101(2) . ?
Zn2 N4 2.204(3) . ?
Cl1 O21 1.304(10) . ?
Cl1 O11 1.291(10) . ?
Cl1 O23 1.347(10) . ?
Cl1 O20 1.394(10) . ?
Cl1 O12 1.403(5) . ?
Cl1 O22 1.435(7) . ?
Cl1 O13 1.433(7) . ?
Cl1 O10 1.459(7) . ?
C1 O1 1.315(4) . ?
C1 C2 1.419(5) . ?
C1 C6 1.430(4) . ?
C2 C3 1.411(5) . ?
C2 C8 1.439(5) . ?
C3 C4 1.366(5) . ?
C4 C5 1.361(6) . ?
C4 C7 1.530(5) . ?
C5 C6 1.405(5) . ?
C6 C13 1.429(5) . ?
C8 N1 1.282(5) . ?
C9 N1 1.464(5) . ?
C9 C10 1.507(6) . ?
C10 N2 1.463(5) . ?
C11 N2 1.467(6) . ?
C12 N2 1.443(5) . ?
C13 N3 1.271(5) . ?
C14 C15 1.473(7) . ?
C14 N3 1.493(5) . ?
C15 N4 1.472(5) . ?
C16 N4 1.462(6) . ?
C17 N4 1.483(7) . ?
C18 O2 1.247(4) . ?
C18 O3 1.266(4) . ?
C18 C19 1.495(5) . ?
C20 O4 1.246(4) . ?
C20 O5 1.260(4) . ?
C20 C21 1.506(4) . ?
O10 O23 0.817(14) . ?
O11 O22 0.676(15) . ?
O11 O20 1.61(2) . ?
O12 O21 1.103(15) . ?
O12 O20 1.568(12) . ?
O13 O21 1.36(2) . ?
O13 O23 1.635(15) . ?
