#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/91/4319159.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_4319159
_publ_author_name                'Andrea Erxleben'
_publ_contact_author_address
; Universitaet Dortmund
  Fachbereich Chemie, ACIII
  Otto-Hahn-Str. 6
  D-44221 Dortmund
  Germany
;
_publ_contact_author_email       AERX@platon.chemie.uni-dortmund.de
_publ_contact_author_fax         +49(0)231-7553797
_publ_contact_author_name        'Dr. Andrea Erxleben'
_publ_contact_author_phone       +49(0)231-7553845
_publ_section_title
;
 Mono- and Dinuclear Zinc Complexes Derived from Unsymmetric Binucleating
 Ligands: Synthesis, Characterization, and Formation of Tetranuclear
 Arrays
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              208
_journal_page_last               213
_journal_paper_doi               10.1021/ic000600z
_journal_volume                  40
_journal_year                    2001
_chemical_formula_structural     '[Zn4(C14H10N2O3)4]*4.5H2O'
_chemical_formula_sum            'C56 H49 N8 O16.5 Zn4'
_chemical_formula_weight         1359.51
_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   mixed
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 115.720(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.669(2)
_cell_length_b                   28.704(5)
_cell_length_c                   15.024(3)
_cell_measurement_reflns_used    4342
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      4.55
_cell_volume                     5310.7(17)
_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
'Siemens SHELXTL Ver. 5.01, (Sheldrick, 1993)'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1035
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4342
_diffrn_reflns_theta_max         24.74
_diffrn_reflns_theta_min         4.55
_exptl_absorpt_coefficient_mu    1.868
_exptl_absorpt_correction_T_max  0.7698
_exptl_absorpt_correction_T_min  0.6561
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       cube
_exptl_crystal_F_000             2772
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.581
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.886
_refine_ls_goodness_of_fit_obs   1.101
_refine_ls_hydrogen_treatment    'isotropically(difmap)/fixed U-values(geom)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     456
_refine_ls_number_reflns         4342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_restrained_S_obs      1.101
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_obs          0.0407
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0439P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0951
_refine_ls_wR_factor_obs         0.0770
_reflns_number_observed          2096
_reflns_number_total             4342
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000600z_1.cif
_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^)+(0.0439P)^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^)+(0.0439P)^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 

The following automatic conversions were performed:
data name '_publ_contact_author_mail' replaced with
'_publ_contact_author_email' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'difmap/geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        5310.7(16)
_cod_original_formula_sum        'C56 H49 N8 O16.50 Zn4'
_cod_database_code               4319159
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 0.14015(5) 0.15307(2) 0.27203(5) 0.0579(2) Uani 1 d . .
Zn2 Zn 0.03549(5) 0.08289(2) 0.37940(5) 0.0590(2) Uani 1 d . .
C1 C 0.0612(4) 0.1856(2) 0.4273(4) 0.0533(13) Uani 1 d . .
C2 C 0.0989(4) 0.2305(2) 0.4186(4) 0.0527(13) Uani 1 d . .
C3 C 0.1079(5) 0.2649(2) 0.4882(5) 0.067(2) Uani 1 d . .
C4 C 0.0829(5) 0.2569(3) 0.5645(6) 0.072(2) Uani 1 d . .
C5 C 0.0493(5) 0.2135(3) 0.5740(5) 0.068(2) Uani 1 d . .
C6 C 0.0373(4) 0.1770(2) 0.5088(4) 0.0558(14) Uani 1 d . .
C7 C -0.0039(5) 0.1314(2) 0.5303(5) 0.070(2) Uani 1 d . .
C8 C 0.1323(4) 0.2461(2) 0.3434(5) 0.063(2) Uani 1 d . .
C9 C 0.1793(6) 0.2470(2) 0.2106(6) 0.064(2) Uani 1 d . .
C10 C 0.2328(4) 0.2144(2) 0.1704(4) 0.0623(15) Uani 1 d . .
C11 C 0.2988(6) 0.2290(3) 0.1283(6) 0.096(3) Uani 1 d . .
C12 C 0.3445(7) 0.1975(4) 0.0895(6) 0.111(3) Uani 1 d . .
C13 C 0.3274(6) 0.1508(4) 0.0967(5) 0.102(2) Uani 1 d . .
C14 C 0.2628(5) 0.1376(3) 0.1408(5) 0.078(2) Uani 1 d . .
C1' C 0.1927(4) 0.0514(2) 0.2826(4) 0.0529(14) Uani 1 d . .
C2' C 0.1650(5) 0.0050(2) 0.2461(4) 0.0612(15) Uani 1 d . .
C3' C 0.2477(7) -0.0291(3) 0.2839(6) 0.082(2) Uani 1 d . .
C4' C 0.3494(8) -0.0198(3) 0.3501(6) 0.089(2) Uani 1 d . .
C5' C 0.3765(6) 0.0259(3) 0.3783(5) 0.076(2) Uani 1 d . .
C6' C 0.3018(4) 0.0623(2) 0.3468(4) 0.0586(14) Uani 1 d . .
C7' C 0.3451(5) 0.1096(2) 0.3896(4) 0.068(2) Uani 1 d . .
C8' C 0.0618(5) -0.0115(2) 0.1753(5) 0.066(2) Uani 1 d . .
C9' C -0.1172(6) -0.0136(2) 0.0559(5) 0.076(2) Uani 1 d . .
C10' C -0.2063(5) 0.0186(3) -0.0078(5) 0.073(2) Uani 1 d . .
C11' C -0.3049(7) 0.0009(4) -0.0752(7) 0.101(3) Uani 1 d . .
C12' C -0.3832(8) 0.0301(5) -0.1311(7) 0.128(3) Uani 1 d . .
H12' H -0.4504(8) 0.0186(5) -0.1754(7) 0.080 Uiso 1 calc R .
C13' C -0.3649(6) 0.0767(4) -0.1235(6) 0.112(3) Uani 1 d . .
H13' H -0.4187(6) 0.0971(4) -0.1636(6) 0.080 Uiso 1 calc R .
C14' C -0.2653(7) 0.0936(3) -0.0554(6) 0.088(2) Uani 1 d . .
N1 N 0.1396(3) 0.22293(15) 0.2755(3) 0.0545(11) Uani 1 d . .
N2 N 0.2158(3) 0.1685(2) 0.1772(3) 0.0639(12) Uani 1 d . .
N1' N -0.0222(4) 0.0124(2) 0.1262(4) 0.0629(12) Uani 1 d . .
N2' N -0.1862(4) 0.0648(2) 0.0036(4) 0.0694(13) Uani 1 d . .
O1 O 0.0469(2) 0.15305(11) 0.3579(2) 0.0503(8) Uani 1 d . .
O2 O -0.0337(3) 0.09879(13) 0.4667(3) 0.0673(10) Uani 1 d . .
O3 O -0.0073(4) 0.12698(15) 0.6108(3) 0.0986(14) Uani 1 d . .
O1' O 0.1124(2) 0.08368(10) 0.2560(2) 0.0505(9) Uani 1 d . .
O2' O 0.2820(3) 0.14156(13) 0.3859(3) 0.0644(10) Uani 1 d . .
O3' O 0.4458(4) 0.1140(2) 0.4281(4) 0.113(2) Uani 1 d . .
O1W O -0.1608(3) 0.1446(2) 0.6897(3) 0.1085(15) Uani 1 d . .
O2W O 0.5941(4) 0.1445(2) 0.6241(4) 0.127(2) Uani 1 d . .
O3W O 0.5000 0.0731(4) 0.2500 0.090(4) Uani 0.50 d SP .
H3 H 0.1279(32) 0.2908(16) 0.4794(32) 0.038(15) Uiso 1 d . .
H4 H 0.0878(38) 0.2792(19) 0.6069(39) 0.072(19) Uiso 1 d . .
H5 H 0.0272(29) 0.2055(13) 0.6203(30) 0.029(12) Uiso 1 d . .
H8 H 0.1480(29) 0.2765(15) 0.3422(28) 0.033(12) Uiso 1 d . .
H9A H 0.1233(38) 0.2567(17) 0.1633(37) 0.058(19) Uiso 1 d . .
H9B H 0.2280(36) 0.2717(16) 0.2473(34) 0.058(16) Uiso 1 d . .
H11 H 0.3100(38) 0.2569(17) 0.1269(37) 0.056(18) Uiso 1 d . .
H12 H 0.3971(50) 0.2090(23) 0.0660(47) 0.124(25) Uiso 1 d . .
H13 H 0.3654(44) 0.1260(20) 0.0789(43) 0.095(22) Uiso 1 d . .
H14 H 0.2459(37) 0.1030(19) 0.1462(35) 0.073(17) Uiso 1 d . .
H3' H 0.2258(38) -0.0549(17) 0.2608(37) 0.054(19) Uiso 1 d . .
H4' H 0.3971(45) -0.0395(20) 0.3657(41) 0.080(22) Uiso 1 d . .
H5' H 0.4471(35) 0.0339(15) 0.4245(33) 0.044(15) Uiso 1 d . .
H8' H 0.0583(33) -0.0458(18) 0.1634(34) 0.065(16) Uiso 1 d . .
H9'A H -0.1711(49) -0.0350(23) 0.0845(45) 0.131(23) Uiso 1 d . .
H9'B H -0.0992(38) -0.0297(18) 0.0162(37) 0.063(18) Uiso 1 d . .
H11' H -0.3119(47) -0.0322(23) -0.0735(46) 0.096(27) Uiso 1 d . .
H14' H -0.2533(37) 0.1276(19) -0.0533(36) 0.062(18) Uiso 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'
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
O2' Zn1 N1 99.1(2) . . ?
O2' Zn1 O1' 90.08(14) . . ?
N1 Zn1 O1' 170.03(14) . . ?
O2' Zn1 N2 92.01(15) . . ?
N1 Zn1 N2 79.5(2) . . ?
O1' Zn1 N2 104.2(2) . . ?
O2' Zn1 O1 95.38(14) . . ?
N1 Zn1 O1 88.5(2) . . ?
O1' Zn1 O1 86.68(12) . . ?
N2 Zn1 O1 166.8(2) . . ?
O2' Zn1 O1 168.48(12) . 2 ?
N1 Zn1 O1 90.36(14) . 2 ?
O1' Zn1 O1 80.10(11) . 2 ?
N2 Zn1 O1 96.21(13) . 2 ?
O1 Zn1 O1 78.18(12) . 2 ?
O2 Zn2 N1' 101.4(2) . 2 ?
O2 Zn2 O1 88.21(14) . . ?
N1' Zn2 O1 168.9(2) 2 . ?
O2 Zn2 N2' 94.6(2) . 2 ?
N1' Zn2 N2' 80.0(2) 2 2 ?
O1 Zn2 N2' 105.0(2) . 2 ?
O2 Zn2 O1' 95.81(14) . 2 ?
N1' Zn2 O1' 86.6(2) 2 2 ?
O1 Zn2 O1' 86.88(12) . 2 ?
N2' Zn2 O1' 164.5(2) 2 2 ?
O2 Zn2 O1' 165.55(13) . . ?
N1' Zn2 O1' 92.15(14) 2 . ?
O1 Zn2 O1' 77.85(11) . . ?
N2' Zn2 O1' 92.71(14) 2 . ?
O1' Zn2 O1' 79.84(11) 2 . ?
O1 C1 C2 119.8(5) . . ?
O1 C1 C6 122.4(5) . . ?
C2 C1 C6 117.8(5) . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 C8 113.9(5) . . ?
C1 C2 C8 126.8(5) . . ?
C4 C3 C2 122.6(6) . . ?
C3 C4 C5 117.8(7) . . ?
C4 C5 C6 123.9(6) . . ?
C5 C6 C1 118.4(5) . . ?
C5 C6 C7 116.1(5) . . ?
C1 C6 C7 125.5(5) . . ?
O3 C7 O2 121.5(6) . . ?
O3 C7 C6 118.3(6) . . ?
O2 C7 C6 120.2(5) . . ?
N1 C8 C2 128.8(6) . . ?
C10 C9 N1 111.3(5) . . ?
N2 C10 C11 120.2(6) . . ?
N2 C10 C9 117.3(5) . . ?
C11 C10 C9 122.5(7) . . ?
C12 C11 C10 120.5(8) . . ?
C11 C12 C13 119.2(8) . . ?
C14 C13 C12 118.4(8) . . ?
N2 C14 C13 122.6(7) . . ?
O1' C1' C6' 121.9(5) . . ?
O1' C1' C2' 118.5(5) . . ?
C6' C1' C2' 119.6(5) . . ?
C3' C2' C1' 117.3(6) . . ?
C3' C2' C8' 115.3(6) . . ?
C1' C2' C8' 127.4(5) . . ?
C4' C3' C2' 123.4(8) . . ?
C3' C4' C5' 118.2(7) . . ?
C4' C5' C6' 123.3(7) . . ?
C5' C6' C1' 117.8(6) . . ?
C5' C6' C7' 115.8(6) . . ?
C1' C6' C7' 126.3(5) . . ?
O2' C7' O3' 123.4(6) . . ?
O2' C7' C6' 120.5(5) . . ?
O3' C7' C6' 116.0(6) . . ?
N1' C8' C2' 127.4(6) . . ?
N1' C9' C10' 111.4(6) . . ?
N2' C10' C11' 122.2(8) . . ?
N2' C10' C9' 117.4(6) . . ?
C11' C10' C9' 120.4(8) . . ?
C12' C11' C10' 119.4(10) . . ?
C11' C12' C13' 120.0(9) . . ?
C12' C13' C14' 119.6(9) . . ?
N2' C14' C13' 121.5(8) . . ?
C8 N1 C9 117.9(5) . . ?
C8 N1 Zn1 123.6(4) . . ?
C9 N1 Zn1 116.4(4) . . ?
C14 N2 C10 119.0(5) . . ?
C14 N2 Zn1 126.1(4) . . ?
C10 N2 Zn1 113.7(4) . . ?
C8' N1' C9' 115.9(5) . . ?
C8' N1' Zn2 127.5(4) . 2 ?
C9' N1' Zn2 116.2(4) . 2 ?
C14' N2' C10' 117.3(6) . . ?
C14' N2' Zn2 127.8(5) . 2 ?
C10' N2' Zn2 114.7(4) . 2 ?
C1 O1 Zn2 123.5(3) . . ?
C1 O1 Zn1 122.2(3) . . ?
Zn2 O1 Zn1 101.39(13) . . ?
C1 O1 Zn1 111.5(3) . 2 ?
Zn2 O1 Zn1 90.07(11) . 2 ?
Zn1 O1 Zn1 101.82(12) . 2 ?
C7 O2 Zn2 125.5(4) . . ?
C1' O1' Zn1 123.4(3) . . ?
C1' O1' Zn2 125.3(3) . 2 ?
Zn1 O1' Zn2 99.97(13) . 2 ?
C1' O1' Zn2 108.8(3) . . ?
Zn1 O1' Zn2 92.20(11) . . ?
Zn2 O1' Zn2 100.15(11) 2 . ?
C7' O2' Zn1 124.2(4) . . ?
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 O2' 1.978(4) . ?
Zn1 N1 2.006(4) . ?
Zn1 O1' 2.022(3) . ?
Zn1 N2 2.138(4) . ?
Zn1 O1 2.172(3) . ?
Zn1 O1 2.453(3) 2 ?
Zn2 O2 1.975(4) . ?
Zn2 N1' 2.029(5) 2 ?
Zn2 O1 2.056(3) . ?
Zn2 N2' 2.112(5) 2 ?
Zn2 O1' 2.158(3) 2 ?
Zn2 O1' 2.496(3) . ?
C1 O1 1.349(6) . ?
C1 C2 1.415(6) . ?
C1 C6 1.420(7) . ?
C2 C3 1.405(8) . ?
C2 C8 1.461(7) . ?
C3 C4 1.351(8) . ?
C4 C5 1.358(8) . ?
C5 C6 1.393(7) . ?
C6 C7 1.514(7) . ?
C7 O3 1.236(6) . ?
C7 O2 1.273(7) . ?
C8 N1 1.257(7) . ?
C9 C10 1.470(8) . ?
C9 N1 1.479(7) . ?
C10 N2 1.348(6) . ?
C10 C11 1.374(8) . ?
C11 C12 1.366(10) . ?
C12 C13 1.374(10) . ?
C13 C14 1.367(8) . ?
C14 N2 1.343(7) . ?
C1' O1' 1.357(5) . ?
C1' C6' 1.415(7) . ?
C1' C2' 1.429(7) . ?
C2' C3' 1.415(8) . ?
C2' C8' 1.430(7) . ?
C3' C4' 1.339(10) . ?
C4' C5' 1.380(9) . ?
C5' C6' 1.392(8) . ?
C6' C7' 1.508(7) . ?
C7' O2' 1.245(6) . ?
C7' O3' 1.246(6) . ?
C8' N1' 1.265(6) . ?
C9' N1' 1.473(7) . ?
C9' C10' 1.496(8) . ?
C10' N2' 1.351(7) . ?
C10' C11' 1.384(9) . ?
C11' C12' 1.333(11) . ?
C12' C13' 1.355(10) . ?
C13' C14' 1.387(9) . ?
C14' N2' 1.344(8) . ?
N1' Zn2 2.029(5) 2 ?
N2' Zn2 2.112(5) 2 ?
O1 Zn1 2.453(3) 2 ?
O1' Zn2 2.158(3) 2 ?
