#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/91/4319161.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_4319161
_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     '[Zn2(C12H15N2O3)2(CH3CO2)2]*6H2O'
_chemical_formula_sum            'C28 H48 N4 O16 Zn2'
_chemical_formula_weight         827.44
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                92.270(10)
_cell_angle_beta                 98.560(10)
_cell_angle_gamma                97.790(10)
_cell_formula_units_Z            1
_cell_length_a                   7.002(2)
_cell_length_b                   9.2000(10)
_cell_length_c                   14.3090(10)
_cell_measurement_reflns_used    2875
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      3.46
_cell_volume                     901.4(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
'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  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0633
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2875
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         3.46
_exptl_absorpt_coefficient_mu    1.406
_exptl_absorpt_correction_T_max  0.8168
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   Scalepack
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.524
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.960
_refine_ls_goodness_of_fit_obs   1.078
_refine_ls_hydrogen_treatment
isotropically(difmap)/Uiso=1.5*U(C(bonded))(geom)
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         2873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_restrained_S_obs      1.078
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_obs          0.0366
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0492P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0881
_refine_ls_wR_factor_obs         0.0833
_reflns_number_observed          2187
_reflns_number_total             2875
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000600z_3.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0492P)^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^)+(0.0492P)^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_database_code               4319161
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 0.05480(5) 0.58659(4) 0.40795(3) 0.03356(15) Uani 1 d . .
C1 C -0.2968(4) 0.3500(3) 0.3937(2) 0.0342(8) Uani 1 d . .
C2 C -0.4634(4) 0.2958(4) 0.4351(2) 0.0377(8) Uani 1 d . .
C3 C -0.6275(5) 0.2166(4) 0.3772(3) 0.0515(10) Uani 1 d . .
C4 C -0.6312(5) 0.1864(5) 0.2829(3) 0.0575(11) Uani 1 d . .
C5 C -0.4693(5) 0.2402(4) 0.2425(3) 0.0461(9) Uani 1 d . .
C6 C -0.3024(4) 0.3220(3) 0.2961(2) 0.0347(8) Uani 1 d . .
C7 C -0.4826(5) 0.3238(4) 0.5330(3) 0.0410(9) Uani 1 d . .
C8 C -0.4124(6) 0.3948(5) 0.6955(3) 0.0425(9) Uani 1 d . .
C9 C -0.3586(6) 0.2754(5) 0.7593(3) 0.0472(9) Uani 1 d . .
C10 C -0.5725(7) 0.3454(7) 0.8736(4) 0.0713(14) Uani 1 d . .
C11 C -0.3098(10) 0.1950(8) 0.9207(4) 0.088(2) Uani 1 d . .
C12 C -0.1398(5) 0.3770(4) 0.2437(2) 0.0394(8) Uani 1 d . .
C13 C -0.0832(4) 0.8608(4) 0.3587(3) 0.0424(9) Uani 1 d . .
C14 C -0.1758(6) 0.9928(4) 0.3849(3) 0.0626(11) Uani 1 d . .
H14A H -0.2052(6) 0.9863(4) 0.4481(3) 0.094 Uiso 1 calc R .
H14B H -0.2940(6) 0.9950(4) 0.3416(3) 0.094 Uiso 1 calc R .
H14C H -0.0870(6) 1.0809(4) 0.3815(3) 0.094 Uiso 1 calc R .
N1 N -0.3484(4) 0.3706(3) 0.6030(2) 0.0377(7) Uani 1 d . .
N2 N -0.3719(4) 0.3157(4) 0.8608(2) 0.0507(8) Uani 1 d . .
O1 O -0.1464(3) 0.4281(2) 0.44831(15) 0.0366(5) Uani 1 d . .
O2 O -0.0150(3) 0.4861(3) 0.2777(2) 0.0496(6) Uani 1 d . .
O3 O -0.1353(4) 0.3155(3) 0.1654(2) 0.0570(7) Uani 1 d . .
O4 O -0.0631(3) 0.7672(3) 0.4199(2) 0.0463(6) Uani 1 d . .
O5 O -0.0359(5) 0.8509(4) 0.2801(2) 0.0804(10) Uani 1 d . .
O1W O -0.1293(8) 0.0151(5) 0.1319(3) 0.101(2) Uani 1 d . .
O2W O -0.2125(7) 0.8634(5) 0.9651(3) 0.131(2) Uani 1 d . .
O3W O -0.1350(4) 0.5650(4) 0.9301(2) 0.0830(10) Uani 1 d . .
H1WA H -0.1225(101) -0.0415(76) 0.1769(47) 0.148(29) Uiso 1 d . .
H1WB H -0.1332(67) 0.0900(53) 0.1412(34) 0.064(16) Uiso 1 d . .
H3 H -0.7327(52) 0.1838(39) 0.4074(24) 0.049(10) Uiso 1 d . .
H2N H -0.2559(64) 0.4039(50) 0.8809(31) 0.085(14) Uiso 1 d . .
H4 H -0.7484(59) 0.1214(45) 0.2413(28) 0.070(12) Uiso 1 d . .
H5 H -0.4672(53) 0.2252(43) 0.1700(30) 0.070(12) Uiso 1 d . .
H7 H -0.6073(55) 0.3005(39) 0.5430(25) 0.053(11) Uiso 1 d . .
H8A H -0.5333(54) 0.4013(38) 0.6839(23) 0.046(10) Uiso 1 d . .
H8B H -0.3468(42) 0.4903(36) 0.7233(21) 0.029(8) Uiso 1 d . .
H9A H -0.2198(46) 0.2557(33) 0.7647(21) 0.034(8) Uiso 1 d . .
H9B H -0.4404(58) 0.1777(46) 0.7415(27) 0.066(12) Uiso 1 d . .
H10A H -0.5654(68) 0.3556(54) 0.9376(36) 0.091(17) Uiso 1 d . .
H10B H -0.6075(82) 0.4643(66) 0.8441(39) 0.135(22) Uiso 1 d . .
H10C H -0.6676(70) 0.2508(54) 0.8442(33) 0.089(16) Uiso 1 d . .
H11A H -0.3113(68) 0.2225(56) 0.9758(36) 0.085(18) Uiso 1 d . .
H11B H -0.1832(71) 0.1797(54) 0.9083(32) 0.087(17) Uiso 1 d . .
H11C H -0.4366(90) 0.0860(69) 0.9007(40) 0.146(24) 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
O4 Zn1 O2 112.83(11) . . ?
O4 Zn1 O1 103.34(10) . . ?
O2 Zn1 O1 86.50(9) . . ?
O4 Zn1 N1 112.42(10) . 2_566 ?
O2 Zn1 N1 92.89(10) . 2_566 ?
O1 Zn1 N1 141.23(10) . 2_566 ?
O4 Zn1 O1 96.47(10) . 2_566 ?
O2 Zn1 O1 148.49(10) . 2_566 ?
O1 Zn1 O1 75.28(9) . 2_566 ?
N1 Zn1 O1 86.02(9) 2_566 2_566 ?
O1 C1 C6 122.9(3) . . ?
O1 C1 C2 118.6(3) . . ?
C6 C1 C2 118.5(3) . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 C7 116.2(3) . . ?
C1 C2 C7 124.5(3) . . ?
C4 C3 C2 122.2(3) . . ?
C3 C4 C5 118.5(3) . . ?
C4 C5 C6 122.0(4) . . ?
C5 C6 C1 119.4(3) . . ?
C5 C6 C12 116.8(3) . . ?
C1 C6 C12 123.7(3) . . ?
N1 C7 C2 128.5(3) . . ?
N1 C8 C9 109.8(3) . . ?
N2 C9 C8 111.5(3) . . ?
O3 C12 O2 121.5(3) . . ?
O3 C12 C6 118.0(3) . . ?
O2 C12 C6 120.4(3) . . ?
O5 C13 O4 124.7(3) . . ?
O5 C13 C14 118.4(4) . . ?
O4 C13 C14 116.9(3) . . ?
C7 N1 C8 116.6(3) . . ?
C7 N1 Zn1 123.7(2) . 2_566 ?
C8 N1 Zn1 119.7(2) . 2_566 ?
C11 N2 C10 111.3(4) . . ?
C11 N2 C9 108.8(4) . . ?
C10 N2 C9 112.3(3) . . ?
C1 O1 Zn1 127.2(2) . . ?
C1 O1 Zn1 128.1(2) . 2_566 ?
Zn1 O1 Zn1 104.72(9) . 2_566 ?
C12 O2 Zn1 132.3(2) . . ?
C13 O4 Zn1 126.6(2) . . ?
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 2.010(2) . ?
Zn1 O1 2.048(2) . ?
Zn1 N1 2.071(3) 2_566 ?
Zn1 O1 2.077(2) 2_566 ?
C1 O1 1.320(4) . ?
C1 C6 1.405(4) . ?
C1 C2 1.425(4) . ?
C2 C3 1.407(5) . ?
C2 C7 1.444(5) . ?
C3 C4 1.363(5) . ?
C4 C5 1.389(5) . ?
C5 C6 1.403(4) . ?
C6 C12 1.497(5) . ?
C7 N1 1.283(4) . ?
C8 N1 1.477(4) . ?
C8 C9 1.507(5) . ?
C9 N2 1.505(5) . ?
C10 N2 1.503(5) . ?
C11 N2 1.501(6) . ?
C12 O3 1.242(4) . ?
C12 O2 1.267(4) . ?
C13 O5 1.223(4) . ?
C13 O4 1.258(4) . ?
C13 C14 1.512(5) . ?
N1 Zn1 2.071(3) 2_566 ?
O1 Zn1 2.077(2) 2_566 ?
