#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/98/2019845.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2019845
loop_
_publ_author_name
'Liu, Huan'
'Lu, Li-Ping'
_publ_section_title
;
 Crystal structure of diaqua(μ2-triethylenetetraminehexaacetato)dizinc
 tetrahydrate
;
_journal_coeditor_code           HB7351
_journal_issue                   3
_journal_name_full
'Acta Crystallographica Section E Crystallographic Communications'
_journal_page_first              m55
_journal_paper_doi               10.1107/S2056989015002108
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Zn2 (C18 H26 N4 O12) (H2 O1)2], 4H2 O'
_chemical_formula_moiety         ' C18 H30 N4 O14 Zn2, 4(H2 O)'
_chemical_formula_sum            'C18 H38 N4 O18 Zn2'
_chemical_formula_weight         729.26
_chemical_name_systematic
;
Diaqua(μ₂-triethylenetetraminehexaacetato)dizinc tetrahydrate
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                103.969(2)
_cell_angle_beta                 101.052(2)
_cell_angle_gamma                100.882(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1330(14)
_cell_length_b                   8.7013(16)
_cell_length_c                   11.979(2)
_cell_measurement_reflns_used    2008
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.908
_cell_measurement_theta_min      2.622
_cell_volume                     686.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2000)
;
_computing_data_collection
;
SMART (Bruker, 2000)
;
_computing_data_reduction
;
SAINT (Bruker, 2000)
;
_computing_molecular_graphics
;
SHELXTL/PC (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL/PC (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       'ω scans'
_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  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3582
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.838
_exptl_absorpt_correction_T_max  0.7100
_exptl_absorpt_correction_T_min  0.6271
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2000)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.765
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             378
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.755
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0342
_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)+(0.0505P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0888
_reflns_number_gt                2080
_reflns_number_total             2384
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hb7351sup1.cf
_cod_data_source_block           I
_cod_database_code               2019845
_cod_database_fobs_code          2019845
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Zn Zn1 0.27323(5) 0.29051(4) 0.29273(3) 0.02494(14) Uani d . 1 1
N N1 0.0979(4) 0.0459(3) 0.2561(2) 0.0249(5) Uani d . 1 1
N N2 0.0131(4) 0.3615(3) 0.3509(2) 0.0257(5) Uani d . 1 1
O O1 0.3853(3) 0.2527(2) 0.45320(18) 0.0296(5) Uani d . 1 1
O O2 0.3234(4) 0.0827(3) 0.5614(2) 0.0516(7) Uani d . 1 1
O O3 0.4168(3) 0.1580(3) 0.17890(19) 0.0331(5) Uani d . 1 1
O O4 0.3493(3) -0.0649(3) 0.0251(2) 0.0390(6) Uani d . 1 1
H H4 0.4574 -0.0369 0.0120 0.058 Uiso d PR 0.50 1
O O5 0.1248(3) 0.3442(3) 0.14014(18) 0.0312(5) Uani d . 1 1
O O6 -0.0748(4) 0.4953(3) 0.0850(2) 0.0437(6) Uani d . 1 1
H H6 -0.0393 0.4897 0.0232 0.065 Uiso d PR 0.50 1
O O7 0.4665(3) 0.5080(2) 0.3369(2) 0.0377(5) Uani d . 1 1
H H71 0.5033 0.5712 0.4042 0.057 Uiso d R 1 1
H H72 0.4553 0.5622 0.2898 0.057 Uiso d R 1 1
C C1 0.3041(5) 0.1170(4) 0.4670(3) 0.0315(7) Uani d . 1 1
C C2 0.1742(5) -0.0156(4) 0.3559(3) 0.0332(7) Uani d . 1 1
H H2A 0.2499 -0.0926 0.3294 0.040 Uiso calc R 1 1
H H2B 0.0634 -0.0747 0.3772 0.040 Uiso calc R 1 1
C C3 0.3124(4) 0.0213(4) 0.1162(3) 0.0293(7) Uani d . 1 1
C C4 0.1217(5) -0.0520(4) 0.1428(3) 0.0300(7) Uani d . 1 1
H H4A 0.0114 -0.0583 0.0789 0.036 Uiso calc R 1 1
H H4B 0.1204 -0.1623 0.1467 0.036 Uiso calc R 1 1
C C5 -0.1051(4) 0.0634(4) 0.2504(3) 0.0341(7) Uani d . 1 1
H H5A -0.1871 -0.0370 0.2539 0.041 Uiso calc R 1 1
H H5B -0.1585 0.0825 0.1756 0.041 Uiso calc R 1 1
C C6 -0.1089(4) 0.2049(4) 0.3529(3) 0.0308(7) Uani d . 1 1
H H6A -0.2438 0.2133 0.3478 0.037 Uiso calc R 1 1
H H6B -0.0602 0.1835 0.4275 0.037 Uiso calc R 1 1
C C7 -0.0878(5) 0.4310(4) 0.2619(3) 0.0383(8) Uani d . 1 1
H H7A -0.0791 0.5449 0.2996 0.046 Uiso calc R 1 1
H H7B -0.2262 0.3740 0.2356 0.046 Uiso calc R 1 1
C C8 -0.0028(5) 0.4194(4) 0.1545(3) 0.0303(7) Uani d . 1 1
C C9 0.0821(4) 0.4801(4) 0.4711(3) 0.0293(7) Uani d . 1 1
H H9A 0.1606 0.5808 0.4657 0.035 Uiso calc R 1 1
H H9B 0.1671 0.4367 0.5221 0.035 Uiso calc R 1 1
O O8 0.4369(4) 0.7275(3) 0.2220(2) 0.0575(7) Uani d . 1 1
H H81 0.5196 0.7918 0.2798 0.086 Uiso d R 1 1
H H82 0.4963 0.6924 0.1731 0.086 Uiso d R 1 1
O O9 0.6210(6) 0.6889(4) 0.0405(3) 0.0923(12) Uani d . 1 1
H H91 0.6512 0.6831 -0.0229 0.138 Uiso d R 1 1
H H92 0.6638 0.6205 0.0673 0.138 Uiso d R 1 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O7 Zn1 O1 . . 91.79(8) n
O7 Zn1 O3 . . 97.19(9) n
O1 Zn1 O3 . . 102.29(8) n
O7 Zn1 O5 . . 88.93(9) n
O1 Zn1 O5 . . 171.03(8) n
O3 Zn1 O5 . . 86.48(8) n
O7 Zn1 N1 . . 172.37(9) n
O1 Zn1 N1 . . 82.46(8) n
O3 Zn1 N1 . . 79.26(9) n
O5 Zn1 N1 . . 97.53(9) n
O7 Zn1 N2 . . 101.71(9) n
O1 Zn1 N2 . . 92.61(9) n
O3 Zn1 N2 . . 155.51(9) n
O5 Zn1 N2 . . 78.50(8) n
N1 Zn1 N2 . . 83.63(9) n
C5 N1 C4 . . 113.2(2) ?
C5 N1 C2 . . 112.3(2) ?
C4 N1 C2 . . 111.4(2) ?
C5 N1 Zn1 . . 104.87(18) ?
C4 N1 Zn1 . . 107.68(17) ?
C2 N1 Zn1 . . 106.79(18) ?
C6 N2 C7 . . 112.4(3) ?
C6 N2 C9 . . 111.3(2) ?
C7 N2 C9 . . 112.1(2) ?
C6 N2 Zn1 . . 103.30(16) ?
C7 N2 Zn1 . . 108.16(17) ?
C9 N2 Zn1 . . 109.12(17) ?
C1 O1 Zn1 . . 115.50(19) ?
C3 O3 Zn1 . . 113.58(19) ?
C3 O4 H4 . . 118.3 ?
C8 O5 Zn1 . . 116.02(19) ?
C8 O6 H6 . . 118.2 ?
Zn1 O7 H71 . . 123.8 ?
Zn1 O7 H72 . . 117.0 ?
H71 O7 H72 . . 108.0 ?
O2 C1 O1 . . 125.6(3) ?
O2 C1 C2 . . 117.1(3) ?
O1 C1 C2 . . 117.3(3) ?
N1 C2 C1 . . 114.6(2) ?
N1 C2 H2A . . 108.6 ?
C1 C2 H2A . . 108.6 ?
N1 C2 H2B . . 108.6 ?
C1 C2 H2B . . 108.6 ?
H2A C2 H2B . . 107.6 ?
O3 C3 O4 . . 124.8(3) ?
O3 C3 C4 . . 120.6(3) ?
O4 C3 C4 . . 114.6(3) ?
N1 C4 C3 . . 111.7(2) ?
N1 C4 H4A . . 109.3 ?
C3 C4 H4A . . 109.3 ?
N1 C4 H4B . . 109.3 ?
C3 C4 H4B . . 109.3 ?
H4A C4 H4B . . 107.9 ?
N1 C5 C6 . . 110.8(2) ?
N1 C5 H5A . . 109.5 ?
C6 C5 H5A . . 109.5 ?
N1 C5 H5B . . 109.5 ?
C6 C5 H5B . . 109.5 ?
H5A C5 H5B . . 108.1 ?
N2 C6 C5 . . 111.6(2) ?
N2 C6 H6A . . 109.3 ?
C5 C6 H6A . . 109.3 ?
N2 C6 H6B . . 109.3 ?
C5 C6 H6B . . 109.3 ?
H6A C6 H6B . . 108.0 ?
N2 C7 C8 . . 113.6(2) ?
N2 C7 H7A . . 108.8 ?
C8 C7 H7A . . 108.8 ?
N2 C7 H7B . . 108.8 ?
C8 C7 H7B . . 108.8 ?
H7A C7 H7B . . 107.7 ?
O5 C8 O6 . . 125.4(3) ?
O5 C8 C7 . . 121.3(3) ?
O6 C8 C7 . . 113.3(3) ?
N2 C9 C9 . 2_566 114.6(3) ?
N2 C9 H9A . . 108.6 ?
C9 C9 H9A 2_566 . 108.6 ?
N2 C9 H9B . . 108.6 ?
C9 C9 H9B 2_566 . 108.6 ?
H9A C9 H9B . . 107.6 ?
H81 O8 H82 . . 107.0 ?
H91 O9 H92 . . 106.8 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 O7 . 2.003(2) y
Zn1 O1 . 2.063(2) y
Zn1 O3 . 2.112(2) y
Zn1 O5 . 2.130(2) y
Zn1 N1 . 2.150(2) y
Zn1 N2 . 2.243(2) y
N1 C5 . 1.474(4) ?
N1 C4 . 1.477(4) ?
N1 C2 . 1.477(4) ?
N2 C6 . 1.480(4) ?
N2 C7 . 1.483(4) ?
N2 C9 . 1.483(4) ?
O1 C1 . 1.277(4) ?
O2 C1 . 1.227(4) ?
O3 C3 . 1.246(4) ?
O4 C3 . 1.270(4) ?
O4 H4 . 0.8200 ?
O5 C8 . 1.232(4) ?
O6 C8 . 1.274(4) ?
O6 H6 . 0.8199 ?
O7 H71 . 0.8199 ?
O7 H72 . 0.8200 ?
C1 C2 . 1.530(4) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.516(4) ?
C4 H4A . 0.9700 ?
C4 H4B . 0.9700 ?
C5 C6 . 1.523(4) ?
C5 H5A . 0.9700 ?
C5 H5B . 0.9700 ?
C6 H6A . 0.9700 ?
C6 H6B . 0.9700 ?
C7 C8 . 1.514(4) ?
C7 H7A . 0.9700 ?
C7 H7B . 0.9700 ?
C9 C9 2_566 1.523(5) ?
C9 H9A . 0.9700 ?
C9 H9B . 0.9700 ?
O8 H81 . 0.8203 ?
O8 H82 . 0.8203 ?
O9 H91 . 0.8207 ?
O9 H92 . 0.8211 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
C9 H9B O1 . 0.97 2.54 3.198(4) 125 y
C2 H2A O8 1_545 0.97 2.52 3.476(4) 168 y
C5 H5B O4 2 0.97 2.48 3.428(4) 166 y
O7 H71 O1 2_666 0.82 1.91 2.720(3) 169 y
O7 H72 O8 . 0.82 1.83 2.627(3) 164 y
O8 H81 O2 2_666 0.82 1.94 2.747(4) 166 y
O8 H82 O9 . 0.82 1.96 2.734(4) 157 y
O9 H91 O5 2_665 0.82 2.33 3.074(4) 151 y
O9 H92 O6 1_655 0.82 2.33 3.033(4) 144 y
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_site_symmetry_4
_geom_torsion
O1 Zn1 N1 C5 . 111.87(18)
O3 Zn1 N1 C5 . -144.02(19)
O5 Zn1 N1 C5 . -59.08(19)
N2 Zn1 N1 C5 . 18.38(18)
O1 Zn1 N1 C4 . -127.26(19)
O3 Zn1 N1 C4 . -23.16(18)
O5 Zn1 N1 C4 . 61.78(19)
N2 Zn1 N1 C4 . 139.24(19)
O1 Zn1 N1 C2 . -7.52(18)
O3 Zn1 N1 C2 . 96.59(19)
O5 Zn1 N1 C2 . -178.48(18)
N2 Zn1 N1 C2 . -101.02(19)
O7 Zn1 N2 C6 . -164.05(17)
O1 Zn1 N2 C6 . -71.68(18)
O3 Zn1 N2 C6 . 56.2(3)
O5 Zn1 N2 C6 . 109.49(18)
N1 Zn1 N2 C6 . 10.43(18)
O7 Zn1 N2 C7 . 76.6(2)
O1 Zn1 N2 C7 . 169.0(2)
O3 Zn1 N2 C7 . -63.1(3)
O5 Zn1 N2 C7 . -9.9(2)
N1 Zn1 N2 C7 . -108.9(2)
O7 Zn1 N2 C9 . -45.53(19)
O1 Zn1 N2 C9 . 46.84(19)
O3 Zn1 N2 C9 . 174.73(19)
O5 Zn1 N2 C9 . -131.99(19)
N1 Zn1 N2 C9 . 128.95(19)
O7 Zn1 O1 C1 . -178.9(2)
O3 Zn1 O1 C1 . -81.1(2)
N1 Zn1 O1 C1 . -3.9(2)
N2 Zn1 O1 C1 . 79.3(2)
O7 Zn1 O3 C3 . -166.2(2)
O1 Zn1 O3 C3 . 100.4(2)
O5 Zn1 O3 C3 . -77.7(2)
N1 Zn1 O3 C3 . 20.6(2)
N2 Zn1 O3 C3 . -25.8(3)
O7 Zn1 O5 C8 . -87.6(2)
O3 Zn1 O5 C8 . 175.2(2)
N1 Zn1 O5 C8 . 96.5(2)
N2 Zn1 O5 C8 . 14.6(2)
Zn1 O1 C1 O2 . -166.3(3)
Zn1 O1 C1 C2 . 14.7(3)
C5 N1 C2 C1 . -97.9(3)
C4 N1 C2 C1 . 133.9(3)
Zn1 N1 C2 C1 . 16.6(3)
O2 C1 C2 N1 . 159.0(3)
O1 C1 C2 N1 . -21.9(4)
Zn1 O3 C3 O4 . 164.5(2)
Zn1 O3 C3 C4 . -13.1(4)
C5 N1 C4 C3 . 138.9(3)
C2 N1 C4 C3 . -93.3(3)
Zn1 N1 C4 C3 . 23.4(3)
O3 C3 C4 N1 . -7.9(4)
O4 C3 C4 N1 . 174.3(2)
C4 N1 C5 C6 . -162.2(3)
C2 N1 C5 C6 . 70.6(3)
Zn1 N1 C5 C6 . -45.0(3)
C7 N2 C6 C5 . 78.5(3)
C9 N2 C6 C5 . -154.9(3)
Zn1 N2 C6 C5 . -37.9(3)
N1 C5 C6 N2 . 59.6(3)
C6 N2 C7 C8 . -107.8(3)
C9 N2 C7 C8 . 126.0(3)
Zn1 N2 C7 C8 . 5.6(3)
Zn1 O5 C8 O6 . 162.7(3)
Zn1 O5 C8 C7 . -16.4(4)
N2 C7 C8 O5 . 6.7(5)
N2 C7 C8 O6 . -172.5(3)
C6 N2 C9 C9 2_566 -58.1(4)
C7 N2 C9 C9 2_566 68.7(4)
Zn1 N2 C9 C9 2_566 -171.5(3)
