#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/93/2239337.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_2239337
loop_
_publ_author_name
'Wang, Xiao-Juan'
'Feng, Yun-Long'
_publ_section_title
;
 Bis[μ-1,3-bis(1H-imidazol-1-yl)propane-κ²N³:N^3'^]bis(dichloridozinc)
 dihydrate
;
_journal_coeditor_code           WM5017
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m184
_journal_paper_doi               10.1107/S1600536814008162
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Zn2 Cl4 (C9 H12 N4)2], 2H2 O'
_chemical_formula_moiety         'C18 H24 Cl4 N8 Zn2, 2(H2 O)'
_chemical_formula_sum            'C18 H28 Cl4 N8 O2 Zn2'
_chemical_formula_weight         661.02
_chemical_name_systematic
'Bis[μ-1,3-bis(1H-imidazol-1-yl)propane-κ²N³:N^3'^]bis(dichloridozinc) dihydrate'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.704(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.1378(4)
_cell_length_b                   9.7173(4)
_cell_length_c                   13.8801(6)
_cell_measurement_reflns_used    6173
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.01
_cell_volume                     1364.50(10)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω and φ-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  0.0333
_diffrn_reflns_av_sigmaI/netI    0.0211
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21184
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.181
_exptl_absorpt_correction_T_max  .770
_exptl_absorpt_correction_T_min  .631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .18
_exptl_crystal_size_min          .12
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         3162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_gt           0.0296
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0432P)²+0.5084P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                2473
_reflns_number_total             3162
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            wm5017sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2239337
_cod_database_fobs_code          2239337
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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 0.34226(3) 0.80572(3) 0.74784(2) 0.04641(11) Uani d . 1 1
Cl Cl1 0.39773(7) 0.82340(8) 0.90676(5) 0.0634(2) Uani d . 1 1
Cl Cl2 0.19959(7) 0.97104(7) 0.69087(6) 0.0684(2) Uani d . 1 1
O O1W 0.1166(3) 0.7064(4) 0.9784(2) 0.1265(12) Uani d . 1 1
H H1WA 0.1788 0.7355 0.9456 0.152 Uiso d R 1 1
H H1WB 0.1429 0.7043 1.0377 0.152 Uiso d R 1 1
N N1 0.25814(18) 0.6260(2) 0.70857(13) 0.0443(4) Uani d . 1 1
N N2 0.21115(19) 0.43655(19) 0.62798(13) 0.0430(4) Uani d . 1 1
N N3 0.29331(19) 0.1944(2) 0.37271(14) 0.0452(4) Uani d . 1 1
N N4 0.49316(19) 0.1728(2) 0.32351(14) 0.0458(5) Uani d . 1 1
C C1 0.1371(2) 0.5783(3) 0.73318(17) 0.0474(6) Uani d . 1 1
H H1A 0.0841 0.6199 0.7771 0.057 Uiso calc R 1 1
C C2 0.2989(2) 0.5376(2) 0.64438(16) 0.0449(5) Uani d . 1 1
H H2A 0.3782 0.5449 0.6146 0.054 Uiso calc R 1 1
C C3 0.1072(2) 0.4622(3) 0.68377(17) 0.0481(6) Uani d . 1 1
H H3A 0.0310 0.4096 0.6869 0.058 Uiso calc R 1 1
C C4 0.2215(3) 0.3244(2) 0.55803(18) 0.0505(6) Uani d . 1 1
H H4A 0.1746 0.2443 0.5797 0.061 Uiso calc R 1 1
H H4B 0.3137 0.2993 0.5542 0.061 Uiso calc R 1 1
C C5 0.1646(2) 0.3666(3) 0.45951(16) 0.0489(5) Uani d . 1 1
H H5A 0.2165 0.4420 0.4363 0.059 Uiso calc R 1 1
H H5B 0.0752 0.3999 0.4651 0.059 Uiso calc R 1 1
C C6 0.1616(2) 0.2514(3) 0.3861(2) 0.0555(6) Uani d . 1 1
H H6A 0.1046 0.1785 0.4068 0.067 Uiso calc R 1 1
H H6B 0.1241 0.2858 0.3247 0.067 Uiso calc R 1 1
C C7 0.3435(3) 0.0752(3) 0.41050(19) 0.0571(6) Uani d . 1 1
H H7A 0.3011 0.0141 0.4498 0.069 Uiso calc R 1 1
C C8 0.3855(2) 0.2498(3) 0.32038(17) 0.0489(6) Uani d . 1 1
H H8A 0.3753 0.3318 0.2862 0.059 Uiso calc R 1 1
C C9 0.4668(3) 0.0622(3) 0.38023(18) 0.0533(6) Uani d . 1 1
H H9A 0.5245 -0.0101 0.3955 0.064 Uiso calc 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'
Cl Cl 0.1484 0.1585 '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
N1 Zn1 N4 . 3_666 108.03(8)
N1 Zn1 Cl1 . . 114.12(6)
N4 Zn1 Cl1 3_666 . 108.26(6)
N1 Zn1 Cl2 . . 105.77(6)
N4 Zn1 Cl2 3_666 . 106.63(6)
Cl1 Zn1 Cl2 . . 113.66(3)
H1WA O1W H1WB . . 109.3
C2 N1 C1 . . 105.7(2)
C2 N1 Zn1 . . 127.09(16)
C1 N1 Zn1 . . 126.64(16)
C2 N2 C3 . . 107.35(19)
C2 N2 C4 . . 125.7(2)
C3 N2 C4 . . 126.8(2)
C8 N3 C7 . . 107.2(2)
C8 N3 C6 . . 126.3(2)
C7 N3 C6 . . 126.5(2)
C8 N4 C9 . . 105.8(2)
C8 N4 Zn1 . 3_666 129.55(17)
C9 N4 Zn1 . 3_666 124.41(16)
C3 C1 N1 . . 109.3(2)
C3 C1 H1A . . 125.3
N1 C1 H1A . . 125.3
N1 C2 N2 . . 111.0(2)
N1 C2 H2A . . 124.5
N2 C2 H2A . . 124.5
C1 C3 N2 . . 106.6(2)
C1 C3 H3A . . 126.7
N2 C3 H3A . . 126.7
N2 C4 C5 . . 111.01(19)
N2 C4 H4A . . 109.4
C5 C4 H4A . . 109.4
N2 C4 H4B . . 109.4
C5 C4 H4B . . 109.4
H4A C4 H4B . . 108.0
C4 C5 C6 . . 113.6(2)
C4 C5 H5A . . 108.8
C6 C5 H5A . . 108.8
C4 C5 H5B . . 108.8
C6 C5 H5B . . 108.8
H5A C5 H5B . . 107.7
N3 C6 C5 . . 112.65(19)
N3 C6 H6A . . 109.1
C5 C6 H6A . . 109.1
N3 C6 H6B . . 109.1
C5 C6 H6B . . 109.1
H6A C6 H6B . . 107.8
C9 C7 N3 . . 106.9(2)
C9 C7 H7A . . 126.5
N3 C7 H7A . . 126.5
N4 C8 N3 . . 111.1(2)
N4 C8 H8A . . 124.4
N3 C8 H8A . . 124.4
C7 C9 N4 . . 108.9(2)
C7 C9 H9A . . 125.5
N4 C9 H9A . . 125.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn1 N1 . 2.0038(19)
Zn1 N4 3_666 2.0053(19)
Zn1 Cl1 . 2.2476(7)
Zn1 Cl2 . 2.2694(7)
O1W H1WA . 0.8500
O1W H1WB . 0.8500
N1 C2 . 1.323(3)
N1 C1 . 1.375(3)
N2 C2 . 1.334(3)
N2 C3 . 1.370(3)
N2 C4 . 1.468(3)
N3 C8 . 1.333(3)
N3 C7 . 1.357(3)
N3 C6 . 1.468(3)
N4 C8 . 1.322(3)
N4 C9 . 1.369(3)
N4 Zn1 3_666 2.0053(19)
C1 C3 . 1.345(3)
C1 H1A . 0.9300
C2 H2A . 0.9300
C3 H3A . 0.9300
C4 C5 . 1.507(3)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 C6 . 1.513(3)
C5 H5A . 0.9700
C5 H5B . 0.9700
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 C9 . 1.350(4)
C7 H7A . 0.9300
C8 H8A . 0.9300
C9 H9A . 0.9300
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
O1W H1WA Cl1 . 0.85 2.47 3.282(3) 160.1
O1W H1WB Cl2 4_576 0.85 2.76 3.473(4) 143.1
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_1
_geom_torsion
N4 Zn1 N1 C2 3_666 -2.4(2)
Cl1 Zn1 N1 C2 . -122.86(18)
Cl2 Zn1 N1 C2 . 111.46(19)
N4 Zn1 N1 C1 3_666 -172.98(18)
Cl1 Zn1 N1 C1 . 66.57(19)
Cl2 Zn1 N1 C1 . -59.12(19)
C2 N1 C1 C3 . 0.2(3)
Zn1 N1 C1 C3 . 172.38(16)
C1 N1 C2 N2 . -0.6(3)
Zn1 N1 C2 N2 . -172.77(14)
C3 N2 C2 N1 . 0.8(3)
C4 N2 C2 N1 . 177.2(2)
N1 C1 C3 N2 . 0.3(3)
C2 N2 C3 C1 . -0.7(2)
C4 N2 C3 C1 . -177.0(2)
C2 N2 C4 C5 . -86.8(3)
C3 N2 C4 C5 . 88.8(3)
N2 C4 C5 C6 . -175.0(2)
C8 N3 C6 C5 . -78.9(3)
C7 N3 C6 C5 . 101.8(3)
C4 C5 C6 N3 . -58.6(3)
C8 N3 C7 C9 . 0.5(3)
C6 N3 C7 C9 . 180.0(2)
C9 N4 C8 N3 . 0.6(3)
Zn1 N4 C8 N3 3_666 174.77(15)
C7 N3 C8 N4 . -0.7(3)
C6 N3 C8 N4 . 179.8(2)
N3 C7 C9 N4 . -0.2(3)
C8 N4 C9 C7 . -0.2(3)
Zn1 N4 C9 C7 3_666 -174.79(17)
