#------------------------------------------------------------------------------
#$Date: 2016-02-18 17:37:37 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176729 $
#$URL: svn://www.crystallography.net/cod/cif/1/51/30/1513035.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_1513035
loop_
_publ_author_name
'Lamshöft, Marc'
'Storp, Jürgen'
'Ivanova, Bojidarka'
'Spiteller, Michael'
_publ_section_title
;
 Gas-phase CT-stabilized Ag(I) and Zn(II) metal-organic
 complexes–experimental vs. theoretical study
;
_journal_name_full               Polyhedron
_journal_page_first              2564
_journal_paper_doi               10.1016/j.poly.2011.07.003
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         '2(C5 H6 N5 O), Cl4 Zn, 2(H2 O)'
_chemical_formula_sum            'C10 H16 Cl4 N10 O4 Zn'
_chemical_formula_weight         547.50
_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                 95.544(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.817(2)
_cell_length_b                   19.633(3)
_cell_length_c                   8.0457(13)
_cell_measurement_temperature    200(2)
_cell_volume                     2015.1(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker GIS'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker APEX2'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART X2S'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  'doubly curved silicon crystal'
_diffrn_radiation_source         'micro-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18765
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    1.791
_exptl_absorpt_correction_T_max  0.8005
_exptl_absorpt_correction_T_min  0.5649
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.805
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         3560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0356P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                3015
_reflns_number_total             3560
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            Struct-200-3-2.cif
_cod_data_source_block           200-3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1513035
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_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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Zn1 Zn 0.27726(2) 0.380349(14) 0.56148(3) 0.03388(11) Uani 1 1 d .
N10 N 1.40250(16) 0.74945(11) -0.0475(2) 0.0384(5) Uani 1 1 d .
H10 H 1.4062 0.7940 -0.0362 0.046 Uiso 1 1 calc R
O2 O 1.30044(17) 0.52667(9) -0.0136(3) 0.0570(6) Uani 1 1 d .
N8 N 1.24742(16) 0.72926(10) 0.0954(2) 0.0343(5) Uani 1 1 d .
Cl2 Cl 0.39391(6) 0.38325(4) 0.79108(8) 0.0511(2) Uani 1 1 d .
Cl3 Cl 0.26117(6) 0.48792(3) 0.45454(10) 0.0564(2) Uani 1 1 d .
N2 N -0.11536(16) 0.69021(10) 0.9127(2) 0.0353(5) Uani 1 1 d .
H2 H -0.1098 0.7348 0.9211 0.042 Uiso 1 1 calc R
C00 C 0.0879(2) 0.61537(12) 0.7051(3) 0.0347(6) Uani 1 1 d .
OW2 O 1.4878(4) 0.46977(17) 0.2380(6) 0.0999(13) Uani 1 1 d .
C9 C -0.0302(2) 0.52676(13) 0.7963(3) 0.0385(6) Uani 1 1 d .
N5 N 0.03883(16) 0.66698(10) 0.7681(2) 0.0342(5) Uani 1 1 d .
OW1 O -0.5847(3) 0.61535(16) 0.4416(7) 0.0947(12) Uani 1 1 d .
C2 C -0.04746(19) 0.64786(12) 0.8394(3) 0.0313(5) Uani 1 1 d .
C3 C 1.1882(2) 0.67754(12) 0.1374(3) 0.0347(6) Uani 1 1 d .
N9 N 1.43932(17) 0.64637(12) -0.1184(3) 0.0424(5) Uani 1 1 d .
H9 H 1.4702 0.6116 -0.1622 0.051 Uiso 1 1 calc R
C4 C 1.35226(19) 0.64311(13) -0.0307(3) 0.0356(6) Uani 1 1 d .
C5 C 1.32845(19) 0.70815(12) 0.0118(3) 0.0321(6) Uani 1 1 d .
N6 N 1.10497(19) 0.68929(12) 0.2180(3) 0.0467(6) Uani 1 1 d .
H6A H 1.089(2) 0.7313(15) 0.244(4) 0.056 Uiso 1 1 calc .
H6B H 1.066(2) 0.6551(16) 0.246(3) 0.056 Uiso 1 1 calc .
N1 N -0.17432(16) 0.58770(11) 0.9387(2) 0.0375(5) Uani 1 1 d .
H1 H -0.2132 0.5533 0.9663 0.045 Uiso 1 1 calc R
C6 C 1.2898(2) 0.58812(13) 0.0157(3) 0.0392(6) Uani 1 1 d .
C7 C 1.4683(2) 0.71059(14) -0.1253(3) 0.0435(7) Uani 1 1 d .
H7 H 1.5268 0.7268 -0.1776 0.052 Uiso 1 1 calc R
C8 C -0.08489(19) 0.58307(12) 0.8554(3) 0.0343(6) Uani 1 1 d .
Cl4 Cl 0.11272(5) 0.35269(4) 0.62134(8) 0.04599(18) Uani 1 1 d .
Cl1 Cl 0.33038(6) 0.30391(4) 0.38136(9) 0.0536(2) Uani 1 1 d .
O1 O -0.04865(15) 0.46594(9) 0.8079(3) 0.0509(5) Uani 1 1 d .
C1 C -0.1909(2) 0.65243(13) 0.9691(3) 0.0384(6) Uani 1 1 d .
H1A H -0.2482 0.6697 1.0231 0.046 Uiso 1 1 calc R
N3 N 0.1732(2) 0.62601(13) 0.6270(3) 0.0479(6) Uani 1 1 d .
H3A H 0.197(2) 0.6677(16) 0.617(3) 0.057 Uiso 1 1 calc .
H3B H 0.206(2) 0.5914(16) 0.585(3) 0.057 Uiso 1 1 calc .
N7 N 1.20876(17) 0.61127(10) 0.1006(3) 0.0383(5) Uani 1 1 d .
H7A H 1.1659 0.5803 0.1347 0.046 Uiso 1 1 calc R
N4 N 0.05601(16) 0.54884(10) 0.7178(3) 0.0383(5) Uani 1 1 d .
H4 H 0.0933 0.5175 0.6725 0.046 Uiso 1 1 calc R
H100 H -0.588(4) 0.593(2) 0.496(7) 0.10(2) Uiso 1 1 d .
H200 H -0.513(7) 0.605(4) 0.403(11) 0.29(5) Uiso 1 1 d .
H300 H 1.440(4) 0.473(3) 0.204(7) 0.12(3) Uiso 1 1 d .
H400 H 1.524(5) 0.498(3) 0.205(8) 0.20(3) Uiso 1 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'
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
Cl1 Zn1 Cl2 109.11(3)
Cl1 Zn1 Cl4 108.87(3)
Cl2 Zn1 Cl4 112.73(3)
Cl1 Zn1 Cl3 113.49(3)
Cl2 Zn1 Cl3 108.24(3)
Cl4 Zn1 Cl3 104.42(3)
C7 N10 C5 108.4(2)
C7 N10 H10 125.8
C5 N10 H10 125.8
C3 N8 C5 112.1(2)
C1 N2 C2 108.6(2)
C1 N2 H2 125.7
C2 N2 H2 125.7
N5 C00 N3 120.4(2)
N5 C00 N4 123.0(2)
N3 C00 N4 116.7(2)
H300 OW2 H400 111(7)
O1 C9 N4 120.4(2)
O1 C9 C8 129.2(3)
N4 C9 C8 110.4(2)
C00 N5 C2 113.0(2)
H100 OW1 H200 102(6)
N5 C2 C8 127.5(2)
N5 C2 N2 126.4(2)
C8 C2 N2 106.2(2)
N6 C3 N8 119.9(2)
N6 C3 N7 117.0(2)
N8 C3 N7 123.1(2)
C7 N9 C4 108.1(2)
C7 N9 H9 126.0
C4 N9 H9 125.9
C5 C4 N9 107.2(2)
C5 C4 C6 120.1(2)
N9 C4 C6 132.6(2)
N8 C5 C4 127.7(2)
N8 C5 N10 125.6(2)
C4 C5 N10 106.7(2)
C3 N6 H6A 116(2)
C3 N6 H6B 121(2)
H6A N6 H6B 123(3)
C1 N1 C8 108.1(2)
C1 N1 H1 126.0
C8 N1 H1 126.0
O2 C6 N7 121.3(2)
O2 C6 C4 128.1(2)
N7 C6 C4 110.7(2)
N9 C7 N10 109.5(2)
N9 C7 H7 125.3
N10 C7 H7 125.2
C2 C8 N1 107.4(2)
C2 C8 C9 120.3(2)
N1 C8 C9 132.3(2)
N1 C1 N2 109.7(2)
N1 C1 H1A 125.1
N2 C1 H1A 125.1
C00 N3 H3A 118(2)
C00 N3 H3B 124(2)
H3A N3 H3B 117(3)
C3 N7 C6 126.4(2)
C3 N7 H7A 116.8
C6 N7 H7A 116.8
C00 N4 C9 125.7(2)
C00 N4 H4 117.1
C9 N4 H4 117.1
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Zn1 Cl1 2.2376(7)
Zn1 Cl2 2.2622(8)
Zn1 Cl4 2.2740(8)
Zn1 Cl3 2.2824(8)
N10 C7 1.337(3)
N10 C5 1.369(3)
N10 H10 0.8800
O2 C6 1.239(3)
N8 C3 1.330(3)
N8 C5 1.356(3)
N2 C1 1.334(3)
N2 C2 1.377(3)
N2 H2 0.8800
C00 N5 1.320(3)
C00 N3 1.328(3)
C00 N4 1.376(3)
OW2 H300 0.65(5)
OW2 H400 0.78(6)
C9 O1 1.223(3)
C9 N4 1.394(3)
C9 C8 1.415(3)
N5 C2 1.347(3)
OW1 H100 0.63(5)
OW1 H200 1.01(8)
C2 C8 1.370(3)
C3 N6 1.321(3)
C3 N7 1.366(3)
N9 C7 1.317(3)
N9 C4 1.378(3)
N9 H9 0.8800
C4 C5 1.364(3)
C4 C6 1.416(4)
N6 H6A 0.87(3)
N6 H6B 0.83(3)
N1 C1 1.316(3)
N1 C8 1.385(3)
N1 H1 0.8800
C6 N7 1.374(3)
C7 H7 0.9500
C1 H1A 0.9500
N3 H3A 0.81(3)
N3 H3B 0.83(3)
N7 H7A 0.8800
N4 H4 0.8800
