#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:58:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179356 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/53/4325353.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_4325353
loop_
_publ_author_name
'Julien Estager'
'Peter Nockemann'
'Kenneth R. Seddon'
'Małgorzata Swadźba-Kwaśny'
'Sophie Tyrrell'
_publ_section_title
;
 Validation of Speciation Techniques: A Study of Chlorozincate(II) Ionic
 Liquids
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5258
_journal_page_last               5271
_journal_paper_doi               10.1021/ic200586u
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration unk
_chemical_formula_moiety         'Cl13 Zn6, C6 H11 N2'
_chemical_formula_sum            'C6 H11 Cl13 N2 Zn6'
_chemical_formula_weight         964.24
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-03-04
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.5080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.6552(4)
_cell_length_b                   9.2453(2)
_cell_length_c                   17.9079(4)
_cell_measurement_reflns_used    19858
_cell_measurement_temperature    120.15
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     2629.76(10)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      120.15
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11623
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.93
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.706
_exptl_absorpt_correction_T_max  27.485
_exptl_absorpt_correction_T_min  2.910
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.357
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         5840
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0389P)²+22.7113P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                4984
_reflns_number_total             5840
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200586u_si_002_3.cif
_cod_data_source_block           2011src0050
_cod_database_code               4325353
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, y, -z'
3 'x+1/2, y+1/2, z'
4 '-x+1/2, y+1/2, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.11349(8) 0.83683(13) 0.53614(7) 0.0186(3) Uani 1 1 d . . .
Zn2 Zn 0.22325(6) 0.17728(14) 0.52756(7) 0.0189(3) Uani 1 1 d . . .
Zn3 Zn 0.27641(7) -0.15567(14) 0.97195(7) 0.0200(3) Uani 1 1 d . . .
Zn4 Zn 0.38656(8) 0.18517(13) 0.96359(7) 0.0186(3) Uani 1 1 d . . .
Zn5 Zn 0.29534(7) 0.50801(14) 0.85586(8) 0.0302(4) Uani 1 1 d . . .
Zn6 Zn 0.20445(7) 0.51466(14) 0.64415(8) 0.0273(3) Uani 1 1 d . . .
Cl7 Cl 0.41418(14) 0.3606(3) 0.88768(14) 0.0217(6) Uani 1 1 d . . .
Cl8 Cl 0.5000 0.0305(4) 1.0000 0.0181(8) Uani 1 2 d S . .
Cl9 Cl 0.31098(14) -0.0867(4) 1.10045(14) 0.0241(6) Uani 1 1 d . . .
Cl10 Cl 0.36554(16) -0.3371(4) 0.97243(17) 0.0269(7) Uani 1 1 d . . .
Cl11 Cl 0.13716(13) 0.7386(3) 0.42850(13) 0.0195(6) Uani 1 1 d . . .
Cl12 Cl 0.23433(17) 0.3318(4) 0.72826(15) 0.0322(7) Uani 1 1 d . . .
Cl13 Cl 0.08543(14) 0.6599(3) 0.61260(14) 0.0215(6) Uani 1 1 d . . .
Cl14 Cl 0.13511(16) 0.3578(4) 0.52821(17) 0.0262(7) Uani 1 1 d . . .
Cl15 Cl 0.0000 0.9892(4) 0.5000 0.0218(8) Uani 1 2 d S . .
Cl16 Cl 0.26559(16) 0.6898(3) 0.77135(15) 0.0294(6) Uani 1 1 d . . .
Cl17 Cl 0.28046(15) 0.0401(3) 0.89447(14) 0.0254(7) Uani 1 1 d . . .
Cl18 Cl 0.13671(13) -0.2192(3) 0.92805(13) 0.0209(6) Uani 1 1 d . . .
Cl19 Cl 0.18949(14) 0.1079(4) 0.39961(13) 0.0218(6) Uani 1 1 d . . .
Cl20 Cl 0.21942(16) -0.0174(3) 0.60571(14) 0.0261(7) Uani 1 1 d . . .
C2AA C 0.5147(3) 0.7707(5) 0.6732(2) 0.0335(15) Uani 1 1 d GU A 1
H2A H 0.5337 0.7348 0.6317 0.040 Uiso 1 1 calc R A 1
N N 0.5266(3) 0.7032(4) 0.7470(2) 0.0343(13) Uani 1 1 d GU A 1
C3 C 0.4887(3) 0.7919(5) 0.79165(18) 0.0325(14) Uani 1 1 d GU A 1
H3 H 0.4872 0.7728 0.8433 0.039 Uiso 1 1 calc R A 1
N2 N 0.4533(3) 0.9142(4) 0.7455(3) 0.0357(14) Uani 1 1 d GU A 1
C5 C 0.4694(3) 0.9011(4) 0.6723(2) 0.0324(14) Uani 1 1 d GU A 1
H5 H 0.4527 0.9678 0.6301 0.039 Uiso 1 1 calc R A 1
C1AA C 0.5230(5) 0.4475(10) 0.7318(5) 0.0486(19) Uani 1 1 d U A .
H1AA H 0.5040 0.4662 0.6754 0.073 Uiso 1 1 calc R . .
H1AB H 0.4742 0.4268 0.7500 0.073 Uiso 1 1 calc R . .
H1AC H 0.5612 0.3642 0.7427 0.073 Uiso 1 1 calc R . .
C C 0.4179(6) 1.0316(11) 0.7709(5) 0.053(2) Uani 1 1 d U . .
HA H 0.3679 1.0006 0.7846 0.079 Uiso 1 1 calc R A 1
HB H 0.4018 1.1042 0.7291 0.079 Uiso 1 1 calc R A 1
HC H 0.4588 1.0737 0.8170 0.079 Uiso 1 1 calc R A 1
C0AA C 0.5671(6) 0.5742(12) 0.7726(6) 0.059(2) Uani 1 1 d U . .
H0AA H 0.5741 0.5638 0.8293 0.070 Uiso 1 1 calc R A 1
H0AB H 0.6239 0.5777 0.7660 0.070 Uiso 1 1 calc R A 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'
Cl Cl 0.1484 0.1585 '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
Cl11 Zn1 Cl13 110.11(11) . .
Cl11 Zn1 Cl15 110.23(8) . .
Cl11 Zn1 Cl20 113.48(10) . 1_565
Cl13 Zn1 Cl15 108.16(10) . .
Cl13 Zn1 Cl20 111.32(11) . 1_565
Cl20 Zn1 Cl15 103.23(12) 1_565 .
Cl11 Zn2 Cl20 101.33(10) 4_546 .
Cl14 Zn2 Cl11 114.55(13) . 4_546
Cl14 Zn2 Cl19 104.64(12) . .
Cl14 Zn2 Cl20 116.49(11) . .
Cl19 Zn2 Cl11 109.44(9) . 4_546
Cl19 Zn2 Cl20 110.41(13) . .
Cl9 Zn3 Cl17 110.14(13) . .
Cl9 Zn3 Cl18 109.76(9) . .
Cl10 Zn3 Cl9 103.82(12) . .
Cl10 Zn3 Cl17 116.97(11) . .
Cl10 Zn3 Cl18 114.33(13) . .
Cl17 Zn3 Cl18 101.88(10) . .
Cl7 Zn4 Cl8 108.62(10) . .
Cl7 Zn4 Cl17 111.35(11) . .
Cl7 Zn4 Cl18 110.75(12) . 4_557
Cl17 Zn4 Cl8 103.04(12) . .
Cl17 Zn4 Cl18 113.06(11) . 4_557
Cl18 Zn4 Cl8 109.67(8) 4_557 .
Cl7 Zn5 Cl10 88.93(10) . 1_565
Cl7 Zn5 Cl12 86.04(10) . .
Cl9 Zn5 Cl7 112.12(11) 4_557 .
Cl9 Zn5 Cl10 98.46(11) 4_557 1_565
Cl9 Zn5 Cl12 85.84(10) 4_557 .
Cl10 Zn5 Cl12 174.34(10) 1_565 .
Cl16 Zn5 Cl7 127.59(10) . .
Cl16 Zn5 Cl9 118.80(11) . 4_557
Cl16 Zn5 Cl10 95.04(12) . 1_565
Cl16 Zn5 Cl12 86.02(9) . .
Cl12 Zn6 Cl13 127.39(11) . .
Cl12 Zn6 Cl14 94.30(11) . .
Cl12 Zn6 Cl16 86.23(9) . .
Cl12 Zn6 Cl19 118.52(11) . 4_556
Cl13 Zn6 Cl14 89.20(10) . .
Cl13 Zn6 Cl16 86.38(9) . .
Cl14 Zn6 Cl16 174.79(9) . .
Cl19 Zn6 Cl13 112.78(11) 4_556 .
Cl19 Zn6 Cl14 98.26(10) 4_556 .
Cl19 Zn6 Cl16 86.00(10) 4_556 .
Zn4 Cl7 Zn5 104.86(10) . .
Zn4 Cl8 Zn4 103.18(17) 2_657 .
Zn3 Cl9 Zn5 117.33(11) . 4_547
Zn3 Cl10 Zn5 106.36(12) . 1_545
Zn1 Cl11 Zn2 103.00(9) . 4_556
Zn6 Cl12 Zn5 93.70(12) . .
Zn1 Cl13 Zn6 104.37(10) . .
Zn2 Cl14 Zn6 107.30(12) . .
Zn1 Cl15 Zn1 104.03(17) . 2_556
Zn5 Cl16 Zn6 94.05(11) . .
Zn4 Cl17 Zn3 107.25(10) . .
Zn4 Cl18 Zn3 102.88(10) 4_547 .
Zn2 Cl19 Zn6 117.67(10) . 4_546
Zn1 Cl20 Zn2 106.90(10) 1_545 .
N C2AA C5 108.0 . .
C2AA N C3 108.0 . .
C0AA N C2AA 127.4(5) . .
C0AA N C3 124.6(5) . .
N2 C3 N 108.0 . .
C5 N2 C3 108.0 . .
C N2 C3 125.4(5) . .
C N2 C5 126.2(5) . .
N2 C5 C2AA 108.0 . .
N C0AA C1AA 114.0(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 Cl11 2.270(3) .
Zn1 Cl13 2.270(3) .
Zn1 Cl15 2.289(3) .
Zn1 Cl20 2.271(3) 1_565
Zn2 Cl11 2.290(2) 4_546
Zn2 Cl14 2.225(3) .
Zn2 Cl19 2.281(3) .
Zn2 Cl20 2.292(3) .
Zn3 Cl9 2.288(3) .
Zn3 Cl10 2.238(3) .
Zn3 Cl17 2.294(3) .
Zn3 Cl18 2.297(3) .
Zn4 Cl7 2.251(3) .
Zn4 Cl8 2.302(3) .
Zn4 Cl17 2.267(3) .
Zn4 Cl18 2.269(3) 4_557
Zn5 Cl7 2.328(3) .
Zn5 Cl9 2.313(3) 4_557
Zn5 Cl10 2.511(3) 1_565
Zn5 Cl12 2.740(3) .
Zn5 Cl16 2.216(3) .
Zn6 Cl12 2.219(3) .
Zn6 Cl13 2.319(3) .
Zn6 Cl14 2.511(3) .
Zn6 Cl16 2.730(3) .
Zn6 Cl19 2.304(3) 4_556
Cl8 Zn4 2.302(3) 2_657
Cl9 Zn5 2.313(3) 4_547
Cl10 Zn5 2.511(3) 1_545
Cl11 Zn2 2.290(2) 4_556
Cl15 Zn1 2.289(3) 2_556
Cl18 Zn4 2.269(3) 4_547
Cl19 Zn6 2.304(3) 4_546
Cl20 Zn1 2.272(3) 1_545
C2AA N 1.4200 .
C2AA C5 1.4200 .
N C3 1.4200 .
N C0AA 1.378(11) .
C3 N2 1.4200 .
N2 C5 1.4200 .
N2 C 1.376(9) .
C1AA C0AA 1.457(13) .
