#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:50:15 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179157 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/18/4311833.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_4311833
loop_
_publ_author_name
'Belli Dell'Amico, Daniela'
'Fausto Calderazzo'
'Matteo Curiardi'
'Luca Labella'
'Fabio Marchetti'
_publ_contact_author
;
      Belli Dell Amico, Daniela 
      Dipartimento di Chimica e Chimica Industriale
      Università di Pisa
      Via Risorgimento,  35
      56126  Pisa
      Italy
;
_publ_contact_author_email       belli@dcci.unipi.it
_publ_contact_author_fax         39()0502219246
_publ_contact_author_phone       39()0502219206
_publ_section_title
;
 Bis-qtpy (qtpy = 2,2':6',2'':6'',2'''-quaterpyridine) Metal Complexes,
 [M(qtpy)₂]²⁺
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5459
_journal_page_last               5465
_journal_paper_doi               10.1021/ic049595f
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[C40 H28 N8 Zn][Cl O4]2[H2 O]4'
_chemical_formula_sum            'C40 H36 Cl2 N8 O12 Zn'
_chemical_formula_weight         957.04
_chemical_name_systematic
;
bis-(2,2':6',2'':6'',2'''-quaterpyridine)-zinc diperchlorate tetraihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.233(6)
_cell_length_b                   8.0247(3)
_cell_length_c                   22.856(4)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.897
_cell_measurement_theta_min      2.665
_cell_volume                     4238.0(14)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Ital Structures XCS'
_computing_data_reduction        Darx2000
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'WINGX-1.64 (Farrugia, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.612
_diffrn_measured_fraction_theta_max 0.612
_diffrn_measurement_device_type  'Ital Structures'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0105
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3357
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         2.15
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.88680
_exptl_absorpt_correction_T_min  0.77781
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.822
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0006(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         2513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.440
_refine_ls_shift/su_mean         0.055
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1449P)²+9.5428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2012
_refine_ls_wR_factor_ref         0.2069
_reflns_number_gt                2377
_reflns_number_total             2513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049595fsi20040326_074308_3.cif
_cod_data_source_block           znqtp
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4238.0(13)
_cod_database_code               4311833
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.0000 -0.05167(13) 0.2500 0.0565(4) Uani 1 2 d S . .
N1 N 0.0410(2) -0.2161(6) 0.3261(2) 0.0650(13) Uani 1 1 d . . .
C1 C 0.0144(3) -0.2928(9) 0.3620(3) 0.078(2) Uani 1 1 d . . .
H1 H -0.0258 -0.2958 0.3504 0.094 Uiso 1 1 calc R . .
C2 C 0.0464(5) -0.3687(10) 0.4169(4) 0.095(2) Uani 1 1 d . . .
H2 H 0.0276 -0.4208 0.4418 0.114 Uiso 1 1 calc R . .
C3 C 0.1049(4) -0.3659(11) 0.4335(4) 0.096(3) Uani 1 1 d . . .
H3 H 0.1267 -0.4165 0.4697 0.116 Uiso 1 1 calc R . .
C4 C 0.1316(3) -0.2878(10) 0.3963(3) 0.088(2) Uani 1 1 d . . .
H4 H 0.1718 -0.2846 0.4072 0.105 Uiso 1 1 calc R . .
C5 C 0.0984(3) -0.2126(8) 0.3418(3) 0.0668(17) Uani 1 1 d . . .
N2 N 0.0850(2) -0.0549(6) 0.2508(2) 0.0583(12) Uani 1 1 d . . .
C6 C 0.1238(3) -0.1289(9) 0.2985(3) 0.0668(16) Uani 1 1 d . . .
C7 C 0.1817(3) -0.1231(11) 0.3037(4) 0.088(2) Uani 1 1 d . . .
H7 H 0.2086 -0.1740 0.3367 0.106 Uiso 1 1 calc R . .
C8 C 0.1995(3) -0.0405(12) 0.2593(4) 0.100(3) Uani 1 1 d . . .
H8 H 0.2387 -0.0327 0.2630 0.120 Uiso 1 1 calc R . .
C9 C 0.1600(3) 0.0282(10) 0.2109(4) 0.086(2) Uani 1 1 d . . .
H9 H 0.1715 0.0805 0.1801 0.103 Uiso 1 1 calc R . .
C10 C 0.1018(3) 0.0201(8) 0.2072(3) 0.0638(16) Uani 1 1 d . . .
N3 N 0.0046(2) 0.1272(6) 0.1695(2) 0.0583(12) Uani 1 1 d . . .
C11 C 0.0544(3) 0.0911(8) 0.1562(3) 0.0633(16) Uani 1 1 d . . .
C12 C 0.0605(4) 0.1114(9) 0.0989(3) 0.082(2) Uani 1 1 d . . .
H12 H 0.0954 0.0875 0.0916 0.099 Uiso 1 1 calc R . .
C13 C 0.0135(4) 0.1682(10) 0.0523(3) 0.095(3) Uani 1 1 d . . .
H13 H 0.0161 0.1803 0.0127 0.114 Uiso 1 1 calc R . .
C14 C -0.0365(4) 0.2064(10) 0.0647(3) 0.086(2) Uani 1 1 d . . .
H14 H -0.0683 0.2449 0.0335 0.103 Uiso 1 1 calc R . .
C15 C -0.0400(3) 0.1875(8) 0.1246(3) 0.0683(17) Uani 1 1 d . . .
N4 N -0.1429(3) 0.2152(9) 0.0953(3) 0.099(2) Uani 1 1 d . . .
C16 C -0.0924(3) 0.2430(9) 0.1397(3) 0.0741(19) Uani 1 1 d . . .
C17 C -0.0876(4) 0.3213(9) 0.1939(3) 0.081(2) Uani 1 1 d . . .
H17 H -0.0519 0.3373 0.2232 0.098 Uiso 1 1 calc R . .
C18 C -0.1395(5) 0.3771(12) 0.2034(4) 0.108(3) Uani 1 1 d . . .
H18 H -0.1394 0.4312 0.2394 0.130 Uiso 1 1 calc R . .
C19 C -0.1898(4) 0.3485(15) 0.1577(6) 0.119(3) Uani 1 1 d . . .
H19 H -0.2247 0.3839 0.1626 0.143 Uiso 1 1 calc R . .
C20 C -0.1898(4) 0.2696(16) 0.1055(5) 0.128(4) Uani 1 1 d . . .
H20 H -0.2250 0.2532 0.0754 0.154 Uiso 1 1 calc R . .
ClA Cl 0.13660(14) 0.5812(5) 0.11096(14) 0.0647(12) Uani 0.572(8) 1 d PG A 1
O1A O 0.0831(4) 0.5007(18) 0.0642(6) 0.207(3) Uiso 0.572(8) 1 d PG A 1
O2A O 0.1772(4) 0.5540(18) 0.0816(6) 0.207(3) Uiso 0.572(8) 1 d PG A 1
O3A O 0.1184(6) 0.7575(7) 0.0998(7) 0.207(3) Uiso 0.572(8) 1 d PG A 1
O4A O 0.1408(5) 0.5384(15) 0.1628(2) 0.207(3) Uiso 0.572(8) 1 d PG A 1
ClB Cl 0.1411(8) 0.582(3) 0.1160(9) 0.290(12) Uani 0.428(8) 1 d P A 2
O1B O 0.1238(10) 0.626(3) 0.1732(9) 0.207(3) Uiso 0.428(8) 1 d PG A 2
O2B O 0.1587(10) 0.423(2) 0.1277(12) 0.207(3) Uiso 0.428(8) 1 d PG A 2
O3B O 0.0877(8) 0.593(3) 0.0693(9) 0.207(3) Uiso 0.428(8) 1 d PG A 2
O4B O 0.1770(9) 0.694(3) 0.1094(11) 0.207(3) Uiso 0.428(8) 1 d PG A 2
O1W O 0.1679(5) -0.0520(13) 0.0239(5) 0.220(5) Uani 1 1 d G . .
H1W H 0.1952 0.1086 0.0615 0.286 Uiso 1 1 d G . .
H2W H 0.1888 0.3040 0.0892 0.286 Uiso 1 1 d G . .
O2W O 0.2193(4) 0.2138(16) 0.0771(8) 0.320(10) Uani 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'
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
_geom_angle_publ_flag
N2 Zn N2 178.6(3) . 2 ?
N2 Zn N1 102.47(19) . 2 ?
N2 Zn N1 76.6(2) 2 2 ?
N2 Zn N1 76.6(2) . . ?
N2 Zn N1 102.47(19) 2 . ?
N1 Zn N1 105.1(3) 2 . ?
N2 Zn N3 74.46(18) . . ?
N2 Zn N3 106.45(18) 2 . ?
N1 Zn N3 82.13(18) 2 . ?
N1 Zn N3 151.08(19) . . ?
N2 Zn N3 106.45(18) . 2 ?
N2 Zn N3 74.46(18) 2 2 ?
N1 Zn N3 151.08(19) 2 2 ?
N1 Zn N3 82.13(18) . 2 ?
N3 Zn N3 105.2(2) . 2 ?
C5 N1 C1 120.3(6) . . ?
C5 N1 Zn 113.1(4) . . ?
C1 N1 Zn 125.6(5) . . ?
N1 C1 C2 120.7(8) . . ?
N1 C1 H1 119.6 . . ?
C2 C1 H1 119.7 . . ?
C3 C2 C1 119.6(8) . . ?
C3 C2 H2 120.2 . . ?
C1 C2 H2 120.1 . . ?
C2 C3 C4 119.1(7) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.5 . . ?
C3 C4 C5 119.9(8) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
N1 C5 C4 120.4(7) . . ?
N1 C5 C6 116.3(5) . . ?
C4 C5 C6 123.3(7) . . ?
C10 N2 C6 120.7(5) . . ?
C10 N2 Zn 121.3(4) . . ?
C6 N2 Zn 117.9(4) . . ?
N2 C6 C7 120.2(7) . . ?
N2 C6 C5 114.4(5) . . ?
C7 C6 C5 125.4(6) . . ?
C8 C7 C6 119.3(7) . . ?
C8 C7 H7 120.3 . . ?
C6 C7 H7 120.4 . . ?
C9 C8 C7 119.8(7) . . ?
C9 C8 H8 120.0 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.3(7) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 120.7(7) . . ?
N2 C10 C11 115.2(5) . . ?
C9 C10 C11 124.1(6) . . ?
C15 N3 C11 118.2(5) . . ?
C15 N3 Zn 126.9(4) . . ?
C11 N3 Zn 107.3(4) . . ?
N3 C11 C12 123.0(6) . . ?
N3 C11 C10 115.7(5) . . ?
C12 C11 C10 121.2(6) . . ?
C11 C12 C13 118.5(7) . . ?
C11 C12 H12 120.8 . . ?
C13 C12 H12 120.7 . . ?
C14 C13 C12 119.5(7) . . ?
C14 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C13 C14 C15 119.9(7) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
N3 C15 C14 120.9(7) . . ?
N3 C15 C16 118.8(5) . . ?
C14 C15 C16 120.2(6) . . ?
C20 N4 C16 116.9(8) . . ?
N4 C16 C17 124.6(7) . . ?
N4 C16 C15 114.9(7) . . ?
C17 C16 C15 120.5(6) . . ?
C16 C17 C18 116.8(8) . . ?
C16 C17 H17 121.6 . . ?
C18 C17 H17 121.6 . . ?
C19 C18 C17 117.4(9) . . ?
C19 C18 H18 121.2 . . ?
C17 C18 H18 121.3 . . ?
C20 C19 C18 121.1(9) . . ?
C20 C19 H19 119.4 . . ?
C18 C19 H19 119.4 . . ?
N4 C20 C19 123.2(10) . . ?
N4 C20 H20 118.4 . . ?
C19 C20 H20 118.4 . . ?
O4A ClA O2A 125.2 . . ?
O4A ClA O3A 111.9 . . ?
O2A ClA O3A 106.8 . . ?
O4A ClA O1A 111.3 . . ?
O2A ClA O1A 99.9 . . ?
O3A ClA O1A 97.8 . . ?
O3B ClB O4B 111.7(15) . . ?
O3B ClB O2B 112(2) . . ?
O4B ClB O2B 119.9(17) . . ?
O3B ClB O1B 102.0(14) . . ?
O4B ClB O1B 108.0(19) . . ?
O2B ClB O1B 101.4(13) . . ?
H1W O2W H2W 105.5 . . ?
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
Zn N2 2.054(5) . ?
Zn N2 2.054(5) 2 ?
Zn N1 2.171(5) 2 ?
Zn N1 2.171(5) . ?
Zn N3 2.364(5) . ?
Zn N3 2.364(5) 2 ?
N1 C5 1.326(8) . ?
N1 C1 1.337(8) . ?
C1 C2 1.401(10) . ?
C1 H1 0.9300 . ?
C2 C3 1.352(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.365(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.400(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.475(9) . ?
N2 C10 1.330(8) . ?
N2 C6 1.343(8) . ?
C6 C7 1.372(9) . ?
C7 C8 1.386(12) . ?
C7 H7 0.9300 . ?
C8 C9 1.345(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.389(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.481(9) . ?
N3 C15 1.336(8) . ?
N3 C11 1.361(8) . ?
C11 C12 1.369(9) . ?
C12 C13 1.381(11) . ?
C12 H12 0.9300 . ?
C13 C14 1.359(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.407(9) . ?
C14 H14 0.9300 . ?
C15 C16 1.481(9) . ?
N4 C20 1.302(12) . ?
N4 C16 1.353(9) . ?
C16 C17 1.362(10) . ?
C17 C18 1.412(11) . ?
C17 H17 0.9300 . ?
C18 C19 1.364(14) . ?
C18 H18 0.9300 . ?
C19 C20 1.350(14) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
ClA O4A 1.2082 . ?
ClA O2A 1.3644 . ?
ClA O3A 1.4812 . ?
ClA O1A 1.5504 . ?
ClB O3B 1.41(2) . ?
ClB O4B 1.29(2) . ?
ClB O2B 1.35(2) . ?
ClB O1B 1.53(2) . ?
O2W H1W 1.0269 . ?
O2W H2W 1.1262 . ?
