#------------------------------------------------------------------------------
#$Date: 2017-03-02 19:20:33 +0200 (Thu, 02 Mar 2017) $
#$Revision: 192782 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/17/4311712.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_4311712
loop_
_publ_author_name
'Carla Bazzicalupi'
'Andrea Bencini'
'Emanuela Berni'
'Antonio Bianchi'
'Patrizia Fornasari'
'Claudia Giorgi'
'Barbara Valtancoli'
_publ_contact_author_address
;
Department of Chemistry,
POlo Scientifico,
University of Florence
via della Lastruccia 3
I-50019 Sesto Fiorentino, Firenze, Italy
;
_publ_contact_author_email       andrea.bencini@unifi.it
_publ_contact_author_name        'Dr. Andrea Bencini'
_publ_section_title
;
 Zn(II) Coordination to Polyamine Macrocycles Containing Dipyridine Units.
 New Insights into the Activity of Dinuclear Zn(II) Complexes in Phosphate
 Ester Hydrolysis
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6255
_journal_page_last               6265
_journal_paper_doi               10.1021/ic049754v
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety
;
(C18 H23 N6 S Zn +), (Cl O4 -)
;
_chemical_formula_sum            'C18 H23 Cl N6 O4 S Zn'
_chemical_formula_weight         520.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 116.63(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.601(3)
_cell_length_b                   10.808(3)
_cell_length_c                   15.685(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      12
_cell_measurement_theta_min      5
_cell_volume                     2212.6(10)
_computing_cell_refinement       'ENRAF NONIUS CAD4'
_computing_data_collection       'ENRAF NONIUS CAD4'
_computing_data_reduction        'ENRAF NONIUS CAD4'
_computing_molecular_graphics    'ORTEP3 Ver. 1.01β (Farrugia, 1997)'
_computing_publication_material  'PARST93 (Nardelli, 1993)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97(Altomare, 1999)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ENRAF NONIUS CAD4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0941
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4030
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.56
_diffrn_standards_interval_count 200
_exptl_absorpt_coefficient_mu    1.363
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1126
_refine_ls_R_factor_gt           0.0612
_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)+(0.1061P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1844
_reflns_number_gt                2520
_reflns_number_total             3882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049754vsi20040225_015926_1.cif
_cod_data_source_block           '[ZnL1(NCS)]ClO4'
_cod_depositor_comments
;
The following automatic conversions were performed:
data name '_publ_contact_author_adress' replaced with
'_publ_contact_author_address' as specified in the replacement file
'/home/antanas/src/cod-tools/trunk/data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 4998 2017-03-02 13:24:31Z antanas 
;
_cod_original_cell_volume        2212.6(9)
_cod_database_code               4311712
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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 0.58471(5) 0.33745(6) 0.32264(5) 0.0388(2) Uani 1 1 d . . .
N1 N 0.4452(4) 0.3635(4) 0.3389(3) 0.0410(11) Uani 1 1 d . . .
N2 N 0.5901(4) 0.5221(4) 0.3760(3) 0.0418(11) Uani 1 1 d . . .
C1 C 0.6726(5) 0.5928(6) 0.3977(4) 0.0489(15) Uani 1 1 d . . .
C2 C 0.6733(6) 0.7150(7) 0.4244(5) 0.0646(19) Uani 1 1 d . . .
H2 H 0.7315 0.7635 0.4411 0.081(10) Uiso 1 1 calc R . .
C3 C 0.5879(7) 0.7634(7) 0.4259(5) 0.068(2) Uani 1 1 d . . .
H3 H 0.5869 0.8464 0.4411 0.081(10) Uiso 1 1 calc R . .
C4 C 0.5029(6) 0.6903(6) 0.4052(5) 0.0600(18) Uani 1 1 d . . .
H4 H 0.4454 0.7222 0.4084 0.081(10) Uiso 1 1 calc R . .
C5 C 0.5057(5) 0.5675(6) 0.3792(4) 0.0444(14) Uani 1 1 d . . .
C6 C 0.4246(4) 0.4757(6) 0.3608(4) 0.0429(14) Uani 1 1 d . . .
C7 C 0.3356(5) 0.4965(7) 0.3705(5) 0.0563(17) Uani 1 1 d . . .
H7 H 0.3213 0.5745 0.3865 0.081(10) Uiso 1 1 calc R . .
C8 C 0.2698(5) 0.4005(8) 0.3561(5) 0.065(2) Uani 1 1 d . . .
H8 H 0.2099 0.4135 0.3619 0.081(10) Uiso 1 1 calc R . .
C9 C 0.2911(5) 0.2840(7) 0.3330(4) 0.0568(17) Uani 1 1 d . . .
H9 H 0.2459 0.2185 0.3221 0.081(10) Uiso 1 1 calc R . .
C10 C 0.3815(4) 0.2681(6) 0.3267(4) 0.0464(15) Uani 1 1 d . . .
C11 C 0.4189(5) 0.1447(6) 0.3108(5) 0.0524(16) Uani 1 1 d . . .
H11A H 0.4592 0.1046 0.3716 0.076(6) Uiso 1 1 calc R . .
H11B H 0.3609 0.0920 0.2733 0.076(6) Uiso 1 1 calc R . .
N5 N 0.4821(4) 0.1631(5) 0.2601(4) 0.0487(12) Uani 1 1 d . . .
H3A H 0.5224 0.0955 0.2684 0.076(6) Uiso 1 1 calc R . .
C12 C 0.4209(6) 0.1864(6) 0.1587(5) 0.0567(17) Uani 1 1 d . . .
H12A H 0.3667 0.2448 0.1489 0.076(6) Uiso 1 1 calc R . .
H12B H 0.3900 0.1100 0.1260 0.076(6) Uiso 1 1 calc R . .
C13 C 0.4908(6) 0.2386(7) 0.1200(5) 0.0632(19) Uani 1 1 d . . .
H13A H 0.5429 0.1779 0.1276 0.076(6) Uiso 1 1 calc R . .
H13B H 0.4513 0.2551 0.0523 0.076(6) Uiso 1 1 calc R . .
N4 N 0.5404(4) 0.3533(5) 0.1693(4) 0.0481(12) Uani 1 1 d . . .
C14 C 0.4688(5) 0.4589(6) 0.1310(5) 0.0597(18) Uani 1 1 d . . .
H14A H 0.5018 0.5332 0.1640 0.076(6) Uiso 1 1 calc R . .
H14B H 0.4089 0.4438 0.1399 0.076(6) Uiso 1 1 calc R . .
H14C H 0.4493 0.4682 0.0642 0.076(6) Uiso 1 1 calc R . .
C15 C 0.6355(6) 0.3782(7) 0.1598(6) 0.067(2) Uani 1 1 d . . .
H15A H 0.6175 0.4080 0.0959 0.076(6) Uiso 1 1 calc R . .
H15B H 0.6736 0.3017 0.1689 0.076(6) Uiso 1 1 calc R . .
C16 C 0.7023(5) 0.4723(7) 0.2310(5) 0.0604(19) Uani 1 1 d . . .
H16A H 0.7644 0.4855 0.2241 0.076(6) Uiso 1 1 calc R . .
H16B H 0.6663 0.5505 0.2208 0.076(6) Uiso 1 1 calc R . .
N3 N 0.7278(4) 0.4251(5) 0.3266(4) 0.0511(13) Uani 1 1 d . . .
H5 H 0.7780 0.3670 0.3430 0.076(6) Uiso 1 1 calc R . .
C17 C 0.7619(5) 0.5242(7) 0.3979(5) 0.0607(18) Uani 1 1 d . . .
H17A H 0.8049 0.5815 0.3845 0.076(6) Uiso 1 1 calc R . .
H17B H 0.8025 0.4891 0.4606 0.076(6) Uiso 1 1 calc R . .
N6 N 0.6699(4) 0.2365(6) 0.4415(4) 0.0624(16) Uani 1 1 d . . .
C18 C 0.6766(4) 0.1654(6) 0.4986(4) 0.0432(14) Uani 1 1 d . . .
S1 S 0.68448(16) 0.06865(19) 0.57985(14) 0.0704(6) Uani 1 1 d . . .
Cl1 Cl 0.98982(12) 0.33032(15) 0.35466(13) 0.0544(4) Uani 1 1 d . . .
O1A O 1.052(3) 0.372(4) 0.4410(14) 0.248(19) Uani 0.50 1 d P . .
O2A O 0.9157(17) 0.253(2) 0.3604(10) 0.063(4) Uani 0.50 1 d P . .
O3A O 0.955(3) 0.427(3) 0.294(3) 0.219(19) Uani 0.50 1 d P . .
O4A O 1.0453(14) 0.2563(13) 0.3193(18) 0.124(6) Uani 0.50 1 d P . .
O1B O 0.9800(11) 0.4312(12) 0.4111(13) 0.085(4) Uani 0.50 1 d P . .
O2B O 0.990(2) 0.387(2) 0.2770(12) 0.135(13) Uani 0.50 1 d P . .
O3B O 1.0794(9) 0.2674(13) 0.4148(14) 0.101(5) Uani 0.50 1 d P . .
O4B O 0.8963(17) 0.259(2) 0.3160(10) 0.064(5) Uani 0.50 1 d P . .
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'
S S 0.1246 0.1234 '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'
O O 0.0106 0.0060 '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
N6 Zn N2 103.9(2) . . ?
N6 Zn N1 100.5(2) . . ?
N2 Zn N1 73.04(18) . . ?
N6 Zn N4 143.5(2) . . ?
N2 Zn N4 107.15(19) . . ?
N1 Zn N4 106.57(18) . . ?
N6 Zn N3 91.3(2) . . ?
N2 Zn N3 74.31(18) . . ?
N1 Zn N3 147.08(19) . . ?
N4 Zn N3 79.2(2) . . ?
N6 Zn N5 88.0(2) . . ?
N2 Zn N5 144.83(18) . . ?
N1 Zn N5 72.29(18) . . ?
N4 Zn N5 77.56(19) . . ?
N3 Zn N5 139.35(19) . . ?
C6 N1 C10 120.9(5) . . ?
C6 N1 Zn 118.6(4) . . ?
C10 N1 Zn 120.5(4) . . ?
C1 N2 C5 121.2(5) . . ?
C1 N2 Zn 120.1(4) . . ?
C5 N2 Zn 118.5(4) . . ?
N2 C1 C2 120.5(6) . . ?
N2 C1 C17 113.7(6) . . ?
C2 C1 C17 125.6(6) . . ?
C3 C2 C1 119.3(7) . . ?
C2 C3 C4 120.6(7) . . ?
C3 C4 C5 118.2(7) . . ?
N2 C5 C4 120.3(6) . . ?
N2 C5 C6 114.6(5) . . ?
C4 C5 C6 125.0(6) . . ?
N1 C6 C7 120.3(6) . . ?
N1 C6 C5 114.2(5) . . ?
C7 C6 C5 125.3(6) . . ?
C8 C7 C6 118.8(7) . . ?
C7 C8 C9 120.8(6) . . ?
C10 C9 C8 117.8(7) . . ?
N1 C10 C9 121.2(6) . . ?
N1 C10 C11 115.1(5) . . ?
C9 C10 C11 123.6(6) . . ?
N5 C11 C10 109.3(5) . . ?
C12 N5 C11 112.7(5) . . ?
C12 N5 Zn 106.5(4) . . ?
C11 N5 Zn 108.7(4) . . ?
N5 C12 C13 108.1(6) . . ?
N4 C13 C12 111.4(5) . . ?
C13 N4 C14 110.2(5) . . ?
C13 N4 C15 111.3(5) . . ?
C14 N4 C15 109.9(5) . . ?
C13 N4 Zn 110.1(4) . . ?
C14 N4 Zn 108.2(4) . . ?
C15 N4 Zn 107.1(4) . . ?
N4 C15 C16 111.8(6) . . ?
N3 C16 C15 108.0(5) . . ?
C16 N3 C17 111.7(5) . . ?
C16 N3 Zn 108.0(4) . . ?
C17 N3 Zn 108.6(4) . . ?
N3 C17 C1 111.3(5) . . ?
C18 N6 Zn 151.1(5) . . ?
N6 C18 S1 178.4(6) . . ?
O1A Cl1 O3A 109(2) . . ?
O1A Cl1 O2B 118.9(15) . . ?
O3A Cl1 O2B 35(2) . . ?
O1A Cl1 O3B 58.2(19) . . ?
O3A Cl1 O3B 142.8(18) . . ?
O2B Cl1 O3B 116.2(15) . . ?
O1A Cl1 O2A 109.4(13) . . ?
O3A Cl1 O2A 116.5(19) . . ?
O2B Cl1 O2A 129.6(12) . . ?
O3B Cl1 O2A 100.5(11) . . ?
O1A Cl1 O4A 110(2) . . ?
O3A Cl1 O4A 105.5(19) . . ?
O2B Cl1 O4A 70.8(14) . . ?
O3B Cl1 O4A 57.5(9) . . ?
O2A Cl1 O4A 106.4(12) . . ?
O1A Cl1 O4B 134.1(13) . . ?
O3A Cl1 O4B 97.4(19) . . ?
O2B Cl1 O4B 104.3(12) . . ?
O3B Cl1 O4B 116.5(11) . . ?
O2A Cl1 O4B 25.4(9) . . ?
O4A Cl1 O4B 97.7(13) . . ?
O1A Cl1 O1B 48(2) . . ?
O3A Cl1 O1B 74.7(17) . . ?
O2B Cl1 O1B 104.5(12) . . ?
O3B Cl1 O1B 105.8(9) . . ?
O2A Cl1 O1B 96.7(12) . . ?
O4A Cl1 O1B 153.3(9) . . ?
O4B Cl1 O1B 108.8(12) . . ?
O1B O1A Cl1 71.8(16) . . ?
O1B O1A O3B 134.7(18) . . ?
Cl1 O1A O3B 63.6(13) . . ?
O4B O2A Cl1 81(4) . . ?
O2B O3A Cl1 74(3) . . ?
O2B O3A O1B 120(4) . . ?
Cl1 O3A O1B 55.3(14) . . ?
O3B O4A Cl1 60.6(8) . . ?
O3B O4A O2B 104.2(12) . . ?
Cl1 O4A O2B 53.1(8) . . ?
O1A O1B Cl1 60.3(14) . . ?
O1A O1B O3A 98(2) . . ?
Cl1 O1B O3A 50.0(11) . . ?
O3A O2B Cl1 72(3) . . ?
O3A O2B O4A 128(3) . . ?
Cl1 O2B O4A 56.1(10) . . ?
O1A O3B O4A 113.9(19) . . ?
O1A O3B Cl1 58.2(12) . . ?
O4A O3B Cl1 61.9(8) . . ?
O2A O4B Cl1 74(4) . . ?
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 N6 2.033(5) . ?
Zn N2 2.152(5) . ?
Zn N1 2.182(5) . ?
Zn N4 2.200(5) . ?
Zn N3 2.270(5) . ?
Zn N5 2.332(5) . ?
N1 C6 1.331(8) . ?
N1 C10 1.343(8) . ?
N2 C1 1.335(8) . ?
N2 C5 1.348(7) . ?
C1 C2 1.383(10) . ?
C1 C17 1.499(9) . ?
C2 C3 1.362(11) . ?
C3 C4 1.381(10) . ?
C4 C5 1.394(9) . ?
C5 C6 1.471(9) . ?
C6 C7 1.393(8) . ?
C7 C8 1.361(10) . ?
C8 C9 1.384(11) . ?
C9 C10 1.378(8) . ?
C10 C11 1.503(9) . ?
C11 N5 1.476(8) . ?
N5 C12 1.455(8) . ?
C12 C13 1.511(10) . ?
C13 N4 1.469(8) . ?
N4 C14 1.481(8) . ?
N4 C15 1.487(9) . ?
C15 C16 1.502(10) . ?
C16 N3 1.464(8) . ?
N3 C17 1.465(9) . ?
N6 C18 1.151(7) . ?
C18 S1 1.612(6) . ?
Cl1 O1A 1.327(16) . ?
Cl1 O3A 1.35(3) . ?
Cl1 O2B 1.365(17) . ?
Cl1 O3B 1.399(11) . ?
Cl1 O2A 1.40(2) . ?
Cl1 O4A 1.417(13) . ?
Cl1 O4B 1.44(2) . ?
Cl1 O1B 1.451(14) . ?
O1A O1B 1.13(4) . ?
O1A O3B 1.33(4) . ?
O2A O4B 0.63(2) . ?
O3A O2B 0.81(5) . ?
O3A O1B 1.70(4) . ?
O4A O3B 1.36(2) . ?
O4A O2B 1.61(3) . ?
