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#$Date: 2016-03-26 02:12:40 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180128 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/26/7102683.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_7102683
loop_
_publ_author_name
'Turner, David R'
'Hursthouse, M B'
'Light, M E'
'Steed, Jonathan W'
_publ_section_title
;
 Linear distortion of octahedral metal centres by multiple hydrogen
 bonds in modular ML(4) systems.
;
_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1354
_journal_page_last               1355
_journal_paper_doi               10.1039/b402884h
_journal_year                    2004
_chemical_formula_sum            'C52 H60 N12 O14 S Zn'
_chemical_formula_weight         1174.55
_chemical_name_common            '[Zn(TUP)4(H2O)2]SO4.2H2O'
_chemical_name_systematic
;
[Zn(TUP)4(H2O)2]SO4.2H2O
;
_space_group_IT_number           85
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4a'
_symmetry_space_group_name_H-M   'P 4/n :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.0760(5)
_cell_length_b                   18.0760(5)
_cell_length_c                   8.1208(3)
_cell_measurement_temperature    120(2)
_cell_volume                     2653.41(14)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Hooft, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 0.71
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4860
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.582
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.665
_refine_diff_density_min         -1.012
_refine_diff_density_rms         0.107
_refine_ls_extinction_coef       0.0066(15)
_refine_ls_extinction_expression Fc^*^==kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0997
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          1.145
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[σ²(Fo²)+(0.0974P)²+0.0000P] where P==(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1639
_reflns_number_gt                2061
_reflns_number_total             3035
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b402884h.txt
_cod_data_source_block           C:\Dave\Structs\DTZn032\DTZN032.CIF
_cod_original_sg_symbol_H-M      P4/n
_cod_database_code               7102683
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/2, x, z'
'-x+1/2, -y+1/2, z'
'y, -x+1/2, z'
'-x, -y, -z'
'y-1/2, -x, -z'
'x-1/2, y-1/2, -z'
'-y, x-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 0.7500 0.7500 0.23992(8) 0.0130(2) Uani 1 4 d S . .
S2 S 0.7500 1.2500 0.5000 0.0146(4) Uani 1 4 d S . .
O2 O 0.7500 0.7500 -0.0295(5) 0.0181(9) Uani 1 4 d S . .
N3 N 0.81921(14) 1.07391(14) 0.7328(3) 0.0183(6) Uani 1 1 d . A .
H3 H 0.8125 1.1184 0.6913 0.022 Uiso 1 1 calc R . .
N2 N 0.77473(14) 1.03628(13) 0.4837(3) 0.0191(6) Uani 1 1 d . A .
H2 H 0.7738 1.0840 0.4619 0.023 Uiso 1 1 calc R . .
C3 C 0.70956(18) 1.01995(17) 0.2308(4) 0.0198(7) Uani 1 1 d . A .
H3A H 0.7024 1.0720 0.2262 0.024 Uiso 1 1 calc R . .
C9 C 0.86765(17) 1.13526(17) 1.1514(4) 0.0205(7) Uani 1 1 d . . .
H9 H 0.8599 1.1780 1.2173 0.025 Uiso 1 1 calc R . .
C5 C 0.76105(16) 0.91244(16) 0.3560(4) 0.0160(6) Uani 1 1 d . A .
H5 H 0.7903 0.8905 0.4401 0.019 Uiso 1 1 calc R . .
N1 N 0.73286(13) 0.86897(14) 0.2371(3) 0.0158(6) Uani 1 1 d . . .
C10 C 0.90971(18) 1.07740(18) 1.2139(4) 0.0225(7) Uani 1 1 d . . .
C1 C 0.69223(17) 0.90034(17) 0.1180(4) 0.0210(7) Uani 1 1 d . . .
H1 H 0.6703 0.8695 0.0367 0.025 Uiso 1 1 calc R . .
C7 C 0.84744(17) 1.07047(16) 0.8958(4) 0.0176(7) Uani 1 1 d . . .
C8 C 0.83663(16) 1.13220(16) 0.9955(4) 0.0189(7) Uani 1 1 d . . .
H8 H 0.8078 1.1725 0.9563 0.023 Uiso 1 1 calc R . .
C11 C 0.9173(2) 1.01504(19) 1.1147(4) 0.0271(8) Uani 1 1 d . . .
H11 H 0.9439 0.9737 1.1560 0.032 Uiso 1 1 calc R . .
O1 O 0.7500 0.7500 0.5026(5) 0.0173(9) Uani 1 4 d S . .
C6 C 0.8016(2) 1.01633(18) 0.6348(4) 0.0258(8) Uani 1 1 d . . .
C2 C 0.68104(19) 0.97545(18) 0.1091(4) 0.0247(8) Uani 1 1 d . . .
H2A H 0.6540 0.9963 0.0201 0.030 Uiso 1 1 calc R . .
C13 C 0.9467(2) 1.0822(2) 1.3785(4) 0.0322(9) Uani 1 1 d . . .
H13A H 0.9988 1.0958 1.3636 0.048 Uiso 1 1 calc R . .
H13B H 0.9437 1.0342 1.4339 0.048 Uiso 1 1 calc R . .
H13C H 0.9219 1.1198 1.4457 0.048 Uiso 1 1 calc R . .
C4 C 0.74866(16) 0.98909(16) 0.3600(4) 0.0161(7) Uani 1 1 d . . .
O3B O 0.8249(4) 0.9514(5) 0.6619(12) 0.032(2) Uani 0.50 1 d P A 2
C12 C 0.88745(19) 1.01115(18) 0.9574(4) 0.0262(8) Uani 1 1 d . . .
H12 H 0.8944 0.9681 0.8923 0.031 Uiso 1 1 calc R . .
O4 O 0.71956(12) 1.18968(12) 0.3977(3) 0.0249(6) Uani 1 1 d . . .
O5 O 0.8433(3) 0.8075(2) 0.7335(5) 0.0876(13) Uani 1 1 d . . .
O3A O 0.7930(4) 0.9517(5) 0.6904(11) 0.0224(16) Uani 0.50 1 d P A 1
H2O H 0.7603 0.7090 -0.0971 0.24(10) Uiso 0.50 1 d PR . .
H1O H 0.7592 0.7045 0.5867 2(2) Uiso 0.50 1 d PR . .
H5A H 0.8495 0.8814 0.7285 0.20(8) Uiso 0.50 1 d PR . .
H5B H 0.9161 0.7973 0.6896 0.06(2) Uiso 0.50 1 d PR . .
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'
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'
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
O1 Zn1 N1 90.61(7) . 2_655
O1 Zn1 N1 90.61(6) . .
N1 Zn1 N1 89.994(2) 2_655 .
O1 Zn1 N1 90.61(6) . 3_665
N1 Zn1 N1 89.994(2) 2_655 3_665
N1 Zn1 N1 178.79(13) . 3_665
O1 Zn1 N1 90.61(7) . 4_565
N1 Zn1 N1 178.79(13) 2_655 4_565
N1 Zn1 N1 89.994(2) . 4_565
N1 Zn1 N1 89.994(2) 3_665 4_565
O1 Zn1 O2 180.000(2) . .
N1 Zn1 O2 89.39(6) 2_655 .
N1 Zn1 O2 89.39(6) . .
N1 Zn1 O2 89.39(6) 3_665 .
N1 Zn1 O2 89.39(6) 4_565 .
O4 S2 O4 108.44(9) . 6_576
O4 S2 O4 108.44(9) . 8_766
O4 S2 O4 111.54(18) 6_576 8_766
O4 S2 O4 111.54(18) . 3_675
O4 S2 O4 108.44(9) 6_576 3_675
O4 S2 O4 108.44(9) 8_766 3_675
C6 N3 C7 127.0(3) . .
C6 N2 C4 127.1(3) . .
C2 C3 C4 120.1(3) . .
C8 C9 C10 121.7(3) . .
N1 C5 C4 122.2(3) . .
C1 N1 C5 118.6(3) . .
C1 N1 Zn1 120.3(2) . .
C5 N1 Zn1 121.10(19) . .
C9 C10 C11 116.9(3) . .
C9 C10 C13 121.8(3) . .
C11 C10 C13 121.3(3) . .
N1 C1 C2 122.4(3) . .
C12 C7 C8 118.9(3) . .
C12 C7 N3 123.9(3) . .
C8 C7 N3 117.2(3) . .
C9 C8 C7 120.4(3) . .
C12 C11 C10 122.3(3) . .
O3A C6 O3B 28.5(4) . .
O3A C6 N3 122.2(5) . .
O3B C6 N3 122.3(5) . .
O3A C6 N2 121.4(5) . .
O3B C6 N2 121.2(5) . .
N3 C6 N2 114.2(3) . .
C3 C2 C1 119.0(3) . .
C3 C4 N2 118.1(3) . .
C3 C4 C5 117.5(3) . .
N2 C4 C5 124.4(3) . .
C7 C12 C11 119.7(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.133(4) .
Zn1 N1 2.173(2) 2_655
Zn1 N1 2.173(2) .
Zn1 N1 2.173(2) 3_665
Zn1 N1 2.173(2) 4_565
Zn1 O2 2.188(4) .
S2 O4 1.477(2) .
S2 O4 1.477(2) 6_576
S2 O4 1.477(2) 8_766
S2 O4 1.477(2) 3_675
N3 C6 1.348(4) .
N3 C7 1.420(4) .
N2 C6 1.368(4) .
N2 C4 1.400(4) .
C3 C2 1.375(4) .
C3 C4 1.382(4) .
C9 C8 1.386(4) .
C9 C10 1.389(5) .
C5 N1 1.345(4) .
C5 C4 1.404(4) .
N1 C1 1.340(4) .
C10 C11 1.392(4) .
C10 C13 1.497(4) .
C1 C2 1.374(4) .
C7 C12 1.387(4) .
C7 C8 1.392(4) .
C11 C12 1.389(5) .
C6 O3A 1.262(10) .
C6 O3B 1.267(10) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N3 H3 O4 0.88 1.97 2.842(3) 173.2 8_766
N2 H2 O4 0.88 2.21 3.028(3) 154.6 .
O2 H2O O5 0.94 1.87 2.762(5) 156.3 4_564
O1 H1O O5 1.08 1.71 2.728(5) 154.4 4_565
O5 H5A O3B 1.34 1.45 2.686(11) 149.0 .
O5 H5A O3A 1.34 1.66 2.782(11) 135.8 .
O5 H5B O3A 1.38 1.75 2.694(9) 118.3 4_565
O5 H5B O3B 1.38 2.31 3.144(10) 114.7 4_565
