#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/01/7050126.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_7050126
loop_
_publ_author_name
'Gudneppanavar Rajsekhar'
'Chebrolu P. Rao'
'Pauli Saarenketo'
'Kalle Nättinen'
'Kari Rissanen'
_publ_section_title
;
 Complexation behaviour of hexadentate ligands possessing N2O4 and
 N2O2S2 cores: differential reactivity towards Co(II), Ni(II) and
 Zn(II) salts and structures of the products
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              75
_journal_page_last               84
_journal_paper_doi               10.1039/b305313j
_journal_volume                  28
_journal_year                    2004
_chemical_formula_sum            'C15 H15 N O3 Zn0.5'
_chemical_formula_weight         289.96
_chemical_name_systematic
;
?
;
_space_group_IT_number           86
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      86
_symmetry_space_group_name_Hall  '-P 4bc'
_symmetry_space_group_name_H-M   'P 42/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            8
_cell_length_a                   13.925(2)
_cell_length_b                   13.925(2)
_cell_length_c                   14.181(3)
_cell_measurement_reflns_used    9053
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      2.91
_cell_volume                     2749.8(8)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       Collect
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    xp
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Rotation in phi and omega, 2 deg.'
_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  0.1048
_diffrn_reflns_av_sigmaI/netI    0.0539
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17541
_diffrn_reflns_theta_full        25.69
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    0.939
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blocks
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2496
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0382
_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)+(0.0218P)²+3.4869P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                1712
_reflns_number_total             2496
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305313j.txt
_cod_data_source_block           importtr_b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
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_sg_symbol_H-M      P4(2)/n
_cod_original_formula_sum        'C15 H15 N O3 Zn0.50'
_cod_database_code               7050126
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-y, x+1/2, z+1/2'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'y, -x-1/2, -z-1/2'
'-y-1/2, x, -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
C2 C 0.7382(2) 0.4353(2) 0.8265(2) 0.0195(7) Uani 1 1 d . . .
C3 C 0.7072(2) 0.5169(2) 0.8795(2) 0.0237(7) Uani 1 1 d . . .
H3 H 0.6500 0.5127 0.9157 0.028 Uiso 1 1 calc R . .
C4 C 0.7597(2) 0.6037(2) 0.8794(2) 0.0297(8) Uani 1 1 d . . .
H4 H 0.7376 0.6561 0.9163 0.036 Uiso 1 1 calc R . .
C5 C 0.8438(2) 0.6140(2) 0.8258(2) 0.0296(8) Uani 1 1 d . . .
H5 H 0.8772 0.6735 0.8240 0.036 Uiso 1 1 calc R . .
C6 C 0.8777(2) 0.5342(2) 0.7747(2) 0.0241(7) Uani 1 1 d . . .
H6 H 0.9351 0.5398 0.7389 0.029 Uiso 1 1 calc R . .
C7 C 0.8272(2) 0.4453(2) 0.77568(19) 0.0196(7) Uani 1 1 d . . .
C9 C 0.9477(2) 0.3482(2) 0.6979(2) 0.0210(7) Uani 1 1 d . . .
H9 H 0.9890 0.4024 0.7012 0.025 Uiso 1 1 calc R . .
C10 C 0.9869(2) 0.2581(2) 0.6575(2) 0.0198(7) Uani 1 1 d . . .
C11 C 1.0896(2) 0.2475(2) 0.6564(2) 0.0267(8) Uani 1 1 d . . .
H11 H 1.1287 0.3002 0.6748 0.032 Uiso 1 1 calc R . .
C12 C 1.1341(2) 0.1607(2) 0.6287(2) 0.0311(8) Uani 1 1 d . . .
H12 H 1.2021 0.1553 0.6287 0.037 Uiso 1 1 calc R . .
C13 C 1.0767(2) 0.0822(2) 0.6012(2) 0.0313(8) Uani 1 1 d . . .
H13 H 1.1062 0.0229 0.5850 0.038 Uiso 1 1 calc R . .
C14 C 0.9748(2) 0.0912(2) 0.5972(2) 0.0259(7) Uani 1 1 d . . .
H14 H 0.9363 0.0388 0.5768 0.031 Uiso 1 1 calc R . .
C15 C 0.9315(2) 0.1789(2) 0.6241(2) 0.0193(7) Uani 1 1 d . . .
C17 C 0.8043(2) 0.2406(2) 0.52943(19) 0.0228(7) Uani 1 1 d . . .
H17A H 0.8224 0.2030 0.4729 0.027 Uiso 1 1 calc R . .
H17B H 0.8397 0.3022 0.5279 0.027 Uiso 1 1 calc R . .
N8 N 0.85934(16) 0.35788(16) 0.72962(15) 0.0173(5) Uani 1 1 d . . .
O1 O 0.68708(14) 0.35210(14) 0.82546(14) 0.0203(5) Uani 1 1 d . . .
O16 O 0.82916(14) 0.18723(14) 0.61458(13) 0.0199(5) Uani 1 1 d . . .
Zn18 Zn 0.7500 0.2500 0.74539(3) 0.01659(13) Uani 1 2 d S . .
O19 O 0.8505(3) 0.50691(18) 0.3758(2) 0.0634(9) Uani 1 1 d D . .
H19 H 0.846(4) 0.4482(9) 0.363(4) 0.095 Uiso 1 1 d D . .
C20 C 0.8426(3) 0.5132(3) 0.4738(3) 0.0475(11) Uani 1 1 d . . .
H20A H 0.8964 0.4793 0.5033 0.071 Uiso 1 1 calc R . .
H20B H 0.7820 0.4839 0.4941 0.071 Uiso 1 1 calc R . .
H20C H 0.8437 0.5808 0.4929 0.071 Uiso 1 1 calc R . .
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'
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
O1 C2 C3 121.7(3) . . ?
O1 C2 C7 121.8(3) . . ?
C3 C2 C7 116.5(3) . . ?
C4 C3 C2 121.6(3) . . ?
C4 C3 H3 119.2 . . ?
C2 C3 H3 119.2 . . ?
C5 C4 C3 121.4(3) . . ?
C5 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C4 C5 C6 118.5(3) . . ?
C4 C5 H5 120.8 . . ?
C6 C5 H5 120.8 . . ?
C5 C6 C7 121.1(3) . . ?
C5 C6 H6 119.5 . . ?
C7 C6 H6 119.5 . . ?
C6 C7 C2 120.9(3) . . ?
C6 C7 N8 124.9(3) . . ?
C2 C7 N8 114.1(2) . . ?
N8 C9 C10 124.2(3) . . ?
N8 C9 H9 117.9 . . ?
C10 C9 H9 117.9 . . ?
C15 C10 C11 117.0(3) . . ?
C15 C10 C9 125.7(3) . . ?
C11 C10 C9 117.2(3) . . ?
C12 C11 C10 121.8(3) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C13 C12 C11 119.5(3) . . ?
C13 C12 H12 120.3 . . ?
C11 C12 H12 120.3 . . ?
C12 C13 C14 120.5(3) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
C15 C14 C13 119.3(3) . . ?
C15 C14 H14 120.4 . . ?
C13 C14 H14 120.4 . . ?
C14 C15 C10 121.8(3) . . ?
C14 C15 O16 117.9(3) . . ?
C10 C15 O16 120.3(2) . . ?
O16 C17 C17 108.72(19) . 2_655 ?
O16 C17 H17A 109.9 . . ?
C17 C17 H17A 109.9 2_655 . ?
O16 C17 H17B 109.9 . . ?
C17 C17 H17B 109.9 2_655 . ?
H17A C17 H17B 108.3 . . ?
C9 N8 C7 121.8(2) . . ?
C9 N8 Zn18 128.7(2) . . ?
C7 N8 Zn18 108.72(17) . . ?
C2 O1 Zn18 112.28(17) . . ?
C15 O16 C17 110.8(2) . . ?
C15 O16 Zn18 115.18(16) . . ?
C17 O16 Zn18 110.86(16) . . ?
O1 Zn18 O1 111.57(11) 2_655 . ?
O1 Zn18 N8 82.75(8) 2_655 2_655 ?
O1 Zn18 N8 104.07(8) . 2_655 ?
O1 Zn18 N8 104.07(8) 2_655 . ?
O1 Zn18 N8 82.75(8) . . ?
N8 Zn18 N8 168.06(12) 2_655 . ?
O1 Zn18 O16 88.75(8) 2_655 . ?
O1 Zn18 O16 156.60(7) . . ?
N8 Zn18 O16 89.43(8) 2_655 . ?
N8 Zn18 O16 81.04(8) . . ?
O1 Zn18 O16 156.60(7) 2_655 2_655 ?
O1 Zn18 O16 88.75(8) . 2_655 ?
N8 Zn18 O16 81.04(8) 2_655 2_655 ?
N8 Zn18 O16 89.43(8) . 2_655 ?
O16 Zn18 O16 74.35(10) . 2_655 ?
C20 O19 H19 106(4) . . ?
O19 C20 H20A 109.5 . . ?
O19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
O19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
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
C2 O1 1.360(3) . ?
C2 C3 1.429(4) . ?
C2 C7 1.441(4) . ?
C3 C4 1.411(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.404(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.408(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.423(4) . ?
C6 H6 0.9500 . ?
C7 N8 1.452(4) . ?
C9 N8 1.317(4) . ?
C9 C10 1.483(4) . ?
C9 H9 0.9500 . ?
C10 C15 1.427(4) . ?
C10 C11 1.439(4) . ?
C11 C12 1.414(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.408(5) . ?
C12 H12 0.9500 . ?
C13 C14 1.426(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.414(4) . ?
C14 H14 0.9500 . ?
C15 O16 1.436(3) . ?
C17 O16 1.459(3) . ?
C17 C17 1.535(6) 2_655 ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
N8 Zn18 2.151(2) . ?
O1 Zn18 2.0195(19) . ?
O16 Zn18 2.328(2) . ?
Zn18 O1 2.0195(19) 2_655 ?
Zn18 N8 2.151(2) 2_655 ?
Zn18 O16 2.328(2) 2_655 ?
O19 C20 1.397(5) . ?
O19 H19 0.840(3) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
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
C17 H17A O1 0.99 2.62 3.134(3) 112.2 4_564
O19 H19 O1 0.840(3) 1.959(8) 2.794(3) 173(5) 4_564
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C2 C3 C4 -179.1(3) . . . . ?
C7 C2 C3 C4 2.1(4) . . . . ?
C2 C3 C4 C5 1.1(5) . . . . ?
C3 C4 C5 C6 -2.7(5) . . . . ?
C4 C5 C6 C7 1.1(5) . . . . ?
C5 C6 C7 C2 2.2(4) . . . . ?
C5 C6 C7 N8 -176.4(3) . . . . ?
O1 C2 C7 C6 177.5(3) . . . . ?
C3 C2 C7 C6 -3.6(4) . . . . ?
O1 C2 C7 N8 -3.8(4) . . . . ?
C3 C2 C7 N8 175.0(2) . . . . ?
N8 C9 C10 C15 17.5(5) . . . . ?
N8 C9 C10 C11 -159.0(3) . . . . ?
C15 C10 C11 C12 -3.5(4) . . . . ?
C9 C10 C11 C12 173.2(3) . . . . ?
C10 C11 C12 C13 0.2(5) . . . . ?
C11 C12 C13 C14 2.6(5) . . . . ?
C12 C13 C14 C15 -1.9(5) . . . . ?
C13 C14 C15 C10 -1.7(4) . . . . ?
C13 C14 C15 O16 176.8(3) . . . . ?
C11 C10 C15 C14 4.3(4) . . . . ?
C9 C10 C15 C14 -172.2(3) . . . . ?
C11 C10 C15 O16 -174.1(3) . . . . ?
C9 C10 C15 O16 9.4(4) . . . . ?
C10 C9 N8 C7 174.8(3) . . . . ?
C10 C9 N8 Zn18 5.9(4) . . . . ?
C6 C7 N8 C9 13.5(4) . . . . ?
C2 C7 N8 C9 -165.1(3) . . . . ?
C6 C7 N8 Zn18 -175.6(2) . . . . ?
C2 C7 N8 Zn18 5.7(3) . . . . ?
C3 C2 O1 Zn18 -179.4(2) . . . . ?
C7 C2 O1 Zn18 -0.6(3) . . . . ?
C14 C15 O16 C17 -100.6(3) . . . . ?
C10 C15 O16 C17 77.9(3) . . . . ?
C14 C15 O16 Zn18 132.6(2) . . . . ?
C10 C15 O16 Zn18 -48.9(3) . . . . ?
C17 C17 O16 C15 -172.4(3) 2_655 . . . ?
C17 C17 O16 Zn18 -43.2(3) 2_655 . . . ?
C2 O1 Zn18 O1 105.34(18) . . . 2_655 ?
C2 O1 Zn18 N8 -167.00(18) . . . 2_655 ?
C2 O1 Zn18 N8 3.03(18) . . . . ?
C2 O1 Zn18 O16 -43.4(3) . . . . ?
C2 O1 Zn18 O16 -86.56(18) . . . 2_655 ?
C9 N8 Zn18 O1 54.7(2) . . . 2_655 ?
C7 N8 Zn18 O1 -115.32(17) . . . 2_655 ?
C9 N8 Zn18 O1 165.2(2) . . . . ?
C7 N8 Zn18 O1 -4.82(16) . . . . ?
C9 N8 Zn18 N8 -69.1(2) . . . 2_655 ?
C7 N8 Zn18 N8 120.86(16) . . . 2_655 ?
C9 N8 Zn18 O16 -31.8(2) . . . . ?
C7 N8 Zn18 O16 158.25(17) . . . . ?
C9 N8 Zn18 O16 -106.0(2) . . . 2_655 ?
C7 N8 Zn18 O16 84.00(17) . . . 2_655 ?
C15 O16 Zn18 O1 -54.05(18) . . . 2_655 ?
C17 O16 Zn18 O1 179.22(17) . . . 2_655 ?
C15 O16 Zn18 O1 97.1(2) . . . . ?
C17 O16 Zn18 O1 -29.6(3) . . . . ?
C15 O16 Zn18 N8 -136.81(18) . . . 2_655 ?
C17 O16 Zn18 N8 96.45(17) . . . 2_655 ?
C15 O16 Zn18 N8 50.40(17) . . . . ?
C17 O16 Zn18 N8 -76.33(17) . . . . ?
C15 O16 Zn18 O16 142.3(2) . . . 2_655 ?
C17 O16 Zn18 O16 15.60(14) . . . 2_655 ?
