#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:20:46 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179242 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/62/4316291.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_4316291
loop_
_publ_author_name
'Guo-Bi Li'
'Hua-Cai Fang'
'Yue-Peng Cai'
'Zheng-Yuan Zhou'
'Praveen K. Thallapally'
'Jian Tian'
_publ_section_title
;
 Construction of a Novel Zn-Ni Trinuclear Schiff Base and a Ni2+
 Chemosensor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7241
_journal_page_last               7243
_journal_paper_doi               10.1021/ic101036m
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C30 H46 N8 O4 S2 Zn'
_chemical_formula_sum            'C30 H46 N8 O4 S2 Zn'
_chemical_formula_weight         712.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.2010(10)
_cell_angle_beta                 77.5160(10)
_cell_angle_gamma                77.0600(10)
_cell_formula_units_Z            1
_cell_length_a                   8.61180(10)
_cell_length_b                   10.48970(10)
_cell_length_c                   10.74850(10)
_cell_measurement_reflns_used    3311
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.45
_cell_measurement_theta_min      2.47
_cell_volume                     918.341(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11498
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.8861
_exptl_absorpt_correction_T_min  0.8017
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'green yellow'
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.368
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         4158
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0772
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0545P)²+5.0765P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2017
_refine_ls_wR_factor_ref         0.2076
_reflns_number_gt                3579
_reflns_number_total             4158
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101036m_si_002.cif
_cod_data_source_block           c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        918.341(16)
_cod_database_code               4316291
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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 0.5000 0.5000 0.5000 0.0434(3) Uani 1 2 d S . .
S1 S 0.98478(18) 0.22556(18) 0.26359(16) 0.0634(5) Uani 1 1 d . . .
O1 O 0.4061(4) 0.5547(3) 0.3190(3) 0.0368(7) Uani 1 1 d . . .
O2 O 0.6270(4) 0.6646(3) 0.4356(3) 0.0415(8) Uani 1 1 d . . .
N1 N 0.5416(5) 0.6453(4) 0.0870(3) 0.0371(9) Uani 1 1 d D . .
H1 H 0.558(7) 0.596(5) 0.155(3) 0.052(16) Uiso 1 1 d D . .
N2 N 0.7868(5) 0.7038(4) 0.2007(4) 0.0400(9) Uani 1 1 d D . .
H2 H 0.737(5) 0.652(4) 0.257(4) 0.034(13) Uiso 1 1 d D . .
N3 N 0.7102(5) 0.3850(4) 0.3885(4) 0.0466(10) Uani 1 1 d . . .
N4 N 0.6399(12) 1.0347(8) -0.1508(7) 0.121(3) Uani 1 1 d DU . .
C1 C 0.1298(6) 0.5327(6) 0.3609(5) 0.0490(13) Uani 1 1 d . . .
H1A H 0.1129 0.5719 0.4391 0.073 Uiso 1 1 calc R . .
H1B H 0.1428 0.4389 0.3799 0.073 Uiso 1 1 calc R . .
H1C H 0.0378 0.5660 0.3200 0.073 Uiso 1 1 calc R . .
C2 C 0.2795(5) 0.5660(4) 0.2731(4) 0.0315(9) Uani 1 1 d . . .
C3 C 0.2733(5) 0.6118(5) 0.1446(4) 0.0379(10) Uani 1 1 d . . .
H3 H 0.1776 0.6146 0.1164 0.046 Uiso 1 1 calc R . .
C4 C 0.4008(6) 0.6533(5) 0.0562(4) 0.0373(10) Uani 1 1 d . . .
C5 C 0.3781(7) 0.7101(7) -0.0763(5) 0.0579(15) Uani 1 1 d . . .
H5A H 0.4511 0.6559 -0.1371 0.087 Uiso 1 1 calc R . .
H5B H 0.4004 0.7974 -0.0927 0.087 Uiso 1 1 calc R . .
H5C H 0.2683 0.7134 -0.0841 0.087 Uiso 1 1 calc R . .
C6 C 0.6767(6) 0.7000(6) 0.0079(4) 0.0467(12) Uani 1 1 d . . .
H6A H 0.6464 0.7952 -0.0040 0.056 Uiso 1 1 calc R . .
H6B H 0.7035 0.6680 -0.0757 0.056 Uiso 1 1 calc R . .
C7 C 0.8212(6) 0.6595(6) 0.0726(5) 0.0476(12) Uani 1 1 d . . .
H7A H 0.8540 0.5644 0.0800 0.057 Uiso 1 1 calc R . .
H7B H 0.9108 0.6961 0.0199 0.057 Uiso 1 1 calc R . .
C8 C 0.8721(9) 0.9128(7) 0.1302(6) 0.0680(18) Uani 1 1 d . . .
H8A H 0.9768 0.8690 0.0893 0.102 Uiso 1 1 calc R . .
H8B H 0.8839 0.9861 0.1685 0.102 Uiso 1 1 calc R . .
H8C H 0.8038 0.9436 0.0676 0.102 Uiso 1 1 calc R . .
C9 C 0.7965(6) 0.8181(5) 0.2322(5) 0.0408(11) Uani 1 1 d . . .
C10 C 0.7405(6) 0.8498(5) 0.3570(5) 0.0434(11) Uani 1 1 d . . .
H10 H 0.7605 0.9268 0.3776 0.052 Uiso 1 1 calc R . .
C11 C 0.6545(6) 0.7710(5) 0.4547(4) 0.0369(10) Uani 1 1 d . . .
C12 C 0.5947(8) 0.8153(6) 0.5851(5) 0.0587(15) Uani 1 1 d . . .
H12A H 0.4902 0.7937 0.6198 0.088 Uiso 1 1 calc R . .
H12B H 0.5860 0.9087 0.5794 0.088 Uiso 1 1 calc R . .
H12C H 0.6696 0.7718 0.6400 0.088 Uiso 1 1 calc R . .
C13 C 0.8240(5) 0.3198(5) 0.3354(4) 0.0339(9) Uani 1 1 d . . .
C14 C 0.7043(9) 1.0677(6) -0.2464(6) 0.0700(18) Uani 1 1 d DU . .
C15 C 0.7926(10) 1.1130(7) -0.3726(6) 0.077(2) Uani 1 1 d DU . .
H15A H 0.8788 1.1519 -0.3616 0.116 Uiso 1 1 calc R . .
H15B H 0.7194 1.1770 -0.4173 0.116 Uiso 1 1 calc R . .
H15C H 0.8371 1.0395 -0.4215 0.116 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'
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
_geom_angle_publ_flag
N3 Zn1 N3 180.000(1) . 2_666 ?
N3 Zn1 O2 94.68(15) . 2_666 ?
N3 Zn1 O2 85.32(15) 2_666 2_666 ?
N3 Zn1 O2 85.32(15) . . ?
N3 Zn1 O2 94.68(15) 2_666 . ?
O2 Zn1 O2 180.0 2_666 . ?
N3 Zn1 O1 86.07(14) . . ?
N3 Zn1 O1 93.93(14) 2_666 . ?
O2 Zn1 O1 94.35(12) 2_666 . ?
O2 Zn1 O1 85.65(12) . . ?
N3 Zn1 O1 93.93(14) . 2_666 ?
N3 Zn1 O1 86.07(14) 2_666 2_666 ?
O2 Zn1 O1 85.65(12) 2_666 2_666 ?
O2 Zn1 O1 94.35(12) . 2_666 ?
O1 Zn1 O1 179.999(1) . 2_666 ?
C2 O1 Zn1 142.2(3) . . ?
C11 O2 Zn1 149.6(3) . . ?
C4 N1 C6 125.8(4) . . ?
C4 N1 H1 116(4) . . ?
C6 N1 H1 118(4) . . ?
C9 N2 C7 128.5(4) . . ?
C9 N2 H2 119(3) . . ?
C7 N2 H2 111(3) . . ?
C13 N3 Zn1 176.2(4) . . ?
C2 C1 H1A 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O1 C2 C3 122.4(4) . . ?
O1 C2 C1 118.5(4) . . ?
C3 C2 C1 119.1(4) . . ?
C4 C3 C2 124.3(4) . . ?
C4 C3 H3 117.9 . . ?
C2 C3 H3 117.9 . . ?
N1 C4 C3 121.2(4) . . ?
N1 C4 C5 118.6(4) . . ?
C3 C4 C5 120.2(4) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N1 C6 C7 109.3(4) . . ?
N1 C6 H6A 109.8 . . ?
C7 C6 H6A 109.8 . . ?
N1 C6 H6B 109.8 . . ?
C7 C6 H6B 109.8 . . ?
H6A C6 H6B 108.3 . . ?
N2 C7 C6 112.2(4) . . ?
N2 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
N2 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C9 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C9 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N2 C9 C10 120.9(4) . . ?
N2 C9 C8 118.5(5) . . ?
C10 C9 C8 120.6(5) . . ?
C9 C10 C11 123.5(4) . . ?
C9 C10 H10 118.2 . . ?
C11 C10 H10 118.2 . . ?
O2 C11 C10 122.0(4) . . ?
O2 C11 C12 118.3(4) . . ?
C10 C11 C12 119.6(5) . . ?
C11 C12 H12A 109.5 . . ?
C11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C13 S1 178.7(5) . . ?
N4 C14 C15 178.8(10) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 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
Zn1 N3 2.167(4) . ?
Zn1 N3 2.167(4) 2_666 ?
Zn1 O2 2.193(3) 2_666 ?
Zn1 O2 2.193(3) . ?
Zn1 O1 2.213(3) . ?
Zn1 O1 2.213(3) 2_666 ?
S1 C13 1.627(5) . ?
O1 C2 1.266(5) . ?
O2 C11 1.247(6) . ?
N1 C4 1.306(6) . ?
N1 C6 1.458(6) . ?
N1 H1 0.847(10) . ?
N2 C9 1.319(7) . ?
N2 C7 1.469(6) . ?
N2 H2 0.856(10) . ?
N3 C13 1.154(6) . ?
N4 C14 1.102(6) . ?
C1 C2 1.500(6) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C3 1.400(6) . ?
C3 C4 1.391(6) . ?
C3 H3 0.9300 . ?
C4 C5 1.493(6) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 C7 1.503(7) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.503(7) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.389(7) . ?
C10 C11 1.416(6) . ?
C10 H10 0.9300 . ?
C11 C12 1.492(7) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C14 C15 1.471(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
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
N1 H1 O1 0.847(10) 2.01(4) 2.645(4) 132(5) .
N2 H2 O2 0.856(10) 1.96(4) 2.621(5) 133(4) .
N1 H1 O1 0.847(10) 2.01(4) 2.645(4) 132(5) .
N2 H2 O2 0.856(10) 1.96(4) 2.621(5) 133(4) .
