#------------------------------------------------------------------------------
#$Date: 2015-05-22 10:36:55 +0300 (Fri, 22 May 2015) $
#$Revision: 137198 $
#$URL: svn://www.crystallography.net/cod/cif/7/22/05/7220543.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_7220543
loop_
_publ_author_name
'Haribabu, Jebiti'
'Jeyalakshmi, Kumaramangalam'
'Arun, Yuvaraj'
'Bhuvanesh, Nattamai S. P.'
'Perumal, Paramasivan Thirumalai'
'Karvembu, Ramasamy'
_publ_section_title
;
 Synthesis, DNA/protein binding, molecular docking, DNA cleavage and in
 vitro anticancer activity of nickel(ii) bis(thiosemicarbazone) complexes
;
_journal_issue                   57
_journal_name_full               'RSC Adv.'
_journal_page_first              46031
_journal_paper_doi               10.1039/C5RA04498G
_journal_volume                  5
_journal_year                    2015
_chemical_formula_moiety         'C10 H10 N4 O S, H2 O'
_chemical_formula_sum            'C10 H12 N4 O2 S'
_chemical_formula_weight         252.30
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2013-12-03
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-03-07 deposited with the CCDC.
2015-05-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.870(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.830(2)
_cell_length_b                   12.980(3)
_cell_length_c                   10.115(3)
_cell_measurement_reflns_used    6880
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.488
_cell_measurement_theta_min      2.312
_cell_volume                     1156.7(5)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            13112
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.522
_diffrn_reflns_theta_min         2.312
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0564 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.9382.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_description       block
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.322
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2656
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0342
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0349P)²+0.7452P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0808
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2449
_reflns_number_total             2656
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5ra04498g2.cif
_cod_data_source_block           il
_cod_database_code               7220543
_shelxl_version_number           2013-4
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB)
2.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C1(H1A), C2(H2), C3(H3A), C4(H4A)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
S1 S 0.00285(4) 0.62176(2) 0.26732(3) 0.01794(10) Uani 1 1 d . .
O1 O 0.30059(11) 0.88929(7) 0.16153(9) 0.0203(2) Uani 1 1 d . .
N1 N 0.40945(12) 1.03554(9) 0.25810(11) 0.0175(2) Uani 1 1 d . .
H1 H 0.4677 1.0539 0.1949 0.021 Uiso 1 1 calc R U
N2 N 0.14710(12) 0.88221(8) 0.41948(11) 0.0150(2) Uani 1 1 d . .
N3 N 0.11616(12) 0.80239(8) 0.33544(11) 0.0165(2) Uani 1 1 d . .
H3 H 0.1498 0.8033 0.2555 0.020 Uiso 1 1 calc R U
N4 N -0.01796(12) 0.72505(8) 0.49403(11) 0.0164(2) Uani 1 1 d . .
H4 H 0.0058 0.7791 0.5436 0.020 Uiso 1 1 calc R U
C1 C 0.48199(15) 1.17396(10) 0.42343(14) 0.0202(3) Uani 1 1 d . .
H1A H 0.5534 1.2063 0.3708 0.024 Uiso 1 1 calc R U
C2 C 0.45454(16) 1.21071(11) 0.54939(14) 0.0228(3) Uani 1 1 d . .
H2 H 0.5090 1.2691 0.5834 0.027 Uiso 1 1 calc R U
C3 C 0.34940(16) 1.16387(11) 0.62624(14) 0.0227(3) Uani 1 1 d . .
H3A H 0.3329 1.1909 0.7113 0.027 Uiso 1 1 calc R U
C4 C 0.26802(15) 1.07775(10) 0.57993(13) 0.0185(3) Uani 1 1 d . .
H4A H 0.1962 1.0456 0.6323 0.022 Uiso 1 1 calc R U
C5 C 0.29475(14) 1.04034(10) 0.45541(12) 0.0149(2) Uani 1 1 d . .
C6 C 0.40083(14) 1.08859(10) 0.37894(13) 0.0160(3) Uani 1 1 d . .
C7 C 0.23821(14) 0.95158(10) 0.38002(12) 0.0143(2) Uani 1 1 d . .
C8 C 0.31689(14) 0.95307(10) 0.25224(13) 0.0159(3) Uani 1 1 d . .
C9 C 0.03268(14) 0.72044(10) 0.37491(12) 0.0145(2) Uani 1 1 d . .
C10 C -0.11136(17) 0.64497(11) 0.54778(14) 0.0224(3) Uani 1 1 d . .
H10A H -0.1966 0.6291 0.4839 0.034 Uiso 1 1 calc R U
H10B H -0.1504 0.6690 0.6308 0.034 Uiso 1 1 calc R U
H10C H -0.0501 0.5828 0.5648 0.034 Uiso 1 1 calc R U
O1W O 0.34702(11) 0.55862(8) 0.39906(10) 0.0252(2) Uani 1 1 d . .
H1WA H 0.2551 0.5667 0.3704 0.038 Uiso 1 1 d R U
H1WB H 0.3528 0.5587 0.4833 0.038 Uiso 1 1 d R U
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C6 N1 H1 124.5
C8 N1 H1 124.5
C8 N1 C6 111.02(11)
C7 N2 N3 116.31(11)
N2 N3 H3 120.0
N2 N3 C9 120.03(10)
C9 N3 H3 120.0
C9 N4 H4 118.4
C9 N4 C10 123.12(11)
C10 N4 H4 118.4
C2 C1 H1A 121.5
C6 C1 H1A 121.5
C6 C1 C2 117.00(13)
C1 C2 H2 119.2
C3 C2 C1 121.60(13)
C3 C2 H2 119.2
C2 C3 H3A 119.6
C2 C3 C4 120.78(13)
C4 C3 H3A 119.6
C3 C4 H4A 120.9
C5 C4 C3 118.14(12)
C5 C4 H4A 120.9
C4 C5 C6 120.42(12)
C4 C5 C7 133.03(12)
C6 C5 C7 106.48(11)
C1 C6 N1 128.21(12)
C1 C6 C5 122.06(13)
C5 C6 N1 109.71(11)
N2 C7 C5 126.28(12)
N2 C7 C8 127.42(12)
C5 C7 C8 106.14(11)
O1 C8 N1 127.23(12)
O1 C8 C7 126.14(12)
N1 C8 C7 106.62(11)
N3 C9 S1 117.69(9)
N4 C9 S1 125.23(10)
N4 C9 N3 117.08(11)
N4 C10 H10A 109.5
N4 C10 H10B 109.5
N4 C10 H10C 109.5
H10A C10 H10B 109.5
H10A C10 H10C 109.5
H10B C10 H10C 109.5
H1WA O1W H1WB 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
S1 C9 1.6900(13)
O1 C8 1.2370(16)
N1 H1 0.8800
N1 C6 1.4094(17)
N1 C8 1.3457(17)
N2 N3 1.3562(15)
N2 C7 1.2886(17)
N3 H3 0.8800
N3 C9 1.3689(16)
N4 H4 0.8800
N4 C9 1.3146(17)
N4 C10 1.4549(17)
C1 H1A 0.9500
C1 C2 1.397(2)
C1 C6 1.3785(19)
C2 H2 0.9500
C2 C3 1.390(2)
C3 H3A 0.9500
C3 C4 1.3928(19)
C4 H4A 0.9500
C4 C5 1.3849(18)
C5 C6 1.4021(18)
C5 C7 1.4515(18)
C7 C8 1.5082(17)
C10 H10A 0.9800
C10 H10B 0.9800
C10 H10C 0.9800
O1W H1WA 0.8499
O1W H1WB 0.8500
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 O1W 0.88 1.95 2.7754(15) 156.1 2_655
N3 H3 O1 0.88 2.02 2.7213(15) 135.4 .
N4 H4 S1 0.88 2.60 3.4001(13) 150.9 4_576
O1W H1WA S1 0.85 2.50 3.3371(13) 169.0 .
O1W H1WB O1 0.85 2.01 2.7965(15) 154.0 4_576
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
N2 N3 C9 S1 -178.09(9)
N2 N3 C9 N4 1.92(17)
N2 C7 C8 O1 3.5(2)
N2 C7 C8 N1 -175.26(12)
N3 N2 C7 C5 -176.16(11)
N3 N2 C7 C8 -1.35(19)
C1 C2 C3 C4 0.3(2)
C2 C1 C6 N1 -178.53(12)
C2 C1 C6 C5 0.2(2)
C2 C3 C4 C5 -0.1(2)
C3 C4 C5 C6 -0.12(19)
C3 C4 C5 C7 176.41(13)
C4 C5 C6 N1 179.00(11)
C4 C5 C6 C1 0.02(19)
C4 C5 C7 N2 -2.4(2)
C4 C5 C7 C8 -178.11(13)
C5 C7 C8 O1 179.16(12)
C5 C7 C8 N1 0.39(13)
C6 N1 C8 O1 -178.13(13)
C6 N1 C8 C7 0.63(14)
C6 C1 C2 C3 -0.4(2)
C6 C5 C7 N2 174.47(12)
C6 C5 C7 C8 -1.23(13)
C7 N2 N3 C9 173.56(11)
C7 C5 C6 N1 1.65(14)
C7 C5 C6 C1 -177.33(12)
C8 N1 C6 C1 177.42(13)
C8 N1 C6 C5 -1.47(14)
C10 N4 C9 S1 -1.65(18)
C10 N4 C9 N3 178.35(12)
