#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:32:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179900 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/96/7019658.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_7019658
loop_
_publ_author_name
'Prabhakaran, R.'
'Kalaivani, P.'
'Poornima, P.'
'Dallemer, F.'
'Paramaguru, G.'
'Vijaya Padma, V.'
'Renganathan, R.'
'Huang, R.'
'Natarajan, K.'
_publ_section_title
;
 One pot synthesis of structurally different mono and dimeric Ni(ii)
 thiosemicarbazone complexes and N-arylation on a coordinated ligand: a
 comparative biological study.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9323
_journal_page_last               9336
_journal_paper_doi               10.1039/c2dt12231f
_journal_volume                  41
_journal_year                    2012
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H26 N3 Ni1 O1 P1 S1'
_chemical_formula_sum            'C32 H26 N3 Ni O P S'
_chemical_formula_weight         590.3
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2011-01-12T11:39:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 92.473(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.4975(2)
_cell_length_b                   10.5710(2)
_cell_length_c                   13.8196(4)
_cell_measurement_reflns_used    12776
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      1.47
_cell_measurement_wavelength     0.71073
_cell_volume                     1386.17(6)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'Omega + Phi scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.065
_diffrn_reflns_av_unetI/netI     0.0704
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12776
_diffrn_reflns_theta_full        28.7
_diffrn_reflns_theta_max         28.7
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.414
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             612
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.251
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6653
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0672P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0988
_refine_ls_wR_factor_ref         0.1259
_reflns_number_gt                5642
_reflns_number_total             6653
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt12231f.txt
_cod_data_source_block           '[Ni(sal-ptsc)(PPh3)]'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7019658
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+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
C1 C 0.3149(4) -0.0779(3) 0.7501(3) 0.0382(7) Uani 1 1 d .
C2 C 0.4515(4) -0.0863(4) 0.7950(3) 0.0557(10) Uani 1 1 d .
H2 H 0.4801 -0.0272 0.8417 0.067 Uiso 1 1 calc R
C3 C 0.5427(5) -0.1817(5) 0.7699(4) 0.0654(13) Uani 1 1 d .
H3 H 0.633 -0.1845 0.7986 0.078 Uiso 1 1 calc R
C4 C 0.5011(5) -0.2737(5) 0.7021(4) 0.0608(11) Uani 1 1 d .
H4 H 0.5621 -0.3388 0.6869 0.073 Uiso 1 1 calc R
C5 C 0.3693(5) -0.2668(4) 0.6584(3) 0.0541(10) Uani 1 1 d .
H5 H 0.3417 -0.3283 0.6134 0.065 Uiso 1 1 calc R
C6 C 0.2740(4) -0.1694(3) 0.6795(3) 0.0399(8) Uani 1 1 d .
C7 C 0.1393(4) -0.1682(3) 0.6306(3) 0.0409(8) Uani 1 1 d .
H7 H 0.1189 -0.2339 0.5875 0.049 Uiso 1 1 calc R
C8 C -0.1726(4) -0.0175(3) 0.5927(3) 0.0380(7) Uani 1 1 d .
C9 C -0.3646(4) -0.1143(3) 0.4843(3) 0.0390(7) Uani 1 1 d .
C10 C -0.3020(4) -0.2284(3) 0.4633(3) 0.0425(8) Uani 1 1 d .
H10 H -0.214 -0.2487 0.4911 0.051 Uiso 1 1 calc R
C11 C -0.3713(4) -0.3123(4) 0.4008(3) 0.0498(10) Uani 1 1 d .
H11 H -0.3287 -0.3888 0.3864 0.06 Uiso 1 1 calc R
C12 C -0.5030(5) -0.2843(4) 0.3593(3) 0.0543(10) Uani 1 1 d .
H12 H -0.5478 -0.3406 0.3165 0.065 Uiso 1 1 calc R
C13 C -0.5671(5) -0.1706(5) 0.3825(3) 0.0559(10) Uani 1 1 d .
H13 H -0.6566 -0.1516 0.3565 0.067 Uiso 1 1 calc R
C14 C -0.4981(4) -0.0857(4) 0.4442(3) 0.0481(9) Uani 1 1 d .
H14 H -0.5408 -0.0093 0.4589 0.058 Uiso 1 1 calc R
C15 C 0.2428(4) 0.2730(3) 0.8609(3) 0.0404(8) Uani 1 1 d .
C16 C 0.3162(4) 0.3681(4) 0.8180(3) 0.0485(9) Uani 1 1 d .
H16 H 0.2745 0.413 0.7665 0.058 Uiso 1 1 calc R
C17 C 0.4534(5) 0.3976(5) 0.8512(4) 0.0646(13) Uani 1 1 d .
H17 H 0.5027 0.4619 0.8215 0.078 Uiso 1 1 calc R
C18 C 0.5147(5) 0.3330(6) 0.9264(4) 0.0756(16) Uani 1 1 d .
H18 H 0.6053 0.3543 0.949 0.091 Uiso 1 1 calc R
C19 C 0.4431(5) 0.2350(6) 0.9701(4) 0.0714(14) Uani 1 1 d .
H19 H 0.4856 0.1905 1.0216 0.086 Uiso 1 1 calc R
C20 C 0.3075(4) 0.2039(4) 0.9361(3) 0.0551(10) Uani 1 1 d .
H20 H 0.26 0.1369 0.9636 0.066 Uiso 1 1 calc R
C21 C -0.0146(3) 0.3720(3) 0.7675(2) 0.0351(7) Uani 1 1 d .
C22 C -0.1005(4) 0.4493(4) 0.8219(3) 0.0465(9) Uani 1 1 d .
H22 H -0.1201 0.427 0.885 0.056 Uiso 1 1 calc R
C23 C -0.1560(4) 0.5587(5) 0.7819(3) 0.0537(9) Uani 1 1 d .
H23 H -0.2131 0.6098 0.8185 0.064 Uiso 1 1 calc R
C24 C -0.1283(5) 0.5937(4) 0.6885(3) 0.0551(11) Uani 1 1 d .
H24 H -0.1649 0.6685 0.6625 0.066 Uiso 1 1 calc R
C25 C -0.0461(5) 0.5165(4) 0.6343(3) 0.0562(10) Uani 1 1 d .
H25 H -0.0275 0.5391 0.571 0.067 Uiso 1 1 calc R
C26 C 0.0091(4) 0.4061(4) 0.6726(3) 0.0466(9) Uani 1 1 d .
H26 H 0.0628 0.3538 0.6346 0.056 Uiso 1 1 calc R
C27 C -0.0299(4) 0.1968(3) 0.9274(3) 0.0381(7) Uani 1 1 d .
C28 C -0.1329(4) 0.1041(4) 0.9270(3) 0.0459(9) Uani 1 1 d .
H28 H -0.1486 0.0536 0.8725 0.055 Uiso 1 1 calc R
C29 C -0.2121(5) 0.0865(4) 1.0071(3) 0.0561(11) Uani 1 1 d .
H29 H -0.2804 0.0235 1.0067 0.067 Uiso 1 1 calc R
C30 C -0.1907(5) 0.1611(5) 1.0868(3) 0.0588(11) Uani 1 1 d .
H30 H -0.2458 0.1493 1.1401 0.071 Uiso 1 1 calc R
C31 C -0.0895(5) 0.2531(4) 1.0894(3) 0.0574(11) Uani 1 1 d .
H31 H -0.0755 0.3032 1.1443 0.069 Uiso 1 1 calc R
C32 C -0.0078(5) 0.2715(4) 1.0100(3) 0.0493(9) Uani 1 1 d .
H32 H 0.0617 0.3335 1.0116 0.059 Uiso 1 1 calc R
N1 N 0.0423(3) -0.0833(3) 0.6407(2) 0.0349(6) Uani 1 1 d .
N2 N -0.0814(3) -0.1083(3) 0.5846(2) 0.0396(6) Uani 1 1 d .
N3 N -0.3019(3) -0.0205(3) 0.5451(2) 0.0461(7) Uani 1 1 d .
H3A H -0.3533 0.0452 0.5536 0.055 Uiso 1 1 calc R
O1 O 0.2334(3) 0.0149(2) 0.77642(19) 0.0423(6) Uani 1 1 d .
P1 P 0.06513(9) 0.22730(7) 0.81721(6) 0.03340(19) Uani 1 1 d .
S1 S -0.13835(11) 0.11940(10) 0.65972(9) 0.0521(3) Uani 1 1 d .
Ni1 Ni 0.06072(4) 0.06070(4) 0.72070(3) 0.03266(12) Uani 1 1 d .
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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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'
Ni Ni 0.3393 1.1124 '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
O1 C1 C6 123.7(3)
O1 C1 C2 117.8(3)
C6 C1 C2 118.5(3)
C3 C2 C1 120.5(4)
C3 C2 H2 119.7
C1 C2 H2 119.7
C2 C3 C4 121.0(4)
C2 C3 H3 119.5
C4 C3 H3 119.5
C5 C4 C3 119.1(4)
C5 C4 H4 120.5
C3 C4 H4 120.5
C4 C5 C6 122.1(4)
C4 C5 H5 119
C6 C5 H5 119
C5 C6 C1 118.8(4)
C5 C6 C7 118.7(4)
C1 C6 C7 122.5(3)
N1 C7 C6 125.7(3)
N1 C7 H7 117.2
C6 C7 H7 117.2
N2 C8 N3 121.9(3)
N2 C8 S1 123.3(3)
N3 C8 S1 114.7(2)
C10 C9 C14 119.9(3)
C10 C9 N3 124.2(3)
C14 C9 N3 115.9(3)
C9 C10 C11 119.5(4)
C9 C10 H10 120.2
C11 C10 H10 120.2
C12 C11 C10 121.2(4)
C12 C11 H11 119.4
C10 C11 H11 119.4
C11 C12 C13 119.1(4)
C11 C12 H12 120.5
C13 C12 H12 120.5
C14 C13 C12 120.1(4)
C14 C13 H13 119.9
C12 C13 H13 119.9
C13 C14 C9 120.2(4)
C13 C14 H14 119.9
C9 C14 H14 119.9
C16 C15 C20 119.4(4)
C16 C15 P1 121.9(3)
C20 C15 P1 118.6(3)
C15 C16 C17 120.4(4)
C15 C16 H16 119.8
C17 C16 H16 119.8
C18 C17 C16 120.2(5)
C18 C17 H17 119.9
C16 C17 H17 119.9
C17 C18 C19 120.5(5)
C17 C18 H18 119.8
C19 C18 H18 119.8
C20 C19 C18 119.4(5)
C20 C19 H19 120.3
C18 C19 H19 120.3
C15 C20 C19 120.1(5)
C15 C20 H20 120
C19 C20 H20 120
C26 C21 C22 118.6(3)
C26 C21 P1 119.4(3)
C22 C21 P1 122.0(3)
C23 C22 C21 119.9(4)
C23 C22 H22 120.1
C21 C22 H22 120.1
C22 C23 C24 121.0(4)
C22 C23 H23 119.5
C24 C23 H23 119.5
C25 C24 C23 119.2(4)
C25 C24 H24 120.4
C23 C24 H24 120.4
C24 C25 C26 120.6(4)
C24 C25 H25 119.7
C26 C25 H25 119.7
C25 C26 C21 120.6(3)
C25 C26 H26 119.7
C21 C26 H26 119.7
C28 C27 C32 119.0(4)
C28 C27 P1 119.6(3)
C32 C27 P1 121.2(3)
C29 C28 C27 120.2(4)
C29 C28 H28 119.9
C27 C28 H28 119.9
C30 C29 C28 120.3(4)
C30 C29 H29 119.9
C28 C29 H29 119.9
C29 C30 C31 120.8(4)
C29 C30 H30 119.6
C31 C30 H30 119.6
C30 C31 C32 119.8(4)
C30 C31 H31 120.1
C32 C31 H31 120.1
C31 C32 C27 119.9(4)
C31 C32 H32 120
C27 C32 H32 120
C7 N1 N2 113.0(3)
C7 N1 Ni1 125.0(3)
N2 N1 Ni1 122.0(2)
C8 N2 N1 111.0(3)
C8 N3 C9 130.4(3)
C8 N3 H3A 114.8
C9 N3 H3A 114.8
C1 O1 Ni1 127.2(2)
C21 P1 C27 104.40(15)
C21 P1 C15 105.31(16)
C27 P1 C15 104.57(17)
C21 P1 Ni1 116.35(11)
C27 P1 Ni1 111.38(12)
C15 P1 Ni1 113.74(11)
C8 S1 Ni1 96.37(12)
O1 Ni1 N1 95.24(11)
O1 Ni1 S1 177.92(8)
N1 Ni1 S1 86.84(9)
O1 Ni1 P1 87.92(8)
N1 Ni1 P1 175.58(9)
S1 Ni1 P1 90.00(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 O1 1.311(4)
C1 C6 1.416(5)
C1 C2 1.416(5)
C2 C3 1.383(6)
C2 H2 0.93
C3 C4 1.396(7)
C3 H3 0.93
C4 C5 1.368(6)
C4 H4 0.93
C5 C6 1.410(5)
C5 H5 0.93
C6 C7 1.421(5)
C7 N1 1.298(4)
C7 H7 0.93
C8 N2 1.301(4)
C8 N3 1.367(5)
C8 S1 1.742(4)
C9 C10 1.381(5)
C9 C14 1.395(6)
C9 N3 1.415(4)
C10 C11 1.385(5)
C10 H10 0.93
C11 C12 1.385(6)
C11 H11 0.93
C12 C13 1.391(7)
C12 H12 0.93
C13 C14 1.383(6)
C13 H13 0.93
C14 H14 0.93
C15 C16 1.373(6)
C15 C20 1.390(6)
C15 P1 1.832(4)
C16 C17 1.398(6)
C16 H16 0.93
C17 C18 1.354(8)
C17 H17 0.93
C18 C19 1.392(9)
C18 H18 0.93
C19 C20 1.392(6)
C19 H19 0.93
C20 H20 0.93
C21 C26 1.388(5)
C21 C22 1.397(5)
C21 P1 1.827(3)
C22 C23 1.377(6)
C22 H22 0.93
C23 C24 1.379(6)
C23 H23 0.93
C24 C25 1.374(6)
C24 H24 0.93
C25 C26 1.376(6)
C25 H25 0.93
C26 H26 0.93
C27 C28 1.384(5)
C27 C32 1.395(5)
C27 P1 1.832(4)
C28 C29 1.377(6)
C28 H28 0.93
C29 C30 1.363(7)
C29 H29 0.93
C30 C31 1.367(7)
C30 H30 0.93
C31 C32 1.385(6)
C31 H31 0.93
C32 H32 0.93
N1 N2 1.405(4)
N1 Ni1 1.885(3)
N3 H3A 0.86
O1 Ni1 1.846(2)
P1 Ni1 2.2085(9)
S1 Ni1 2.1290(10)
