#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:25:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179789 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/85/7008593.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_7008593
loop_
_publ_author_name
'Kumar Singh, Akhilesh'
'Mukherjee, Rabindranath'
_publ_section_title
;
 Structure and properties of bivalent nickel and copper complexes with
 pyrazine-amide-thioether coordination: stabilization of trivalent
 nickel.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2886
_journal_page_last               2891
_journal_paper_doi               10.1039/b504893a
_journal_year                    2005
_chemical_formula_moiety         'C25 H22 N6 Ni O3 S2'
_chemical_formula_sum            'C25 H22 N6 Ni O3 S2'
_chemical_formula_weight         577.32
_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                106.821(13)
_cell_angle_beta                 100.367(14)
_cell_angle_gamma                98.199(13)
_cell_formula_units_Z            2
_cell_length_a                   8.937(7)
_cell_length_b                   10.803(8)
_cell_length_c                   14.305(11)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      2.1
_cell_volume                     1272.3(17)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'Bruker SAINT PLUS'
_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    'SIR97(Altomare, et. al. 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.905
_diffrn_measured_fraction_theta_max 0.905
_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  0.0438
_diffrn_reflns_av_sigmaI/netI    0.1184
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7450
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         2.10
_exptl_absorpt_coefficient_mu    0.967
_exptl_absorpt_correction_T_max  0.8301
_exptl_absorpt_correction_T_min  0.7602
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             596
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.040
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         5726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0678P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1229
_refine_ls_wR_factor_ref         0.1400
_reflns_number_gt                3649
_reflns_number_total             5726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b504893a.txt
_cod_data_source_block           3junbm
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' 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_cell_volume        1272.4(17)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7008593
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
Ni Ni 0.30330(5) 0.32927(4) 0.71648(3) 0.03227(16) Uani 1 1 d . . .
S1 S 0.10056(10) 0.31574(9) 0.80536(7) 0.0381(2) Uani 1 1 d . . .
S2 S 0.35486(10) 0.12707(8) 0.73945(7) 0.0351(2) Uani 1 1 d . . .
O1 O 0.0728(3) 0.2132(4) 0.4191(2) 0.0746(10) Uani 1 1 d . . .
O2 O 0.6583(3) 0.6179(3) 0.9168(2) 0.0561(8) Uani 1 1 d . . .
O1S O 0.1254(11) 0.2414(16) 0.1830(6) 0.389(10) Uani 1 1 d . . .
H1S H 0.1432 0.3107 0.1680 0.583 Uiso 1 1 calc R . .
N1 N 0.4273(3) 0.3269(3) 0.6050(2) 0.0390(7) Uani 1 1 d . . .
N2 N 0.5419(5) 0.3413(4) 0.4387(3) 0.0725(12) Uani 1 1 d . . .
N3 N 0.1283(3) 0.2479(3) 0.5921(2) 0.0344(7) Uani 1 1 d . . .
N4 N 0.4901(3) 0.4137(3) 0.8349(2) 0.0344(7) Uani 1 1 d . . .
N5 N 0.3383(4) 0.7984(3) 0.7849(3) 0.0584(10) Uani 1 1 d . . .
N6 N 0.3002(3) 0.5264(3) 0.7348(2) 0.0370(7) Uani 1 1 d . . .
C1 C 0.5793(5) 0.3646(4) 0.6126(3) 0.0497(10) Uani 1 1 d . . .
H1 H 0.6507 0.3873 0.6757 0.060 Uiso 1 1 calc R . .
C2 C 0.6334(5) 0.3708(5) 0.5283(4) 0.0643(13) Uani 1 1 d . . .
H2 H 0.7421 0.3979 0.5360 0.077 Uiso 1 1 calc R . .
C3 C 0.3896(5) 0.3010(5) 0.4313(3) 0.0627(12) Uani 1 1 d . . .
H3 H 0.3191 0.2768 0.3677 0.075 Uiso 1 1 calc R . .
C4 C 0.3322(4) 0.2939(4) 0.5143(3) 0.0431(9) Uani 1 1 d . . .
C5 C 0.1602(4) 0.2471(4) 0.5040(3) 0.0462(10) Uani 1 1 d . . .
C6 C -0.0195(4) 0.1931(3) 0.5998(3) 0.0351(8) Uani 1 1 d . . .
C7 C -0.1400(4) 0.1096(4) 0.5187(3) 0.0438(9) Uani 1 1 d . . .
H7 H -0.1275 0.0935 0.4520 0.053 Uiso 1 1 calc R . .
C8 C -0.2767(4) 0.0508(4) 0.5355(3) 0.0496(10) Uani 1 1 d . . .
H8 H -0.3562 -0.0057 0.4799 0.059 Uiso 1 1 calc R . .
C9 C -0.2995(4) 0.0728(4) 0.6315(3) 0.0505(11) Uani 1 1 d . . .
H9 H -0.3931 0.0306 0.6416 0.061 Uiso 1 1 calc R . .
C10 C -0.1855(4) 0.1564(4) 0.7126(3) 0.0441(9) Uani 1 1 d . . .
H10 H -0.2021 0.1740 0.7785 0.053 Uiso 1 1 calc R . .
C11 C -0.0458(4) 0.2152(3) 0.6979(3) 0.0352(8) Uani 1 1 d . . .
C12 C 0.1509(4) 0.1937(4) 0.8632(3) 0.0433(10) Uani 1 1 d . . .
H12A H 0.2376 0.2375 0.9230 0.052 Uiso 1 1 calc R . .
H12B H 0.0605 0.1596 0.8863 0.052 Uiso 1 1 calc R . .
C13 C 0.1978(4) 0.0788(4) 0.7945(3) 0.0407(9) Uani 1 1 d . . .
H13A H 0.1062 0.0271 0.7398 0.049 Uiso 1 1 calc R . .
H13B H 0.2300 0.0203 0.8330 0.049 Uiso 1 1 calc R . .
C14 C 0.5150(4) 0.1990(3) 0.8452(3) 0.0324(8) Uani 1 1 d . . .
C15 C 0.5871(4) 0.1168(4) 0.8885(3) 0.0447(9) Uani 1 1 d . . .
H15 H 0.5449 0.0244 0.8643 0.054 Uiso 1 1 calc R . .
C16 C 0.7183(5) 0.1660(4) 0.9657(3) 0.0542(11) Uani 1 1 d . . .
H16 H 0.7659 0.1089 0.9953 0.065 Uiso 1 1 calc R . .
C17 C 0.7796(5) 0.3007(4) 0.9994(3) 0.0527(11) Uani 1 1 d . . .
H17 H 0.8714 0.3358 1.0517 0.063 Uiso 1 1 calc R . .
C18 C 0.7084(4) 0.3849(4) 0.9577(3) 0.0459(10) Uani 1 1 d . . .
H18 H 0.7521 0.4770 0.9823 0.055 Uiso 1 1 calc R . .
C19 C 0.5736(4) 0.3370(3) 0.8801(3) 0.0330(8) Uani 1 1 d . . .
C20 C 0.5374(4) 0.5443(3) 0.8587(3) 0.0379(8) Uani 1 1 d . . .
C21 C 0.4218(4) 0.6055(3) 0.8046(3) 0.0396(9) Uani 1 1 d . . .
C22 C 0.4401(5) 0.7416(4) 0.8292(3) 0.0506(10) Uani 1 1 d . . .
H22 H 0.5282 0.7963 0.8793 0.061 Uiso 1 1 calc R . .
C23 C 0.2189(5) 0.7186(4) 0.7166(3) 0.0552(11) Uani 1 1 d . . .
H23 H 0.1434 0.7555 0.6841 0.066 Uiso 1 1 calc R . .
C24 C 0.1984(5) 0.5824(4) 0.6899(3) 0.0492(10) Uani 1 1 d . . .
H24 H 0.1108 0.5282 0.6391 0.059 Uiso 1 1 calc R . .
C1S C 0.1298(14) 0.1453(7) 0.1119(12) 0.306(11) Uani 1 1 d . . .
H1S1 H 0.1751 0.1763 0.0632 0.459 Uiso 1 1 calc R . .
H1S2 H 0.0241 0.0937 0.0794 0.459 Uiso 1 1 calc R . .
H1S3 H 0.1936 0.0897 0.1367 0.459 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 Ni N4 175.71(11) . . ?
N3 Ni N6 98.17(12) . . ?
N4 Ni N6 81.08(12) . . ?
N3 Ni N1 79.83(13) . . ?
N4 Ni N1 95.92(13) . . ?
N6 Ni N1 88.88(11) . . ?
N3 Ni S2 97.31(9) . . ?
N4 Ni S2 83.66(9) . . ?
N6 Ni S2 164.32(9) . . ?
N1 Ni S2 96.30(9) . . ?
N3 Ni S1 84.50(10) . . ?
N4 Ni S1 99.72(10) . . ?
N6 Ni S1 90.67(8) . . ?
N1 Ni S1 164.09(9) . . ?
S2 Ni S1 88.34(4) . . ?
C11 S1 C12 100.94(18) . . ?
C11 S1 Ni 95.35(13) . . ?
C12 S1 Ni 100.37(13) . . ?
C14 S2 C13 103.06(17) . . ?
C14 S2 Ni 97.09(12) . . ?
C13 S2 Ni 102.14(13) . . ?
C4 N1 C1 117.5(3) . . ?
C4 N1 Ni 111.6(2) . . ?
C1 N1 Ni 130.5(3) . . ?
C2 N2 C3 116.0(4) . . ?
C5 N3 C6 122.4(3) . . ?
C5 N3 Ni 117.5(2) . . ?
C6 N3 Ni 120.1(2) . . ?
C20 N4 C19 122.6(3) . . ?
C20 N4 Ni 115.4(2) . . ?
C19 N4 Ni 121.6(2) . . ?
C23 N5 C22 116.4(4) . . ?
C21 N6 C24 117.8(3) . . ?
C21 N6 Ni 111.3(2) . . ?
C24 N6 Ni 131.0(3) . . ?
N1 C1 C2 120.2(4) . . ?
N2 C2 C1 123.4(4) . . ?
N2 C3 C4 121.9(4) . . ?
N1 C4 C3 121.0(4) . . ?
N1 C4 C5 118.1(3) . . ?
C3 C4 C5 120.9(4) . . ?
O1 C5 N3 130.3(4) . . ?
O1 C5 C4 117.9(3) . . ?
N3 C5 C4 111.8(3) . . ?
N3 C6 C7 125.2(3) . . ?
N3 C6 C11 117.4(3) . . ?
C7 C6 C11 117.1(3) . . ?
C8 C7 C6 120.6(4) . . ?
C9 C8 C7 121.3(4) . . ?
C10 C9 C8 119.7(3) . . ?
C9 C10 C11 120.1(3) . . ?
C10 C11 C6 121.1(3) . . ?
C10 C11 S1 118.3(3) . . ?
C6 C11 S1 120.6(2) . . ?
C13 C12 S1 114.0(3) . . ?
C12 C13 S2 113.8(2) . . ?
C15 C14 C19 120.8(3) . . ?
C15 C14 S2 118.9(3) . . ?
C19 C14 S2 120.2(3) . . ?
C16 C15 C14 121.4(4) . . ?
C15 C16 C17 118.6(4) . . ?
C16 C17 C18 120.8(4) . . ?
C17 C18 C19 121.4(4) . . ?
C18 C19 N4 125.9(3) . . ?
C18 C19 C14 116.9(3) . . ?
N4 C19 C14 117.2(3) . . ?
O2 C20 N4 129.2(3) . . ?
O2 C20 C21 118.3(3) . . ?
N4 C20 C21 112.4(3) . . ?
N6 C21 C22 120.3(4) . . ?
N6 C21 C20 118.8(3) . . ?
C22 C21 C20 120.9(4) . . ?
N5 C22 C21 122.3(4) . . ?
N5 C23 C24 122.5(4) . . ?
N6 C24 C23 120.7(4) . . ?
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
Ni N3 2.021(3) . ?
Ni N4 2.036(3) . ?
Ni N6 2.074(3) . ?
Ni N1 2.096(3) . ?
Ni S2 2.3958(19) . ?
Ni S1 2.4046(17) . ?
S1 C11 1.777(3) . ?
S1 C12 1.814(4) . ?
S2 C14 1.779(4) . ?
S2 C13 1.814(3) . ?
O1 C5 1.241(5) . ?
O2 C20 1.242(4) . ?
O1S C1S 1.237(15) . ?
N1 C4 1.334(5) . ?
N1 C1 1.337(5) . ?
N2 C2 1.314(6) . ?
N2 C3 1.343(5) . ?
N3 C5 1.340(4) . ?
N3 C6 1.405(4) . ?
N4 C20 1.336(4) . ?
N4 C19 1.405(4) . ?
N5 C23 1.308(5) . ?
N5 C22 1.335(5) . ?
N6 C21 1.326(4) . ?
N6 C24 1.333(5) . ?
C1 C2 1.392(6) . ?
C3 C4 1.392(5) . ?
C4 C5 1.515(5) . ?
C6 C7 1.409(5) . ?
C6 C11 1.421(5) . ?
C7 C8 1.388(5) . ?
C8 C9 1.382(6) . ?
C9 C10 1.380(5) . ?
C10 C11 1.397(5) . ?
C12 C13 1.508(5) . ?
C14 C15 1.388(5) . ?
C14 C19 1.413(5) . ?
C15 C16 1.376(5) . ?
C16 C17 1.386(6) . ?
C17 C18 1.390(5) . ?
C18 C19 1.400(5) . ?
C20 C21 1.518(5) . ?
C21 C22 1.387(5) . ?
C23 C24 1.385(5) . ?
