#------------------------------------------------------------------------------
#$Date: 2016-03-26 18:22:14 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180424 $
#$URL: svn://www.crystallography.net/cod/cif/7/20/93/7209327.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_7209327
loop_
_publ_author_name
'Ana B. Caballero'
'Antonio Rodríguez-Diéguez'
'Elisa Barea'
'Miguel Quirós'
'Juan M. Salas'
_publ_contact_author_email       antonio5@ugr.es
_publ_contact_author_name        'Antonio Rodríguez-Diéguez'
_publ_section_title
;
 Influence of Pseudohalide Ligands on the Structural Versatility and
 Properties of Novel Ternary Metal Complexes with
 1,2,4-Triazolo[1,5-a]pyrimidine
;
_journal_name_full               CrystEngComm
_journal_page_first              3038
_journal_page_last               3045
_journal_paper_doi               10.1039/c003285a
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C24 H20 N20 Ni2 O2 S4'
_chemical_formula_sum            'C24 H20 N20 Ni2 O2 S4'
_chemical_formula_weight         866.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.818(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3178(8)
_cell_length_b                   12.8907(8)
_cell_length_c                   12.1015(8)
_cell_measurement_reflns_used    2706
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.4
_cell_measurement_theta_min      2.4
_cell_volume                     1729.73(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART (Bruker, 1999)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1999)'
_computing_molecular_graphics    'Xtal_GX (Hall & du Boulay, 1997)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Bruker SMART APEX CCD system'
_diffrn_measurement_method       'φ and ω 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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19963
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        0.4
_diffrn_standards_number         106
_exptl_absorpt_coefficient_mu    1.389
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS (Bruker, 1999)'
_exptl_crystal_colour            light_blue
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       planar
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.495
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4078
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0751
_refine_ls_R_factor_gt           0.0462
_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)+(0.0400P)²+1.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.1058
_reflns_number_gt                2840
_reflns_number_total             4078
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            niscntp2.cif
_cod_data_source_block           niscntp
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7209327
_cod_database_fobs_code          7209327
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ni1 Ni 0.5000 0.5000 0.5000 0.02414(13) Uani 1 2 d S
Ni2 Ni 0.0000 0.5000 0.5000 0.02757(14) Uani 1 2 d S
N1A N 0.1276(2) 0.48209(19) 0.4258(2) 0.0328(6) Uani 1 1 d .
C2A C 0.2429(2) 0.5024(2) 0.4870(3) 0.0332(7) Uani 1 1 d .
H2A H 0.2758 0.5265 0.5674 0.040 Uiso 1 1 d R
N3A N 0.3112(2) 0.48647(18) 0.4267(2) 0.0285(5) Uani 1 1 d .
C3AA C 0.2306(2) 0.4529(2) 0.3162(2) 0.0275(6) Uani 1 1 d .
N4A N 0.2492(2) 0.4271(2) 0.2192(2) 0.0359(6) Uani 1 1 d .
C5A C 0.1526(3) 0.3943(3) 0.1220(3) 0.0490(9) Uani 1 1 d .
H5A H 0.1621 0.3741 0.0529 0.059 Uiso 1 1 d R
C6A C 0.0375(3) 0.3885(3) 0.1172(3) 0.0503(9) Uani 1 1 d .
H6A H -0.0270 0.3647 0.0465 0.060 Uiso 1 1 d R
C7A C 0.0201(3) 0.4174(3) 0.2154(3) 0.0420(8) Uani 1 1 d .
H7A H -0.0558 0.4156 0.2145 0.050 Uiso 1 1 d R
N8A N 0.1194(2) 0.44930(18) 0.3156(2) 0.0286(5) Uani 1 1 d .
N1B N 0.4932(3) 0.7925(2) 0.3297(3) 0.0508(8) Uani 1 1 d .
C2B C 0.5209(3) 0.6948(3) 0.3583(3) 0.0422(8) Uani 1 1 d .
H2B H 0.5639 0.6567 0.3253 0.051 Uiso 1 1 d R
N3B N 0.4840(2) 0.65235(18) 0.4381(2) 0.0297(5) Uani 1 1 d .
C3AB C 0.4286(3) 0.7310(2) 0.4635(3) 0.0315(7) Uani 1 1 d .
N4B N 0.3776(2) 0.7331(2) 0.5408(2) 0.0387(6) Uani 1 1 d .
C5B C 0.3292(3) 0.8230(3) 0.5479(3) 0.0521(9) Uani 1 1 d .
H5B H 0.2918 0.8277 0.5999 0.063 Uiso 1 1 d R
C6B C 0.3309(4) 0.9117(3) 0.4817(4) 0.0580(10) Uani 1 1 d .
H6B H 0.2955 0.9729 0.4905 0.070 Uiso 1 1 d R
C7B C 0.3841(3) 0.9077(3) 0.4053(3) 0.0515(9) Uani 1 1 d .
H7B H 0.3868 0.9651 0.3600 0.062 Uiso 1 1 d R
N8B N 0.4334(2) 0.81608(19) 0.3980(2) 0.0386(6) Uani 1 1 d .
N1T N 0.0802(2) 0.6376(2) 0.5773(3) 0.0428(7) Uani 1 1 d .
C1T C 0.1076(3) 0.7103(2) 0.6385(3) 0.0358(7) Uani 1 1 d .
S1 S 0.14719(11) 0.81142(8) 0.72705(10) 0.0657(3) Uani 1 1 d .
N2T N 0.1186(2) 0.4252(2) 0.6569(2) 0.0432(7) Uani 1 1 d .
C2T C 0.1839(3) 0.3811(2) 0.7412(3) 0.0408(8) Uani 1 1 d .
S2 S 0.27801(12) 0.32036(8) 0.86398(11) 0.0856(4) Uani 1 1 d .
O1W O 0.49864(19) 0.45490(17) 0.33360(19) 0.0327(5) Uani 1 1 d D
H11W H 0.4300(14) 0.444(3) 0.282(2) 0.039 Uiso 1 1 d D
H12W H 0.528(3) 0.3974(13) 0.338(3) 0.039 Uiso 1 1 d 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 0.0000 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
N3B Ni1 N3B 180.0 . 3_666
N3B Ni1 O1W 92.52(9) . 3_666
N3B Ni1 O1W 87.48(9) 3_666 3_666
N3B Ni1 O1W 87.47(9) . .
N3B Ni1 O1W 92.53(9) 3_666 .
O1W Ni1 O1W 180.0 3_666 .
N3B Ni1 N3A 89.30(9) . 3_666
N3B Ni1 N3A 90.70(9) 3_666 3_666
O1W Ni1 N3A 91.56(9) 3_666 3_666
O1W Ni1 N3A 88.45(9) . 3_666
N3B Ni1 N3A 90.71(9) . .
N3B Ni1 N3A 89.30(9) 3_666 .
O1W Ni1 N3A 88.44(9) 3_666 .
O1W Ni1 N3A 91.55(9) . .
N3A Ni1 N3A 180.0 3_666 .
N1T Ni2 N1T 180.0 . 3_566
N1T Ni2 N2T 91.30(11) . 3_566
N1T Ni2 N2T 88.70(11) 3_566 3_566
N1T Ni2 N2T 88.70(11) . .
N1T Ni2 N2T 91.30(11) 3_566 .
N2T Ni2 N2T 179.998(1) 3_566 .
N1T Ni2 N1A 89.36(10) . .
N1T Ni2 N1A 90.64(10) 3_566 .
N2T Ni2 N1A 91.13(10) 3_566 .
N2T Ni2 N1A 88.87(10) . .
N1T Ni2 N1A 90.64(10) . 3_566
N1T Ni2 N1A 89.36(10) 3_566 3_566
N2T Ni2 N1A 88.87(10) 3_566 3_566
N2T Ni2 N1A 91.13(10) . 3_566
N1A Ni2 N1A 180.0 . 3_566
C2A N1A N8A 102.4(2) . .
C2A N1A Ni2 123.79(19) . .
N8A N1A Ni2 133.82(18) . .
N1A C2A N3A 116.2(2) . .
N1A C2A H2A 121.9 . .
N3A C2A H2A 121.9 . .
C3AA N3A C2A 102.9(2) . .
C3AA N3A Ni1 130.38(19) . .
C2A N3A Ni1 126.47(18) . .
N4A C3AA N3A 128.4(3) . .
N4A C3AA N8A 122.9(3) . .
N3A C3AA N8A 108.7(2) . .
C5A N4A C3AA 115.4(3) . .
N4A C5A C6A 123.8(3) . .
N4A C5A H5A 118.1 . .
C6A C5A H5A 118.1 . .
C7A C6A C5A 119.8(3) . .
C7A C6A H6A 120.1 . .
C5A C6A H6A 120.1 . .
C6A C7A N8A 116.3(3) . .
C6A C7A H7A 121.8 . .
N8A C7A H7A 121.9 . .
C7A N8A N1A 128.5(2) . .
C7A N8A C3AA 121.7(2) . .
N1A N8A C3AA 109.8(2) . .
C2B N1B N8B 101.6(3) . .
N1B C2B N3B 116.6(3) . .
N1B C2B H2B 121.6 . .
N3B C2B H2B 121.7 . .
C3AB N3B C2B 102.9(2) . .
C3AB N3B Ni1 127.86(19) . .
C2B N3B Ni1 129.2(2) . .
N3B C3AB N4B 128.5(3) . .
N3B C3AB N8B 108.7(3) . .
N4B C3AB N8B 122.8(3) . .
C5B N4B C3AB 115.2(3) . .
N4B C5B C6B 123.9(3) . .
N4B C5B H5B 118.1 . .
C6B C5B H5B 118.0 . .
C7B C6B C5B 119.6(3) . .
C7B C6B H6B 120.2 . .
C5B C6B H6B 120.2 . .
N8B C7B C6B 116.5(3) . .
N8B C7B H7B 121.7 . .
C6B C7B H7B 121.8 . .
C7B N8B N1B 127.9(3) . .
C7B N8B C3AB 122.0(3) . .
N1B N8B C3AB 110.2(3) . .
C1T N1T Ni2 161.5(3) . .
N1T C1T S1 178.9(3) . .
C2T N2T Ni2 177.7(3) . .
N2T C2T S2 178.6(3) . .
Ni1 O1W H11W 111(2) . .
Ni1 O1W H12W 112(2) . .
H11W O1W H12W 100(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 N3B 2.080(2) .
Ni1 N3B 2.080(2) 3_666
Ni1 O1W 2.089(2) 3_666
Ni1 O1W 2.089(2) .
Ni1 N3A 2.105(2) 3_666
Ni1 N3A 2.105(2) .
Ni2 N1T 2.048(3) .
Ni2 N1T 2.048(3) 3_566
Ni2 N2T 2.062(3) 3_566
Ni2 N2T 2.062(3) .
Ni2 N1A 2.135(2) .
Ni2 N1A 2.135(2) 3_566
N1A C2A 1.311(3) .
N1A N8A 1.361(3) .
C2A N3A 1.347(3) .
C2A H2A 0.9300 .
N3A C3AA 1.343(3) .
C3AA N4A 1.333(4) .
C3AA N8A 1.367(4) .
N4A C5A 1.326(4) .
C5A C6A 1.396(5) .
C5A H5A 0.9300 .
C6A C7A 1.348(5) .
C6A H6A 0.9300 .
C7A N8A 1.358(4) .
C7A H7A 0.9300 .
N1B C2B 1.312(4) .
N1B N8B 1.360(4) .
C2B N3B 1.349(4) .
C2B H2B 0.9300 .
N3B C3AB 1.331(4) .
C3AB N4B 1.334(4) .
C3AB N8B 1.369(4) .
N4B C5B 1.323(4) .
C5B C6B 1.400(5) .
C5B H5B 0.9300 .
C6B C7B 1.348(5) .
C6B H6B 0.9300 .
C7B N8B 1.348(4) .
C7B H7B 0.9300 .
N1T C1T 1.150(4) .
C1T S1 1.622(3) .
N2T C2T 1.138(4) .
C2T S2 1.632(4) .
O1W H11W 0.815(10) .
O1W H12W 0.816(10) .
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
O1W H11W N4A 0.815(10) 2.028(17) 2.789(3) 155(3) .
O1W H12W N4B 0.816(10) 2.20(2) 2.914(3) 146(3) 3_666
