#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/49/2214962.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2214962
loop_
_publ_author_name
'Liang-Gui Wang'
_publ_section_title
Dibromidobis(2-methyl-5-phenyl-s-triazolo[3,4-b][1,3,4]thiadiazole-κN)nickel(II)
_journal_coeditor_code           BG2086
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2345
_journal_page_last               m2345
_journal_paper_doi               10.1107/S160053680703958X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni Br2 (C10 H8 N4 S)2]'
_chemical_formula_moiety         'C20 H16 Br2 N8 Ni S2'
_chemical_formula_sum            'C20 H16 Br2 N8 Ni S2'
_chemical_formula_weight         651.06
_chemical_name_systematic
;
Dibromidobis(2-methyl-5-phenyl-s-triazolo[3,4-b][1,3,4]thiadiazole-
\kN)nickel(II)
;
_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                98.442(2)
_cell_angle_beta                 105.614(3)
_cell_angle_gamma                108.859(2)
_cell_formula_units_Z            1
_cell_length_a                   6.8286(10)
_cell_length_b                   8.5231(13)
_cell_length_c                   11.3654(16)
_cell_measurement_reflns_used    2383
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.92
_cell_volume                     582.69(15)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'APEX2 (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  'SHELXTL (Bruker, 1998)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.92
_diffrn_measured_fraction_theta_max 0.89
_diffrn_measurement_device_type  'Bruker APEX II area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.1013
_diffrn_reflns_av_sigmaI/netI    0.1038
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4173
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.467
_exptl_absorpt_correction_T_max  0.53
_exptl_absorpt_correction_T_min  0.37
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.929
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2383
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0443
_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)+(0.0555P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1114
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                1595
_reflns_number_total             2383
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bg2086.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     ' -P 1 '
_cod_original_sg_symbol_H-M      ' P-1 '
_cod_database_code               2214962
_cod_database_fobs_code          2214962
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Br Br1 0.85222(9) 0.72697(7) 0.06809(5) 0.0707(2) Uani d . 1
Ni Ni1 0.5000 0.5000 0.0000 0.0321(2) Uani d S 1
S S1 0.3986(2) 0.08844(13) 0.13109(10) 0.0434(3) Uani d . 1
N N1 0.5616(6) 0.4522(4) 0.1689(3) 0.0392(8) Uani d . 1
N N2 0.6704(6) 0.5816(4) 0.2827(3) 0.0392(8) Uani d . 1
N N3 0.6002(6) 0.3343(4) 0.3279(3) 0.0330(7) Uani d . 1
N N4 0.5781(6) 0.1933(4) 0.3771(3) 0.0383(8) Uani d . 1
C C1 0.8738(8) 0.7807(6) 0.5409(4) 0.0435(10) Uani d . 1
H H1 0.8615 0.8379 0.4772 0.052 Uiso calc R 1
C C2 0.9710(8) 0.8729(6) 0.6677(4) 0.0504(12) Uani d . 1
H H2 1.0233 0.9921 0.6892 0.060 Uiso calc R 1
C C3 0.9889(8) 0.7861(6) 0.7604(4) 0.0497(12) Uani d . 1
H H3 1.0536 0.8479 0.8447 0.060 Uiso calc R 1
C C5 0.8172(8) 0.5181(6) 0.6055(4) 0.0424(10) Uani d . 1
H H4 0.7674 0.3990 0.5852 0.051 Uiso calc R 1
C C6 0.7950(7) 0.6011(5) 0.5107(4) 0.0340(9) Uani d . 1
C C4 0.9134(8) 0.6106(6) 0.7314(4) 0.0511(12) Uani d . 1
H H6 0.9264 0.5541 0.7954 0.061 Uiso calc R 1
C C8 0.5192(7) 0.3049(5) 0.2004(4) 0.0358(9) Uani d . 1
C C9 0.4777(8) 0.0564(5) 0.2839(4) 0.0425(10) Uani d . 1
C C10 0.4262(9) -0.1189(6) 0.3024(5) 0.0629(15) Uani d . 1
H H17A 0.4750 -0.1124 0.3911 0.094 Uiso calc R 1
H H17B 0.4999 -0.1755 0.2613 0.094 Uiso calc R 1
H H17C 0.2703 -0.1826 0.2667 0.094 Uiso calc R 1
C C7 0.6932(7) 0.5085(5) 0.3759(4) 0.0327(9) Uani d . 1
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'
Br Br -0.2901 2.4595 '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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Ni1 N1 . 2_665 180.00(19) ?
N1 Ni1 Br1 . . 90.80(10) y
N1 Ni1 Br1 2_665 . 89.20(10) ?
N1 Ni1 Br1 . 2_665 89.20(10) ?
N1 Ni1 Br1 2_665 2_665 90.80(10) ?
Br1 Ni1 Br1 . 2_665 180.0 ?
C8 S1 C9 . . 87.73(19) ?
C8 N1 N2 . . 106.4(3) ?
C8 N1 Ni1 . . 130.3(3) ?
N2 N1 Ni1 . . 123.3(2) ?
C7 N2 N1 . . 108.2(3) ?
C8 N3 C7 . . 106.6(3) ?
C8 N3 N4 . . 117.5(3) ?
C7 N3 N4 . . 135.9(3) ?
C9 N4 N3 . . 108.2(3) ?
C2 C1 C6 . . 119.2(4) ?
C2 C1 H1 . . 120.4 ?
C6 C1 H1 . . 120.4 ?
C3 C2 C1 . . 119.5(4) ?
C3 C2 H2 . . 120.3 ?
C1 C2 H2 . . 120.3 ?
C4 C3 C2 . . 121.5(4) ?
C4 C3 H3 . . 119.2 ?
C2 C3 H3 . . 119.2 ?
C6 C5 C4 . . 120.5(4) ?
C6 C5 H4 . . 119.7 ?
C4 C5 H4 . . 119.7 ?
C5 C6 C1 . . 119.9(4) ?
C5 C6 C7 . . 122.5(4) ?
C1 C6 C7 . . 117.6(4) ?
C3 C4 C5 . . 119.3(4) ?
C3 C4 H6 . . 120.3 ?
C5 C4 H6 . . 120.3 ?
N1 C8 N3 . . 109.8(3) ?
N1 C8 S1 . . 140.1(3) ?
N3 C8 S1 . . 110.1(3) ?
N4 C9 C10 . . 122.8(4) ?
N4 C9 S1 . . 116.4(3) ?
C10 C9 S1 . . 120.8(4) ?
C9 C10 H17A . . 109.5 ?
C9 C10 H17B . . 109.5 ?
H17A C10 H17B . . 109.5 ?
C9 C10 H17C . . 109.5 ?
H17A C10 H17C . . 109.5 ?
H17B C10 H17C . . 109.5 ?
N2 C7 N3 . . 109.0(3) ?
N2 C7 C6 . . 124.7(4) ?
N3 C7 C6 . . 126.3(3) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ni1 Br1 . 2.3826(6) y
Ni1 N1 . 1.984(3) y
Ni1 N1 2_665 1.984(3) ?
Ni1 Br1 2_665 2.3826(6) ?
S1 C8 . 1.716(4) ?
S1 C9 . 1.765(4) ?
N1 C8 . 1.319(5) ?
N1 N2 . 1.405(4) ?
N2 C7 . 1.305(5) ?
N3 C8 . 1.358(5) ?
N3 C7 . 1.368(5) ?
N3 N4 . 1.380(4) ?
N4 C9 . 1.297(6) ?
C1 C2 . 1.396(6) ?
C1 C6 . 1.402(6) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.375(6) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.369(7) ?
C3 H3 . 0.9300 ?
C5 C6 . 1.375(6) ?
C5 C4 . 1.389(6) ?
C5 H4 . 0.9300 ?
C6 C7 . 1.473(5) ?
C4 H6 . 0.9300 ?
C9 C10 . 1.481(6) ?
C10 H17A . 0.9600 ?
C10 H17B . 0.9600 ?
C10 H17C . 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C10 H17C Br1 1_445 0.96 2.90 3.769(5) 150.3
C5 H4 N4 . 0.93 2.45 3.123(6) 129.2
