[1-(5-Bromo-2-oxidobenzylidene)thiosemicarbazidato-κ^3^<i>O</i>,<i>N</i>^1^,<i>S</i>](pyridine-κ<i>N</i>)nickel(II)
Pederzolli, Fernanda Rosi Soares; Bresolin, Leandro; Beck, Johannes; Daniels, Jörg; de Oliveira, Adriano Bof; Acta Crystallographica Section E 68 (2012) m1138–; doi:10.1107/S1600536812028917

data_2236763
_publ_section_title
;
 [1-(5-Bromo-2-oxidobenzylidene)thiosemicarbazidato-\k^3^<i>O</i>,<i>N</i>^1^,<i>S</i>](pyridine-\k<i>N</i>)nickel(II)
;
_journal_coeditor_code           ZL2486
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1138
_journal_paper_doi               10.1107/S1600536812028917
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Ni (C8 H6 Br N3 O S) (C5 H5 N)]'
_chemical_formula_moiety         'C13 H11 Br N4 Ni O S'
_chemical_formula_sum            'C13 H11 Br N4 Ni O S'
_chemical_formula_weight         409.94
_chemical_name_systematic
;
[1-(5-Bromo-2-oxidobenzylidene)thiosemicarbazidato-
\k^3^<i>O</i>,<i>N</i>^1^,<i>S</i>](pyridine-\k<i>N</i>)nickel(II)
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 112.6460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2447(4)
_cell_length_b                   4.11350(10)
_cell_length_c                   31.1380(11)
_cell_measurement_reflns_used    17227
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.91
_cell_volume                     1447.46(8)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
'DENZO and SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            13946
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    4.247
_exptl_absorpt_correction_T_max  0.8303
_exptl_absorpt_correction_T_min  0.4429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Blessing, 1995)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.928
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.045
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.663
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.6555P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0831
_reflns_number_gt                2697
_reflns_number_total             3224
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            zl2486.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2236763
_cod_database_fobs_code          2236763