Crystal structures of two nickel compounds comprising neutral Ni^II^ hydrazone complexes and dicarboxylic acids
Nakanishi, Takumi; Sato, Osamu; Acta Crystallographica Section E 73 (2017) 103–106; doi:10.1107/S2056989016020326

data_2242006
_publ_section_title
;
 Crystal structures of two nickel compounds comprising neutral Ni^II^
 hydrazone complexes and dicarboxylic acids
;
_journal_coeditor_code           HB7631
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              103
_journal_page_last               106
_journal_paper_doi               10.1107/S2056989016020326
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          '[Ni (C13 H11 N4 O)2] (C8 H4 Br2 O4)'
_chemical_formula_moiety         'C26 H22 N8 Ni O2, C8 H4 Br2 O4'
_chemical_formula_sum            'C34 H26 Br2 N8 Ni O6'
_chemical_formula_weight         861.14
_chemical_name_systematic
'Bis{<i>N</i>-[1-(pyridin-2-yl-\k<i>N</i>)ethyl]pyridine-4-carbohydrazonato-\k^2^<i>N</i>',<i>O</i>}nickel(II)--2,5-dibromoterephthalic acid (1/1)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                75.040(9)
_cell_angle_beta                 82.162(10)
_cell_angle_gamma                86.007(11)
_cell_formula_units_Z            2
_cell_length_a                   7.8740(14)
_cell_length_b                   8.9716(15)
_cell_length_c                   24.233(4)
_cell_measurement_reflns_used    6236
_cell_measurement_temperature    123
_cell_measurement_theta_max      30.84
_cell_measurement_theta_min      1.75
_cell_volume                     1637.3(5)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2014)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2014)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2014)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2014)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2014)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR97 (Altomare et al., 1999)
;
_diffrn_ambient_temperature      123
_diffrn_detector_area_resol_mean 14.222
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28760
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.439
_diffrn_reflns_theta_min         3.056
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.101
_exptl_absorpt_correction_T_max  0.538
_exptl_absorpt_correction_T_min  0.467
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>REQAB</i>; Rigaku, 1998)
;
_exptl_crystal_colour            Brown
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             864.00
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     464
_refine_ls_number_reflns         7439
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0360P)^2^+2.3422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1030
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                6665
_reflns_number_total             7439
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            hb7631sup1.cif
_cod_data_source_block           1-Br
_cod_database_code               2242006
_cod_database_fobs_code          2242006