Bis{<i>N</i>-[bis(6-bromopyridin-2-yl)methylene-κ<i>N</i>]ethane-1,2-diamine-κ^2^<i>N</i>,<i>N</i>'}nickel(II) bis(perchlorate)
Knight, James C.; Amoroso, Angelo J.; Prabaharan, Ravi; Edwards, Peter G.; Acta Crystallographica Section E 63 (2007) m1046–m1047; doi:10.1107/S1600536807010653

data_2212764
_publ_section_title
;Bis{<i>N</i>-[bis(6-bromopyridin-2-yl)methylene-\k<i>N</i>]ethane-1,2-diamine-\k^2^<i>N</i>,<i>N</i>'}nickel(II)
 bis(perchlorate)
;
_journal_coeditor_code           BG2034
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1046
_journal_page_last               m1047
_journal_paper_doi               10.1107/S1600536807010653
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Ni (C13 H12 Br2 N4)2] (Cl O4)2'
_chemical_formula_moiety         'C26 H24 Br4 N8 Ni, 2(Cl O4)'
_chemical_formula_sum            'C26 H24 Br4 Cl2 N8 Ni O8'
_chemical_formula_weight         1025.78
_chemical_name_systematic
;
Bis{N-[bis(6-bromopyridin-2-yl)methylene-\kN]ethane-1,2-diamine-
\k^2^N,N'}nickel(II) bis(perchlorate)
;
_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                110.077(2)
_cell_angle_beta                 95.308(2)
_cell_angle_gamma                94.573(2)
_cell_formula_units_Z            2
_cell_length_a                   9.1897(3)
_cell_length_b                   12.9937(3)
_cell_length_c                   15.0869(5)
_cell_measurement_reflns_used    24601
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.71
_cell_volume                     1672.76(9)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction
'SCALEPACK and DENZO (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIFF99 (Beurskens <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f and \w'
_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  0.1561
_diffrn_reflns_av_sigmaI/netI    0.1231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            26603
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.96
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.578
_exptl_absorpt_correction_T_max  0.31
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.348
_refine_diff_density_min         -0.934
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7570
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1171
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+4.0795P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1288
_refine_ls_wR_factor_ref         0.1483
_reflns_number_gt                4801
_reflns_number_total             7570
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg2034.cif
_cod_data_source_block           I
_cod_database_code               2212764
_cod_database_fobs_code          2212764