Bis[μ~3~-<i>N</i>'-oxidopyridine-2-carboximidamidato(2{-})]bis[μ~2~-<i>N</i>'-oxidopyridine-2-carboximidamidato(1{-})]tetrapyridinetetranickel(II) dinitrate
Deng, Xiao-Hui; Ran, Jing-Wen; Acta Crystallographica Section E 68 (2012) m40–; doi:10.1107/S1600536811052524

data_2233079
_publ_section_title
;
 Bis[\m~3~-<i>N</i>'-oxidopyridine-2-carboximidamidato(2{-})]bis[\m~2~-<i>N</i>'-oxidopyridine-2-carboximidamidato(1{-})]tetrapyridinetetranickel(II)
 dinitrate
;
_journal_coeditor_code           BH2397
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m40
_journal_paper_doi               10.1107/S1600536811052524
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac
'[Ni4 (C6 H5 N3 O)2 (C6 H6 N3 O)2 (C5 H5 N)4] (N O3)2'
_chemical_formula_moiety         'C44 H42 N16 Ni4 O4 2+, 2(N O3 -)'
_chemical_formula_sum            'C44 H42 N18 Ni4 O10'
_chemical_formula_weight         1217.80
_chemical_name_systematic
;
Bis[\m~3~-<i>N</i>'-oxidopyridine-2-carboximidamidato(2-)]bis[\m~2~-<i>N</i>'-
oxidopyridine-2-carboximidamidato(1-)]tetrapyridinetetranickel(II)
dinitrate
;
_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                92.041(6)
_cell_angle_beta                 98.240(5)
_cell_angle_gamma                100.870(5)
_cell_formula_units_Z            1
_cell_length_a                   10.4356(6)
_cell_length_b                   10.7190(8)
_cell_length_c                   11.2908(9)
_cell_measurement_reflns_used    1738
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.76
_cell_measurement_theta_min      3.05
_cell_volume                     1224.96(15)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type
;
Bruker SMART APEXII CCD area-detector
;
_diffrn_measurement_method       '\f and \w 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  0.0392
_diffrn_reflns_av_sigmaI/netI    0.0565
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9481
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.591
_exptl_absorpt_correction_T_max  0.6059
_exptl_absorpt_correction_T_min  0.5686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.517
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4286
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0408
_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^)+(0.0420P)^2^+0.4034P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1000
_reflns_number_gt                3180
_reflns_number_total             4286
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bh2397.cif
_cod_data_source_block           I
_cod_database_code               2233079
_cod_database_fobs_code          2233079