Bis[μ-<i>N</i>'-(2-methyl-1-oxidopropanylidene)-2-oxidobenzohydrazidato]tetrapyridinetrinickel(II)
Chen, Xiao-Hua; Xie, Chun-Ling; Yang, Ming-Xing; Chen, Li-Juan; Acta Crystallographica Section E 67 (2011) m1308–m1309; doi:10.1107/S1600536811034362

data_2231732
_publ_section_title
;
 Bis[\m-<i>N</i>'-(2-methyl-1-oxidopropanylidene)-2-oxidobenzohydrazidato]tetrapyridinetrinickel(II)
;
_journal_coeditor_code           XU5275
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1308
_journal_page_last               m1309
_journal_paper_doi               10.1107/S1600536811034362
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Ni3 (C11 H11 N2 O3) (C5 H5 N)4]'
_chemical_formula_moiety         'C42 H42 N8 Ni3 O6'
_chemical_formula_sum            'C42 H42 N8 Ni3 O6'
_chemical_formula_weight         930.97
_chemical_name_systematic
;
Bis[\m-<i>N</i>'-(2-methyl-1-oxidopropanylidene)-2-
oxidobenzohydrazidato]tetrapyridinetrinickel(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           SHELXL97
_cell_angle_alpha                109.324(15)
_cell_angle_beta                 96.474(13)
_cell_angle_gamma                93.516(13)
_cell_formula_units_Z            2
_cell_length_a                   9.866(3)
_cell_length_b                   12.325(5)
_cell_length_c                   18.240(7)
_cell_measurement_reflns_used    5875
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.11
_cell_volume                     2068.1(13)
_computing_cell_refinement
'TEXRAY (Molecular Structure Corporation, 1999)'
_computing_data_collection
'TEXRAY (Molecular Structure Corporation, 1999)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_molecular_graphics    'ORTEX (McArdle, 1995)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20490
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TEXRAY (Molecular Structure Corporation, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.460
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     539
_refine_ls_number_reflns         9360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0318P)^2^+0.8559P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                5875
_reflns_number_total             9360
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu5275.cif
_cod_data_source_block           I
_cod_original_cell_volume        2068.2(13)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2231732
_cod_database_fobs_code          2231732