[3-Hydroxy-<i>N</i>'-(2-oxidobenzylidene)-2-naphthohydrazidato-κ^3^<i>O</i>,<i>N</i>,<i>O</i>']tris(pyridine-κ<i>N</i>)nickel(II) pyridine trisolvate
Shi-Zhu Sun; Wen-Jun Kang; Da-Cheng Li; Da-Qi Wang; Jian-Min Dou; Acta Crystallographica Section E 64 (2008) m438–m438; doi:10.1107/S1600536808002900

data_2217690
_publ_section_title
;[3-Hydroxy-<i>N</i>'-(2-oxidobenzylidene)-2-naphthohydrazidato-\k^3^<i>O</i>,<i>N</i>,<i>O</i>']tris(pyridine-\k<i>N</i>)nickel(II)
 pyridine trisolvate
;
_journal_coeditor_code           XU2364
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m438
_journal_page_last               m438
_journal_paper_doi               10.1107/S1600536808002900
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Ni (C18 H12 N2 O3) (C5 H5 N)3], 3C5 H5 N'
_chemical_formula_moiety         'C33 H27 N5 Ni O3, 3(C5 H5 N)'
_chemical_formula_sum            'C48 H42 N8 Ni O3'
_chemical_formula_weight         837.59
_chemical_name_systematic
;
[3-Hydroxy-N'-(2-oxidobenzylidene)-2-naphthohydrazidato-
\k^3^O,N,O']tris(pyridine-\kN)nickel(II) pyridine trisolvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.378(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.370(2)
_cell_length_b                   27.720(3)
_cell_length_c                   16.862(2)
_cell_measurement_reflns_used    4738
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      20.496
_cell_measurement_theta_min      2.202
_cell_volume                     8586.2(17)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD area-detector'
_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  0.0787
_diffrn_reflns_av_sigmaI/netI    0.1300
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35434
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.33
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  0.8719
_exptl_absorpt_correction_T_min  0.7869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.676
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1081
_refine_ls_number_reflns         14836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.1999
_refine_ls_R_factor_gt           0.0809
_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^)+(0.1595P)^2^+3.0585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2276
_refine_ls_wR_factor_ref         0.3209
_reflns_number_gt                5715
_reflns_number_total             14836
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu2364.cif
_cod_data_source_block           I
_cod_original_cell_volume        8586.3(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217690
_cod_database_fobs_code          2217690