Bis(butane-2,3-dione monooxime benzoylhydrazone-κ^3^<i>O,N,N</i>')nickel(II) sulfate salicylhydroxamic acid
Gao, Shan; Huo, Li-Hua; Zhao, Hui; Ng, Seik Weng; Acta Crystallographica Section E 60 (2004) m1750–m1751; doi:10.1107/S1600536804027102

data_2204612
_publ_section_title
;
 Bis(butane-2,3-dione monooxime
 benzoylhydrazone-\k^3^<i>O,N,N</i>')nickel(II) sulfate
 salicylhydroxamic acid
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1750
_journal_page_last               m1751
_journal_paper_doi               10.1107/S1600536804027102
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          '[Ni (C11 H13 N3 O2)2] S O4, C7 H7 N O3'
_chemical_formula_moiety         'C22 H26 N6 O4 Ni 2+, S O4 2-, C7 H7 N O3'
_chemical_formula_sum            'C29 H33 N7 Ni O11 S'
_chemical_formula_weight         746.39
_chemical_name_systematic
;Bis(butane-2,3-dione monooxime benzoylhydrazone-\k^3^O,N,N')nickel(II)
 sulfate
salicylhydroxamic acid
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.82(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.986(2)
_cell_length_b                   23.781(5)
_cell_length_c                   17.868(4)
_cell_measurement_reflns_used    21088
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     3308.8(14)
_computing_cell_refinement       RAPID-AUTO
_computing_data_collection       'RAPID-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_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  0.0689
_diffrn_reflns_av_sigmaI/netI    0.0575
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29244
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.10
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.870
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.19
_refine_diff_density_min         -0.33
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0767P)^2^+1.6714P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1354
_refine_ls_wR_factor_ref         0.1519
_reflns_number_gt                4963
_reflns_number_total             7483
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6553.cif
_cod_data_source_block           I
_cod_original_cell_volume        3309.0(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2204612
_cod_database_fobs_code          2204612