Hydrolysis of 4-(4-oxopentan-2-ylideneamino)benzoic acid and in-situ formation of nickel(II), zinc(II) and cadmium(II) complexes of 4-aminobenzoic acid
Nithi Phukan; Jubaraj B. Baruah; Inorganica Chimica Acta 394 (2013) 430–435; doi:10.1016/j.ica.2012.09.005

data_1512767
_publ_section_title
;
 Hydrolysis of 4-(4-oxopentan-2-ylideneamino)benzoic acid and in-situ
 formation of nickel(II), zinc(II) and cadmium(II) complexes of
 4-aminobenzoic acid
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              430
_journal_page_last               435
_journal_paper_doi               10.1016/j.ica.2012.09.005
_journal_volume                  394
_journal_year                    2013
_chemical_formula_sum            'C18 H32 N2 Ni O14'
_chemical_formula_weight         559.17
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 97.332(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.7822(3)
_cell_length_b                   18.1737(9)
_cell_length_c                   10.6188(5)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.50
_cell_measurement_theta_min      2.23
_cell_volume                     1298.15(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0143
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21520
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         28.50
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.815
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         3221
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.7278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                2953
_reflns_number_total             3221
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-430-435-2.cif
_cod_data_source_block           nithi
_cod_original_sg_symbol_H-M      'P2(1)/n  '
_cod_database_code               1512767