Two nickel(II) bis[(pyridin-2-yl)methyl]amine complexes with homophthalic and benzene-1,2,4,5-tetracarboxylic acids
Atria, Ana María; Garland, Maria Teresa; Baggio, Ricardo; Acta Crystallographica Section C 70 (2014) 541–546; doi:10.1107/S2053229614008134

data_2019543
_publ_section_title
;
 Two nickel(II) bis[(pyridin-2-yl)methyl]amine complexes with homophthalic
 and benzene-1,2,4,5-tetracarboxylic acids
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              541
_journal_page_last               546
_journal_paper_doi               10.1107/S2053229614008134
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ni (C9 H6 O4) (C12 H13 N3) (H2 O)]'
_chemical_formula_moiety         'C21 H21 N3 Ni O5'
_chemical_formula_sum            'C21 H21 N3 Ni O5'
_chemical_formula_weight         454.12
_chemical_name_systematic
<i>catena</i>-Poly[[aqua{bis[(pyridin-2-yl)methyl]amine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}nickel(II)]-\m-2-(2-carboxylatophenyl)aceteto-\k^2^<i>O</i>:<i>O</i>']
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.081(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   18.233(3)
_cell_length_b                   10.4511(14)
_cell_length_c                   20.898(3)
_cell_measurement_reflns_used    2835
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.79
_cell_measurement_theta_min      2.24
_cell_volume                     3976.5(10)
_computing_cell_refinement       'SAINT-NT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-NT (Bruker, 2002)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
'SHELXTL (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0233
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15811
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.80
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.723
_refine_diff_density_min         -0.373
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.434
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4399
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.434
_refine_ls_R_factor_all          0.0622
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0538P)^2^+2.6787P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                3562
_reflns_number_total             4399
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3094sup1.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 2019543--2019544.cif.'
_cod_original_cell_volume        3976.3(9)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2019543
_cod_database_fobs_code          2019543