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_2019544
_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
;
[Ni2 (C10 H2 O8) (C12 H13 N3)2 (H2 O)2],
[Ni (C12 H13 N3) (H2 O)3]2 (C10 H2 O8), 6H2 O'
;
_chemical_formula_moiety
'C34 H32 N6 Ni2 O10, 2(C12 H19 N3 Ni O3 2+), C10 H2 O8 4-, 6(H2 O)'
_chemical_formula_sum            'C68 H84 N12 Ni4 O30'
_chemical_formula_weight         1784.32
_chemical_name_systematic
;(\m-Benzene-1,2,4,5-tetracarboxylato-\k^4^<i>O</i>^1^,<i>O</i>^2^:<i>O</i>^4^,<i>O</i>^5^)bis(aqua{bis[(pyridin-2-yl)methyl]amine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}nickel(II))
bis{triaquabis[(pyridin-2-yl)methyl]amine-\k^3^<i>N</i>,<i>N</i>',<i>N</i>''}nickel(II)}
benzene-1,2,4,5-tetracarboxylate hexahydrate
;
_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           SHELXL-97
_cell_angle_alpha                85.0080(10)
_cell_angle_beta                 82.8230(10)
_cell_angle_gamma                65.2930(8)
_cell_formula_units_Z            1
_cell_length_a                   9.8485(6)
_cell_length_b                   10.7208(6)
_cell_length_c                   19.4924(11)
_cell_measurement_reflns_used    6234
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.12
_cell_measurement_theta_min      2.34
_cell_volume                     1853.65(19)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.892
_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  0.0151
_diffrn_reflns_av_sigmaI/netI    0.0237
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15507
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.91
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.096
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS in SAINT-NT; Bruker, 2002)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.313
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         7916
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0481P)^2^+0.4178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0836
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                6969
_reflns_number_total             7916
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            uk3094sup1.cif
_cod_data_source_block           II
_cod_depositor_comments
'Adding full bibliography for 2019543--2019544.cif.'
_cod_original_sg_symbol_H-M      ' P -1'
_cod_database_code               2019544
_cod_database_fobs_code          2019544