2,9-Dimethyl-1,10-phenanthrolin-1-ium (6-carboxy-4-hydroxypyridine-2-carboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)(4-hydroxypyridine-2,6-dicarboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)nickelate(II) 2.35-hydrate: a proton-transfer compound
Derakhshandeh, Maryam; Derikvand, Zohreh; Nemati, Andya; Stoeckli-Evans, Helen; Acta Crystallographica Section E 66 (2010) m1084–m1085; doi:10.1107/S1600536810031399

data_2227768
_publ_section_title
;
 2,9-Dimethyl-1,10-phenanthrolin-1-ium
 (6-carboxy-4-hydroxypyridine-2-carboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)(4-hydroxypyridine-2,6-dicarboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)nickelate(II)
 2.35-hydrate: a proton-transfer compound
;
_journal_coeditor_code           LH5110
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1084
_journal_page_last               m1085
_journal_paper_doi               10.1107/S1600536810031399
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac
'(C14 H13 N2) [Ni (C7 H3 N O5) (C7 H4 N O5)], 2.35H2 O'
_chemical_formula_moiety         'C28 H20 N4 Ni O10, 2.35(H2 O)'
_chemical_formula_sum            'C28 H24.7 N4 Ni O12.35'
_chemical_formula_weight         673.53
_chemical_name_systematic
;
2,9-Dimethyl-1,10-phenanthrolin-1-ium (6-carboxy-4-hydroxypyridine-2-
carboxylato-\k^3^O^2^,<i>N</i>,<i>O</i>^6^)(4-hydroxypyridine-2,6-dicarboxylato-
\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)nickelate(II) 2.35-hydrate
;
_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                 94.330(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1663(8)
_cell_length_b                   9.7296(9)
_cell_length_c                   25.698(2)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.15
_cell_volume                     2784.0(4)
_computing_cell_refinement       'CELL (Stoe & Cie, 2000)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 2000)'
_computing_molecular_graphics
'PLATON (Spek, 2009) and Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material
'SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f rotation'
_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  0.0493
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            21508
_diffrn_reflns_theta_full        26.10
_diffrn_reflns_theta_max         26.10
_diffrn_reflns_theta_min         2.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.774
_exptl_absorpt_correction_T_max  0.839
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULscanABS in PLATON; Spek, 2009)'
_exptl_crystal_colour            pale-blue
_exptl_crystal_density_diffrn    1.607
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1390
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.286
_refine_diff_density_min         -0.494
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         5442
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0379P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0711
_reflns_number_gt                3321
_reflns_number_total             5442
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            lh5110.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C28 H24.70 N4 Ni O12.35'
_cod_database_code               2227768
_cod_database_fobs_code          2227768