The crystal structure of a new polymorph of hexaaquanickel(II) bis(6-oxo-1,6-dihydropyridine-3-carboxylate)
Pérez-Aguirre, Rubén; Pérez-Yáñez, Sonia; Beobide, Garikoitz; Castillo, Oscar; Gutiérrez-Zorrilla, Juan Manuel; Luque, Antonio; Acta Crystallographica Section E 71 (2015) m238–m239; doi:10.1107/S2056989015022422

data_2241358
_publ_section_title
;
 The crystal structure of a new polymorph of hexaaquanickel(II)
 bis(6-oxo-1,6-dihydropyridine-3-carboxylate)
;
_journal_coeditor_code           WM5241
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m238
_journal_page_last               m239
_journal_paper_doi               10.1107/S2056989015022422
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (H2 O)6] (C6 H4 N O3)2'
_chemical_formula_moiety         'H12 Ni O6 2+, 2(C6 H4 N O3 -)'
_chemical_formula_sum            'C12 H20 N2 Ni O12'
_chemical_formula_weight         443.01
_chemical_name_systematic
;
Hexaaquanickel(II) bis(6-oxo-1,6-dihydropyridine-3-carboxylate)
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                102.461(8)
_cell_angle_beta                 96.754(7)
_cell_angle_gamma                114.823(8)
_cell_formula_units_Z            1
_cell_length_a                   6.2620(5)
_cell_length_b                   7.1053(7)
_cell_length_c                   10.7101(10)
_cell_measurement_reflns_used    2781
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.239
_cell_measurement_theta_min      2.003
_cell_volume                     410.49(8)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2012)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2012)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method       'thin-slice \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2781
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.239
_diffrn_reflns_theta_min         2.003
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.888
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
(<i>CrysAlisRED</i>; Oxford Diffraction, 2003)
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             230
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1801
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0191P)^2^+0.3293P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                1654
_reflns_number_total             1801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5241sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        410.49(7)
_cod_database_code               2241358
_cod_database_fobs_code          2241358
_shelx_res_checksum              62834