Hydrothermal synthesis and crystal structure of novel bis(6-carboxypyridine-2-carboxylato-κ^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)nickel(II) trihydrate, Ni(Hpydc)~2~·3H~2~O
Sanotra, Sumit; Gupta, Rimpy; Sheikh, Haq Nawaz; Kalsotra, Bansi Lal; Gupta, Vivek K.; Rajnikant; Acta Crystallographica Section B 68 (2012) 619–624; doi:10.1107/S0108768112043972

data_2105291
_publ_section_title
;
 Hydrothermal synthesis and crystal structure of novel
 bis(6-carboxypyridine-2-carboxylato-\k^3^<i>O</i>^2^,<i>N</i>,<i>O</i>^6^)nickel(II)
 trihydrate, Ni(Hpydc)~2~&#x00B7;3H~2~O
;
_journal_coeditor_code           BP5046
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              619
_journal_page_last               624
_journal_paper_doi               10.1107/S0108768112043972
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C14 H8 N2 Ni O8, 3(H2 O)'
_chemical_formula_sum            'C14 H14 N2 Ni O11'
_chemical_formula_weight         444.98
_chemical_name_systematic
;
bis (2,6-pyridinedicarboxylato)nickelate(II) trihydrate
;
_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                 115.166(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6825(3)
_cell_length_b                   10.0465(2)
_cell_length_c                   13.7770(4)
_cell_measurement_reflns_used    12492
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9500
_cell_measurement_theta_min      3.4245
_cell_volume                     1714.04(8)
_computing_cell_refinement       'CrysAlisPro, Diff.Ltd,Ver 1.171.34.40'
_computing_data_collection       'CrysAlisPro,Diff.Ltd,Ver 1.171.34.40'
_computing_data_reduction        'CrysAlisPro, Diff.Ltd,Ver 1.171.34.40'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'PLATON(Spek,1999)& PARST(1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '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  0.0325
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            24855
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    1.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82716
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crys Alis RED'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.724
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.671
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3353
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0475P)^2^+0.7877P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                2779
_reflns_number_total             3353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bp5046.cif
_cod_data_source_block           I
_cod_original_cell_volume        1714.04(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105291