Disappearing and Concomitant Polymorphism of Nickel(II) Complexes with 6-Hydroxypicolinic Acid. Structural and Density Functional Theory Studies
Kukovec, Boris-Marko; Vaz, Pedro D.; Calhorda, Maria José; Popović, Zora; Crystal Growth & Design 10 (2010) 3685–; doi:10.1021/cg100536m

data_4501845
_publ_section_title
;
 Disappearing and Concomitant Polymorphism of Nickel(II) Complexes with
 6-Hydroxypicolinic Acid. Structural and Density Functional Theory Studies
;
_journal_issue                   8
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3685
_journal_paper_doi               10.1021/cg100536m
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety         'C22 H18 N4 Ni O6'
_chemical_formula_sum            'C22 H18 N4 Ni O6'
_chemical_formula_weight         493.11
_chemical_name_common
;
trans-bis(6-hydroxypicolinato-N,O)bis(pyridine)nickel(II)
;
_chemical_name_systematic
;
trans-bis(6-hydroxypyridine-2-carboxylato-N,O)bis(pyridine)
nickel(II)- monoclinic polymorph
;
_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                 96.991(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.3358(3)
_cell_length_b                   27.5392(7)
_cell_length_c                   9.4855(3)
_cell_measurement_reflns_used    3834
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      34.00
_cell_measurement_theta_min      3.66
_cell_volume                     2161.31(12)
_computing_cell_refinement       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis (Oxford Diffraction, 2006)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 2001), MERCURY 1.4.2 (CCDC, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type
'Oxford Diffraction Xcalibur2 diffractometer with Sapphire 3 CCD detector'
_diffrn_measurement_method       \w-scan
_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  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0836
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            13268
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.67
_diffrn_standards_interval_count '1 ref frame per 50 dc frames'
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_T_max  0.85
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlis, Version 171.31.5 (Oxford Diffraction, 2006)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4667
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0908
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0994
_reflns_number_gt                2432
_reflns_number_total             4667
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg100536m_si_001.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4501845