Zn and Ni complexes of pyridine-2,6-di-carboxyl-ates: crystal field stabilization matters!
Kremer, Marius; Englert, Ulli; Acta crystallographica. Section E, Crystallographic communications 75 (2019) 903–911; doi:10.1107/S2056989019007461

data_2311595
_publ_section_title
;
 Zn and Ni complexes of pyridine-2,6-di-carboxyl-ates: crystal field
 stabilization matters!
;
_journal_coeditor_code           WM5493
_journal_issue                   'Pt 6'
_journal_name_full
'Acta crystallographica. Section E, Crystallographic communications'
_journal_page_first              903
_journal_page_last               911
_journal_paper_doi               10.1107/S2056989019007461
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Ni (C7 H3 N O5) (H2 O)3], 1.7H2 O'
_chemical_formula_moiety         'C7 H9 N Ni O8, 1.7 (H2 O)'
_chemical_formula_sum            'C7 H12.4 N Ni O9.7'
_chemical_formula_weight         324.49
_chemical_name_systematic
;
Triaqua(4-hydroxypyridine-2,6-dicarboxylato)nickel(II) 1.7-hydrate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90.3550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.7249(11)
_cell_length_b                   6.8538(5)
_cell_length_c                   22.3510(16)
_cell_measurement_reflns_used    5539
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.77
_cell_volume                     2255.7(3)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2009)
;
_computing_data_collection
;
SMART (Bruker, 2001)
;
_computing_data_reduction
;
SAINT-Plus (Bruker, 2009)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i> (2006)
;
_computing_publication_material
;
SHELXL-2013 (Sheldrick, 2015b)
;
_computing_structure_refinement
;
SHELXL-2013 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.936
_diffrn_measurement_device_type  'Bruker APEX CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            16693
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.027
_diffrn_reflns_theta_min         2.767
_exptl_absorpt_coefficient_mu    1.771
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5692
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Bruker, 2008)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.911
_exptl_crystal_description       block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.521
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.165
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3368
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.0447
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0471P)^2^+5.9483P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1056
_reflns_number_gt                2963
_reflns_number_total             3368
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5493sup1.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C7 H12.40 N Ni O9.70'
_cod_database_code               2311595
_shelx_estimated_absorpt_t_min   0.593
_shelx_estimated_absorpt_t_max   0.816
_shelx_hkl_checksum              31174
_shelx_res_checksum              49969
_shelxl_version_number           20.13