Synthesis, characterization and crystal structure of the new pentahydrate of bis(2,2'-bipyridine-κ^2^<i>N</i>,<i>N</i>')(oxalato-κ^2^<i>O</i>^1^,<i>O</i>^2^)nickel(II)
Farkašová, Nela; Černák, Juraj; Tomás, Milagros; Falvello, Larry R.; Acta Crystallographica Section C 70 (2014) 477–481; doi:10.1107/S2053229614007499

data_2019518
_publ_section_title
;
 Synthesis, characterization and crystal structure of the new pentahydrate
 of
 bis(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')(oxalato-\k^2^<i>O</i>^1^,<i>O</i>^2^)nickel(II)
;
_journal_coeditor_code           FN3166
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              477
_journal_page_last               481
_journal_paper_doi               10.1107/S2053229614007499
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Ni (C2 O4) (C10 H8 N2)2] , 5H2 O'
_chemical_formula_moiety         'C22 H16 N4 Ni O4, 5(H2 O)'
_chemical_formula_sum            'C22 H26 N4 Ni O9'
_chemical_formula_weight         549.18
_chemical_name_systematic
'Bis(2,2'-bipyridine-\k^2^<i>N</i>,<i>N</i>')(oxalato-\k^2^<i>O</i>^1^,<i>O</i>^2^)nickel(II) pentahydrate'
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.390(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7474(4)
_cell_length_b                   22.7052(9)
_cell_length_c                   9.9647(5)
_cell_measurement_reflns_used    4223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      1.00000
_cell_measurement_theta_min      0.77869
_cell_volume                     2365.50(18)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            21922
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         4.16
_diffrn_standards_number         23587
_exptl_absorpt_coefficient_mu    0.881
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77869
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2012)'
_exptl_crystal_colour            'light purple'
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.290
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0348P)^2^+1.1619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0767
_reflns_number_gt                4730
_reflns_number_total             5415
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3166sup1.cf
_cod_data_source_block           I
_cod_depositor_comments          'Adding full bibliography for 2019518.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2019518
_cod_database_fobs_code          2019518