Functionalization of krebs-type polyoxometalates with n,o-chelating ligands: a systematic study.
Artetxe, Beñat; Reinoso, Santiago; San Felices, Leire; Vitoria, Pablo; Pache, Aroa; Martín-Caballero, Jagoba; Gutiérrez-Zorrilla, Juan M; Inorganic chemistry 54 (2015) 241–252; doi:10.1021/ic502232v

data_4341640
_publ_section_title
;
 Functionalization of krebs-type polyoxometalates with n,o-chelating
 ligands: a systematic study.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              241
_journal_page_last               252
_journal_paper_doi               10.1021/ic502232v
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C8 H10 N4 Ni O6'
_chemical_formula_sum            'C8 H10 N4 Ni O6'
_chemical_formula_weight         316.91
_chemical_name_systematic
;
Diaqua-<i>trans</i>-bis(pyrazole-3-carboxylate-\k^2^<i>N</i>,<i>O</i>)
nickel(II) 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-02-18T15:39:04-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 97.216(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.0879(3)
_cell_length_b                   11.2855(6)
_cell_length_c                   9.2686(6)
_cell_measurement_reflns_used    1367
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      72.96
_cell_measurement_theta_min      6.188
_cell_volume                     527.98(5)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'Olex2 (Dolomanov et al., 2009)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector_area_resol_mean 10.4023
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0538962
_diffrn_orient_matrix_UB_12      0.1297923
_diffrn_orient_matrix_UB_13      0.0461067
_diffrn_orient_matrix_UB_21      -0.0095811
_diffrn_orient_matrix_UB_22      0.036036
_diffrn_orient_matrix_UB_23      -0.1608608
_diffrn_orient_matrix_UB_31      -0.3002923
_diffrn_orient_matrix_UB_32      0.0221103
_diffrn_orient_matrix_UB_33      -0.0080355
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2552
_diffrn_reflns_theta_full        64.97
_diffrn_reflns_theta_max         64.97
_diffrn_reflns_theta_min         6.21
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.031
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.97078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
        (compiled Feb  1 2013,16:14:44)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.993
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             324
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.061
_refine_diff_density_max         0.309
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         893
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0244
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.1956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0632
_reflns_number_gt                791
_reflns_number_total             893
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502232v_si_002.cif
_cod_data_source_block           Ni-pzc
_cod_depositor_comments
'Adding full bibliography for 4341628--4341641.cif.'
_cod_original_cell_volume        527.99(6)
_cod_database_code               4341640