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_4341639
_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_sum            'C8 H10 Co N4 O6'
_chemical_formula_weight         317.13
_chemical_name_systematic
;
Diaqua-<i>trans</i>-bis(pyrazole-3-carboxylate-\k^2^<i>N</i>,<i>O</i>)
cobalt(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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-21T12:02:35-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.932(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.08740(10)
_cell_length_b                   11.4002(3)
_cell_length_c                   9.2880(2)
_cell_measurement_temperature    100(2)
_cell_volume                     534.74(2)
_computing_cell_refinement       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_collection       'CrysAlisPro (Agilent Technologies, 2011)'
_computing_data_reduction        'CrysAlisPro (Agilent Technologies, 2011)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material
'WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'OLEX2 (Dolomanov, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.2439
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
  1 omega   23.00   48.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -23.5000   57.0000  -30.0000 25

  2 omega   43.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329  178.0000 -120.0000 65

  3 omega   29.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   57.0000   60.0000 61

  4 omega   -7.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   57.0000  -60.0000 107

  5 omega   -2.00   35.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   77.0000   60.0000 37

  6 omega   58.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   77.0000   60.0000 37

  7 omega    4.00  105.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   77.0000  -30.0000 101

  8 omega   35.00   90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329   57.0000 -150.0000 55

  9 omega   93.00  118.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.9329 -178.0000  -90.0000 25
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0482658000
_diffrn_orient_matrix_UB_12      -0.0521726000
_diffrn_orient_matrix_UB_13      -0.0353911000
_diffrn_orient_matrix_UB_21      -0.0178279000
_diffrn_orient_matrix_UB_22      0.0303353000
_diffrn_orient_matrix_UB_23      -0.0672205000
_diffrn_orient_matrix_UB_31      0.1306205000
_diffrn_orient_matrix_UB_32      -0.0151492000
_diffrn_orient_matrix_UB_33      -0.0122830000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4004
_diffrn_reflns_theta_full        26.5
_diffrn_reflns_theta_max         26.5
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96178
_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            orange
_exptl_crystal_density_diffrn    1.97
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             322
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.283
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1110
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0229
_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^)+(0.0233P)^2^+0.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.054
_refine_ls_wR_factor_ref         0.0555
_reflns_number_gt                1025
_reflns_number_total             1110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502232v_si_002.cif
_cod_data_source_block           Co-pzc
_cod_depositor_comments
'Adding full bibliography for 4341628--4341641.cif.'
_cod_database_code               4341639