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_4341637
_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_compound_source        'synthesis as described'
_chemical_formula_moiety
'C8 H74.40 K6 N3.20 Na6 O109 Sb2 W20.40 Zn1.60'
_chemical_formula_sum            'C8 H74.4 K6 N3.2 Na6 O109 Sb2 W20.4 Zn1.6'
_chemical_formula_weight         6431.08
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-24T12:41:48-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                65.534(3)
_cell_angle_beta                 67.844(3)
_cell_angle_gamma                78.232(2)
_cell_formula_units_Z            1
_cell_length_a                   12.2715(3)
_cell_length_b                   15.9492(6)
_cell_length_c                   16.0131(5)
_cell_measurement_reflns_used    11936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3059
_cell_measurement_theta_min      1.6142
_cell_measurement_wavelength     0.71073
_cell_volume                     2637.79(16)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
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_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_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0223164
_diffrn_orient_matrix_UB_12      -0.0317846
_diffrn_orient_matrix_UB_13      -0.0238765
_diffrn_orient_matrix_UB_21      -0.0217004
_diffrn_orient_matrix_UB_22      -0.0368902
_diffrn_orient_matrix_UB_23      0.0448976
_diffrn_orient_matrix_UB_31      -0.0542079
_diffrn_orient_matrix_UB_32      0.0048802
_diffrn_orient_matrix_UB_33      -0.0082897
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17726
_diffrn_reflns_theta_full        26
_diffrn_reflns_theta_max         26
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    23.383
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.25984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.048
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.863
_refine_diff_density_min         -2.834
_refine_diff_density_rms         0.361
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         10357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0384
_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^)+(0.0395P)^2^+68.4571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0943
_refine_ls_wR_factor_ref         0.0969
_reflns_number_gt                9486
_reflns_number_total             10357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502232v_si_002.cif
_cod_data_source_block           3-SbZn
_cod_depositor_comments
'Adding full bibliography for 4341628--4341641.cif.'
_cod_original_cell_volume        2637.79(14)
_cod_original_formula_sum
'C8 H74.40 K6 N3.20 Na6 O109 Sb2 W20.40 Zn1.60'
_cod_database_code               4341637