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_4341629
_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 H99.60 Co2.40 N4 Na12 O120 Sb2 W19.60'
_chemical_formula_sum            'C8 H99.6 Co2.4 N4 Na12 O120 Sb2 W19.6'
_chemical_formula_weight         6436.79
_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             2014-09-12T11:16:59-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                68.763(5)
_cell_angle_beta                 71.840(5)
_cell_angle_gamma                87.406(4)
_cell_formula_units_Z            1
_cell_length_a                   13.6242(7)
_cell_length_b                   14.7481(6)
_cell_length_c                   15.6620(9)
_cell_measurement_reflns_used    6351
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.0047
_cell_measurement_theta_min      3.1894
_cell_volume                     2779.0(3)
_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
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
        (compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
        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)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_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 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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      0.0602088
_diffrn_orient_matrix_UB_12      0.0036868
_diffrn_orient_matrix_UB_13      -0.10251
_diffrn_orient_matrix_UB_21      0.0283224
_diffrn_orient_matrix_UB_22      -0.1056104
_diffrn_orient_matrix_UB_23      0.0426105
_diffrn_orient_matrix_UB_31      -0.0990844
_diffrn_orient_matrix_UB_32      -0.038288
_diffrn_orient_matrix_UB_33      -0.0076047
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_av_unetI/netI     0.0932
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18695
_diffrn_reflns_theta_full        67
_diffrn_reflns_theta_max         67
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    44.529
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.198
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    3.846
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2885
_exptl_crystal_size_max          0.0627
_exptl_crystal_size_mid          0.0275
_exptl_crystal_size_min          0.0229
_refine_diff_density_max         2.519
_refine_diff_density_min         -2.589
_refine_diff_density_rms         0.389
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.99
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9901
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.99
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0572P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1336
_reflns_number_gt                7585
_reflns_number_total             9901
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502232v_si_002.cif
_cod_data_source_block           1-SbCo
_cod_depositor_comments
'Adding full bibliography for 4341628--4341641.cif.'
_cod_original_cell_volume        2779.0(2)
_cod_original_formula_sum        'C8 H99.60 Co2.40 N4 Na12 O120 Sb2 W19.60'
_cod_database_code               4341629