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_4341628
_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 Mn2.40 N4 Na12 O120 Sb2 W19.60'
_chemical_formula_sum            'C8 H99.6 Mn2.4 N4 Na12 O120 Sb2 W19.6'
_chemical_formula_weight         6427.21
_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             2014-09-12T10:32:45-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                69.160(3)
_cell_angle_beta                 71.318(3)
_cell_angle_gamma                87.719(2)
_cell_formula_units_Z            1
_cell_length_a                   13.8331(4)
_cell_length_b                   14.6798(3)
_cell_length_c                   15.7557(5)
_cell_measurement_reflns_used    10357
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3384
_cell_measurement_theta_min      1.5563
_cell_volume                     2822.65(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
;
        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    'OLEX 2 (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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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      0.0524017
_diffrn_orient_matrix_UB_12      0.0121718
_diffrn_orient_matrix_UB_13      -0.0091687
_diffrn_orient_matrix_UB_21      0.0124618
_diffrn_orient_matrix_UB_22      -0.0039332
_diffrn_orient_matrix_UB_23      -0.045808
_diffrn_orient_matrix_UB_31      -0.0070164
_diffrn_orient_matrix_UB_32      0.0502809
_diffrn_orient_matrix_UB_33      -0.0204286
_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  0.037
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14573
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    20.781
_exptl_absorpt_correction_T_max  0.34
_exptl_absorpt_correction_T_min  0.027
_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            orange
_exptl_crystal_density_diffrn    3.781
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2880
_exptl_crystal_size_max          0.5723
_exptl_crystal_size_mid          0.0747
_exptl_crystal_size_min          0.0592
_refine_diff_density_max         3.84
_refine_diff_density_min         -4.771
_refine_diff_density_rms         0.457
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         9892
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0818P)^2^+8.4330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1264
_reflns_number_gt                9096
_reflns_number_total             9892
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502232v_si_002.cif
_cod_data_source_block           1-SbMn
_cod_depositor_comments
'Adding full bibliography for 4341628--4341641.cif.'
_cod_original_cell_volume        2822.65(13)
_cod_original_formula_sum        'C8 H99.60 Mn2.40 N4 Na12 O120 Sb2 W19.60'
_cod_database_code               4341628