Catalysis of “outer-phase” oxygen atom exchange reactions by encapsulated “inner-phase” water in {V15Sb6}-type polyoxovanadates
Wendt, Michael; Warzok, Ulrike; Näther, Christian; van Leusen, Jan; Kögerler, Paul; Schalley, Christoph A.; Bensch, Wolfgang; Chem. Sci. 7 (2016) 2684–; doi:10.1039/C5SC04571A

data_1541933
_publ_section_title
;
 Catalysis of &#x201C;outer-phase&#x201D; oxygen atom exchange reactions
 by encapsulated &#x201C;inner-phase&#x201D; water in {V15Sb6}-type
 polyoxovanadates
;
_journal_issue                   4
_journal_name_full               'Chem. Sci.'
_journal_page_first              2684
_journal_paper_doi               10.1039/C5SC04571A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety         'V15Sb6O42, NiC6H24N6, C2H8N2, H2O'
_chemical_formula_sum            'C18 H72 N18 Ni3 O42 Sb6 V15'
_chemical_formula_weight         2883.66
_chemical_name_common            '[Ni(ethylendiamine)3]3{V15Sb6O42}*xH2O'
_chemical_name_systematic
;
 '[Ni(C2H8N2)3]3{V15Sb6O42}*xH2O' 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           150
_space_group_name_Hall           'P 3 2"'
_space_group_name_H-M_alt        'P 3 2 1'
_symmetry_space_group_name_Hall  'P 3 2"'
_symmetry_space_group_name_H-M   'P 3 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   23.7437(5)
_cell_length_b                   23.7437(5)
_cell_length_c                   14.9586(3)
_cell_measurement_reflns_used    38040
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.002
_cell_measurement_theta_min      1.361
_cell_volume                     7303.3(3)
_computing_cell_refinement       'STOE-IPDS Program Package'
_computing_data_collection       'STOE-IPDS Program Package'
_computing_data_reduction        'STOE-IPDS Program Package'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe Imaging Plate Diffraction System'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0717
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            38040
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.002
_diffrn_reflns_theta_min         1.361
_exptl_absorpt_coefficient_mu    3.631
_exptl_absorpt_correction_T_max  0.6543
_exptl_absorpt_correction_T_min  0.5900
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 2013)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4131
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.338
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Flack x determined using 2597 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.028(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         8614
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0896P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1438
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_full    0.973
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7047
_reflns_number_total             8614
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04571a2.cif
_cod_data_source_block           mh1117
_cod_depositor_comments
'Adding full bibliography for 1541930--1541933.cif.'
_cod_database_code               1541933
_shelxl_version_number           2013-4
_shelx_res_checksum              82242