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_1541930
_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 H92 N18 Ni3 O52 Sb6 V15'
_chemical_formula_weight         3063.82
_chemical_name_common            '[Ni(ethylendiamine)3]3{V15Sb6O42(H2O)}*9H2O'
_chemical_name_systematic
;
  '[Ni(C2H8N2)3]3{V15Sb6O42(H2O)}*9H2O'
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 126.449(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.2404(7)
_cell_length_b                   22.7636(7)
_cell_length_c                   14.3542(5)
_cell_measurement_reflns_used    8392
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.65
_cell_volume                     4794.2(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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.986
_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  0.0274
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14462
_diffrn_reflns_point_group_measured_fraction_full 0.810
_diffrn_reflns_point_group_measured_fraction_max 0.799
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.002
_diffrn_reflns_theta_min         1.651
_exptl_absorpt_coefficient_mu    3.702
_exptl_absorpt_correction_T_max  0.6693
_exptl_absorpt_correction_T_min  0.4902
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2954
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.258
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_details
;
 Flack x determined using 2492 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         8392
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0385
_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^)+(0.0623P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.580
_reflns_Friedel_fraction_full    0.622
_reflns_Friedel_fraction_max     0.602
_reflns_number_gt                7488
_reflns_number_total             8392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc04571a2.cif
_cod_data_source_block           mh21
_cod_depositor_comments
'Adding full bibliography for 1541930--1541933.cif.'
_cod_database_code               1541930
_shelxl_version_number           2014-3
_shelx_res_checksum              3182