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_1541931
_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, CoC6H24N6, C2H8N2, H2O'
_chemical_formula_sum            'C18 H90 Co3 N18 O51 Sb6 V15'
_chemical_formula_weight         3046.47
_chemical_name_common            '[Co(ethylendiamine)3]3{V15Sb6O42}*9H2O'
_chemical_name_systematic
; 
 '[Co(C2H8N2)3]3{V15Sb6O42}*9H2O'  
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-10-23 deposited with the CCDC.
2016-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 126.360(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.2302(14)
_cell_length_b                   22.6142(16)
_cell_length_c                   14.4067(11)
_cell_measurement_reflns_used    10404
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.52
_cell_volume                     4783.0(8)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0647
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            19592
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.639
_exptl_absorpt_correction_T_max  0.6407
_exptl_absorpt_correction_T_min  0.5249
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-Shape (STOE & CIE, 1998)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2928
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
;
_refine_diff_density_max         1.867
_refine_diff_density_min         -1.609
_refine_diff_density_rms         0.177
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         10404
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0453
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0854P)^2^+1.8281P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1149
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                9465
_reflns_number_total             10404
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc04571a2.cif
_cod_data_source_block           mh133
_cod_depositor_comments
'Adding full bibliography for 1541930--1541933.cif.'
_cod_original_cell_volume        4783.0(6)
_cod_original_sg_symbol_H-M      C2
_cod_database_code               1541931