Redox-controlled delta-Dawson {Mn2^III^W17} polyoxometalate with photocatalytic H2 evolution activity
Yan-Qing Jiao; Chao Qin; Xin-Long Wang; Fu-Hong Liu; Peng Huang; Chun-Gang Wang; Kui-Zhan Shao; Zhong-Min Su; Chem.Commun. 50 (2014) 5961–; doi:10.1039/C3CC47703G

data_7113913
_publ_section_title
;
 Redox-controlled delta-Dawson {Mn2^III^W17} polyoxometalate with
 photocatalytic H2 evolution activity
;
_journal_name_full               Chem.Commun.
_journal_page_first              5961
_journal_paper_doi               10.1039/C3CC47703G
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C12 H68 Cl2 Mn2 N6 O66 W17'
_chemical_formula_sum            'C12 H68 Cl2 Mn2 N6 O66 W17'
_chemical_formula_weight         4658.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 90.000(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   17.607(5)
_cell_length_b                   21.831(5)
_cell_length_c                   22.897(5)
_cell_measurement_reflns_used    7927
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.00
_cell_measurement_theta_min      1.000
_cell_volume                     8801(4)
_computing_cell_refinement       'SMART (Bruker, 1997)'
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1170
_diffrn_reflns_av_sigmaI/netI    0.1122
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21611
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    22.544
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_correction_T_min  0.000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 1996)'
_exptl_crystal_colour            rufous
_exptl_crystal_density_diffrn    3.516
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8208
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.25
_platon_squeeze_details
'                                                                      '
_refine_diff_density_max         2.804
_refine_diff_density_min         -2.448
_refine_diff_density_rms         0.443
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         7915
_refine_ls_number_restraints     1424
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0591
_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^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1564
_reflns_number_gt                6278
_reflns_number_total             7915
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47703g2.cif
_cod_data_source_block           919424
_cod_original_sg_symbol_H-M      cmc2(1)
_cod_database_code               7113913