Waugh type [CoMo9O32]6- cluster with atomically dispersed Co3+ derives from Anderson type [CoMo6O24]3- for photocatalytic oxygen molecule activation
Chen, Yongdong; Zhang, Chaolei; Caoping, Yang; Zhang, Jiangwei; zheng, Kai; Fang, Qihua; Li, Gao; Nanoscale  (2017) –; doi:10.1039/C7NR04373B

data_1546536
_publ_section_title
;
 Waugh type [CoMo9O32]6- cluster with atomically dispersed Co3+ derives
 from Anderson type [CoMo6O24]3- for photocatalytic oxygen molecule
 activation
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/C7NR04373B
_journal_year                    2017
_chemical_formula_moiety         '1(Co1 Mo9 O32), 12(H2 O), 6(H4 N)'
_chemical_formula_sum            'Co H48 Mo9 N6 O44'
_chemical_formula_weight         1758.78
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   difmap
_audit_creation_date             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2.9988
_cell_length_a                   16.1035(7)
_cell_length_b                   16.1035(7)
_cell_length_c                   12.2637(6)
_cell_measurement_reflns_used    1382
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.240
_cell_measurement_theta_min      3.361
_cell_volume                     2754.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2287
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.240
_diffrn_reflns_theta_min         3.361
_exptl_absorpt_coefficient_mu    3.551
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.431
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            atrovirens
_exptl_crystal_density_diffrn    3.209
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2586
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.066
_refine_diff_density_min         -1.582
_refine_diff_density_rms         0.357
_refine_ls_abs_structure_details
;
 Flack x determined using 547 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.49(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     131
_refine_ls_number_reflns         1598
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0682P)^2^+18.8678P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.678
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.751
_reflns_number_gt                1582
_reflns_number_total             1598
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr04373b2.cif
_cod_data_source_block           compound1
_cod_original_cell_volume        2754.2(3)
_cod_database_code               1546536
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 O7-O7_$1
 2.1 with sigma of 0.02
 N1-H1B_$2 = N1-H1D_$2 = N1-H1A_$2 = N1-H1C_$2
 0.9 with sigma of 0.02
 N2-H2D_$3 = N2-H2C_$3 = N2-H2B_$3 = N2-H2A_$3
 0.9 with sigma of 0.02
 O8_$4-O8
 2.1 with sigma of 0.02
 O8-H8A
 0.9 with sigma of 0.02
 O8-H8B
 0.9 with sigma of 0.02
 H8B-H8A
 1.2 with sigma of 0.02
 H1A-H1C \\sim H1A-H1B \\sim H1A-H1D \\sim H1C-H1B \\sim H1C-H1D \\sim H1B-H1D
 with sigma of 0.02
 H2A-H2B \\sim H2A-H2D \\sim H2A-H2C \\sim H2B-H2D \\sim H2B-H2C \\sim H2D-H2C
 with sigma of 0.02
3. Others
 Fixed Sof: H2A(0.5) H2B(0.5) H1D(0.5)
4.a Free rotating group:
 O7(H7A,H7B), N2(H2A,H2B)
;