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_1546537
_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         'Co H8 Mo6 O24, 8(H2 O), (H4 N)'
_chemical_formula_sum            'Co H28 Mo6 N O32'
_chemical_formula_weight         1188.78
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-05-15
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.86(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.432(2)
_cell_length_b                   10.997(2)
_cell_length_c                   11.725(2)
_cell_measurement_reflns_used    3293
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.000
_cell_measurement_theta_min      3.302
_cell_volume                     1452.3(5)
_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 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0897
_diffrn_reflns_av_unetI/netI     0.0820
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13481
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.430
_diffrn_reflns_theta_min         3.302
_exptl_absorpt_coefficient_mu    3.179
_exptl_absorpt_correction_T_max  0.530
_exptl_absorpt_correction_T_min  0.237
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1162
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.087
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.207
_refine_ls_extinction_coef       0.0094(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3293
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0757P)^2^+7.8400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1184
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3060
_reflns_number_total             3293
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7nr04373b2.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        1452.2(5)
_cod_database_code               1546537
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All O(H) groups
 At 1.5 times of:
  All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 O6-H6
 0.9 with sigma of 0.02
 H2A-H2B \\sim H2A-H2C \\sim H2A-H2D \\sim H2B-H2C \\sim H2B-H2D \\sim H2C-H2D
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B), O15(H15A,H15B), N2(H2A,H2B), O13(H13A,H13B), O14(H14A,H14B)
3.b Ternary CH refined with riding coordinates:
 O2(H2), O3(H3), O0AA(H0AA)
;