Visible-light CO2 photoreduction of polyoxometalate-based hybrids with different cobalt clusters
Yao, Wei; Qin, Chao; Xu, Na; Zhou, Jie; Sun, Chunyi; Liu, Li; Su, Zhongmin; CrystEngComm 21 (2019) 6423–; doi:10.1039/C9CE01218D

data_7234154
_publ_section_title
;
 Visible-light CO2 photoreduction of polyoxometalate-based hybrids with
 different cobalt clusters
;
_journal_issue                   42
_journal_name_full               CrystEngComm
_journal_page_first              6423
_journal_paper_doi               10.1039/C9CE01218D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C12 H24 Cl Co3 N18 O43 Si W12, Cl, 6(O)'
_chemical_formula_sum            'C12 H36 Cl2 Co3 N18 O49 Si W12'
_chemical_formula_weight         3698.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                92.8590(10)
_cell_angle_beta                 90.2200(10)
_cell_angle_gamma                95.7360(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7994(10)
_cell_length_b                   13.1541(11)
_cell_length_c                   18.1961(15)
_cell_measurement_reflns_used    3546
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.558
_cell_volume                     3044.3(4)
_computing_cell_refinement       'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection       'APEX2(Bruker, 2005)'
_computing_data_reduction        'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'Shelxl2014 (Sheldrick, 2015b)'
_computing_structure_solution    'ShelXT2014 (Sheldrick, 2015a)'
_diffrn_ambient_temperature      296.15
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II Quazar'
_diffrn_measurement_method       '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_detector       'Bruker APEX II'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17621
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.558
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    23.585
_exptl_absorpt_correction_T_max  0.005
_exptl_absorpt_correction_T_min  0.002
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    4.035
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3286
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.535
_refine_diff_density_min         -1.910
_refine_diff_density_rms         0.351
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.980
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     886
_refine_ls_number_reflns         10690
_refine_ls_number_restraints     1575
_refine_ls_restrained_S_all      0.961
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8086
_reflns_number_total             10690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01218d2.cif
_cod_data_source_block           1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7234153--7234154.cif.'
_cod_database_code               7234154
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.54
_shelx_estimated_absorpt_t_min   0.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9
\\sim N10 \\sim N11 \\sim N12 \\sim N13 \\sim N14 \\sim N15 \\sim N16 \\sim N17
\\sim N18 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim
C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 3.8A with sigma of 0.01 and
sigma for terminal atoms of 0.03
Cl1 \\sim O12 \\sim O26 \\sim O27 \\sim O31 \\sim O37 \\sim O40 \\sim N1 \\sim
N2 \\sim N3 \\sim H3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim H7 \\sim N8
\\sim N9 \\sim N10 \\sim N11 \\sim N12 \\sim N13 \\sim N14 \\sim H14 \\sim N15
\\sim N16 \\sim N17 \\sim N18 \\sim C1 \\sim H1 \\sim C2 \\sim H2 \\sim C3
\\sim C4 \\sim C5 \\sim H5 \\sim C6 \\sim H6 \\sim C7 \\sim C8 \\sim H8 \\sim
C9 \\sim C10 \\sim H10 \\sim C11 \\sim H11 \\sim C12 \\sim H12C \\sim Cl2 \\sim
O1W \\sim O2W \\sim O3W \\sim O4W \\sim O5W \\sim O7W \\sim O6W: within 3.8A
with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(O17) \\sim Ueq, Uanis(O34) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.002
3. Others
 Fixed Sof: O7W(0.5) O6W(0.5)
4.a Rotating group:
 O12(H12A,H12B), O27(H27A,H27B), O40(H40A,H40B)
4.b Aromatic/amide H refined with riding coordinates:
 N3(H3), N7(H7), N12(H12), N13(H13), N14(H14), N16(H16), C1(H1), C2(H2),
 C3(H3A), C4(H4), C5(H5), C6(H6), C7(H7A), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12C)
;
_olex2_submission_special_instructions 'No special instructions were received'