Dye-Polyoxometalate Coordination Polymer as Photodriven Electron Pump for Photocatalytic Radical Coupling Reactions
Ming, Zheng; Zhang, Tiexin; Tian, Wenming; Li, Jianing; Liu, Zhenhui; Liu, Renhai; Liu, Zhongmin; Duan, Chunying; Chemical Communications  (2021) –; doi:10.1039/D1CC04209B

data_7129154
_publ_section_title
;
 Dye-Polyoxometalate Coordination Polymer as Photodriven Electron Pump for
 Photocatalytic Radical Coupling Reactions
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC04209B
_journal_year                    2021
_chemical_formula_moiety
'C264 H192 Cd6 N32 O120 Si3 V6 W30, 17(C3 H7 N O)'
_chemical_formula_sum            'C315 H311 Cd6 N49 O137 Si3 V6 W30'
_chemical_formula_weight         13554.92
_space_group_crystal_system      cubic
_space_group_IT_number           229
_space_group_name_Hall           '-I 4 2 3'
_space_group_name_H-M_alt        'I m -3 m'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2020-10-08 deposited with the CCDC.	2021-10-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.8105(9)
_cell_length_b                   29.8105(9)
_cell_length_c                   29.8105(9)
_cell_measurement_reflns_used    9864
_cell_measurement_temperature    220.01
_cell_measurement_theta_max      26.895
_cell_measurement_theta_min      2.366
_cell_volume                     26491.6(14)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      220.01
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            91696
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.976
_diffrn_reflns_theta_min         2.160
_exptl_absorpt_coefficient_mu    6.889
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5695
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1002 before and 0.0661 after correction.
The Ratio of minimum to maximum transmission is 0.7639.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_description       block
_exptl_crystal_F_000             12656
_platon_squeeze_details
;
TITL 1                I m -3 m     R = 0.12
CELL   29.8105   29.8105   29.8105     90.00     90.00     90.00
SPGR Im-3m
Q101 1.000 0.672-0.003 !       7.90 eA-3
Q102 0.500 0.617 0.000 !       7.53 eA-3
Q103 0.500 0.883 0.117 !       6.74 eA-3
C104 0.250 1.000 0.000 !       6.64 eA-3
Q105 0.373 1.000 0.000 !       6.36 eA-3
C106 0.169 0.497 0.172 !       6.31 eA-3
Q107 0.500 0.258-0.002 !       5.24 eA-3
Q108 0.500 0.500 0.000 !       3.58 eA-3
Q109 0.583 0.947 0.438 !       3.45 eA-3
Q110 0.559 0.679 0.085 !       3.21 eA-3
C111 0.142 0.502 0.141 !       2.83 eA-3
Q112 0.882 0.328 0.004 !       2.81 eA-3
C113 1.000 0.023 0.003 !       2.78 eA-3
C114 1.000 0.086-0.001 !       2.43 eA-3
Q115 0.937 0.454 0.063 !       2.41 eA-3
C116 0.057 0.292 0.053 !       2.08 eA-3
C117 0.063 0.938 0.062 !       2.08 eA-3
Q118 0.480 0.978 0.384 !       2.07 eA-3
C119 0.977 0.023 0.023 !       2.02 eA-3
C120 0.500 0.799 0.193 !       1.98 eA-3
Q121 0.139 0.530 0.169 !       1.84 eA-3
C122 0.139 0.858 0.142 !       1.73 eA-3
Q123 0.163 0.163 0.163 !       1.71 eA-3
Q124 0.303 0.838 0.044 !       1.70 eA-3
C125 0.219 0.995 0.023 !       1.66 eA-3
C126 0.977 0.975 0.148 !       1.66 eA-3
C127 0.500 0.585 0.249 !       1.66 eA-3
C128 0.500 0.615 0.202 !       1.65 eA-3
C129 0.008 0.123 0.013 !       1.65 eA-3
Q130 0.030 0.687 0.000 !       1.64 eA-3
C131 1.000 0.188 0.006 !       1.59 eA-3
C132 0.259 0.016 0.089 !       1.53 eA-3
C133 0.139 0.124 0.124 !       1.53 eA-3
C134 0.533 0.435 0.468 !       1.52 eA-3
C135 0.467 0.565 0.532 !       1.52 eA-3
C136 1.000 0.029 0.251 !       1.50 eA-3
C137 0.469 0.580 0.230 !       1.48 eA-3
Q138 0.591 0.541 0.032 !       1.47 eA-3
C139 0.626 0.377 0.398 !       1.47 eA-3
C140 0.856 0.910 0.149 !       1.47 eA-3
C141 0.044 0.044 0.044 !       1.46 eA-3
C142 1.000 0.041 0.282 !       1.46 eA-3
C143 0.534 0.421 0.437 !       1.45 eA-3
C144 0.966 0.079 0.063 !       1.45 eA-3
C145 0.466 0.579 0.563 !       1.45 eA-3
C146 0.466 0.563 0.579 !       1.45 eA-3
C147 0.607 0.228 0.496 !       1.42 eA-3
Q148 0.876 0.526 0.147 !       1.42 eA-3
C149 0.500 0.651 0.218 !       1.41 eA-3
C150 0.644 0.647 0.475 !       1.40 eA-3
C151 0.726 0.062 0.001 !       1.40 eA-3
Q152 0.090 0.500 0.562 !       1.39 eA-3
Q153 0.590 1.000 0.062 !       1.39 eA-3
Q154 0.063 0.996 0.594 !       1.39 eA-3
Q155 0.408 0.945 0.982 !       1.38 eA-3
Q156 0.189 0.814 0.186 !       1.36 eA-3
Q157 0.054 0.293 0.419 !       1.35 eA-3
C158 0.029 0.732 0.029 !       1.35 eA-3
C159 1.000 0.049 0.115 !       1.34 eA-3
Q160 0.533 0.859-0.002 !       1.32 eA-3
C161 0.471 0.642 0.225 !       1.29 eA-3
C162 0.280 0.038 0.121 !       1.29 eA-3
C163 0.166 0.049 0.165 !       1.29 eA-3
Q164 0.332 0.116 0.116 !       1.26 eA-3
C165 0.148 0.105 0.104 !       1.23 eA-3
Q166 0.729 0.278 0.123 !       1.21 eA-3
Q167 1.000 0.355 0.470 !       1.21 eA-3
C168 0.500 0.587 0.442 !       1.18 eA-3
C169 0.905 0.036 0.941 !       1.17 eA-3
C170 0.524 0.687 0.471 !       1.17 eA-3
Q171 0.873 0.545 0.038 !       1.17 eA-3
C172 0.021 0.925 0.977 !       1.17 eA-3
C173 1.000 0.156-0.003 !       1.16 eA-3
C174 0.122 0.094-0.004 !       1.15 eA-3
C175 0.796 0.455 0.477 !       1.15 eA-3
C176 0.641 0.521 0.204 !       1.15 eA-3
Q177 0.165 0.469 0.029 !       1.13 eA-3
C178 0.880 0.885 0.036 !       1.12 eA-3
Q179 0.759 0.756 0.165 !       1.12 eA-3
Q180 0.296 0.906 0.463 !       1.11 eA-3
C181 0.488 0.396 0.464 !       1.11 eA-3
C182 0.035 0.008 0.049 !       1.11 eA-3
C183 0.048 0.126 0.047 !       1.10 eA-3
Q184 0.436 0.559 0.134 !       1.10 eA-3
Q185 0.576 0.087 0.087 !       1.09 eA-3
Q186 0.765 0.677 0.356 !       1.08 eA-3
C187 0.820 0.234 0.002 !       1.05 eA-3
C188 0.087 0.179 0.094 !       1.05 eA-3
C189 0.906 0.014 0.104 !       1.05 eA-3
Q190 0.979 0.821 0.422 !       1.03 eA-3
Q191 0.408 0.205 0.432 !       1.02 eA-3
Q192 0.420 0.172 0.325 !       1.02 eA-3
Q193 0.938 0.414 0.063 !       1.01 eA-3
C194 0.067 0.087 0.148 !       1.00 eA-3
Q195 0.314 0.420 0.212 !       1.00 eA-3
Q196 0.964 0.959 0.363 !       1.00 eA-3
C197 0.561 0.567 0.249 !       0.99 eA-3
Q198 0.467 1.000 0.023 !       0.99 eA-3
C199 0.239 0.520 0.245 !       0.99 eA-3
;
_refine_diff_density_max         3.935
_refine_diff_density_min         -2.277
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2752
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0776
_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^)+(0.1046P)^2^+1411.4800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2039
_refine_ls_wR_factor_ref         0.2385
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2082
_reflns_number_total             2752
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc04209b2.cif
_cod_data_source_block           1_sq
_cod_original_cell_volume        26492(2)
_cod_database_code               7129154
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{W1, V1}
{V2, W2}
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(V2) = Uanis(W2)
Uanis(W1) = Uanis(V1)
4. Rigid body (RIGU) restrains
 N1, N2, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 V2, O4, O3, V1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: W1(0.41667) W2(0.20833) O5(0.25) N1(0.5) C1(0.5) H1(0.5) C2(0.5)
 H2(0.5) C3(0.5) H3(0.5) C4(0.5) H4(0.5) C5(0.5) C6(0.5) H6(0.5) C7(0.5)
 H7(0.5) C8(0.5) H9(0.5) C10(0.5) C11(0.5) H11(0.5) V1(0.08333) V2(0.04167)
6.a Riding coordinates:
 C9(H9)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C7(H7), C11(H11)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'