Four POM-based complexes modified by multi-nuclear clusters: structures, photocatalytic, supercapacitor and chromogenic properties
Ma, Shufang; Ying, Jun; Zhang, Yanping; Tian, Aixiang; CrystEngComm  (2022) –; doi:10.1039/D2CE00255H

data_7244635
_publ_section_title
;
 Four POM-based complexes modified by multi-nuclear clusters: structures,
 photocatalytic, supercapacitor and chromogenic properties
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00255H
_journal_year                    2022
_chemical_formula_moiety         '4(Mo12 O40 P), C54 H104 Cl2 Cu3 N24 O6'
_chemical_formula_sum            'C54 H104 Cl2 Cu3 Mo48 N24 O166 P4'
_chemical_formula_weight         8736.13
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc29cm2d
_audit_creation_date             2021-12-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.06.28 svn.raecde09e for OlexSys, GUI svn.r6132)
;
_audit_update_record
;
2021-12-21 deposited with the CCDC.	2022-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.5050(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   19.1589(6)
_cell_length_b                   25.1934(8)
_cell_length_c                   21.8895(7)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.28
_cell_volume                     10532.9(6)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_unetI/netI     0.0983
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            77120
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.451
_diffrn_reflns_theta_min         1.338
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.211
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5149
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0999 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.6905.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'deep green'
_exptl_crystal_density_diffrn    2.755
_exptl_crystal_description       block
_exptl_crystal_F_000             8242
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
TITL 2_a.res in P2(1)/c
CELL   19.1589   25.1934   21.8895     90.00     94.50     90.00
SPGR P21/c
C101 0.647 0.571 0.350 !       5.75 eA-3
C102 0.900 0.694 0.358 !       5.57 eA-3
Q103 0.267 0.945 0.267 !       5.18 eA-3
C104 0.771 0.377 0.165 !       3.14 eA-3
C105 0.118 0.977 0.171 !       3.12 eA-3
C106 0.271 0.922 0.282 !       3.07 eA-3
C107 0.220 0.852 0.338 !       3.00 eA-3
C108 0.909 0.602 0.295 !       2.81 eA-3
Q109 0.765 0.305 0.485 !       2.79 eA-3
C110 1.006 0.477 0.156 !       2.78 eA-3
C111 0.046 0.044 0.321 !       2.61 eA-3
C112 0.865 0.470 0.309 !       2.59 eA-3
C113 0.069 0.041 0.295 !       2.57 eA-3
C114 0.014 0.538 0.971 !       2.53 eA-3
Q115 0.192 0.945 0.689 !       2.51 eA-3
Q116 0.740 0.805 0.725 !       2.50 eA-3
C117 0.048 0.063 0.368 !       2.49 eA-3
C118 0.080 0.499 0.804 !       2.48 eA-3
Q119 0.404 0.601 0.077 !       2.47 eA-3
Q120 0.622 0.055 0.273 !       2.44 eA-3
C121 0.958 0.938 0.605 !       2.44 eA-3
C122 0.982 0.540 0.180 !       2.39 eA-3
C123 0.109 0.077 0.365 !       2.28 eA-3
C124 0.924 0.515 0.165 !       2.28 eA-3
Q125 0.061 0.407 0.350 !       2.27 eA-3
Q126 0.272 0.836 0.780 !       2.26 eA-3
Q127 0.667 0.892 0.052 !       2.25 eA-3
Q128 0.111 0.649 0.093 !       2.21 eA-3
C129 0.080 0.977 0.333 !       2.19 eA-3
C130 0.993 0.047 0.425 !       2.17 eA-3
C131 0.970 0.546 0.142 !       2.17 eA-3
C132 0.980 0.978 0.495 !       2.14 eA-3
Q133 0.348 0.796 0.483 !       2.14 eA-3
Q134 0.626 0.860 0.154 !       2.13 eA-3
Q135 0.316 0.079 0.814 !       2.13 eA-3
Q136 0.733 0.890 0.212 !       2.11 eA-3
C137 0.034 0.954 0.339 !       2.11 eA-3
Q138 0.916 0.890 0.166 !       2.10 eA-3
Q139 0.763 0.234 0.486 !       2.08 eA-3
C140 0.874 0.553 0.917 !       2.07 eA-3
C141 1.003 0.422 0.928 !       2.07 eA-3
C142 0.964 0.991 0.435 !       2.05 eA-3
Q143 0.381 0.298 0.349 !       2.05 eA-3
Q144 0.594 0.156 0.243 !       2.02 eA-3
Q145 0.777 0.054 0.455 !       2.02 eA-3
Q146 0.589 0.249 0.940 !       2.02 eA-3
C147 0.064 0.070 0.430 !       2.01 eA-3
Q148 0.892 0.181 0.382 !       2.01 eA-3
Q149 0.953 0.062 0.428 !       2.01 eA-3
Q150 0.193 0.765 0.173 !       2.01 eA-3
Q151 0.389 0.280 0.076 !       2.00 eA-3
Q152 0.980 0.328 0.406 !       1.99 eA-3
Q153 0.607 0.125 0.262 !       1.98 eA-3
C154 0.925 0.930 0.800 !       1.98 eA-3
Q155 0.780 0.688 0.468 !       1.98 eA-3
Q156 0.372 0.733 0.538 !       1.97 eA-3
Q157 0.346 0.712 0.704 !       1.97 eA-3
Q158 0.710 0.148 0.062 !       1.96 eA-3
C159 0.912 0.562 0.094 !       1.95 eA-3
C160 0.024 0.437 0.023 !       1.95 eA-3
C161 0.178 0.093 0.184 !       1.95 eA-3
C162 0.917 0.547 0.157 !       1.94 eA-3
C163 0.965 0.524 0.102 !       1.94 eA-3
Q164 0.796 0.454 0.972 !       1.94 eA-3
Q165 0.504 0.297 0.848 !       1.93 eA-3
C166 0.934 0.596 0.103 !       1.93 eA-3
Q167 0.596 0.040 0.417 !       1.92 eA-3
Q168 0.893 0.422 0.148 !       1.91 eA-3
C169 0.811 0.556 0.313 !       1.91 eA-3
Q170 0.853 0.897 0.779 !       1.90 eA-3
C171 0.997 0.515 0.926 !       1.90 eA-3
C172 0.063 0.460 0.133 !       1.90 eA-3
Q173 0.875 0.998 0.464 !       1.89 eA-3
C174 0.825 0.915 0.504 !       1.89 eA-3
C175 0.175 0.085 0.496 !       1.89 eA-3
Q176 0.886 0.446 0.328 !       1.88 eA-3
Q177 0.142 0.047 0.610 !       1.87 eA-3
C178 0.935 0.485 0.144 !       1.87 eA-3
Q179 0.839 0.709 0.046 !       1.86 eA-3
C180 0.908 0.991 0.626 !       1.86 eA-3
C181 0.986 0.494 0.133 !       1.86 eA-3
Q182 0.165 0.680 0.109 !       1.85 eA-3
Q183 0.923 0.649 0.026 !       1.84 eA-3
Q184 0.079 0.681 0.079 !       1.84 eA-3
C185 0.917 0.579 0.253 !       1.83 eA-3
Q186 0.905 0.274 0.357 !       1.83 eA-3
Q187 0.529 0.671 0.172 !       1.83 eA-3
C188 0.011 0.031 0.610 !       1.82 eA-3
Q189 0.408 0.812 0.048 !       1.82 eA-3
Q190 0.957 0.412 0.115 !       1.82 eA-3
Q191 0.954 0.759 0.733 !       1.82 eA-3
Q192 0.750 0.712 0.350 !       1.81 eA-3
Q193 0.736 0.351 0.146 !       1.81 eA-3
C194 0.018 0.024 0.460 !       1.81 eA-3
Q195 0.591 0.250 0.837 !       1.80 eA-3
Q196 0.592 0.321 0.359 !       1.79 eA-3
C197 0.023 0.992 0.475 !       1.79 eA-3
Q198 0.114 0.883 0.346 !       1.79 eA-3
Q199 0.151 0.312 0.975 !       1.79 eA-3
;
_refine_diff_density_max         1.687
_refine_diff_density_min         -1.376
_refine_diff_density_rms         0.196
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1357
_refine_ls_number_reflns         26502
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      9.708
_refine_ls_R_factor_all          0.1216
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0493P)^2^+3.0343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1301
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15871
_reflns_number_total             26502
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00255h2.cif
_cod_data_source_block           3_sq
_cod_database_code               7244635
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 O5-O80_$1
 2.8 with sigma of 0.01
 O5-O80_$1 = O30-O63_$1
 3.1 with sigma of 0.01
 O5-O80
 3 with sigma of 0.01
 O41-O78
 3 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 N1(H1), N8(H8), N12(H12)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12a,H12b), C22(H22a,H22b), C23(H23a,H23b), C14(H14a,H14b), C13(H13a,
 H13b), C25(H25a,H25b), C24(H24a,H24b), C21(H21a,H21b), C26(H26a,H26b),
 C15(H15a,H15b), C16(H16a,H16b), C6(H6a,H6b), C5(H5a,H5b), C27(H27a,H27b),
 C7(H7a,H7b), C18(H18a,H18b), C3(H3a,H3b), C1(H1a,H1b), C17(H17a,H17b), C4(H4a,
 H4b), C2(H2a,H2b)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C19(H19), C20(H20), N10(H10a), C8(H8a), C9(H9)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'