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_7244634
_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         'C54 H106 Co3 Mo26 N24 O92'
_chemical_formula_sum            'C54 H106 Co3 Mo26 N24 O92'
_chemical_formula_weight         5234.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc29cpds
_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                98.809(2)
_cell_angle_beta                 102.976(2)
_cell_angle_gamma                93.813(2)
_cell_formula_units_Z            1
_cell_length_a                   12.4509(17)
_cell_length_b                   16.733(2)
_cell_length_c                   19.224(3)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.64
_cell_volume                     3835.6(9)
_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 0.990
_diffrn_measured_fraction_theta_max 0.973
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0563
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27348
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.421
_diffrn_reflns_theta_min         1.688
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.455
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5151
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0719 before and 0.0432 after correction.
The Ratio of minimum to maximum transmission is 0.6908.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.266
_exptl_crystal_description       block
_exptl_crystal_F_000             2507
_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 P-1
CELL   12.4509   16.7330   19.2240     98.81    102.98     93.81
SPGR P-1
Q101 0.901 0.823 0.167 !       9.13 eA-3
C102 0.809 0.296 0.338 !       6.16 eA-3
Q103 0.688 0.437 0.469 !       4.58 eA-3
Q104 1.000 0.500 0.500 !       4.43 eA-3
C105 0.860 0.322 0.239 !       4.10 eA-3
C106 0.876 0.137 0.383 !       3.44 eA-3
C107 0.058 0.054 0.459 !       3.32 eA-3
C108 0.361 0.935 0.024 !       2.74 eA-3
C109 0.767 0.906 0.080 !       2.70 eA-3
C110 0.812 0.093 0.215 !       2.56 eA-3
Q111 0.404 0.130 0.421 !       2.41 eA-3
Q112 0.374 0.450 0.153 !       2.31 eA-3
C113 0.859 0.020-0.003 !       2.31 eA-3
C114 0.763 0.221 0.370 !       2.30 eA-3
Q115 0.501 0.586 0.421 !       2.21 eA-3
Q116 0.860 0.489 0.007 !       2.11 eA-3
Q117 0.738 0.757 0.437 !       2.09 eA-3
C118 0.562 0.992 0.080 !       2.07 eA-3
Q119 0.095 0.455 0.158 !       2.02 eA-3
Q120 0.047 0.639 0.121 !       2.01 eA-3
Q121 0.512 0.835 0.395 !       2.01 eA-3
Q122 0.627 0.023 0.483 !       1.98 eA-3
Q123 0.452 0.846 0.407 !       1.96 eA-3
Q124 0.346 0.155 0.435 !       1.93 eA-3
Q125 0.687 0.889 0.346 !       1.92 eA-3
Q126 0.186 0.329 0.023 !       1.92 eA-3
Q127 0.574 0.039 0.499 !       1.90 eA-3
Q128 0.283 0.579 0.279 !       1.84 eA-3
Q129 0.450 0.609 0.435 !       1.84 eA-3
Q130 0.327 0.452 0.176 !       1.82 eA-3
Q131 0.453 0.114 0.411 !       1.82 eA-3
Q132 0.534 0.989 0.303 !       1.80 eA-3
C133 0.606 0.983 0.114 !       1.79 eA-3
Q134 0.374 0.140 0.393 !       1.79 eA-3
C135 0.874 0.222 0.012 !       1.75 eA-3
Q136 0.563 0.812 0.444 !       1.73 eA-3
Q137 0.984 0.641 0.080 !       1.72 eA-3
Q138 0.781 0.730 0.490 !       1.67 eA-3
Q139 0.294 0.599 0.258 !       1.67 eA-3
Q140 0.081 0.509 0.018 !       1.66 eA-3
Q141 0.408 0.428 0.205 !       1.66 eA-3
Q142 0.740 0.867 0.333 !       1.65 eA-3
Q143 0.343 0.986 0.488 !       1.64 eA-3
Q144 0.127 0.324 0.050 !       1.63 eA-3
Q145 0.562 0.818 0.374 !       1.62 eA-3
C146 0.942 0.217 0.136 !       1.60 eA-3
Q147 0.457 0.608 0.369 !       1.59 eA-3
Q148 0.310 0.500 0.157 !       1.58 eA-3
Q149 0.190 0.511 0.027 !       1.57 eA-3
Q150 0.072 0.627 0.159 !       1.54 eA-3
Q151 0.345 0.585 0.251 !       1.54 eA-3
Q152 0.483 0.999 0.316 !       1.53 eA-3
Q153 0.145 0.317-0.001 !       1.52 eA-3
Q154 0.799 0.737 0.422 !       1.51 eA-3
Q155 0.167 0.446 0.207 !       1.51 eA-3
C156 0.922 0.177 0.060 !       1.51 eA-3
C157 0.922 0.183 0.187 !       1.50 eA-3
Q158 0.358 0.596 0.301 !       1.49 eA-3
Q159 0.468 0.112 0.471 !       1.48 eA-3
C160 0.956 0.133 0.082 !       1.48 eA-3
Q161 0.499 0.991 0.269 !       1.48 eA-3
Q162 0.032 0.473 0.168 !       1.48 eA-3
Q163 0.685 0.008 0.466 !       1.48 eA-3
C164 0.777 0.188 0.124 !       1.47 eA-3
Q165 0.687 0.772 0.452 !       1.46 eA-3
C166 0.986 0.165 0.114 !       1.42 eA-3
Q167 0.453 0.448 0.193 !       1.42 eA-3
Q168 0.717 0.730 0.407 !       1.41 eA-3
Q169 0.686 0.758 0.401 !       1.39 eA-3
Q170 0.373 0.624 0.438 !       1.38 eA-3
Q171 0.983 0.640 0.147 !       1.37 eA-3
Q172 0.705 0.894 0.298 !       1.35 eA-3
Q173 0.795 0.865 0.309 !       1.35 eA-3
Q174 0.154 0.453 0.136 !       1.33 eA-3
Q175 0.653 0.704 0.269 !       1.33 eA-3
Q176 0.529 0.912 0.488 !       1.32 eA-3
C177 0.846 0.251 0.026 !       1.31 eA-3
Q178 0.607 0.981 0.347 !       1.30 eA-3
Q179 0.328 0.424 0.115 !       1.29 eA-3
C180 0.769 0.947 0.158 !       1.28 eA-3
Q181 0.577 0.039 0.438 !       1.28 eA-3
Q182 0.904 0.478 0.050 !       1.27 eA-3
Q183 0.470 0.865 0.355 !       1.26 eA-3
Q184 0.464 0.073 0.421 !       1.26 eA-3
Q185 0.222 0.607 0.281 !       1.23 eA-3
Q186 0.545 0.597 0.452 !       1.23 eA-3
C187 0.933 0.154 0.249 !       1.22 eA-3
Q188 0.162 0.081 0.484 !       1.22 eA-3
Q189 0.871 0.610 0.317 !       1.22 eA-3
C190 0.768 0.240 0.107 !       1.22 eA-3
C191 0.688 0.923 0.110 !       1.22 eA-3
Q192 0.411 0.566 0.233 !       1.22 eA-3
Q193 0.280 0.552 0.489 !       1.22 eA-3
C194 0.968 0.071 0.001 !       1.21 eA-3
Q195 0.048 0.671 0.090 !       1.21 eA-3
Q196 0.235 0.312 0.017 !       1.21 eA-3
Q197 0.234 0.350 0.076 !       1.20 eA-3
Q198 0.532 0.013 0.442 !       1.20 eA-3
C199 0.876 0.182 0.154 !       1.20 eA-3
;
_refine_diff_density_max         1.808
_refine_diff_density_min         -2.366
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     899
_refine_ls_number_reflns         18771
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      11.852
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0531
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^+18.0662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1477
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14456
_reflns_number_total             18771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00255h2.cif
_cod_data_source_block           4_sq
_cod_database_code               7244634
_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
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O4-N8
 3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Mo7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O1W(H1Wa,H1Wb)
4.b Ternary CH refined with riding coordinates:
 N4(H4), N8(H8), N12(H12)
4.c Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C3(H3a,H3b), C21(H21a,H21b), C6(H6a,H6b), C13(H13a,H13b), C4(H4a,
 H4b), C22(H22a,H22b), C23(H23a,H23b), C14(H14a,H14b), C7(H7a,H7b), C12(H12a,
 H12b), C24(H24a,H24b), C9(H9a,H9b), C16(H16a,H16b), C15(H15a,H15b), C18(H18a,
 H18b), C25(H25a,H25b), C8(H8a,H8b), C27(H27a,H27b), C17(H17a,H17b), C26(H26a,
 H26b)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C19(H19), C20(H20), C11(H11), C1(H1), C10(H10)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'