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_7244632
_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
'2(Mo12 O40 P), C18 H41 Cu N8 O5, 4(H2 O), C9 H17 N4 O'
_chemical_formula_sum            'C27 H66 Cu Mo24 N12 O90 P2'
_chemical_formula_weight         4426.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc29cp4j
_audit_creation_date             2021-12-15
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7092(4)
_cell_length_b                   22.2121(6)
_cell_length_c                   30.2861(8)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.27
_cell_volume                     9895.1(5)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0472
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            73422
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.258
_diffrn_reflns_theta_min         1.137
_diffrn_source_current           30.0
_diffrn_source_power             1.2
_diffrn_source_voltage           40.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.295
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5693
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0750 before and 0.0370 after correction.
The Ratio of minimum to maximum transmission is 0.7634.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.972
_exptl_crystal_description       block
_exptl_crystal_F_000             8396
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.651
_refine_diff_density_min         -1.409
_refine_diff_density_rms         0.171
_refine_ls_abs_structure_details
;
 Flack x determined using 7966 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1423
_refine_ls_number_reflns         24459
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0435P)^2^+8.3578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0938
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                20144
_reflns_number_total             24459
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00255h2.cif
_cod_data_source_block           2
_cod_database_code               7244632
_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
 H87B-H21B
 2.55 with sigma of 0.01
 H4-H85A
 2.22 with sigma of 0.01
 H4-H85B
 2.15 with sigma of 0.01
 H87A-H12
 2.15 with sigma of 0.01
 H6-H90A
 2.15 with sigma of 0.01
 H86A-H88A
 2.15 with sigma of 0.01
 Cu1-H88A \\sim Cu1-H88B
 with sigma of 0.02
 Cu1-H89A \\sim Cu1-H89B
 with sigma of 0.02
3. Rigid bond restraints
 O86
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.0025
4. Uiso/Uaniso restraints and constraints
Uanis(O86) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O90) \\sim Ueq, Uanis(O86) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5.a Free rotating group:
 O85(H85A,H85B), O84(H84A,H84B), O88(H88A,H88B), O89(H89A,H89B), O86(H86A,
 H86B), O87(H87A,H87B)
5.b Ternary CH refined with riding coordinates:
 N4(H4), N8(H8), N12(H12)
5.c Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C5(H5A,H5B), C6(H6A,H6B), C17(H17A,H17B),
 C12(H12A,H12B), C27(H27A,H27B), C16(H16A,H16B), C14(H14A,H14B), C7(H7A,H7B),
 C25(H25A,H25B), C23(H23A,H23B), C26(H26A,H26B), C9(H9A,H9B), C18(H18A,H18B),
 C3(H3A,H3B), C8(H8A,H8B), C24(H24A,H24B), C4(H4A,H4B), C22(H22A,H22B),
 C21(H21A,H21B)
5.d Aromatic/amide H refined with riding coordinates:
 N6(H6), C10(H10), C1(H1), C2(H2), C11(H11), C20(H20), C19(H19)
5.e X=CH2 refined with riding coordinates:
 O90(H90A,H90B)
;
_olex2_submission_special_instructions 'No special instructions were received'