A {Cd4Cl2O14} cluster functionalized sandwich-type tungsto-arsenate as conformation modulator for misfolding Aβ peptide
Hua, Jiai; Wei, Xueman; Ma, Xiang; Jiao, Jinzhe; Chai, Binghui; Wu, Chenbin; Zhang, Changli; Niu, Yulan; CrystEngComm  (2022) –; doi:10.1039/D1CE01637G

data_7244171
_publ_section_title
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 A {Cd4Cl2O14} cluster functionalized sandwich-type tungsto-arsenate as
 conformation modulator for misfolding A\b peptide
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01637G
_journal_year                    2022
_chemical_formula_moiety         'As2 Cd4 Cl2 O68 W18, 6(C3 H12 N2), 6(O)'
_chemical_formula_sum            'C18 H88 As2 Cd4 Cl2 N12 O76 W18'
_chemical_formula_weight         5668.64
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-07-21 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                99.623(3)
_cell_angle_beta                 98.647(3)
_cell_angle_gamma                112.828(2)
_cell_formula_units_Z            1
_cell_length_a                   12.5169(15)
_cell_length_b                   12.5282(16)
_cell_length_c                   15.952(3)
_cell_measurement_reflns_used    1512
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.50
_cell_volume                     2208.5(6)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0939
_diffrn_reflns_av_unetI/netI     0.1708
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11082
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         25.099
_diffrn_reflns_theta_min         1.817
_exptl_absorpt_coefficient_mu    25.189
_exptl_absorpt_correction_T_max  0.0928
_exptl_absorpt_correction_T_min  0.0375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    4.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         4.819
_refine_diff_density_min         -4.747
_refine_diff_density_rms         0.775
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         7727
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0950
_refine_ls_R_factor_gt           0.0799
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0005P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1771
_refine_ls_wR_factor_ref         0.1896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5496
_reflns_number_total             7727
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01637g2.cif
_cod_data_source_block           njy1
_cod_database_code               7244171
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.093
_shelx_estimated_absorpt_t_min   0.037
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H,H) groups
2. Restrained distances
 N5-C7 = C7-C8
 1.47 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(As1) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O7) \\sim
Ueq, Uanis(O9) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq,
Uanis(O13) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O4) \\sim Ueq,
Uanis(O24) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23)
\\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O28) \\sim Ueq,
Uanis(O29) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33)
\\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O14) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(N3) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O3W) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C2(H2), C5(H5), C8(H8)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E), C4(H4D,H4E), C7(H7A,H7B)
4.c Me refined with riding coordinates:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C), N3(H3D,H3E,H3F), N4(H4A,H4B,H4C), N5(H5A,
 H5B,H5C), N6(H6D,H6E,H6F), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C)
;
_shelx_res_checksum              98513
_shelx_hkl_checksum              92216
_olex2_submission_special_instructions 'No special instructions were received'