Polyoxometalate templated silver-bisphosphine sandwich: structurally tunable hybrid materials
Yao, Sheng-Jie; Qi, Zhen-Qing; Jiang, Zhan-Guo; Zhan, Cai-Hong; CrystEngComm 26 (2024) 1798–1805; doi:10.1039/D4CE00106K

data_7248223
_publ_section_title
;
 Polyoxometalate templated silver-bisphosphine sandwich: structurally
 tunable hybrid materials
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1798
_journal_page_last               1805
_journal_paper_doi               10.1039/D4CE00106K
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'O40 P W12, 2(C54 H52 Ag2 P4)'
_chemical_formula_sum            'C108 H104 Ag4 O40 P9 W12'
_chemical_formula_weight         4958.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-05
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6392)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-02-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.668(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.7042(10)
_cell_length_b                   22.4607(16)
_cell_length_c                   20.2442(15)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.25
_cell_volume                     6966.9(8)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'BRUKER D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1065
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            92378
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.248
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.580
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1151 before and 0.0804 after correction.
The Ratio of minimum to maximum transmission is 0.6753.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.364
_exptl_crystal_description       block
_exptl_crystal_F_000             4566
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.852
_refine_diff_density_min         -3.256
_refine_diff_density_rms         0.369
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13212
_refine_ls_number_restraints     1014
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1177P)^2^+94.1975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1911
_refine_ls_wR_factor_ref         0.2166
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8949
_reflns_number_total             13212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00106k2.cif
_cod_data_source_block           1234_a
_cod_depositor_comments
'Adding full bibliography for 7248221--7248224.cif.'
_cod_database_code               7248223
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.418
_shelx_estimated_absorpt_t_min   0.363
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within
3.8A
3. Others
 Fixed Sof: O22(0.5) O19(0.5) O20(0.5) O21(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C26(H26A,H26B), C25(H25A,H25B), C27(H27A,H27B), C26(H26A,
 H26B), C25(H25A,H25B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11),
 C12(H12), C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20),
  C21(H21), C23(H23), C24(H24), C2(H2), C3(H3), C5(H5), C6(H6), C1(H1), C7(H7),
 C8(H8), C9(H9), C11(H11), C12(H12), C18(H18), C17(H17), C15(H15), C14(H14),
 C13(H13), C19(H19), C20(H20), C21(H21), C23(H23), C24(H24)
4.c Fitted hexagon refined as free rotating group:
 C1(C2,C3,C4,C5,C6), C7(C8,C9,C10,C11,C12), C13(C14,C15,C16,C17,C18), C19(C20,
 C21,C22,C23,C24), C2(C3,C4,C5,C6,C1), C7(C8,C9,C10,C11,C12), C18(C17,C16,C15,
 C14,C13), C19(C20,C21,C22,C23,C24)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56882
_shelx_fab_checksum              24184
_olex2_submission_special_instructions 'No special instructions were received'