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_7248224
_publ_section_title
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 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         '3(C54 H52 Ag2 P4), 2(Mo12 O40 P)'
_chemical_formula_sum            'C162 H156 Ag6 Mo24 O80 P14'
_chemical_formula_weight         6766.22
_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             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                100.6530(10)
_cell_angle_beta                 93.370(2)
_cell_angle_gamma                109.7070(10)
_cell_formula_units_Z            1
_cell_length_a                   14.0626(4)
_cell_length_b                   14.8889(3)
_cell_length_c                   27.6698(7)
_cell_measurement_reflns_used    9433
_cell_measurement_temperature    297.00
_cell_measurement_theta_max      76.00
_cell_measurement_theta_min      3.23
_cell_volume                     5314.0(2)
_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      297.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  'BRUKER D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0707
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            77753
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.156
_diffrn_reflns_theta_min         3.230
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.179
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.114
_exptl_crystal_description       prism
_exptl_crystal_F_000             3268
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.393
_refine_diff_density_min         -1.859
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1315
_refine_ls_number_reflns         22600
_refine_ls_number_restraints     468
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1021
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0533P)^2^+26.1338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1547
_refine_ls_wR_factor_ref         0.1778
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14594
_reflns_number_total             22600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00106k2.cif
_cod_data_source_block           1021_a
_cod_depositor_comments
'Adding full bibliography for 7248221--7248224.cif.'
_cod_database_code               7248224
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.340
_shelx_estimated_absorpt_t_min   0.183
_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 2A with sigma of 0.02 and sigma for terminal atoms of 3.8 within 2A
O5_3 \\sim O21_3 \\sim O16_3 \\sim O20_3 \\sim O22_3 \\sim O6_3 \\sim O18_3
\\sim O8_3 \\sim O9_3 \\sim O17_3 \\sim O19_3 \\sim O14_3 \\sim O10_3 \\sim
O12_3 \\sim O7_3 \\sim O13_3 \\sim O11_3 \\sim O15_3: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
3. Others
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) O4(0.5) O1(0.5) O2(0.5) O3(0.5) O4(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C52(H52A,H52B), C53(H53A,
 H53B), C54(H54A,H54B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
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), C28(H28), C29(H29), C30(H30), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41),
  C42(H42), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50),
 C51(H51), 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)
4.c Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C17,C18)
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_shelx_res_checksum              24871
_olex2_submission_special_instructions 'No special instructions were received'