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_7248221
_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
'2(C54 H52 Ag2 P4), 2(C2 H3 N), 2(C3 H7 N O), Mo8 O26'
_chemical_formula_sum            'C118 H124 Ag4 Mo8 N4 O28 P8'
_chemical_formula_weight         3492.96
_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             2023-10-04
_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                 97.1750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2663(4)
_cell_length_b                   20.3743(6)
_cell_length_c                   22.7754(5)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    293.00
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.46
_cell_volume                     6568.2(3)
_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      293.00
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0411
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44774
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.402
_diffrn_reflns_theta_min         2.193
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.766
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     799
_refine_ls_number_reflns         13449
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0434
_refine_ls_R_factor_gt           0.0295
_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^)+(0.0299P)^2^+2.8903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0762
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10669
_reflns_number_total             13449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00106k2.cif
_cod_data_source_block           23_a
_cod_depositor_comments
'Adding full bibliography for 7248221--7248224.cif.'
_cod_database_code               7248221
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.866
_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
2. Restrained distances
 C2_4-N1_4
 1.5 with sigma of 0.02
3. Rigid bond restraints
 N1_3, C1_3, C2_3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
C2'_4 \\sim C3_4 \\sim C3'_4 \\sim C1_4 \\sim C1'_4 \\sim C2_4: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C1_3 \\sim N1_3 \\sim C2_3: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 O1_4, N1_4, C1_4, C2_4, C3_4, C1'_4, C2'_4, C3'_4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
6. Others
 Sof(C1')=Sof(H1')=Sof(C2')=Sof(H2'A)=Sof(H2'B)=Sof(H2'C)=Sof(C3')=Sof(H3'A)=
 Sof(H3'B)=Sof(H3'C)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(H3C)=FVAR(1)
7.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C25(H25A,H25B), C26(H26A,
 H26B), C27(H27A,H27B)
7.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), 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), C1(H1), C1'(H1')
7.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C2'(H2'A,H2'B,H2'C),
 C3'(H3'A,H3'B,H3'C)
;
_shelx_res_checksum              54946
_olex2_submission_special_instructions 'No special instructions were received'