Two Inorganic-Organic Hybrid Silver-Polyoxometalates as Reusable Catalyst for One-Pot Synthesis of Propargylamines via Three-Component Coupling Reaction at Room Temperature
Dou, Ming-Yu; Huang, Xianqiang; Yang, Guo-Yu; CrystEngComm  (2020) –; doi:10.1039/D0CE00042F

data_7240124
_publ_section_title
;
 Two Inorganic-Organic Hybrid Silver-Polyoxometalates as Reusable Catalyst
 for One-Pot Synthesis of Propargylamines via Three-Component Coupling
 Reaction at Room Temperature
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00042F
_journal_year                    2020
_chemical_formula_sum            'C40 H58 Ag3 N10 O46 P S6 W12'
_chemical_formula_weight         4168.10
_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   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-10-17 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                98.1610(10)
_cell_angle_beta                 101.089(2)
_cell_angle_gamma                101.148(2)
_cell_formula_units_Z            1
_cell_length_a                   11.6301(11)
_cell_length_b                   13.3660(12)
_cell_length_c                   15.5869(13)
_cell_measurement_reflns_used    2288
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.163
_cell_measurement_theta_min      2.265
_cell_volume                     2292.1(4)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.1352
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11714
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         2.265
_exptl_absorpt_coefficient_mu    15.849
_exptl_absorpt_correction_T_max  0.1626
_exptl_absorpt_correction_T_min  0.1282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.020
_exptl_crystal_description       block
_exptl_crystal_F_000             1876
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         5.814
_refine_diff_density_min         -2.531
_refine_diff_density_rms         0.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.923
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         7930
_refine_ls_number_restraints     1797
_refine_ls_restrained_S_all      0.860
_refine_ls_R_factor_all          0.1331
_refine_ls_R_factor_gt           0.0815
_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^)+(0.1280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2284
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4246
_reflns_number_total             7930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00042f2.cif
_cod_data_source_block           160227b
_cod_database_code               7240124
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.128
_shelx_estimated_absorpt_t_max   0.163
_shelx_res_checksum              52836