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_7240125
_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            'C76 H112 Ag4 N20 O54 S10 Si W12'
_chemical_formula_weight         5156.23
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2019-10-17 deposited with the CCDC.	2020-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                97.1360(10)
_cell_angle_beta                 108.793(2)
_cell_angle_gamma                104.501(2)
_cell_formula_units_Z            1
_cell_length_a                   14.1080(13)
_cell_length_b                   15.0509(14)
_cell_length_c                   16.3421(15)
_cell_measurement_reflns_used    2918
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.447
_cell_volume                     3099.9(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_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_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_sigmaI/netI    0.1263
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15867
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    11.967
_exptl_absorpt_correction_T_max  0.2219
_exptl_absorpt_correction_T_min  0.1878
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.762
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2390
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         5.641
_refine_diff_density_min         -3.712
_refine_diff_density_rms         0.387
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         10734
_refine_ls_number_restraints     2522
_refine_ls_restrained_S_all      0.913
_refine_ls_R_factor_all          0.1372
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.187
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1943
_refine_ls_wR_factor_ref         0.2223
_reflns_number_gt                5896
_reflns_number_total             10734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d0ce00042f2.cif
_cod_data_source_block           160412f
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_sg_symbol_H-M      'P-1   '
_cod_database_code               7240125