New Ag(I)-Iminophosphorane Coordination Polymers as Efficient Catalysts Precursors for the MW-Assisted Meyer-Schuster Rearrangement of Propargylic Alcohols in Water
Joaquín García-Álvarez; Josefina Díez; Cristian Vidal; Cristian Vicent; Inorganic Chemistry 52 (2013) 6533–6542; doi:10.1021/ic400511d

data_4335086
_publ_contact_author
;     Josefina D\'iez
      Departamento de Qu\'imica Org\'anica e Inorg\'anica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33006 Oviedo
      Spain
;
_publ_contact_author_email       jdv@uniovi.es
_publ_contact_author_fax         '0034 98 5103446'
_publ_contact_author_phone       '0034 98 5102960'
_publ_section_title
;
 New Ag(I)-Iminophosphorane Coordination Polymers as Efficient Catalysts
 Precursors for the MW-Assisted Meyer-Schuster Rearrangement of
 Propargylic Alcohols in Water
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6533
_journal_page_last               6542
_journal_paper_doi               10.1021/ic400511d
_journal_volume                  52
_journal_year                    2013
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C52 H104 Ag4 N16 O16 P8 S4, 4(F6 Sb)'
_chemical_formula_sum            'C52 H104 Ag4 F24 N16 O16 P8 S4 Sb4'
_chemical_formula_weight         2959.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_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
_cell_angle_alpha                92.271(3)
_cell_angle_beta                 91.468(3)
_cell_angle_gamma                93.049(3)
_cell_formula_units_Z            2
_cell_length_a                   13.3063(5)
_cell_length_b                   14.7998(5)
_cell_length_c                   25.4223(8)
_cell_measurement_reflns_used    13343
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6683
_cell_measurement_theta_min      2.9934
_cell_volume                     4993.5(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'DIRDIF-2008 ( Beurskens, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.2640
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_device
; 
165 mm Onyx CCD detector in \k-geometry diffractometer
;
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nova (Cu) x-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37861
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         74.50
_diffrn_reflns_theta_min         2.99
_exptl_absorpt_coefficient_mu    17.545
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.969
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.261
_refine_diff_density_min         -1.662
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1168
_refine_ls_number_reflns         18020
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1104
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0883P)^2^+54.2637P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1775
_refine_ls_wR_factor_ref         0.2031
_reflns_number_gt                11929
_reflns_number_total             18020
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400511d_si_002_1.cif
_cod_data_source_block           6a
_cod_database_code               4335086