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_4335087
_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         'C18 H22 Ag N4 O2 P2 S, F6 Sb'
_chemical_formula_sum            'C18 H22 Ag F6 N4 O2 P2 S Sb'
_chemical_formula_weight         764.02
_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                84.351(2)
_cell_angle_beta                 88.7160(10)
_cell_angle_gamma                76.4820(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6584(3)
_cell_length_b                   10.8702(2)
_cell_length_c                   10.9832(3)
_cell_measurement_reflns_used    3899
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_volume                     1231.24(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker, 2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2007)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13103
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         25.24
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    2.177
_exptl_absorpt_correction_T_max  1.066
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 R.H. Blessing, Acta Cryst. (1995), A51, 33-38
;
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       Prism
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.773
_refine_diff_density_min         -1.135
_refine_diff_density_rms         0.272
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4429
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.149
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0839P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                3745
_reflns_number_total             4429
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic400511d_si_002_2.cif
_cod_data_source_block           5b
_cod_database_code               4335087