Pd(ii)-catalyzed cycloisomerisation of γ-alkynoic acids and one-pot tandem cycloisomerisation/CuAAC reactions in water
García-Álvarez, Joaquín; Díez, Josefina; Vidal, Cristian; Green Chemistry 14 (2012) 3190–; doi:10.1039/c2gc36176k

data_7215081
_publ_section_title
;
 Pd(ii)-catalyzed cycloisomerisation of \g-alkynoic acids and one-pot
 tandem cycloisomerisation/CuAAC reactions in water
;
_journal_issue                   11
_journal_name_full               'Green Chemistry'
_journal_page_first              3190
_journal_paper_doi               10.1039/c2gc36176k
_journal_volume                  14
_journal_year                    2012
_chemical_compound_source        synthesis
_chemical_formula_moiety
'C20 H44 Cl4 N8 O4 P4 Pd2 S2, C4 H10 O, C H2 Cl2'
_chemical_formula_sum            'C25 H56 Cl6 N8 O5 P4 Pd2 S2'
_chemical_formula_weight         1162.28
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.006(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8415(5)
_cell_length_b                   13.0797(5)
_cell_length_c                   28.1381(12)
_cell_measurement_reflns_used    7473
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_volume                     4468.5(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowki & 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, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, 1994)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.051
_diffrn_reflns_av_sigmaI/netI    0.1137
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            31922
_diffrn_reflns_theta_full        25.45
_diffrn_reflns_theta_max         25.45
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.728
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.870
_refine_diff_density_min         -1.208
_refine_diff_density_rms         0.347
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         8114
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0826
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1290
_refine_ls_wR_factor_ref         0.1580
_reflns_number_gt                5223
_reflns_number_total             8114
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2gc36176k.txt
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7215081