Oxidant-induced intramolecular triazole formation.
Abraham, Maria L.; Schulze, A. Carina; Korthaus, Alexander; Oppel, Iris M.; Dalton transactions (Cambridge, England : 2003) 42 (2013) 16066–16072; doi:10.1039/c3dt51490k

data_7023577
_publ_section_title
;
 Oxidant-induced intramolecular triazole formation.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16066
_journal_page_last               16072
_journal_paper_doi               10.1039/c3dt51490k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C28 H28 Br3 N6 O3 P Pd'
_chemical_formula_weight         873.63
_chemical_name_common            '[Pd(PEt3)H2Br3L']'
_chemical_name_systematic
;
 (2,4-Dihydro-5-(5-bromo-2-hydroxyphenyl)-4-((5-bromo-2-hydroxyphenyl)
 methyleneamino)-1,2,4-triazol-3-ylidene 5-bromo-2-oxybenzaldehyde 
 hydrazono)-(triethylphosphine)-palladium(ii) 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 111.9570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.2940(8)
_cell_length_b                   20.8512(14)
_cell_length_c                   14.0096(10)
_cell_measurement_reflns_used    6611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.57
_cell_measurement_theta_min      2.18
_cell_volume                     3059.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    SHELXL-97
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42613
_diffrn_reflns_theta_full        28.68
_diffrn_reflns_theta_max         28.68
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    4.618
_exptl_absorpt_correction_T_max  0.5641
_exptl_absorpt_correction_T_min  0.2595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Medium Absorber'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.896
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         4.888
_refine_diff_density_min         -1.174
_refine_diff_density_rms         0.225
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.178(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         15386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0932P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1383
_refine_ls_wR_factor_ref         0.1448
_reflns_number_gt                13496
_reflns_number_total             15386
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51490k.txt
_cod_data_source_block           10-[(pdpet3)h2br3l']
_cod_original_formula_sum        'C28 H28 Br3 N6 O3 P1 Pd1'
_cod_database_code               7023577