Abnormal carbenes derived from the 1,5-cycloaddition product between azides and alkynes: structural characterization of Pd(ii) complexes and their catalytic properties.
Hohloch, Stephan; Frey, Wolfgang; Su, Cheng-Yong; Sarkar, Biprajit; Dalton transactions (Cambridge, England : 2003) 42 (2013) 11355–11358; doi:10.1039/c3dt51083b

data_7021733
_publ_section_title
;
 Abnormal carbenes derived from the 1,5-cycloaddition product between
 azides and alkynes: structural characterization of Pd(ii) complexes and
 their catalytic properties.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11355
_journal_page_last               11358
_journal_paper_doi               10.1039/c3dt51083b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_sum            'C32 H30 Cl2 N6 Pd'
_chemical_formula_weight         675.92
_chemical_name_systematic
;
?
;
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                 116.214(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.427(3)
_cell_length_b                   8.2599(12)
_cell_length_c                   12.1501(17)
_cell_measurement_reflns_used    1868
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      1.87
_cell_volume                     1479.0(4)
_computing_cell_refinement       'Bruker Kappa Apex II suite, 2008'
_computing_data_collection       'Bruker Kappa Apex II suite, 2008'
_computing_data_reduction        'Bruker Kappa Apex II suite, 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker Kappa Apex II duo'
_diffrn_measurement_method       'Omega psi scan'
_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  0.0501
_diffrn_reflns_av_sigmaI/netI    0.0967
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4408
_diffrn_reflns_theta_full        25.18
_diffrn_reflns_theta_max         25.18
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.521
_refine_diff_density_min         -2.666
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2328
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0620
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0525P)^2^+18.2510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1591
_reflns_number_gt                1868
_reflns_number_total             2328
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51083b.txt
_cod_data_source_block           c:\rechne\sar32
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7021733