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_7021734
_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            'C36 H38 Cl2 N6 Pd'
_chemical_formula_weight         732.02
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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                 113.010(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.7893(14)
_cell_length_b                   15.1436(9)
_cell_length_c                   19.3799(11)
_cell_measurement_temperature    100(2)
_cell_volume                     6696.4(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.928
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            38116
_diffrn_reflns_theta_full        66.54
_diffrn_reflns_theta_max         66.54
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    6.210
_exptl_absorpt_correction_T_max  0.5756
_exptl_absorpt_correction_T_min  0.3698
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.104
_refine_diff_density_min         -0.698
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         10976
_refine_ls_number_restraints     815
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+52.7814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2283
_refine_ls_wR_factor_ref         0.2356
_reflns_number_gt                9820
_reflns_number_total             10976
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51083b.txt
_cod_data_source_block           pd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7021734