Formation of CC-type palladacycles with assistance from an apparently innocent NH(CO) functional group
Jhen-Yi Lee; Yao-Huei Huang; Shu-Ya Liu; Shun-Chu Cheng; Yang-Ming Jhou; Jenn-Huei Lii; Hon Man Lee; Chem.Commun. 48 (2012) 5632–; doi:10.1039/c2cc31299a

data_7107754
_publ_section_title
;
 Formation of CC-type palladacycles with assistance from an apparently
 innocent NH(CO) functional group
;
_journal_name_full               Chem.Commun.
_journal_page_first              5632
_journal_paper_doi               10.1039/c2cc31299a
_journal_volume                  48
_journal_year                    2012
_chemical_formula_moiety         'C33 H27 Cl N4 O Pd, C H2 Cl2'
_chemical_formula_sum            'C34 H29 Cl3 N4 O Pd'
_chemical_formula_weight         722.36
_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                80.665(2)
_cell_angle_beta                 89.264(2)
_cell_angle_gamma                73.218(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8587(2)
_cell_length_b                   11.1511(3)
_cell_length_c                   15.0170(4)
_cell_measurement_reflns_used    2842
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2.6
_cell_volume                     1558.65(7)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'DIAMOND (Brandenburg, 2006)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0627
_diffrn_reflns_av_sigmaI/netI    0.0937
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22102
_diffrn_reflns_theta_full        28.75
_diffrn_reflns_theta_max         28.75
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.887
_exptl_absorpt_correction_T_max  0.8425
_exptl_absorpt_correction_T_min  0.8087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.981
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         8024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0631
_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^)+(0.0333P)^2^+8.9357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1592
_reflns_number_gt                5539
_reflns_number_total             8024
_reflns_threshold_expression     I>2\s
_cod_data_source_file            c2cc31299a.txt
_cod_data_source_block           grl034
_cod_database_code               7107754