Pd(ii) complexes with amide-based macrocycles: syntheses, properties and applications in cross-coupling reactions
Kumar, Sushil; Jha, Rajeev Ranjan; Yadav, Sunil; Gupta, Rajeev; New J. Chem. 39 (2015) 2042–; doi:10.1039/C4NJ01300J

data_7054630
_publ_section_title
;
 Pd(ii) complexes with amide-based macrocycles: syntheses, properties and
 applications in cross-coupling reactions
;
_journal_issue                   3
_journal_name_full               'New J. Chem.'
_journal_page_first              2042
_journal_paper_doi               10.1039/C4NJ01300J
_journal_volume                  39
_journal_year                    2015
_chemical_formula_moiety         'C17 H24 N4 O2 Pd'
_chemical_formula_sum            'C17 H24 N4 O2 Pd'
_chemical_formula_weight         422.80
_chemical_name_systematic
;
?
;
_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
_audit_update_record
;
2011-10-16 deposited with the CCDC.
2015-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 106.046(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   9.864(5)
_cell_length_b                   10.537(5)
_cell_length_c                   17.033(5)
_cell_measurement_reflns_used    2355
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      67.45
_cell_measurement_theta_min      5.10
_cell_volume                     1701.4(13)
_computing_cell_refinement       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlisPro, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.872
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4748
_diffrn_reflns_theta_full        67.46
_diffrn_reflns_theta_max         67.46
_diffrn_reflns_theta_min         4.99
_exptl_absorpt_coefficient_mu    8.944
_exptl_absorpt_correction_T_max  0.5347
_exptl_absorpt_correction_T_min  0.1680
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.183
_refine_diff_density_min         -1.669
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.0014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         2680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0589
_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^)+(0.1225P)^2^+13.1922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2052
_reflns_number_gt                2355
_reflns_number_total             2680
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01300j2.cif
_cod_data_source_block           skpdl12-2
_cod_depositor_comments
'Adding full bibliography for 7054627--7054630.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7054630