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_7054629
_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 O4 Pd'
_chemical_formula_sum            'C17 H24 N4 O4 Pd'
_chemical_formula_weight         454.80
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90.00
_cell_angle_beta                 99.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.4774(4)
_cell_length_b                   10.9664(3)
_cell_length_c                   16.1533(6)
_cell_measurement_reflns_used    3611
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.20
_cell_measurement_theta_min      5.00
_cell_volume                     1829.31(11)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            8698
_diffrn_reflns_theta_full        73.39
_diffrn_reflns_theta_max         73.39
_diffrn_reflns_theta_min         4.90
_exptl_absorpt_coefficient_mu    8.452
_exptl_absorpt_correction_T_max  0.2827
_exptl_absorpt_correction_T_min  0.2467
_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       prism
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         3611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0349
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0429P)^2^+1.0150P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0860
_reflns_number_gt                3228
_reflns_number_total             3611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4nj01300j2.cif
_cod_data_source_block           skpdl-13
_cod_depositor_comments
'Adding full bibliography for 7054627--7054630.cif.'
_cod_original_cell_volume        1829.30(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7054629