Controlled interaction of benzaldehyde thiosemicarbazones with palladium: formation of bis-complexes with cis-geometry and organopalladium complexes, and their catalytic application in C‒C and C‒N coupling
Dutta, Jayita; Bhattacharya, Samaresh; RSC Advances 3 (2013) 10707–; doi:10.1039/c3ra40829a

data_7235261
_publ_section_title
;
 Controlled interaction of benzaldehyde thiosemicarbazones with palladium:
 formation of bis-complexes with cis-geometry and organopalladium
 complexes, and their catalytic application in C--C and C--N coupling
;
_journal_issue                   27
_journal_name_full               'RSC Advances'
_journal_page_first              10707
_journal_paper_doi               10.1039/c3ra40829a
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C30 H14 Cl2 N6 Pd S2'
_chemical_formula_weight         531.77
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.686(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.908(4)
_cell_length_b                   26.302(14)
_cell_length_c                   9.794(5)
_cell_measurement_temperature    273(2)
_cell_volume                     2037.0(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0938
_diffrn_reflns_av_sigmaI/netI    0.1014
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9566
_diffrn_reflns_theta_full        20.96
_diffrn_reflns_theta_max         20.96
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.851
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056.0
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         3.022
_refine_diff_density_min         -2.038
_refine_diff_density_rms         0.301
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.80(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4042
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.972
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.1218
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3070
_refine_ls_wR_factor_ref         0.3127
_reflns_number_gt                3668
_reflns_number_total             4042
_reflns_threshold_expression     &gt;2sigma(I)
_cod_data_source_file            c3ra40829a.cif
_cod_data_source_block           jdds6
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7235261