Mononuclear palladium and heterodinuclear palladium‒ruthenium complexes of semicarbazone ligands. Synthesis, characterization, and application in C‒C cross-coupling reactions
Datta, Sayanti; Kumar Seth, Dipravath; Halder, Sarmistha; Sheldrick, William S.; Mayer-Figge, Heike; Drew, Michael G. B.; Bhattacharya, Samaresh; RSC Advances 2 (2012) 5254–; doi:10.1039/c2ra20105d

data_7238607
_publ_section_title
;
 Mononuclear palladium and heterodinuclear palladium--ruthenium complexes
 of semicarbazone ligands. Synthesis, characterization, and application in
 C--C cross-coupling reactions
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              5254
_journal_paper_doi               10.1039/c2ra20105d
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C67 H57 Cl N5 O3 P3 Pd Ru'
_chemical_formula_weight         1316.01
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                99.3150(10)
_cell_angle_beta                 103.3020(10)
_cell_angle_gamma                100.3930(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2779(2)
_cell_length_b                   13.7689(2)
_cell_length_c                   22.0341(3)
_cell_measurement_temperature    296(2)
_cell_volume                     2916.58(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.769
_diffrn_measured_fraction_theta_max 0.769
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            44521
_diffrn_reflns_theta_full        40.60
_diffrn_reflns_theta_max         40.60
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.748
_exptl_absorpt_correction_T_max  0.869
_exptl_absorpt_correction_T_min  0.849
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1340.0
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.19
_refine_diff_density_max         1.601
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     730
_refine_ls_number_reflns         28857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_gt           0.0415
_refine_ls_shift/su_max          0.100
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'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          0.1180
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                21050
_reflns_number_total             28857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra20105d.txt
_cod_data_source_block           ms12
_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.

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' 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.

data item '_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7238607