Palladacycles of Thioethers Catalyzing Suzuki‒Miyaura C‒C Coupling: Generation and Catalytic Activity of Nanoparticles
Rao, Gyandshwar Kumar; Kumar, Arun; Kumar, Satyendra; Dupare, Umesh B.; Singh, Ajai K.; Organometallics 32 (2013) 2452–; doi:10.1021/om4001956

data_4080637
_publ_section_title
;
 Palladacycles of Thioethers Catalyzing Suzuki--Miyaura C--C Coupling:
 Generation and Catalytic Activity of Nanoparticles
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2452
_journal_paper_doi               10.1021/om4001956
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C23 H24 Cl N O2 Pd S, C H Cl3'
_chemical_formula_sum            'C24 H25 Cl4 N O2 Pd S'
_chemical_formula_weight         639.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                86.059(5)
_cell_angle_beta                 86.844(5)
_cell_angle_gamma                80.961(5)
_cell_formula_units_Z            2
_cell_length_a                   8.948(2)
_cell_length_b                   10.178(3)
_cell_length_c                   14.684(4)
_cell_measurement_reflns_used    1543
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.34
_cell_measurement_theta_min      2.31
_cell_volume                     1316.3(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0953
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9472
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.216
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_meas      1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Cube
_exptl_crystal_F_000             644.0
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.295
_exptl_crystal_size_min          0.207
_refine_diff_density_max         1.012
_refine_diff_density_min         -1.339
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         4578
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.1041
_refine_ls_R_factor_gt           0.0792
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.4524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                3656
_reflns_number_total             4578
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4001956_si_002.cif
_cod_data_source_block           gyn77m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        1316.2(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080637