Sonogashira (Cu and amine free) and Suzuki coupling in air catalyzed <i>via</i> nanoparticles formed <i>in situ</i> from Pd( <scp>ii</scp> ) complexes of chalcogenated Schiff bases of 1-naphthaldehyde and their reduced forms
Bhaskar, Renu; Sharma, Alpesh K.; Yadav, Manoj K.; Singh, Ajai K.; Dalton Transactions 46 (2017) 15235–15248; doi:10.1039/C7DT02701J

data_1547502
_publ_section_title
;
 Sonogashira (Cu and amine free) and Suzuki coupling in air catalyzed
 <i>via</i> nanoparticles formed <i>in situ</i> from Pd( <scp>ii</scp> )
 complexes of chalcogenated Schiff bases of 1-naphthaldehyde and their
 reduced forms
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              15235
_journal_page_last               15248
_journal_paper_doi               10.1039/C7DT02701J
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C19 H19 Cl2 N Pd S, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C19.5 H20 Cl3 N Pd S'
_chemical_formula_weight         513.17
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-09-01 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                84.460(4)
_cell_angle_beta                 82.473(4)
_cell_angle_gamma                72.438(4)
_cell_formula_units_Z            4
_cell_length_a                   9.2268(17)
_cell_length_b                   11.055(2)
_cell_length_c                   21.199(4)
_cell_measurement_reflns_used    1156
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.81
_cell_measurement_theta_min      2.42
_cell_volume                     2040.1(7)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.1209
_diffrn_reflns_Laue_measured_fraction_full 0.958
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10511
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.971
_exptl_absorpt_coefficient_mu    1.408
_exptl_absorpt_correction_T_max  0.694
_exptl_absorpt_correction_T_min  0.670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2014)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       Rod
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.819
_refine_diff_density_min         -0.683
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7072
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1330
_refine_ls_R_factor_gt           0.0736
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0603P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4175
_reflns_number_total             7072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02701j2.cif
_cod_data_source_block           C3
_cod_depositor_comments
;

2019-01-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C19 H19 Cl2 N Pd S), C H2 Cl2'
_cod_original_formula_sum        'C39 H40 Cl6 N2 Pd2 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     1026.35
_cod_database_code               1547502
_shelx_estimated_absorpt_t_min   0.670
_shelx_estimated_absorpt_t_max   0.694
_shelxl_version_number           2014-3
_shelx_res_checksum              53448