Synthesis, characterization, photophysical properties, and catalytic activity of an SCS bis(N-heterocyclic thione) (SCS-NHT) Pd pincer complex.
Tyson, Ginger E.; Tokmic, Kenan; Oian, Casey S.; Rabinovich, Daniel; Valle, Henry U.; Hollis, T. Keith; Kelly, John T.; Cuellar, Kristina A.; McNamara, Louis E.; Hammer, Nathan I.; Webster, Charles Edwin; Oliver, Allen G.; Zhang, Min; Dalton transactions (Cambridge, England : 2003) 44 (2015) 14475–14482; doi:10.1039/c4dt03324h

data_7035759
_publ_section_title
;
 Synthesis, characterization, photophysical properties, and catalytic
 activity of an SCS bis(N-heterocyclic thione) (SCS-NHT) Pd pincer
 complex.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14475
_journal_page_last               14482
_journal_paper_doi               10.1039/c4dt03324h
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C20 H25 Cl N4 Pd S2, C0.5 H Cl'
_chemical_formula_sum            'C20.5 H26 Cl2 N4 Pd S2'
_chemical_formula_weight         569.87
_chemical_properties_physical
'Air-sensitive, Hygroscopic, Oxygen-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-11 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 120.004(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.218(4)
_cell_length_b                   9.2969(11)
_cell_length_c                   18.482(3)
_cell_measurement_reflns_used    9957
_cell_measurement_temperature    120.04
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.22
_cell_volume                     4645.2(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.04
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41942
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.288
_diffrn_reflns_theta_min         1.506
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.9903
_exptl_absorpt_correction_T_min  0.8325
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0440 before and 0.0410 after correction.
The Ratio of minimum to maximum transmission is 0.8407.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.630
_exptl_crystal_description       plate
_exptl_crystal_F_000             2312
_exptl_crystal_recrystallization_method 'Vapour Deposition'
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.992
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         5207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0211P)^2^+10.2658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0521
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4542
_reflns_number_total             5207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03324h2.cif
_cod_data_source_block           get1146
_cod_depositor_comments
'Adding full bibliography for 7035758--7035759.cif.'
_cod_original_formula_sum        'C20.50 H26 Cl2 N4 Pd S2'
_cod_database_code               7035759
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.769
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H28A(0.5) H28B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C21(H21A,H21B), C22(H22A,H22B), C26(H26A,H26B), C29(H29A,
 H29B), C30(H30A,H30B), C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C15(H15), C18(H18), C20(H20), C23(H23), C25(H25), C27(H27)
3.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C24(H24A,H24B,H24C)
;
_shelx_res_checksum              4818
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'