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_7035758
_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 H26 N4 S2'
_chemical_formula_sum            'C20 H26 N4 S2'
_chemical_formula_weight         386.57
_chemical_name_systematic        KmTB
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_audit_update_record
;
2015-05-08 deposited with the CCDC.
2015-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.585(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.212(2)
_cell_length_b                   6.9974(6)
_cell_length_c                   26.698(2)
_cell_measurement_reflns_used    8175
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      24.22
_cell_measurement_theta_min      2.33
_cell_volume                     4145.3(6)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      120.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            64400
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.147
_diffrn_reflns_theta_min         0.918
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9161
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0595 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.9161.
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    1.239
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.145
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     472
_refine_ls_number_reflns         9135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0300P)^2^+3.3200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7044
_reflns_number_total             9135
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03324h2.cif
_cod_data_source_block           kmtb
_cod_depositor_comments
'Adding full bibliography for 7035758--7035759.cif.'
_cod_original_cell_volume        4145.4(6)
_cod_database_code               7035758
_shelxl_version_number           2013-3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H1BC)=Sof(H1BD)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=
 Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(1)
 Sof(H1AA)=Sof(H1AB)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=
 Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1AA,H1AB), C1(H1BC,H1BD), C2(H2A,H2B), C3(H3A,H3B), C2A(H2AA,H2AB),
 C3A(H3AA,H3AB), C16(H16A,H16B), C34(H34A,H34B), C36(H36A,H36B), C38(H38A,H38B),
  C40(H40A,H40B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C47(H47A,H47B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C27(H27), C29(H29), C30(H30), C33(H33), C35(H35), C37(H37),
  C39(H39)
3.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C4A(H4AA,H4AB,H4AC), C46(H46A,H46B,H46C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              47138