Sulfonate-tagged 1,4-diazabutadiene (DAD(S)) ligands and their noble-metal complexes - synthesis, characterization and immobilization in ionic liquids.
Oelkers, Benjamin; Sundermeyer, Jörg; Dalton transactions (Cambridge, England : 2003) 40 (2011) 12727–12741; doi:10.1039/c1dt10939a

data_7017287
_publ_section_title
;
 Sulfonate-tagged 1,4-diazabutadiene (DAD(S)) ligands and their
 noble-metal complexes - synthesis, characterization and immobilization in
 ionic liquids.
;
_journal_issue                   47
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12727
_journal_page_last               12741
_journal_paper_doi               10.1039/c1dt10939a
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C20 H22 N2 O6 S2, 2(C6 H16 N)'
_chemical_formula_sum            'C32 H54 N4 O6 S2'
_chemical_formula_weight         654.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.533(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.7780(14)
_cell_length_b                   7.2899(9)
_cell_length_c                   14.6759(11)
_cell_measurement_reflns_used    4816
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     1758.8(3)
_computing_cell_refinement       'STOE Cell'
_computing_data_collection       'STOE Expose'
_computing_data_reduction        'STOE Integrate'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'STOE IPDS 1'
_diffrn_measurement_method       'rotation method'
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13370
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.90
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.9665
_exptl_absorpt_correction_T_min  0.9528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular plate'
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.761
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3200
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.761
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0381P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0828
_reflns_number_gt                1562
_reflns_number_total             3200
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt10939a.txt
_cod_data_source_block           compound4a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017287