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_7017288
_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(C8 H15 N2)'
_chemical_formula_sum            'C36 H52 N6 O6 S2'
_chemical_formula_weight         728.96
_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                88.301(14)
_cell_angle_beta                 88.487(14)
_cell_angle_gamma                85.669(15)
_cell_formula_units_Z            1
_cell_length_a                   8.6734(10)
_cell_length_b                   9.4661(12)
_cell_length_c                   11.6547(13)
_cell_measurement_reflns_used    7938
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     953.5(2)
_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 0.907
_diffrn_measured_fraction_theta_max 0.897
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0434
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8973
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.9882
_exptl_absorpt_correction_T_min  0.9208
_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    1.270
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             390
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0668P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1080
_reflns_number_gt                2506
_reflns_number_total             3378
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt10939a.txt
_cod_data_source_block           compound6
_cod_original_cell_volume        953.46(19)
_cod_database_code               7017288