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_7017290
_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         'C28 H38 N2 O6 S2, 2(C9 H17 N2)'
_chemical_formula_sum            'C46 H72 N6 O6 S2'
_chemical_formula_weight         869.22
_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                 93.811(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   18.7969(13)
_cell_length_b                   8.4216(6)
_cell_length_c                   14.6542(11)
_cell_measurement_reflns_used    1966
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.48
_cell_measurement_theta_min      2.65
_cell_volume                     2314.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE IPDS 2'
_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  0.1533
_diffrn_reflns_av_sigmaI/netI    0.3566
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12521
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9835
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'irregular block'
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.208
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.576
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.576
_refine_ls_R_factor_all          0.2121
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0785
_reflns_number_gt                1353
_reflns_number_total             4879
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt10939a.txt
_cod_data_source_block           compound8c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7017290