Filling Gaps in the Series of Noninnocent Hetero-1,3-diene Chelate Ligands: Ruthenium Complexes of Redox-Active α-Azocarbonyl and α-Azothiocarbonyl Ligands RNNC(R')E, E = O or S
Fabian Ehret; Martina Bubrin; Ralph Hübner; David Schweinfurth; Ingo Hartenbach; Stanislav Záliš; Wolfgang Kaim; Inorganic Chemistry 51 (2012) 6237–6244; doi:10.1021/ic300439h

data_4329347
_publ_contact_author_address
;
Universitaet Stuttgart,
Institut fuer Anorganische Chemie,
Pfaffenwaldring 55,
Stuttgart, D-70569
Germany
;
_publ_contact_author_email       ehret@iac.uni-stuttgart.de
_publ_contact_author_fax         '++49(0)711 685 64170'
_publ_contact_author_name        'Ehret Fabian'
_publ_contact_author_phone       '++49(0)711 685 64165'
_publ_section_title
;
 Filling Gaps in the Series of Noninnocent Hetero-1,3-diene Chelate
 Ligands: Ruthenium Complexes of Redox-Active \a-Azocarbonyl and
 \a-Azothiocarbonyl Ligands RNNC(R')E, E = O or S
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6237
_journal_page_last               6244
_journal_paper_doi               10.1021/ic300439h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C24 H28 N2 O6 Ru'
_chemical_formula_weight         541.55
_chemical_name_systematic
; 
 ? 
;
_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                70.921(3)
_cell_angle_beta                 70.309(3)
_cell_angle_gamma                74.557(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7692(4)
_cell_length_b                   12.2019(8)
_cell_length_c                   12.5343(9)
_cell_measurement_reflns_used    5056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.10
_cell_measurement_theta_min      0.41
_cell_volume                     1174.87(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Kappa CCD (Nonius)'
_diffrn_measurement_method       CCD
_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  0.1026
_diffrn_reflns_av_sigmaI/netI    0.1402
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9755
_diffrn_reflns_theta_full        27.12
_diffrn_reflns_theta_max         27.12
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    0.709
_exptl_absorpt_correction_T_max  0.9312
_exptl_absorpt_correction_T_min  0.8680
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Scalepack (W. Minor & Z. Otwinowski)'
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_description       block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1247
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.005
_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^+8.2033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                3541
_reflns_number_total             5140
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300439h_si_002_1.cif
_cod_data_source_block           c:\crystal\x-red\feaug10a
_cod_database_code               4329347