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_4329348
_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_moiety         'C33 H26 N6 O Ru, F6 P'
_chemical_formula_sum            'C33 H26 F6 N6 O P Ru'
_chemical_formula_weight         768.64
_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                 101.689(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9570(6)
_cell_length_b                   16.4648(7)
_cell_length_c                   16.8146(7)
_cell_measurement_reflns_used    8831
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.57
_cell_measurement_theta_min      1.60
_cell_volume                     3512.7(3)
_computing_cell_refinement       'Bruker APEX II Software Suite, 2008'
_computing_data_collection       'Bruker APEX II Software Suite, 2008'
_computing_data_reduction        'Bruker APEX II Software Suite, 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_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  0.0222
_diffrn_reflns_av_sigmaI/netI    0.0246
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38159
_diffrn_reflns_theta_full        30.57
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6784
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_description       plate
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.522
_exptl_crystal_size_mid          0.458
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.7191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0797
_reflns_number_gt                8831
_reflns_number_total             10714
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300439h_si_002_2.cif
_cod_data_source_block           ac15
_cod_database_code               4329348