Structure and Spectroelectrochemical Response of Arene‒Ruthenium and Arene‒Osmium Complexes with Potentially Hemilabile Noninnocent Ligands
Bubrin, Martina; Schweinfurth, David; Ehret, Fabian; Záliš, Stanislav; Kvapilová, Hana; Fiedler, Jan; Zeng, Qiang; Hartl, František; Kaim, Wolfgang; Organometallics 33 (2014) 4973–; doi:10.1021/om5002815

data_4083194
_publ_section_title
;
 Structure and Spectroelectrochemical Response of Arene--Ruthenium and
 Arene--Osmium Complexes with Potentially Hemilabile Noninnocent
 Ligands
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4973
_journal_paper_doi               10.1021/om5002815
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C32 H12 B F24, C31 H41 N O Ru S'
_chemical_formula_sum            'C63 H53 B F24 N O Ru S'
_chemical_formula_weight         1440.00
_chemical_name_systematic        '[RuCymQSMe]BArF'
_chemical_properties_physical
'air-sensitive, oxygen-sensitive, paramagnetic'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                67.150(3)
_cell_angle_beta                 77.622(3)
_cell_angle_gamma                77.104(3)
_cell_formula_units_Z            4
_cell_length_a                   16.1476(9)
_cell_length_b                   22.7330(11)
_cell_length_c                   22.7580(13)
_cell_measurement_reflns_used    32389
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      1.62
_cell_volume                     7428.1(7)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX II Duo'
_diffrn_measurement_method       'Omega + Phi Scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0662
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            121649
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.335
_exptl_absorpt_correction_T_max  0.9785
_exptl_absorpt_correction_T_min  0.8291
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            dark-purple
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2908
_exptl_crystal_recrystallization_method Benzene
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
;
_refine_diff_density_max         1.425
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1671
_refine_ls_number_reflns         32389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0644P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1187
_refine_ls_wR_factor_ref         0.1285
_reflns_number_gt                22018
_reflns_number_total             32389
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5002815_si_001.cif
_cod_data_source_block           ac162
_cod_database_code               4083194