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_4083188
_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         'C30 H39 N O Ru'
_chemical_formula_sum            'C30 H39 N O Ru'
_chemical_formula_weight         530.69
_chemical_name_systematic        '[RuCymQH]'
_chemical_properties_physical    'air-sensitive, oxygen-sensitive'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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                 93.308(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.1014(4)
_cell_length_b                   22.4260(8)
_cell_length_c                   21.4064(7)
_cell_measurement_reflns_used    9128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.47
_cell_measurement_theta_min      2.86
_cell_volume                     5320.5(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 0.974
_diffrn_measured_fraction_theta_max 0.974
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0391
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33359
_diffrn_reflns_theta_full        66.47
_diffrn_reflns_theta_max         66.47
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.917
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Blessing,1995
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             2224
_exptl_crystal_recrystallization_method Pentane
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         9128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0263
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0267P)^2^+2.6580P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0601
_refine_ls_wR_factor_ref         0.0647
_reflns_number_gt                7566
_reflns_number_total             9128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5002815_si_001.cif
_cod_data_source_block           ac95
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4083188