Low-Valent Ruthenium Complexes of the Non-innocent 2,6-Bis(imino)pyridine Ligand
Gallagher, Michelle; Wieder, Noah L.; Dioumaev, Vladimir K.; Carroll, Patrick J.; Berry, Donald H.; Organometallics 29 (2010) 591–; doi:10.1021/om9009075

data_4067376
_publ_section_title
;
 Low-Valent Ruthenium Complexes of the Non-innocent 2,6-Bis(imino)pyridine
 Ligand
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              591
_journal_paper_doi               10.1021/om9009075
_journal_volume                  29
_journal_year                    2010
_chemical_formula_sum            'C62 H78 N8 Ru2'
_chemical_formula_weight         1137.46
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.895(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.799(3)
_cell_length_b                   26.768(3)
_cell_length_c                   14.9788(17)
_cell_measurement_temperature    143(1)
_cell_volume                     6705.8(14)
_computing_data_collection       'CrystalClear (Rigaku, 1999)'
_computing_data_reduction        'CrystalClear (Rigaku, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      143(1)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       'phi and omega rotations'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18633
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.59
_exptl_absorpt_coefficient_mu    0.489
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  Shape and scale corrections using equivalent reflections.
   Shape function based on spherical harmonics.
   Highest even and odd order for spherical harmonics:  4  and  3
   Laue group:  2/m
   Friedel opposites are equivalent.
;
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
The program SQUUEZE (PLATON) was used to correct the data for disordered 
solvent. Two voids were found that were found to contain electron density 
equal to approximately 12 electrons.
;
_refine_diff_density_max         0.967
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         11719
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1218
_reflns_number_gt                7503
_reflns_number_total             11719
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om9009075_si_002.cif
_cod_data_source_block           UP5031
_cod_original_cell_volume        6706.0(13)
_cod_original_sg_symbol_H-M      'C c      '
_cod_database_code               4067376