Heterometallic Hydride Complexes of Rare-Earth Metals and Ruthenium through C‒H Bond Activation
Sobaczynski, Adam P.; Bauer, Tobias; Kempe, Rhett; Organometallics 32 (2013) 1363–; doi:10.1021/om301039g

data_4080278
_publ_section_title
;
 Heterometallic Hydride Complexes of Rare-Earth Metals and Ruthenium
 through C--H Bond Activation
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1363
_journal_paper_doi               10.1021/om301039g
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C71 H104 Lu2 O2 P4 Ru2'
_chemical_formula_weight         1665.50
_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                97.095(4)
_cell_angle_beta                 112.040(3)
_cell_angle_gamma                110.461(4)
_cell_formula_units_Z            2
_cell_length_a                   15.0930(7)
_cell_length_b                   15.5230(8)
_cell_length_c                   18.3880(8)
_cell_measurement_reflns_used    23032
_cell_measurement_temperature    133(2)
_cell_volume                     3576.8(4)
_computing_cell_refinement       X-AREA-STOE
_computing_data_collection       X-AREA-STOE
_computing_data_reduction        X-AREA-STOE
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR-97
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  STOE-IPDSII
_diffrn_measurement_method       Omega-Scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1239
_diffrn_reflns_av_sigmaI/netI    0.1104
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12016
_diffrn_reflns_theta_full        24.63
_diffrn_reflns_theta_max         24.63
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    3.280
_exptl_absorpt_correction_T_max  0.6143
_exptl_absorpt_correction_T_min  0.3130
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.281
_refine_diff_density_min         -1.649
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.742
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         12016
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.743
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                7201
_reflns_number_total             12016
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om301039g_si_004.cif
_cod_data_source_block           t277apma
_cod_original_cell_volume        3576.8(3)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4080278
_cell_measurement_2theta_min     2.50
_cell_measurement_2theta_max     50.04