β-Diketiminate Rare Earth Borohydride Complexes: Synthesis, Structure, and Catalytic Activity in the Ring-Opening Polymerization of ε-Caprolactone and Trimethylene Carbonate
Schmid, Matthias; Guillaume, Sophie M.; Roesky, Peter W.; Organometallics 33 (2014) 5392–; doi:10.1021/om500708x

data_4084713
_publ_section_title
;
 \b-Diketiminate Rare Earth Borohydride Complexes: Synthesis, Structure,
 and Catalytic Activity in the Ring-Opening Polymerization of
 \e-Caprolactone and Trimethylene Carbonate
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5392
_journal_paper_doi               10.1021/om500708x
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C37 H61 B N2 O2 Yb'
_chemical_formula_sum            'C37 H61 B N2 O2 Yb'
_chemical_formula_weight         749.74
_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                75.7709(25)
_cell_angle_beta                 84.403(3)
_cell_angle_gamma                85.904(3)
_cell_formula_units_Z            2
_cell_length_a                   8.7800(3)
_cell_length_b                   12.3442(4)
_cell_length_c                   17.6886(5)
_cell_measurement_reflns_used    54479
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.65
_cell_measurement_theta_min      1.70
_cell_volume                     1847.21(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_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  0.0789
_diffrn_reflns_av_sigmaI/netI    0.0501
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22654
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    2.563
_exptl_absorpt_correction_T_max  0.9483
_exptl_absorpt_correction_T_min  0.5960
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.432
_exptl_crystal_size_mid          0.199
_exptl_crystal_size_min          0.062
_refine_diff_density_max         2.973
_refine_diff_density_min         -1.351
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0406
_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^)+(0.0156P)^2^+12.6133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1173
_refine_ls_wR_factor_ref         0.1177
_reflns_number_gt                6521
_reflns_number_total             6703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500708x_si_004.cif
_cod_data_source_block           ms281
_cod_original_cell_volume        1847.22(10)
_cod_database_code               4084713