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_4084711
_publ_contact_author
;
      Prof. Dr. Peter W. Roesky
      Karlsruher Institut fuer Technologie (KIT), CS
      Institut fuer Anorganische Chemie (AOC)
      Lehrstuhl fuer Anorganische Funktionsmaterialien
      Engesserstr. 15, Geb. 30.45
      76131 Karlsruhe 
      Bundesrepublik Deutschland
;
_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         'C33 H57 B2 Lu N2 O, C4 H8 O'
_chemical_formula_sum            'C37 H65 B2 Lu N2 O2'
_chemical_formula_weight         766.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-08-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                65.951(2)
_cell_angle_beta                 86.995(3)
_cell_angle_gamma                82.341(3)
_cell_formula_units_Z            2
_cell_length_a                   11.7844(4)
_cell_length_b                   12.8442(4)
_cell_length_c                   14.2905(4)
_cell_measurement_reflns_used    53025
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      1.56
_cell_volume                     1957.64(11)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0698
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56498
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.560
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    2.552
_exptl_absorpt_correction_T_max  0.7185
_exptl_absorpt_correction_T_min  0.4674
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Red & X-Shape'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       prism
_exptl_crystal_F_000             796
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.276
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.864
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     457
_refine_ls_number_reflns         7695
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6427
_reflns_number_total             7695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500708x_si_007.cif
_cod_data_source_block           ms568_1
_cod_original_cell_volume        1957.65(11)
_cod_database_code               4084711
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H30A(0.66667) H30B(0.66667) H30C(0.33333) H30D(0.33333)
 H33A(0.66667) H33B(0.66667) H33C(0.33333) H33D(0.33333) C31A(0.66667)
 H31A(0.66667) H31B(0.66667) C32A(0.66667) H32A(0.66667) H32B(0.66667)
 C31B(0.33333) H31C(0.33333) H31D(0.33333) C32B(0.33333) H32C(0.33333)
 H32D(0.33333)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C30(H30C,H30D), C33(H33A,H33B), C33(H33C,H33D), C31A(H31A,
 H31B), C32A(H32A,H32B), C31B(H31C,H31D), C32B(H32C,H32D), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C34A(H34A,H34B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
3.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              19726
_shelx_hkl_checksum              33955
_olex2_submission_special_instructions 'No special instructions were received'