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_4084712
_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 N2 O Sm'
_chemical_formula_sum            'C33 H57 B2 N2 O Sm'
_chemical_formula_weight         669.77
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 110.19(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.579(6)
_cell_length_b                   10.445(2)
_cell_length_c                   23.642(5)
_cell_measurement_reflns_used    64227
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.13
_cell_measurement_theta_min      1.34
_cell_volume                     7087(3)
_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      150
_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 0.992
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            60353
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.666
_diffrn_reflns_theta_min         1.419
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    1.682
_exptl_absorpt_correction_T_max  0.7143
_exptl_absorpt_correction_T_min  0.6085
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-Red & X-Shape'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       prism
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.291
_exptl_crystal_size_min          0.247
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.728
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         13353
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0220
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0236P)^2^+1.4983P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0476
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11599
_reflns_number_total             13353
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500708x_si_005.cif
_cod_data_source_block           ms304_1
_cod_database_code               4084712
_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
 Sof(H63C)=Sof(H63D)=Sof(C64B)=Sof(H64C)=Sof(H64D)=Sof(H65C)=Sof(H65D)=1-FVAR(1)
 Sof(H63A)=Sof(H63B)=Sof(C64A)=Sof(H64A)=Sof(H64B)=Sof(H65A)=Sof(H65B)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C45(H45), C48(H48), C57(H57), C60(H60)
3.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C63(H63A,
 H63B), C63(H63C,H63D), C64A(H64A,H64B), C64B(H64C,H64D), C65(H65A,H65B),
 C65(H65C,H65D), C66(H66A,H66B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C36(H36),
 C41(H41), C42(H42), C43(H43), C53(H53), C54(H54), C55(H55)
3.d Idealised Me refined as rotating group:
 C1(H1E,H1F,H1G), 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), C34(H34A,H34B,H34C), C38(H38A,
 H38B,H38C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C),
 C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,
 H61C), C62(H62A,H62B,H62C)
;
_shelx_res_checksum              41324
_shelx_hkl_checksum              70961
_olex2_submission_special_instructions 'No special instructions were received'