Stereo-selectivity switchable ROP of rac-β-butyrolactone initiated by salan-ligated rare-earth metal amide complexes: the key role of the substituents on ligand frameworks.
Zhuo, Zhixing; Zhang, Chen; Luo, Yunjie; Wang, Yaorong; Yao, Yingming; Yuan, Dan; Cui, Dongmei; Chemical communications (Cambridge, England) 54 (2018) 11998–12001; doi:10.1039/c8cc05469j

data_7125340
_publ_section_title
;
 Stereo-selectivity switchable ROP of rac-\b-butyrolactone initiated by
 salan-ligated rare-earth metal amide complexes: the key role of the
 substituents on ligand frameworks.
;
_journal_issue                   85
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11998
_journal_page_last               12001
_journal_paper_doi               10.1039/c8cc05469j
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         '2(C50 H88 N3 O2 Si2 Y), 3(C7H8)'
_chemical_formula_sum            'C121 H200 N6 O4 Si4 Y2'
_chemical_formula_weight         2093.05
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-04-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-06-29 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 92.992(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   23.3487(9)
_cell_length_b                   12.1983(5)
_cell_length_c                   21.8684(9)
_cell_measurement_reflns_used    6712
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.3540
_cell_measurement_theta_min      3.0870
_cell_volume                     6219.9(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.0970
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44381
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2268
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.076
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         12704
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1002P)^2^+5.5644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2003
_reflns_number_gt                8223
_reflns_number_total             12704
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8cc05469j2.cif
_cod_data_source_block           g161223b
_cod_database_code               7125340
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26-C27 = C26-C28 = C26-C29
 1.53 with sigma of 0.02
 C26-C27A = C26-C28A = C26-C29A
 1.53 with sigma of 0.02
 C51-C57
 1.52 with sigma of 0.01
 H56-H57B
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C27A) = Uanis(C28A) = Uanis(C29A)
Uanis(C27) = Uanis(C28) = Uanis(C29)
Uiso(C51) = Uiso(C52) = Uiso(C53) = Uiso(C54) = Uiso(C55) = Uiso(C56) =
Uiso(C57)
4. Others
 Fixed Sof: C27(0.5) H27A(0.5) H27B(0.5) H27C(0.5) C28(0.5) H28A(0.5)
 H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C27A(0.5) H27D(0.5)
 H27E(0.5) H27F(0.5) C28A(0.5) H28D(0.5) H28E(0.5) H28F(0.5) C29A(0.5)
 H29D(0.5) H29E(0.5) H29F(0.5)
5.a Ternary CH refined with riding coordinates:
 C3(H3), C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C21(H21A,H21B), C36(H36A,H36B)
5.c Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C27A(H27D,H27E,
 H27F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F)
5.d Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C32(H32), C34(H34), C52(H52), C53(H53), C54(H54),
 C55(H55), C56(H56)
5.e Fitted hexagon refined as free rotating group:
 C51(C52,C53,C54,C55,C56)
5.f Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C57(H57A,H57B,H57C)
;
_olex2_submission_special_instructions 'No special instructions were received'