Lutetium and yttrium complexes supported by an anilido-oxazoline ligand for polymerization of 1,3-conjugated dienes and ε-caprolactone
Li, Wenqiang; Jiang, Xinxin; So, Yat-Ming; He, Gaohong; Pan, Yu; New Journal of Chemistry 44 (2020) 121–128; doi:10.1039/C9NJ05081G

data_7059138
_publ_section_title
;
 Lutetium and yttrium complexes supported by an anilido-oxazoline ligand
 for polymerization of 1,3-conjugated dienes and \e-caprolactone
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              121
_journal_page_last               128
_journal_paper_doi               10.1039/C9NJ05081G
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C31 H51 Lu N2 O2 Si2'
_chemical_formula_sum            'C31 H51 Lu N2 O2 Si2'
_chemical_formula_weight         714.89
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-22 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.9110(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8355(6)
_cell_length_b                   9.5060(3)
_cell_length_c                   20.6821(7)
_cell_measurement_reflns_used    9854
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.79
_cell_volume                     3454.2(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150.02
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27335
_diffrn_reflns_theta_full        26.03
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         2.79
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  0.701
_exptl_absorpt_correction_T_min  0.502
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'yellowish yellow'
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.703
_refine_diff_density_min         -1.284
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6792
_refine_ls_number_restraints     3918
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0215P)^2^+5.9006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                5955
_reflns_number_total             6792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9nj05081g2.cif
_cod_data_source_block           1a
_cod_depositor_comments
;Adding full bibliography for 7059138--7059139.cif.

 Adding full bibliography for 7059138--7059139.cif.
;
_cod_database_code               7059138
_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. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27
\\sim C28 \\sim C21 \\sim C22 \\sim C29 \\sim C30 \\sim C31 \\sim C21A \\sim
C22A \\sim C29A \\sim C30A \\sim C31A: within 9.2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Si1 \\sim Si1 \\sim C29 \\sim C31: within 2A with sigma of 0.007 and sigma for
terminal atoms of 0.001
All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Others
 Sof(C29A)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=
 Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
 Sof(H23C)=Sof(H23D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(2)
 Sof(H23A)=Sof(H23B)=Sof(C22)=Sof(H22A)=Sof(H22B)=FVAR(2)
 Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(3)
 Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C20(H20A,H20B), C20(H20C,H20D), C23(H23A,H23B), C23(H23C,H23D),
 C24(H24A,H24B), C28(H28A,H28B), C21(H21A,H21B), C22(H22A,H22B), C21A(H21C,
 H21D), C22A(H22C,H22D)
4.b Me refined with riding coordinates:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C14(H14), C15(H15), C16(H16)
4.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C29A(H29D,H29E,
 H29F), C30A(H30D,H30E,H30F), C31A(H31D,H31E,H31F)
;
_olex2_submission_special_instructions 'No special instructions were received'