Cationic half-sandwich rare-earth metal alkyl species catalyzed polymerization and copolymerization of aryl isocyanides possessing polar, bulky, or chiral substituents
Yan, Xinwen; Zhang, Shaowen; Peng, Deqian; Zhang, Pengfei; Zhi, Junge; Wu, Xiaolu; Wang, Lin; Dong, Yuping; Li, Xiaofang; Polymer Chemistry 9 (2018) 984–; doi:10.1039/C8PY00007G

data_1548724
_publ_section_title
;
 Cationic half-sandwich rare-earth metal alkyl species catalyzed
 polymerization and copolymerization of aryl isocyanides possessing polar,
 bulky, or chiral substituents
;
_journal_issue                   8
_journal_name_full               'Polymer Chemistry'
_journal_page_first              984
_journal_paper_doi               10.1039/C8PY00007G
_journal_volume                  9
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H49 Lu O3 Si2'
_chemical_formula_sum            'C26 H49 Lu O3 Si2'
_chemical_formula_weight         640.80
_chemical_name_systematic        3
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-10-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-12-04 deposited with the CCDC.
2018-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.76(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.2286(16)
_cell_length_b                   17.857(4)
_cell_length_c                   10.889(2)
_cell_measurement_reflns_used    5486
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.4855
_cell_measurement_theta_min      2.2915
_cell_volume                     1505.8(6)
_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 (Sheldrick, 2008)'
_diffrn_ambient_temperature      153.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0637
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11051
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.936
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.489
_diffrn_reflns_theta_min         2.630
_exptl_absorpt_coefficient_mu    3.380
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7110
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             656
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.583
_refine_diff_density_min         -1.571
_refine_diff_density_rms         0.134
_refine_ls_abs_structure_details
;
 Flack x determined using 2679 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         6491
_refine_ls_number_restraints     169
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0382P)^2^+1.8171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.877
_reflns_number_gt                6287
_reflns_number_total             6491
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00007g2.cif
_cod_data_source_block           bwn17072_pl
_cod_depositor_comments
'Adding full bibliography for 1548723--1548725.cif.'
_cod_database_code               1548724
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.498
_shelx_estimated_absorpt_t_min   0.462
_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
 C24-C23 = C24A-C23A = C25-C24 = C25A-C24A = C26-C25 = C26A-C25A
 1.54 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C26A \\sim C26 \\sim C25A \\sim C25 \\sim C24A \\sim C24 \\sim C23 \\sim C23A
\\sim O3: within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C23A) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C24A)
\\sim Ueq, Uanis(C25A) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C26A) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(O3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
4. Others
 Sof(C25A)=Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C23A)=
 Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C19(H19A,H19B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,
 H25B), C26(H26A,H26B), C25A(H25C,H25D), C26A(H26C,H26D), C23A(H23C,H23D),
 C24A(H24C,H24D)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_olex2_submission_special_instructions 'No special instructions were received'