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_1548725
_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_formula_moiety         'C28 H53 Lu O3 Si2'
_chemical_formula_sum            'C28 H53 Lu O3 Si2'
_chemical_formula_weight         668.85
_chemical_name_systematic        6
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-12-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2017-12-05 deposited with the CCDC.
2018-01-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.6700(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3321(6)
_cell_length_b                   15.5971(7)
_cell_length_c                   16.0371(7)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.64
_cell_volume                     3226.1(2)
_computing_cell_refinement       'SAINT V8.35A (?, 2016)'
_computing_data_reduction        'SAINT V8.35A (?, 2016)'
_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      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            70881
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.556
_diffrn_reflns_theta_min         2.612
_exptl_absorpt_coefficient_mu    3.158
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1162 before and 0.0561 after correction.
The Ratio of minimum to maximum transmission is 0.7619.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.42
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.568
_refine_diff_density_max         0.426
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7422
_refine_ls_number_restraints     262
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0195P)^2^+8.3770P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6722
_reflns_number_total             7422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8py00007g2.cif
_cod_data_source_block           a
_cod_depositor_comments
'Adding full bibliography for 1548723--1548725.cif.'
_cod_database_code               1548725
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.351
_shelx_estimated_absorpt_t_min   0.331
_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
 C19A-C17 = C19-C17 = C21-C14 = C21A-C14 = C23-C22 = C23A-C22
 1.52 with sigma of 0.02
 C28-C27 = C27-C26 = C28-C27A = C27A-C26
 1.52 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16 \\sim C16A \\sim O2A \\sim O2 \\sim C15 \\sim C15A \\sim O1 \\sim O1A:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
C27 \\sim C27A \\sim C19A \\sim C19 \\sim C23A \\sim C23 \\sim C21A \\sim C21:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.01
C28 \\sim C28A \\sim C26 \\sim C26A: 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(O1A) \\sim Ueq, Uanis(O1)
\\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16A) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C27A) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C26A) \\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C28A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
4. Others
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(O2A)=Sof(O1A)=1-FVAR(1)
 Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(O1)=Sof(O2)=FVAR(1)
 Sof(C27A)=Sof(H27C)=Sof(H27D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=Sof(C28A)=
 Sof(H28C)=Sof(H28D)=1-FVAR(2)
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(C28)=Sof(H28A)=
 Sof(H28B)=FVAR(2)
 Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(3)
 Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(3)
 Sof(C23A)=Sof(H23D)=Sof(H23E)=Sof(H23F)=1-FVAR(4)
 Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=FVAR(4)
 Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(5)
 Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(5)
5.a Riding coordinates:
 C25(H25A,H25B)
5.b Ternary CH refined with riding coordinates:
 C15(H15), C16(H16), C15A(H15A), C16A(H16A)
5.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C5(H5A,H5B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B),
 C27A(H27C,H27D), C26A(H26C,H26D), C28A(H28C,H28D)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11)
5.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C19A(H19D,H19E,H19F), C23A(H23D,H23E,H23F), C21A(H21D,H21E,H21F)
;
_olex2_submission_special_instructions 'No special instructions were received'