Metal and Counteranion Nuclearity Effects in Organoscandium-Catalyzed Isoprene Polymerization and Copolymerization
Chen, Jiazhen; Gao, Yanshan; Xiong, Shuoyan; Delferro, Massimiliano; Lohr, Tracy L.; Marks, Tobin J.; ACS Catalysis 7 (2017) 5214–; doi:10.1021/acscatal.7b01621

data_4514160
_publ_section_title
;
 Metal and Counteranion Nuclearity Effects in Organoscandium-Catalyzed
 Isoprene Polymerization and Copolymerization
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              5214
_journal_paper_doi               10.1021/acscatal.7b01621
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C48 H100 O2 Sc2 Si6'
_chemical_formula_sum            'C48 H100 O2 Sc2 Si6'
_chemical_formula_weight         967.73
_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   geom
_audit_creation_date             2015-10-15
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.009(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3075(14)
_cell_length_b                   24.950(2)
_cell_length_c                   17.0373(16)
_cell_measurement_reflns_used    9495
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.134
_cell_measurement_theta_min      2.414
_cell_volume                     6022.5(10)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.05
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            143090
_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         30.146
_diffrn_reflns_theta_min         1.457
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1123 before and 0.0587 after correction.
The Ratio of minimum to maximum transmission is 0.8385.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.067
_exptl_crystal_description       plate
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.445
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.850
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     557
_refine_ls_number_reflns         17663
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0586
_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^)+(0.0592P)^2^+6.0317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1292
_refine_ls_wR_factor_ref         0.1513
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12099
_reflns_number_total             17663
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b01621_si_004.cif
_cod_data_source_block           cx0584a
_cod_depositor_comments
'Adding full bibliography for 4514159--4514160.cif.'
_cod_original_cell_volume        6022.6(10)
_cod_database_code               4514160
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.851
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  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(H22C)=Sof(H22D)=Sof(C23B)=Sof(H23C)=Sof(H23D)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H24A)=Sof(H24B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C17(H17A,H17B), C21(H21A,H21B), C22(H22A,H22B),
 C22(H22C,H22D), C23(H23A,H23B), C23B(H23C,H23D), C24(H24A,H24B), C24(H24C,
 H24D), C6A(H6AA,H6AB), C13A(H13C,H13D), C17A(H17C,H17D), C21A(H21C,H21D),
 C22A(H22E,H22F), C23A(H23E,H23F), C24A(H24E,H24F)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,
 H20B,H20C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C9A(H9AA,H9AB,H9AC),
 C10A(H10D,H10E,H10F), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F), C14A(H14D,
 H14E,H14F), C15A(H15D,H15E,H15F), C16A(H16D,H16E,H16F), C18A(H18D,H18E,H18F),
 C19A(H19D,H19E,H19F), C20A(H20D,H20E,H20F)
;
_shelx_res_checksum              82935
_shelx_hkl_checksum              44094
_olex2_date_sample_data_collection 2015-10-14
_olex2_date_sample_submission    2015-10-13
_olex2_submission_original_sample_id cx0584a
_olex2_submission_special_instructions 'No special instructions were received'