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_4514183
_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         'C46 H96 O2 Sc2 Si6'
_chemical_formula_sum            'C46 H96 O2 Sc2 Si6'
_chemical_formula_weight         939.68
_chemical_name_systematic
;
 ?
;
_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   geom
_audit_creation_date             2016-01-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 111.842(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2889(6)
_cell_length_b                   18.1841(7)
_cell_length_c                   18.6875(6)
_cell_measurement_reflns_used    7415
_cell_measurement_temperature    99.93
_cell_measurement_theta_max      63.714
_cell_measurement_theta_min      3.562
_cell_volume                     5768.7(4)
_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      99.93
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.903
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22783
_diffrn_reflns_point_group_measured_fraction_full 0.903
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.709
_diffrn_reflns_theta_min         2.886
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    3.441
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0967 before and 0.0638 after correction.
The Ratio of minimum to maximum transmission is 0.6435.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.082
_exptl_crystal_description       plate
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.393
_exptl_crystal_size_mid          0.359
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.723
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         9410
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0820
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+25.4516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2147
_refine_ls_wR_factor_ref         0.2436
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6494
_reflns_number_total             9410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b01621_si_003.cif
_cod_data_source_block           cx0648
_cod_database_code               4514183
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.345
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C46(H46A,H46B), C39(H39A,H39B), C1(H1A,H1B), C12(H12A,H12B), C5(H5A,H5B),
 C9(H9A,H9B), C35(H35A,H35B), C10(H10A,H10B), C43(H43A,H43B), C45(H45A,H45B),
 C44(H44A,H44B), C11(H11A,H11B)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C31(H31A,H31B,H31C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C36(H36A,H36B,H36C), C4(H4A,H4B,H4C), C41(H41A,H41B,H41C),
 C33(H33A,H33B,H33C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C), C37(H37A,H37B,H37C), C19(H19A,
 H19B,H19C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C38(H38A,H38B,H38C), C3(H3A,H3B,
 H3C), C2(H2A,H2B,H2C)
;
_shelx_res_checksum              7932
_shelx_hkl_checksum              27058
_olex2_date_sample_data_collection 2016-01-06
_olex2_date_sample_submission    2016-01-06
_olex2_submission_original_sample_id cx0648
_olex2_submission_special_instructions 'No special instructions were received'