Lithium achieves sequence selective ring-opening terpolymerisation (ROTERP) of ternary monomer mixtures
Plajer, Alex Johannes; Pröhm, Patrick; Rupf, Susanne M.; Chemical Science  (2022) –; doi:10.1039/D2SC01776H

data_1566926
_publ_section_title
;
 Lithium achieves sequence selective ring-opening terpolymerisation
 (ROTERP) of ternary monomer mixtures
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01776H
_journal_year                    2022
_chemical_formula_moiety         'C40 H58 Li2 O10 S2'
_chemical_formula_sum            'C40 H58 Li2 O10 S2'
_chemical_formula_weight         776.86
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2b6bxt
_audit_creation_date             2022-01-04
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2022-02-09 deposited with the CCDC.	2022-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.544(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2936(6)
_cell_length_b                   21.8827(10)
_cell_length_c                   17.1083(7)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.56
_cell_volume                     4214.8(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7771
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.421
_diffrn_reflns_theta_min         2.034
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 211417 reflections, Rint = 0.1308
 (86043 with I > 3sig(I), Rint = 0.0613)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       needle
_exptl_crystal_F_000             1664
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: tetrahydrofurane'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.257
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         7771
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0561
_refine_ls_R_factor_gt           0.0472
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0290P)^2^+3.1353P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0929
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7066
_reflns_number_total             7771
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01776h2.cif
_cod_data_source_block           p21_n_twin
_cod_database_code               1566926
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.900
_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. Others
 Fixed Sof: O7(0.66667) O8(0.33333) C2(0.5) H2A(0.5) H2B(0.5) C3(0.6) H3A(0.6)
 H3B(0.6) C4(0.5) H4A(0.5) H4B(0.5) C5(0.4) H5A(0.4) H5B(0.4) C6(0.6) H6A(0.6)
 H6B(0.6) C7(0.4) H7A(0.4) H7B(0.4) H50A(0.5) H50B(0.5) H50C(0.5) H50D(0.5)
 C51(0.5) H51A(0.5) H51B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5) H55A(0.5) H55B(0.5) H55C(0.5) H55D(0.5)
 H56C(0.5) H56D(0.5) H56A(0.5) H56B(0.5) C60(0.5) H60A(0.5) H60B(0.5) C61(0.5)
 H61A(0.5) H61B(0.5) C62(0.5) H62A(0.5) H62B(0.5) C63(0.5) H63A(0.5) H63B(0.5)
 C64(0.5) H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5) H66C(0.5) H66D(0.5)
 H66A(0.5) H66B(0.5) C109(0.66667) H10A(0.66667) H10B(0.66667) H10C(0.66667)
 C110(0.33333) H11J(0.33333) H11K(0.33333) H11L(0.33333) C111(0.66667)
 H11A(0.66667) H11B(0.66667) H11C(0.66667) C112(0.33333) H11D(0.33333)
 H11E(0.33333) H11F(0.33333) C113(0.66667) H11M(0.66667) H11N(0.66667)
 H11O(0.66667) C114(0.33333) H11G(0.33333) H11H(0.33333) H11I(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C50(H50A,H50B),
  C50(H50C,H50D), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,
 H54B), C55(H55A,H55B), C55(H55C,H55D), C56(H56C,H56D), C56(H56A,H56B),
 C60(H60A,H60B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
  C65(H65A,H65B), C66(H66C,H66D), C66(H66A,H66B)
3.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C202(H202), C203(H203),
 C204(H204), C205(H205)
3.c Idealised Me refined as rotating group:
 C109(H10A,H10B,H10C), C110(H11J,H11K,H11L), C111(H11A,H11B,H11C), C112(H11D,
 H11E,H11F), C113(H11M,H11N,H11O), C114(H11G,H11H,H11I), C209(H20A,H20B,H20C),
 C210(H21A,H21B,H21C), C211(H21D,H21E,H21F)
;
_shelx_res_checksum              15938
_olex2_submission_special_instructions 'No special instructions were received'