Lithium catalysed sequence selective ring opening terpolymerisation: a mechanistic study
Deglmann, Peter; Machleit, Sara; Gallizioli, Cesare; Rupf, Susanne M.; Plajer, Alex J.; Catalysis Science & Technology 13 (2023) 2937–2945; doi:10.1039/D3CY00301A

data_1568827
_publ_section_title
;
 Lithium catalysed sequence selective ring opening terpolymerisation: a
 mechanistic study
;
_journal_issue                   10
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2937
_journal_page_last               2945
_journal_paper_doi               10.1039/D3CY00301A
_journal_volume                  13
_journal_year                    2023
_chemical_compound_source        THF
_chemical_formula_moiety         'C8 H17 Li O S'
_chemical_formula_sum            'C8 H17 Li O S'
_chemical_formula_weight         168.21
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-01-18
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2023-01-18 deposited with the CCDC.	2023-04-09 downloaded from the CCDC.
;
_cell_angle_alpha                113.372(7)
_cell_angle_beta                 102.438(7)
_cell_angle_gamma                98.398(8)
_cell_formula_units_Z            4
_cell_length_a                   8.1843(17)
_cell_length_b                   11.066(3)
_cell_length_c                   13.037(3)
_cell_measurement_reflns_used    6553
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.91
_cell_volume                     1022.5(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.983
_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  0.0850
_diffrn_reflns_av_unetI/netI     0.0684
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18312
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.863
_diffrn_reflns_theta_min         2.638
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.262
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1164 before and 0.0849 after correction.
The Ratio of minimum to maximum transmission is 0.7111.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.093
_exptl_crystal_description       needle
_exptl_crystal_F_000             368
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.371
_refine_diff_density_rms         0.061
_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     234
_refine_ls_number_reflns         3884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0358P)^2^+0.7748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1221
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2927
_reflns_number_total             3884
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00301a2.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 1568826--1568827.cif.'
_cod_database_code               1568827
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.859
_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, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C103) = Uanis(C104)
3. Others
 Fixed Sof: H24A(0.75) H24B(0.75) H24C(0.75) H24D(0.25) H24E(0.25) H24F(0.25)
 H10G(0.8) H10H(0.8) H10I(0.2) H10J(0.2) C21(0.75) H21A(0.75) H21B(0.75)
 H21C(0.75) C23(0.75) H23(0.75) C26(0.75) H26A(0.75) H26B(0.75) C104(0.8)
 H10K(0.8) H10L(0.8) C20(0.25) H20I(0.25) H20J(0.25) H20K(0.25) C22(0.25)
 H22(0.25) C25(0.25) H25A(0.25) H25B(0.25) C103(0.2) H10M(0.2) H10N(0.2)
4.a Ternary CH refined with riding coordinates:
 C11(H11), C23(H23), C22(H22)
4.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C100(H10E,H10F), C101(H10C,H10D), C102(H10G,H10H), C102(H10I,
 H10J), C200(H20A,H20B), C201(H20G,H20H), C202(H20E,H20F), C203(H20C,H20D),
 C26(H26A,H26B), C104(H10K,H10L), C25(H25A,H25B), C103(H10M,H10N)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C), C24(H24D,H24E,
 H24F), C21(H21A,H21B,H21C), C20(H20I,H20J,H20K)
;
_shelx_res_checksum              65096
_shelx_hkl_checksum              76786
_olex2_submission_special_instructions 'No special instructions were received'