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_1568826
_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_formula_moiety         'C8 H17 Li O2'
_chemical_formula_sum            'C8 H17 Li O2'
_chemical_formula_weight         152.15
_chemical_properties_physical    Moisture-sensitive,Hygroscopic
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   19.3447(15)
_cell_length_b                   19.3447(15)
_cell_length_c                   10.3928(10)
_cell_measurement_reflns_used    2412
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.53
_cell_measurement_theta_min      2.98
_cell_volume                     3889.2(6)
_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    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0338
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3821
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.116
_diffrn_reflns_theta_max         25.116
_diffrn_reflns_theta_min         2.106
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0915 before and 0.0562 after correction.
The Ratio of minimum to maximum transmission is 0.8655.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.039
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.453
_exptl_crystal_size_min          0.433
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.030
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0823P)^2^+1.8693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1476
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1341
_reflns_number_total             1711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cy00301a2.cif
_cod_data_source_block           i41_a
_cod_depositor_comments
'Adding full bibliography for 1568826--1568827.cif.'
_cod_original_cell_volume        3889.2(7)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               1568826
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.966
_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. Shared sites
{C11, C11B}
3. Uiso/Uaniso restraints and constraints
Uanis(C11) = Uanis(C11B)
4. Others
 Fixed Sof: O2(0.6) O3(0.4) H10A(0.4) H10(0.6) C11(0.6) C11B(0.4) H11A(0.6)
 H11B(0.6) H11C(0.6) H11D(0.4) H11E(0.4) C12(0.6) H12A(0.6) H12B(0.6) C13(0.4)
 H13A(0.4) H13B(0.4) H13C(0.4) C14(0.4) H14A(0.4) H14B(0.4) H14C(0.4) C15(0.6)
 H15A(0.6) H15B(0.6) H15C(0.6) C20(0.6) H20A(0.6) H20B(0.6) C21(0.6) H21A(0.6)
 H21B(0.6) H22A(0.6) H22B(0.6) H22C(0.4) H22D(0.4) H23A(0.6) H23B(0.6)
 H23C(0.4) H23D(0.4) C30(0.4) H30A(0.4) H30B(0.4) C31(0.4) H31A(0.4) H31B(0.4)
5.a Ternary CH refined with riding coordinates:
 C10(H10A), C10(H10)
5.b Secondary CH2 refined with riding coordinates:
 C11B(H11D,H11E), C12(H12A,H12B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,
 H22B), C22(H22C,H22D), C23(H23A,H23B), C23(H23C,H23D), C30(H30A,H30B),
 C31(H31A,H31B)
5.c Idealised Me refined as rotating group:
 C11B(H11A,H11B,H11C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,
 H15C)
;
_shelx_res_checksum              50178
_shelx_hkl_checksum              12341
_olex2_submission_special_instructions 'No special instructions were received'