The Role of Neutral Donor Ligands in the Isoselective Ring-Opening Polymerization of rac-β-Butyrolactone
Dong, Xiang; Robinson, Jerome; Chemical Science  (2020) –; doi:10.1039/D0SC03507F

data_1558609
_publ_section_title
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 The Role of Neutral Donor Ligands in the Isoselective Ring-Opening
 Polymerization of rac-\b-Butyrolactone
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03507F
_journal_year                    2020
_chemical_formula_moiety         'C49 H83 La N2 O4 Si2'
_chemical_formula_sum            'C49 H83 La N2 O4 Si2'
_chemical_formula_weight         959.26
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-26
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-01-26 deposited with the CCDC.	2020-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.851(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0458(16)
_cell_length_b                   16.5877(16)
_cell_length_c                   19.5942(17)
_cell_measurement_reflns_used    9263
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.65
_cell_measurement_theta_min      2.45
_cell_volume                     5105.5(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.2
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  'Bruker D8-Quest, Photon 100 CMOS Detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1329
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            192582
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.936
_diffrn_reflns_theta_min         1.785
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.925
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0982 before and 0.0836 after correction.
The Ratio of minimum to maximum transmission is 0.8719.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       block
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     549
_refine_ls_number_reflns         11709
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0527
_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^)+(0.0144P)^2^+19.0668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8606
_reflns_number_total             11709
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc03507f2.cif
_cod_data_source_block           jrr20190425_1-La
_cod_database_code               1558609
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C23(H23A,H23B), C42(H42A,H42B), C43(H43A,
 H43B), C44(H44A,H44B), C45(H45A,H45B), C47(H47A,H47B), C48(H48A,H48B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
 C31(H31)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C46(H46A,H46B,H46C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              51622
_olex2_submission_special_instructions 'No special instructions were received'