New lanthanoid biphenolate complexes, their further reactivity with trimethylaluminium and catalytic activity for the polymerisation of rac-lactide
Shephard, Angus; Ali, Safaa; Wang, Jun; Guo, Zhifang; Davies, Murray S.; Deacon, Glen B.; Junk, Peter Courtney; Dalton Transactions  (2021) –; doi:10.1039/D1DT02513A

data_7708372
_publ_section_title
;
 New lanthanoid biphenolate complexes, their further reactivity with
 trimethylaluminium and catalytic activity for the polymerisation of
 rac-lactide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02513A
_journal_year                    2021
_chemical_formula_moiety         'C56 H82 Al O6 Y, 2(C6 H6)'
_chemical_formula_sum            'C68 H94 Al O6 Y'
_chemical_formula_weight         1123.32
_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
_audit_creation_date             2021-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-07-26 deposited with the CCDC.	2021-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.845(2)
_cell_length_b                   19.536(4)
_cell_length_c                   32.429(7)
_cell_measurement_reflns_used    10557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6219(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0746
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            76823
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.218
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_exptl_transmission_factor_max   0.9
_exptl_transmission_factor_min   0.8
_refine_diff_density_max         7.678
_refine_diff_density_min         -2.060
_refine_diff_density_rms         0.149
_refine_ls_extinction_coef       0.0020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         10557
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0998
_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^)+(0.1851P)^2^+21.6418P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2581
_refine_ls_wR_factor_ref         0.2733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8678
_reflns_number_total             10557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           complex8
_cod_database_code               7708372
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.898
_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. Rigid bond restraints
 C56, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15, C14
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C56, O6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Uiso/Uaniso restraints and constraints
C63 \\sim C68: within 1.4A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.4A
C56 \\sim C55: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C15 \\sim C14: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
C15 \\sim C16: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.001 within 2A
C16: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C56: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C56 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
4.a Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C52(H52A,H52B), C35(H35A,H35B), C50(H50A,H50B), C55(H55A,
 H55B), C51(H51A,H51B), C56(H56A,H56B), C53(H53A,H53B), C54(H54A,H54B),
 C12(H12A,H12B)
4.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C8(H8), C6(H6), C32(H32), C29(H29), C40(H40), C14(H14), C17(H17),
 C58(H58), C59(H59), C61(H61), C62(H62), C57(H57), C65(H65), C66(H66), C67(H67),
  C68(H68), C63(H63), C64(H64), C60(H60)
4.c Fitted hexagon refined as free rotating group:
 C65(C66,C67,C68,C63,C64)
4.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C2(H2A,H2B,H2C), C47(H47A,H47B,H47C), C1(H1A,H1B,H1C),
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C), C44(H44A,H44B,H44C), C11(H11A,H11B,
 H11C), C39(H39A,H39B,H39C), C48(H48A,H48B,H48C), C3(H3A,H3B,H3C), C25(H25A,
 H25B,H25C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C21(H21A,H21B,H21C),
 C31(H31A,H31B,H31C), C45(H45A,H45B,H45C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              85683
_olex2_submission_special_instructions 'No special instructions were received'