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_7708378
_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         'C28 H41 Al O3, C7 H8'
_chemical_formula_sum            'C35 H49 Al O3'
_chemical_formula_weight         544.72
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-09-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-20 deposited with the CCDC.	2021-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.39(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.725(3)
_cell_length_b                   16.410(3)
_cell_length_c                   24.286(5)
_cell_measurement_reflns_used    5741
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.685
_cell_measurement_theta_min      1.767
_cell_volume                     6325(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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.953
_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  0.0412
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            38583
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.685
_diffrn_reflns_theta_min         1.767
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.096
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.8
_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    1.144
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5741
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0841P)^2^+3.1808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1391
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4767
_reflns_number_total             5741
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           complex10
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7708378
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Others
 Fixed Sof: H28A(0.85) H28B(0.85) H28C(0.15) H28D(0.15) H26A(0.85) H26B(0.85)
 H26C(0.15) H26D(0.15) C27(0.85) H27A(0.85) H27B(0.85) C27A(0.15) H27C(0.15)
 H27D(0.15)
 Fixed Uiso: H12A(0.045) H12B(0.045) H14(0.045) H17(0.045) H9(0.045) H6(0.046)
 H22A(0.063) H22B(0.063) H22C(0.063) H2A(0.068) H2B(0.068) H2C(0.068)
 H8A(0.066) H8B(0.066) H8C(0.066) H21A(0.067) H21B(0.067) H21C(0.067)
 H25A(0.06) H25B(0.06) H3A(0.067) H3B(0.067) H3C(0.067) H24A(0.069) H24B(0.069)
 H24C(0.069) H23A(0.071) H23B(0.071) H23C(0.071) H16A(0.069) H16B(0.069)
 H16C(0.069) H1A(0.07) H1B(0.07) H1C(0.07) H34(0.06) H32(0.065) H29(0.069)
 H28A(0.069) H28B(0.069) H28C(0.069) H28D(0.069) H26A(0.07) H26B(0.07)
 H26C(0.07) H26D(0.07) H30(0.069) H31(0.069) H35A(0.092) H35B(0.092)
 H35C(0.092) H27A(0.071) H27B(0.071) H27C(0.075) H27D(0.075) H8AA(0.069)
 H8AB(0.069) H8AC(0.069) H35D(0.133) H35E(0.133) H35F(0.133)
 Fixed X: H12A(0.399287) H12B(0.33709) H14(0.433115) H17(0.437548)
 H9(0.346681) H6(0.098035) H22A(0.36502) H22B(0.442066) H22C(0.355143) H2A(-
 0.087644) H2B(-0.01563) H2C(-0.025701) H8A(0.238713) H8B(0.206978)
 H8C(0.303561) H21A(0.369846) H21B(0.449869) H21C(0.37057) H25A(0.27781)
 H25B(0.186272) H3A(0.053903) H3B(0.038767) H3C(-0.039413) H24A(0.104444)
 H24B(0.157306) H24C(0.087481) H23A(0.22568) H23B(0.233393) H23C(0.237858)
 H16A(0.55251) H16B(0.469611) H16C(0.497449) H1A(0.010203) H1B(0.043442) H1C(-
 0.052348) H34(0.555878) H32(0.66776) H29(0.509625) H28A(0.266512)
 H28B(0.349399) H28C(0.277297) H28D(0.365268) H26A(0.30684) H26B(0.234826)
 H26C(0.237004) H26D(0.330507) H30(0.54216) H31(0.621416) H35A(0.686667)
 H35B(0.664787) H35C(0.59432) H27A(0.355104) H27B(0.400045) H27C(0.354923)
 H27D(0.257131) H8AA(0.283002) H8AB(0.187453) H8AC(0.259379) H35D(0.634862)
 H35E(0.703151) H35F(0.610088)
 Fixed Y: H12A(0.343384) H12B(0.279839) H14(0.472012) H17(0.464969)
 H9(0.454083) H6(0.48196) H22A(0.21615) H22B(0.240188) H22C(0.2094)
 H2A(0.395267) H2B(0.401564) H2C(0.472205) H8A(0.597678) H8B(0.538507)
 H8C(0.536767) H21A(0.430365) H21B(0.371222) H21C(0.346791) H25A(0.173534)
 H25B(0.136054) H3A(0.245129) H3B(0.26424) H3C(0.261858) H24A(0.219813)
 H24B(0.136796) H24C(0.154294) H23A(0.301152) H23B(0.388171) H23C(0.3066)
 H16A(0.544749) H16B(0.596608) H16C(0.581938) H1A(0.446046) H1B(0.358279)
 H1C(0.369557) H34(0.339126) H32(0.20358) H29(0.219376) H28A(0.039812)
 H28B(0.095519) H28C(0.056286) H28D(0.090625) H26A(0.044735) H26B(0.007423)
 H26C(0.016519) H26D(0.052277) H30(0.092861) H31(0.08635) H35A(0.386765)
 H35B(0.347816) H35C(0.397321) H27A(-0.022661) H27B(0.061856) H27C(-0.015569)
 H27D(-0.030208) H8AA(0.582287) H8AB(0.574159) H8AC(0.519291) H35D(0.407327)
 H35E(0.356044) H35F(0.367773)
 Fixed Z: H12A(0.209995) H12B(0.225297) H14(0.265356) H17(0.431831)
 H9(0.147178) H6(0.068338) H22A(0.47532) H22B(0.452774) H22C(0.407754)
 H2A(0.063761) H2B(0.033479) H2C(0.07624) H8A(0.079357) H8B(0.024363)
 H8C(0.064252) H21A(0.488607) H21B(0.502741) H21C(0.522718) H25A(0.152305)
 H25B(0.14579) H3A(0.140116) H3B(0.072971) H3C(0.097572) H24A(0.308815)
 H24B(0.318816) H24C(0.257596) H23A(0.385204) H23B(0.416195) H23C(0.45316)
 H16A(0.388185) H16B(0.383573) H16C(0.327068) H1A(0.18189) H1B(0.20791)
 H1C(0.167971) H34(0.379456) H32(0.522507) H29(0.326059) H28A(0.274713)
 H28B(0.300169) H28C(0.291345) H28D(0.286116) H26A(0.133709) H26B(0.157487)
 H26C(0.13556) H26D(0.151549) H30(0.371308) H31(0.469145) H35A(0.477105)
 H35B(0.531046) H35C(0.482527) H27A(0.233837) H27B(0.226641) H27C(0.218334)
 H27D(0.210555) H8AA(0.085454) H8AB(0.044359) H8AC(0.032447) H35D(0.464871)
 H35E(0.51362) H35F(0.517504)
;
_shelx_res_checksum              26889
_olex2_submission_special_instructions 'No special instructions were received'