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_7708376
_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         'C54 H77 O6 Y, C7 H8'
_chemical_formula_sum            'C61 H85 O6 Y'
_chemical_formula_weight         1003.19
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-09-16 deposited with the CCDC.	2021-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                106.74(3)
_cell_angle_beta                 106.42(3)
_cell_angle_gamma                93.08(3)
_cell_formula_units_Z            2
_cell_length_a                   12.386(3)
_cell_length_b                   14.465(3)
_cell_length_c                   17.062(3)
_cell_measurement_reflns_used    7923
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     2777.4(13)
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_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  0.0404
_diffrn_reflns_av_unetI/netI     0.0325
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            34526
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.026
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         1.312
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.098
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       block
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.182
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0177(10)
_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   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         9003
_refine_ls_number_restraints     283
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0745P)^2^+1.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7923
_reflns_number_total             9003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           1b
_cod_original_cell_volume        2777.3(11)
_cod_database_code               7708376
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.898
_shelx_estimated_absorpt_t_min   0.810
_olex2_refinement_description
;
1. Others
 Fixed Sof: H51A(0.7) H51B(0.7) H51C(0.3) H51D(0.3) H50A(0.75) H50B(0.75)
 H50C(0.25) H50D(0.25) H53A(0.7) H53B(0.7) H53C(0.3) H53D(0.3) H48A(0.75)
 H48B(0.75) H48C(0.25) H48D(0.25) C49(0.75) H49A(0.75) H49B(0.75) C52(0.68)
 H52A(0.68) H52B(0.68) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5) C56(0.5) C57(0.5)
 H57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5) C61(0.5)
 H61(0.5) C52A(0.32) H52C(0.32) H52D(0.32) C65(0.5) H65(0.5) C66(0.5) H66(0.5)
 C67(0.5) H67(0.5) C68(0.5) H68(0.5) C63(0.5) C64(0.5) H64(0.5) C62(0.5)
 H62A(0.5) H62B(0.5) H62C(0.5) C49A(0.25) H49C(0.25) H49D(0.25)
 Fixed Uiso: H1(0.036) H6(0.029) H3A(0.041) H3B(0.041) H3C(0.041) H16(0.032)
 H39(0.035) H2A(0.045) H2B(0.045) H2C(0.045) H8(0.031) H22A(0.043) H22B(0.043)
 H22C(0.043) H29(0.034) H37(0.039) H14(0.031) H47A(0.034) H47B(0.034)
 H31(0.033) H1A(0.04) H1B(0.04) H1C(0.04) H45A(0.043) H45B(0.043) H45C(0.043)
 H35A(0.031) H35B(0.031) H51A(0.042) H51B(0.042) H51C(0.042) H51D(0.042)
 H46A(0.046) H46B(0.046) H46C(0.046) H50A(0.039) H50B(0.039) H50C(0.039)
 H50D(0.039) H25A(0.058) H25B(0.058) H25C(0.058) H54A(0.035) H54B(0.035)
 H21A(0.049) H21B(0.049) H21C(0.049) H11A(0.064) H11B(0.064) H11C(0.064)
 H12A(0.03) H12B(0.03) H34A(0.063) H34B(0.063) H34C(0.063) H24A(0.056)
 H24B(0.056) H24C(0.056) H44A(0.05) H44B(0.05) H44C(0.05) H26A(0.058)
 H26B(0.058) H26C(0.058) H23A(0.05) H23B(0.05) H23C(0.05) H19A(0.055)
 H19B(0.055) H19C(0.055) H53A(0.051) H53B(0.051) H53C(0.051) H53D(0.051)
 H48A(0.056) H48B(0.056) H48C(0.056) H48D(0.056) H42A(0.081) H42B(0.081)
 H42C(0.081) H49A(0.05) H49B(0.05) H52A(0.043) H52B(0.043) H55A(0.152)
 H55B(0.152) H55C(0.152) H57(0.084) H58(0.112) H59(0.138) H60(0.14) H61(0.115)
 H52C(0.042) H52D(0.042) H65(0.061) H66(0.052) H67(0.054) H68(0.062) H64(0.066)
 H62A(0.087) H62B(0.087) H62C(0.087) H49C(0.04) H49D(0.04)
 Fixed X: H6(0.897205) H3A(0.671931) H3B(0.662814) H3C(0.587711) H16(0.195845)
 H39(0.334198) H2A(0.933887) H2B(0.874279) H2C(0.874804) H8(0.728217)
 H22A(0.143148) H22B(0.043611) H22C(0.173867) H29(0.183818) H37(0.068971)
 H14(0.52743) H47A(0.489722) H47B(0.469791) H31(0.101436) H1A(0.817159)
 H1B(0.760078) H1C(0.681594) H45A(0.661251) H45B(0.569967) H45C(0.569579)
 H35A(0.080624) H35B(0.196333) H51A(0.2102) H51B(0.296258) H51C(0.335055)
 H51D(0.218103) H46A(0.506258) H46B(0.465537) H46C(0.597128) H50A(0.631245)
 H50B(0.703015) H50C(0.632464) H50D(0.684796) H25A(0.240797) H25B(0.134596)
 H25C(0.238259) H54A(0.470835) H54B(0.341723) H21A(0.119188) H21B(-0.000166)
 H21C(0.104705) H11A(0.987895) H11B(0.898386) H11C(0.948453) H12A(0.568447)
 H12B(0.512589) H34A(0.037262) H34B(0.055221) H34C(0.154871) H24A(0.423178)
 H24B(0.444341) H24C(0.43244) H44A(0.611264) H44B(0.482855) H44C(0.51967)
 H26A(0.280766) H26B(0.293759) H26C(0.17175) H23A(0.02892) H23B(-0.043556)
 H23C(0.050867) H19A(0.366616) H19B(0.322675) H19C(0.455521) H53A(0.324308)
 H53B(0.457185) H53C(0.452757) H53D(0.368229) H48A(0.680889) H48B(0.631687)
 H48C(0.635608) H48D(0.659268) H42A(0.059962) H42B(0.073147) H42C(0.161423)
 H49A(0.67015) H49B(0.776482) H52A(0.422644) H52B(0.303014) H55A(-0.099668)
 H55B(-0.155025) H55C(-0.208733) H57(-0.146495) H58(-0.032257) H59(0.124759)
 H60(0.169667) H61(0.049649) H52C(0.196852) H52D(0.268888) H65(0.025952)
 H66(0.165928) H67(0.110933) H68(-0.077697) H64(-0.163748) H62A(-0.240416)
 H62B(-0.246305) H62C(-0.258071) H49C(0.767921) H49D(0.770958)
 Fixed Y: H6(0.921274) H3A(1.001147) H3B(1.014027) H3C(0.923889) H16(0.773472)
 H39(0.800267) H2A(0.93679) H2B(1.025727) H2C(1.002029) H8(0.731658)
 H22A(0.862485) H22B(0.793517) H22C(0.786355) H29(0.263621) H37(0.659379)
 H14(0.742592) H47A(0.559262) H47B(0.464858) H31(0.482826) H1A(0.79186)
 H1B(0.862545) H1C(0.784688) H45A(0.782144) H45B(0.694658) H45C(0.724398)
 H35A(0.637768) H35B(0.672523) H51A(0.898599) H51B(0.881062) H51C(0.917656)
 H51D(0.863303) H46A(0.88237) H46B(0.95302) H46C(0.940998) H50A(0.54586)
 H50B(0.630123) H50C(0.514727) H50D(0.628415) H25A(0.368068) H25B(0.381218)
 H25C(0.468457) H54A(0.907684) H54B(0.896231) H21A(0.614079) H21B(0.607757)
 H21C(0.567746) H11A(0.821099) H11B(0.830808) H11C(0.924499) H12A(0.617471)
 H12B(0.63174) H34A(0.318126) H34B(0.230116) H34C(0.274737) H24A(0.459907)
 H24B(0.36021) H24C(0.365498) H44A(0.893253) H44B(0.912198) H44C(0.81)
 H26A(0.225093) H26B(0.217496) H26C(0.223776) H23A(0.686598) H23B(0.731106)
 H23C(0.801202) H19A(0.741183) H19B(0.841419) H19C(0.833367) H53A(1.043997)
 H53B(1.059438) H53C(1.046576) H53D(1.059327) H48A(0.553798) H48B(0.438794)
 H48C(0.429495) H48D(0.527811) H42A(0.779387) H42B(0.668957) H42C(0.756919)
 H49A(0.427592) H49B(0.5069) H52A(1.021622) H52B(1.058234) H55A(1.025934)
 H55B(0.920057) H55C(1.01444) H57(1.094336) H58(1.107602) H59(1.025284)
 H60(0.932282) H61(0.912776) H52C(0.983872) H52D(1.043259) H65(0.40416)
 H66(0.50197) H67(0.602914) H68(0.625436) H64(0.42637) H62A(0.482061)
 H62B(0.461216) H62C(0.567631) H49C(0.602119) H49D(0.495388)
 Fixed Z: H6(0.532635) H3A(0.318788) H3B(0.412952) H3C(0.332698) H16(0.575038)
 H39(-0.11138) H2A(0.417646) H2B(0.458437) H2C(0.360967) H8(0.603665)
 H22A(0.400361) H22B(0.318358) H22C(0.323797) H29(0.025207) H37(-0.079784)
 H14(0.625403) H47A(0.076773) H47B(0.105788) H31(-0.070352) H1A(0.299977)
 H1B(0.248487) H1C(0.266579) H45A(0.072386) H45B(0.000015) H45C(0.097823)
 H35A(0.053869) H35B(0.132307) H51A(0.23573) H51B(0.179015) H51C(0.201454)
 H51D(0.200016) H46A(0.163258) H46B(0.107156) H46C(0.137796) H50A(0.306988)
 H50B(0.290157) H50C(0.283029) H50D(0.311709) H25A(0.307924) H25B(0.234725)
 H25C(0.285991) H54A(0.410774) H54B(0.412573) H21A(0.288779) H21B(0.307343)
 H21C(0.360469) H11A(0.653501) H11B(0.706103) H11C(0.688499) H12A(0.497651)
 H12B(0.406226) H34A(-0.16301) H34B(-0.123609) H34C(-0.150654) H24A(0.253921)
 H24B(0.192945) H24C(0.285068) H44A(-0.007095) H44B(-0.041525) H44C(-0.084045)
 H26A(0.218723) H26B(0.126469) H26C(0.140728) H23A(0.477696) H23B(0.407296)
 H23C(0.492142) H19A(0.728654) H19B(0.721608) H19C(0.742445) H53A(0.402801)
 H53B(0.411244) H53C(0.371323) H53D(0.42955) H48A(0.104242) H48B(0.068832)
 H48C(0.094685) H48D(0.072707) H42A(-0.184708) H42B(-0.229799) H42C(-0.224999)
 H49A(0.206311) H49B(0.221132) H52A(0.270883) H52B(0.274465) H55A(0.166076)
 H55B(0.098881) H55C(0.084747) H57(-0.000524) H58(-0.084326) H59(-0.081236)
 H60(0.012509) H61(0.090879) H52C(0.300203) H52D(0.259837) H65(0.394453)
 H66(0.520317) H67(0.630039) H68(0.612034) H64(0.373949) H62A(0.513586)
 H62B(0.41501) H62C(0.471122) H49C(0.201741) H49D(0.213029)
;
_shelx_res_checksum              60841
_olex2_submission_special_instructions 'No special instructions were received'