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_7708374
_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         'C58 H85 O7 Y, 3(C4 H8 O1)'
_chemical_formula_sum            'C70 H109 O10 Y'
_chemical_formula_weight         1199.48
_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   geom
_audit_creation_date             2021-08-25
_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                90
_cell_angle_beta                 93.72(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.254(3)
_cell_length_b                   17.600(4)
_cell_length_c                   28.387(6)
_cell_measurement_reflns_used    15405
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6608(3)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.973
_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  0.0632
_diffrn_reflns_av_unetI/netI     0.0363
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            83342
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.911
_diffrn_reflns_theta_min         1.362
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.938
_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    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0145(5)
_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   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         15405
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0576P)^2^+7.5401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12242
_reflns_number_total             15405
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           1
_cod_original_cell_volume        6608(2)
_cod_database_code               7708374
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.835
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.053) H1A(0.069) H1B(0.069) H1C(0.069) H2A(0.063) H2B(0.063)
 H2C(0.063) H3A(0.067) H3B(0.067) H3C(0.067) H6(0.041) H8(0.049) H11A(0.076)
 H11B(0.076) H11C(0.076) H12A(0.057) H12B(0.057) H14(0.044) H16(0.045)
 H20A(0.092) H20B(0.092) H20C(0.092) H21A(0.085) H21B(0.085) H21C(0.085)
 H22A(0.061) H22B(0.061) H22C(0.061) H23A(0.074) H23B(0.074) H23C(0.074)
 H24A(0.067) H24B(0.067) H24C(0.067) H25A(0.059) H25B(0.059) H25C(0.059)
 H26A(0.06) H26B(0.06) H26C(0.06) H29(0.037) H31(0.035) H34A(0.058) H34B(0.058)
 H34C(0.058) H35A(0.032) H35B(0.032) H37(0.039) H39(0.039) H42A(0.081)
 H42B(0.081) H42C(0.081) H44A(0.059) H44B(0.059) H44C(0.059) H45A(0.056)
 H45B(0.056) H45C(0.056) H46A(0.056) H46B(0.056) H46C(0.056) H47A(0.068)
 H47B(0.068) H47C(0.068) H47D(0.068) H48A(0.062) H48B(0.062) H48C(0.067)
 H48D(0.067) H49A(0.078) H49B(0.078) H49C(0.07) H49D(0.07) H50A(0.065)
 H50B(0.065) H50C(0.065) H50D(0.065) H51A(0.052) H51B(0.052) H51C(0.056)
 H51D(0.056) H52A(0.071) H52B(0.071) H52C(0.065) H52D(0.065) H53A(0.073)
 H53B(0.073) H53C(0.065) H53D(0.065) H54A(0.052) H54B(0.052) H54C(0.04)
 H54D(0.04) H55A(0.073) H55B(0.073) H56A(0.089) H56B(0.089) H57A(0.076)
 H57B(0.076) H58A(0.053) H58B(0.053) H59A(0.046) H59B(0.046) H60A(0.077)
 H60B(0.077) H61A(0.077) H61B(0.077) H62A(0.081) H62B(0.081) H59C(0.107)
 H59D(0.107) H60C(0.081) H60D(0.081) H61C(0.091) H61D(0.091) H62C(0.191)
 H62D(0.191) H63A(0.12) H63B(0.12) H64A(0.084) H64B(0.084) H65A(0.137)
 H65B(0.137) H66A(0.178) H66B(0.178) H63C(0.125) H63D(0.125) H64C(0.101)
 H64D(0.101) H65C(0.132) H65D(0.132) H66C(0.105) H66D(0.105) H67A(0.11)
 H67B(0.11) H68A(0.072) H68B(0.072) H69A(0.096) H69B(0.096) H70A(0.183)
 H70B(0.183) H67C(0.199) H67D(0.199) H68C(0.147) H68D(0.147) H69C(0.161)
 H69D(0.161) H70C(0.296) H70D(0.296)
 Fixed X: H1(0.244442) H1A(0.283364) H1B(0.166368) H1C(0.231777) H2A(0.106773)
 H2B(0.039476) H2C(0.080424) H3A(0.146744) H3B(0.110681) H3C(0.226001)
 H6(0.313796) H8(0.489094) H11A(0.506895) H11B(0.507091) H11C(0.414492)
 H12A(0.376359) H12B(0.40726) H14(0.559245) H16(0.795103) H20A(0.773853)
 H20B(0.762955) H20C(0.66426) H21A(0.830694) H21B(0.862855) H21C(0.87327)
 H22A(0.600168) H22B(0.704821) H22C(0.657678) H23A(0.787628) H23B(0.708454)
 H23C(0.801052) H24A(0.365118) H24B(0.46009) H24C(0.477438) H25A(0.581095)
 H25B(0.561764) H25C(0.536641) H26A(0.357635) H26B(0.384912) H26C(0.291013)
 H29(0.370029) H31(0.308937) H34A(0.328316) H34B(0.338334) H34C(0.232128)
 H35A(0.391779) H35B(0.385574) H37(0.216862) H39(-0.00509) H42A(-0.023419)
 H42B(0.074672) H42C(0.004019) H44A(-0.016909) H44B(-0.043962) H44C(-0.076918)
 H45A(0.009876) H45B(0.036884) H45C(0.124489) H46A(0.220092) H46B(0.131959)
 H46C(0.16121) H47A(0.482244) H47B(0.476859) H47C(0.432412) H47D(0.50656)
 H48A(0.359654) H48B(0.416474) H48C(0.402508) H48D(0.430942) H49A(0.224314)
 H49B(0.289761) H49C(0.265411) H49D(0.24133) H50A(0.299009) H50B(0.220864)
 H50C(0.221049) H50D(0.290777) H51A(0.190325) H51B(0.304036) H51C(0.199153)
 H51D(0.286682) H52A(0.158215) H52B(0.253828) H52C(0.179336) H52D(0.102635)
 H53A(0.126988) H53B(0.064005) H53C(0.037228) H53D(0.059527) H54A(0.220527)
 H54B(0.138052) H54C(0.141489) H54D(0.200235) H55A(0.465244) H55B(0.557923)
 H56A(0.657123) H56B(0.590364) H57A(0.482354) H57B(0.589536) H58A(0.560284)
 H58B(0.446694) H59A(-0.043294) H59B(0.062542) H60A(-0.019685) H60B(0.099421)
 H61A(0.111496) H61B(-0.010267) H62A(-0.000711) H62B(0.118406) H59C(0.165566)
 H59D(0.062236) H60C(-0.027597) H60D(-0.087966) H61C(-0.029744) H61D(0.076737)
 H62C(0.127263) H62D(0.015353) H63A(0.343624) H63B(0.287095) H64A(0.099891)
 H64B(0.175627) H65A(0.112722) H65B(0.228588) H66A(0.156209) H66B(0.249177)
 H63C(0.261169) H63D(0.206202) H64C(0.023727) H64D(0.087374) H65C(0.117917)
 H65D(0.188769) H66C(0.225597) H66D(0.306011) H67A(0.219035) H67B(0.102033)
 H68A(0.065021) H68B(0.183882) H69A(0.052543) H69B(0.166101) H70A(0.130107)
 H70B(0.236755) H67C(0.257104) H67D(0.173528) H68C(0.243205) H68D(0.165211)
 H69C(0.132552) H69D(0.051828) H70C(-0.011322) H70D(0.077383)
 Fixed Y: H1(0.426681) H1A(0.32967) H1B(0.307311) H1C(0.319732) H2A(0.415618)
 H2B(0.407208) H2C(0.488985) H3A(0.497945) H3B(0.412811) H3C(0.43655)
 H6(0.526735) H8(0.590332) H11A(0.59456) H11B(0.65635) H11C(0.652673)
 H12A(0.465767) H12B(0.553291) H14(0.426307) H16(0.430785) H20A(0.616381)
 H20B(0.621438) H20C(0.623583) H21A(0.428764) H21B(0.505787) H21C(0.498728)
 H22A(0.516854) H22B(0.508196) H22C(0.436859) H23A(0.416761) H23B(0.348001)
 H23C(0.347851) H24A(0.350031) H24B(0.399482) H24C(0.322604) H25A(0.393881)
 H25B(0.470345) H25C(0.46735) H26A(0.511951) H26B(0.51068) H26C(0.462455)
 H29(0.266912) H31(0.238749) H34A(0.142948) H34B(0.12514) H34C(0.151858)
 H35A(0.420137) H35B(0.334141) H37(0.277035) H39(0.418287) H42A(0.261338)
 H42B(0.224368) H42C(0.280269) H44A(0.52549) H44B(0.607109) H44C(0.531594)
 H45A(0.576595) H45B(0.652814) H45C(0.605451) H46A(0.596679) H46B(0.647046)
 H46C(0.566945) H47A(0.746654) H47B(0.664682) H47C(0.674342) H47D(0.711139)
 H48A(0.70045) H48B(0.780852) H48C(0.79499) H48D(0.821771) H49A(0.755368)
 H49B(0.826292) H49C(0.840025) H49D(0.771644) H50A(0.775328) H50B(0.710268)
 H50C(0.707562) H50D(0.76392) H51A(0.712387) H51B(0.712086) H51C(0.707564)
 H51D(0.681277) H52A(0.705745) H52B(0.650714) H52C(0.613842) H52D(0.67867)
 H53A(0.561622) H53B(0.610175) H53C(0.602057) H53D(0.539849) H54A(0.507061)
 H54B(0.538385) H54C(0.526442) H54D(0.497796) H55A(0.763306) H55B(0.717483)
 H56A(0.732715) H56B(0.808929) H57A(0.753297) H57B(0.717693) H58A(0.605867)
 H58B(0.626094) H59A(0.41596) H59B(0.458379) H60A(0.275839) H60B(0.256976)
 H61A(0.246369) H61B(0.246563) H62A(0.36129) H62B(0.367703) H59C(0.366079)
 H59D(0.4057) H60C(0.217493) H60D(0.295335) H61C(0.313298) H61D(0.273065)
 H62C(0.398168) H62D(0.424893) H63A(0.737053) H63B(0.663966) H64A(0.786389)
 H64B(0.858496) H65A(0.807019) H65B(0.831821) H66A(0.676132) H66B(0.713207)
 H63C(0.676796) H63D(0.651665) H64C(0.767389) H64D(0.774547) H65C(0.846278)
 H65D(0.846346) H66C(0.769626) H66D(0.785286) H67A(0.167895) H67B(0.191513)
 H68A(0.096879) H68B(0.084233) H69A(-0.003353) H69B(-0.024156) H70A(0.002892)
 H70B(0.028167) H67C(0.12405) H67D(0.112752) H68C(0.010102) H68D(-0.002085)
 H69C(-0.016124) H69D(-0.018638) H70C(0.070159) H70D(0.078143)
 Fixed Z: H1(0.136103) H1A(0.000141) H1B(0.000422) H1C(0.049201) H2A(0.074417)
 H2B(0.02582) H2C(0.042663) H3A(-0.037533) H3B(-0.049105) H3C(-0.054256) H6(-
 0.021113) H8(0.092668) H11A(-0.020208) H11B(0.021157) H11C(-0.017862)
 H12A(0.173604) H12B(0.172772) H14(0.11252) H16(0.208835) H20A(0.249829)
 H20B(0.305557) H20C(0.269983) H21A(0.289793) H21B(0.316712) H21C(0.261032)
 H22A(0.319183) H22B(0.350133) H22C(0.321512) H23A(0.103258) H23B(0.100819)
 H23C(0.13991) H24A(0.48421) H24B(0.503823) H24C(0.475348) H25A(0.42154)
 H25B(0.450102) H25C(0.394226) H26A(0.409106) H26B(0.46485) H26C(0.442768)
 H29(0.425968) H31(0.286795) H34A(0.398212) H34B(0.343429) H34C(0.361548)
 H35A(0.252464) H35B(0.23471) H37(0.215082) H39(0.167804) H42A(0.192479)
 H42B(0.171698) H42C(0.139672) H44A(0.128444) H44B(0.14904) H44C(0.175435)
 H45A(0.250214) H45B(0.222982) H45C(0.251127) H46A(0.175962) H46B(0.15056)
 H46C(0.12851) H47A(0.222092) H47B(0.197487) H47C(0.179767) H47D(0.221056)
 H48A(0.143756) H48B(0.152867) H48C(0.163174) H48D(0.21625) H49A(0.172154)
 H49B(0.192415) H49C(0.214903) H49D(0.177604) H50A(0.267389) H50B(0.248187)
 H50C(0.241224) H50D(0.273259) H51A(0.333246) H51B(0.357829) H51C(0.348765)
 H51D(0.386831) H52A(0.412455) H52B(0.424333) H52C(0.42878) H52D(0.408111)
 H53A(0.416363) H53B(0.37635) H53C(0.349048) H53D(0.390102) H54A(0.363495)
 H54B(0.324048) H54C(0.310635) H54D(0.358658) H55A(0.316314) H55B(0.295808)
 H56A(0.362735) H56B(0.365877) H57A(0.415009) H57B(0.434053) H58A(0.393963)
 H58B(0.406718) H59A(0.356901) H59B(0.369489) H60A(0.312318) H60B(0.312879)
 H61A(0.39119) H61B(0.388794) H62A(0.425182) H62B(0.418014) H59C(0.386563)
 H59D(0.399964) H60C(0.348148) H60D(0.356188) H61C(0.285011) H61D(0.299961)
 H62C(0.312747) H62D(0.325081) H63A(0.525956) H63B(0.504607) H64A(0.473718)
 H64B(0.47768) H65A(0.553743) H65B(0.553513) H66A(0.555007) H66B(0.588313)
 H63C(0.512194) H63D(0.558346) H64C(0.516234) H64D(0.470399) H65C(0.548801)
 H65D(0.505) H66C(0.591333) H66D(0.551624) H67A(0.079994) H67B(0.078445)
 H68A(0.116091) H68B(0.126793) H69A(0.071284) H69B(0.090763) H70A(0.000519)
 H70B(0.025831) H67C(0.064766) H67D(0.103486) H68C(0.045774) H68D(0.085658)
 H69C(-0.002184) H69D(0.037282) H70C(0.00884) H70D(-0.027104)
;
_shelx_res_checksum              49142
_olex2_submission_special_instructions 'No special instructions were received'