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_7708380
_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 Tm, 3(C4 H8 O1)'
_chemical_formula_sum            'C70 H109 O10 Tm'
_chemical_formula_weight         1279.50
_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
_atom_sites_solution_primary     dual
_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                 93.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.200(3)
_cell_length_b                   17.530(4)
_cell_length_c                   28.420(6)
_cell_measurement_reflns_used    11559
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6565(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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.927
_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  0.0450
_diffrn_reflns_av_unetI/netI     0.0165
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            157911
_diffrn_reflns_point_group_measured_fraction_full 0.943
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         1.365
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  0.8
_exptl_absorpt_correction_T_min  0.7
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_description       block
_exptl_crystal_F_000             2712
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.697
_refine_diff_density_min         -1.281
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         11559
_refine_ls_number_restraints     428
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0756P)^2^+8.0789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1271
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10263
_reflns_number_total             11559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           6
_cod_original_cell_volume        6565(2)
_cod_database_code               7708380
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.872
_shelx_estimated_absorpt_t_min   0.766
_olex2_refinement_description
;
1. Shared sites
{H50B, H50D}
2. Others
 Fixed Uiso: H1(0.09) H1A(0.105) H1B(0.105) H1C(0.105) H2A(0.099) H2B(0.099)
 H2C(0.099) H3A(0.104) H3B(0.104) H3C(0.104) H6(0.07) H8(0.078) H11A(0.111)
 H11B(0.111) H11C(0.111) H12A(0.091) H12B(0.091) H14(0.072) H16(0.073)
 H20A(0.125) H20B(0.125) H20C(0.125) H21A(0.121) H21B(0.121) H21C(0.121)
 H22A(0.099) H22B(0.099) H22C(0.099) H23A(0.109) H23B(0.109) H23C(0.109)
 H24A(0.108) H24B(0.108) H24C(0.108) H25A(0.093) H25B(0.093) H25C(0.093)
 H26A(0.098) H26B(0.098) H26C(0.098) H29(0.065) H31(0.065) H34A(0.096)
 H34B(0.096) H34C(0.096) H35A(0.061) H35B(0.061) H37(0.066) H39(0.066)
 H42A(0.115) H42B(0.115) H42C(0.115) H44A(0.094) H44B(0.094) H44C(0.094)
 H45A(0.091) H45B(0.091) H45C(0.091) H46A(0.091) H46B(0.091) H46C(0.091)
 H47A(0.1) H47B(0.1) H47C(0.1) H47D(0.1) H48A(0.086) H48B(0.086) H48C(0.098)
 H48D(0.098) H49A(0.108) H49B(0.108) H49C(0.101) H49D(0.101) H50A(0.092)
 H50B(0.092) H50C(0.092) H50D(0.092) H51A(0.08) H51B(0.08) H51C(0.085)
 H51D(0.085) H52A(0.094) H52B(0.094) H52C(0.09) H52D(0.09) H53A(0.096)
 H53B(0.096) H53C(0.096) H53D(0.096) H54A(0.086) H54B(0.086) H54C(0.077)
 H54D(0.077) H55A(0.098) H55B(0.098) H56A(0.107) H56B(0.107) H57A(0.099)
 H57B(0.099) H58A(0.08) H58B(0.08) H59A(0.079) H59B(0.079) H60A(0.107)
 H60B(0.107) H61A(0.112) H61B(0.112) H62A(0.113) H62B(0.113) H59C(0.147)
 H59D(0.147) H60C(0.116) H60D(0.116) H61C(0.125) H61D(0.125) H62C(0.197)
 H62D(0.197) H63A(0.148) H63B(0.148) H64A(0.118) H64B(0.118) H65A(0.161)
 H65B(0.161) H66A(0.194) H66B(0.194) H63C(0.144) H63D(0.144) H64C(0.126)
 H64D(0.126) H65C(0.142) H65D(0.142) H66C(0.123) H66D(0.123) H67A(0.126)
 H67B(0.126) H68A(0.102) H68B(0.102) H69A(0.121) H69B(0.121) H70A(0.208)
 H70B(0.208) H67C(0.21) H67D(0.21) H68C(0.148) H68D(0.148) H69C(0.162)
 H69D(0.162) H70C(0.198) H70D(0.198)
 Fixed X: H1(0.259488) H1A(0.282967) H1B(0.16546) H1C(0.231025) H2A(0.105246)
 H2B(0.037847) H2C(0.076078) H3A(0.142765) H3B(0.112185) H3C(0.226507)
 H6(0.313747) H8(0.487874) H11A(0.505313) H11B(0.507897) H11C(0.413609)
 H12A(0.37413) H12B(0.402089) H14(0.558137) H16(0.794282) H20A(0.774846)
 H20B(0.757789) H20C(0.662421) H21A(0.828567) H21B(0.862291) H21C(0.87024)
 H22A(0.597126) H22B(0.701796) H22C(0.65647) H23A(0.789425) H23B(0.709949)
 H23C(0.80113) H24A(0.362089) H24B(0.456952) H24C(0.475075) H25A(0.579346)
 H25B(0.558905) H25C(0.535013) H26A(0.353343) H26B(0.379644) H26C(0.286287)
 H29(0.367692) H31(0.311762) H34A(0.331804) H34B(0.336132) H34C(0.232051)
 H35A(0.392388) H35B(0.386883) H37(0.217577) H39(-0.00561) H42A(-0.026025)
 H42B(0.074107) H42C(0.007142) H44A(-0.017312) H44B(-0.046102) H44C(-0.078247)
 H45A(0.004643) H45B(0.037198) H45C(0.121029) H46A(0.218512) H46B(0.129573)
 H46C(0.163202) H47A(0.484206) H47B(0.474028) H47C(0.432441) H47D(0.506209)
 H48A(0.359468) H48B(0.418602) H48C(0.429835) H48D(0.400468) H49A(0.225456)
 H49B(0.292758) H49C(0.239742) H49D(0.265041) H50A(0.296678) H50B(0.218961)
 H50C(0.290371) H50D(0.219335) H51A(0.19398) H51B(0.307329) H51C(0.194369)
 H51D(0.281907) H52A(0.157848) H52B(0.251749) H52C(0.175238) H52D(0.097686)
 H53A(0.123714) H53B(0.060559) H53C(0.035247) H53D(0.051851) H54A(0.211578)
 H54B(0.132487) H54C(0.142595) H54D(0.200421) H55A(0.462205) H55B(0.555323)
 H56A(0.655055) H56B(0.58932) H57A(0.476932) H57B(0.583995) H58A(0.558089)
 H58B(0.44343) H59A(0.061266) H59B(-0.046442) H60A(0.118757) H60B(-0.002213)
 H61A(0.118825) H61B(-0.002547) H62A(-0.02182) H62B(0.098644) H59C(0.160671)
 H59D(0.051034) H60C(-0.020571) H60D(-0.085514) H61C(-0.033286) H61D(0.075935)
 H62C(0.126192) H62D(0.012966) H63A(0.348456) H63B(0.261951) H64A(0.099164)
 H64B(0.178227) H65A(0.117335) H65B(0.229518) H66A(0.173298) H66B(0.275292)
 H63C(0.259828) H63D(0.199517) H64C(0.024957) H64D(0.096217) H65C(0.113352)
 H65D(0.185851) H66C(0.229128) H66D(0.306083) H67A(0.230806) H67B(0.120471)
 H68A(0.063701) H68B(0.181084) H69A(0.055818) H69B(0.173479) H70A(0.230276)
 H70B(0.120046) H67C(0.26818) H67D(0.189795) H68C(0.246358) H68D(0.170949)
 H69C(0.059059) H69D(0.131464) H70C(-0.019588) H70D(0.040127)
 Fixed Y: H1(0.418948) H1A(0.328542) H1B(0.306313) H1C(0.318699) H2A(0.416666)
 H2B(0.404175) H2C(0.487925) H3A(0.497482) H3B(0.41125) H3C(0.439433)
 H6(0.526448) H8(0.589766) H11A(0.59562) H11B(0.656429) H11C(0.654529)
 H12A(0.460957) H12B(0.549489) H14(0.424033) H16(0.429929) H20A(0.614631)
 H20B(0.620296) H20C(0.622037) H21A(0.427427) H21B(0.506029) H21C(0.495889)
 H22A(0.514573) H22B(0.507239) H22C(0.43494) H23A(0.41673) H23B(0.347758)
 H23C(0.346401) H24A(0.34925) H24B(0.399224) H24C(0.32236) H25A(0.394687)
 H25B(0.471237) H25C(0.468485) H26A(0.512529) H26B(0.510948) H26C(0.46215)
 H29(0.266914) H31(0.237767) H34A(0.139978) H34B(0.12367) H34C(0.150349)
 H35A(0.420551) H35B(0.334339) H37(0.276227) H39(0.417352) H42A(0.260985)
 H42B(0.221686) H42C(0.276447) H44A(0.525147) H44B(0.606464) H44C(0.529884)
 H45A(0.578245) H45B(0.654014) H45C(0.604282) H46A(0.598798) H46B(0.646365)
 H46C(0.565563) H47A(0.741056) H47B(0.659406) H47C(0.668688) H47D(0.708044)
 H48A(0.699639) H48B(0.779172) H48C(0.818399) H48D(0.788396) H49A(0.755412)
 H49B(0.82496) H49C(0.76713) H49D(0.837552) H50A(0.771829) H50B(0.706894)
 H50C(0.762276) H50D(0.704535) H51A(0.71387) H51B(0.710969) H51C(0.706283)
 H51D(0.680428) H52A(0.706949) H52B(0.64999) H52C(0.608658) H52D(0.67399)
 H53A(0.56122) H53B(0.61238) H53C(0.599212) H53D(0.537116) H54A(0.507)
 H54B(0.544734) H54C(0.517585) H54D(0.494795) H55A(0.761503) H55B(0.715928)
 H56A(0.730054) H56B(0.807339) H57A(0.751868) H57B(0.716907) H58A(0.603753)
 H58B(0.622909) H59A(0.456173) H59B(0.418396) H60A(0.263884) H60B(0.272515)
 H61A(0.248863) H61B(0.238268) H62A(0.353058) H62B(0.367193) H59C(0.371379)
 H59D(0.402135) H60C(0.215276) H60D(0.290253) H61C(0.316771) H61D(0.278064)
 H62C(0.401897) H62D(0.427987) H63A(0.712135) H63B(0.652945) H64A(0.785802)
 H64B(0.856454) H65A(0.800821) H65B(0.833541) H66A(0.67911) H66B(0.723042)
 H63C(0.675008) H63D(0.652363) H64C(0.764109) H64D(0.773947) H65C(0.843925)
 H65D(0.853356) H66C(0.768094) H66D(0.784347) H67A(0.160149) H67B(0.196993)
 H68A(0.100819) H68B(0.085456) H69A(-0.007058) H69B(-0.023375) H70A(0.033679)
 H70B(0.008965) H67C(0.122215) H67D(0.110613) H68C(0.00708) H68D(-0.004725)
 H69C(-0.026044) H69D(-0.003975) H70C(0.078806) H70D(0.093022)
 Fixed Z: H1(0.139315) H1A(-0.000289) H1B(0.000307) H1C(0.04885) H2A(0.074995)
 H2B(0.026978) H2C(0.041715) H3A(-0.036712) H3B(-0.049394) H3C(-0.053979) H6(-
 0.020644) H8(0.093277) H11A(-0.020211) H11B(0.021841) H11C(-0.016165)
 H12A(0.173335) H12B(0.173885) H14(0.112941) H16(0.208347) H20A(0.2506)
 H20B(0.305784) H20C(0.268372) H21A(0.290198) H21B(0.315099) H21C(0.259472)
 H22A(0.318613) H22B(0.349623) H22C(0.321193) H23A(0.103574) H23B(0.099742)
 H23C(0.139379) H24A(0.484413) H24B(0.503872) H24C(0.475164) H25A(0.421972)
 H25B(0.450603) H25C(0.394776) H26A(0.409568) H26B(0.465241) H26C(0.442955)
 H29(0.425818) H31(0.287045) H34A(0.397633) H34B(0.342381) H34C(0.363476)
 H35A(0.252717) H35B(0.234608) H37(0.216011) H39(0.168556) H42A(0.193449)
 H42B(0.175466) H42C(0.141019) H44A(0.128779) H44B(0.14984) H44C(0.17576)
 H45A(0.249673) H45B(0.223004) H45C(0.252071) H46A(0.176922) H46B(0.149845)
 H46C(0.129687) H47A(0.221452) H47B(0.196354) H47C(0.179975) H47D(0.220308)
 H48A(0.143462) H48B(0.153697) H48C(0.213227) H48D(0.161073) H49A(0.172619)
 H49B(0.193695) H49C(0.176785) H49D(0.212505) H50A(0.268591) H50B(0.248278)
 H50C(0.273512) H50D(0.24295) H51A(0.33218) H51B(0.357169) H51C(0.34873)
 H51D(0.386769) H52A(0.411572) H52B(0.423737) H52C(0.42722) H52D(0.407871)
 H53A(0.414289) H53B(0.375714) H53C(0.346737) H53D(0.388403) H54A(0.359657)
 H54B(0.321257) H54C(0.311752) H54D(0.361105) H55A(0.315054) H55B(0.294039)
 H56A(0.361234) H56B(0.364068) H57A(0.412702) H57B(0.432792) H58A(0.392368)
 H58B(0.405033) H59A(0.372309) H59B(0.356761) H60A(0.317544) H60B(0.312813)
 H61A(0.394023) H61B(0.386666) H62A(0.421633) H62B(0.423954) H59C(0.391774)
 H59D(0.404178) H60C(0.349479) H60D(0.360692) H61C(0.289378) H61D(0.300819)
 H62C(0.317147) H62D(0.329083) H63A(0.518602) H63B(0.50269) H64A(0.475747)
 H64B(0.478019) H65A(0.554243) H65B(0.552329) H66A(0.565562) H66B(0.586562)
 H63C(0.51348) H63D(0.558618) H64C(0.513974) H64D(0.470854) H65C(0.553247)
 H65D(0.50987) H66C(0.591904) H66D(0.550541) H67A(0.079713) H67B(0.084203)
 H68A(0.115882) H68B(0.130125) H69A(0.074156) H69B(0.089388) H70A(0.02116)
 H70B(-0.000595) H67C(0.065239) H67D(0.106764) H68C(0.044963) H68D(0.086205)
 H69C(0.036442) H69D(-0.004766) H70C(0.029595) H70D(-0.017975)
;
_shelx_res_checksum              98673
_olex2_submission_special_instructions 'No special instructions were received'