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_7708379
_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 Nd O7, 3(C4 H8 O)'
_chemical_formula_sum            'C70 H109 Nd O10'
_chemical_formula_weight         1254.81
_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             2021-09-15
_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                 93.50(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.176(3)
_cell_length_b                   17.631(4)
_cell_length_c                   28.491(6)
_cell_measurement_reflns_used    11605
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6606(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)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0748
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            76138
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.359
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.4864
_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    1.262
_exptl_crystal_description       block
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.472
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.232
_refine_ls_extinction_coef       0.105(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   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     941
_refine_ls_number_reflns         11605
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.1965
_refine_ls_R_factor_gt           0.1274
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2981
_refine_ls_wR_factor_ref         0.3659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6036
_reflns_number_total             11605
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           2
_cod_original_cell_volume        6606(2)
_cod_database_code               7708379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.850
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.165) H1A(0.182) H1B(0.182) H1C(0.182) H2A(0.179) H2B(0.179)
 H2C(0.179) H3A(0.178) H3B(0.178) H3C(0.178) H6(0.132) H8(0.133) H11A(0.185)
 H11B(0.185) H11C(0.185) H12A(0.135) H12B(0.135) H14(0.132) H16(0.136)
 H20A(0.191) H20B(0.191) H20C(0.191) H21A(0.201) H21B(0.201) H21C(0.201)
 H22A(0.183) H22B(0.183) H22C(0.183) H23A(0.192) H23B(0.192) H23C(0.192)
 H24A(0.185) H24B(0.185) H24C(0.185) H25A(0.169) H25B(0.169) H25C(0.169)
 H26A(0.174) H26B(0.174) H26C(0.174) H29(0.127) H31(0.125) H34A(0.175)
 H34B(0.175) H34C(0.175) H35A(0.126) H35B(0.126) H37(0.127) H39(0.128)
 H42A(0.197) H42B(0.197) H42C(0.197) H44A(0.181) H44B(0.181) H44C(0.181)
 H45A(0.168) H45B(0.168) H45C(0.168) H46A(0.171) H46B(0.171) H46C(0.171)
 H47A(0.144) H47B(0.144) H47C(0.144) H47D(0.144) H48A(0.147) H48B(0.147)
 H48C(0.175) H48D(0.175) H49A(0.16) H49B(0.16) H49C(0.174) H49D(0.174)
 H50A(0.151) H50B(0.151) H50C(0.151) H50D(0.151) H51A(0.144) H51B(0.144)
 H51C(0.147) H51D(0.147) H52A(0.144) H52B(0.144) H52C(0.146) H52D(0.146)
 H53A(0.167) H53B(0.167) H53C(0.157) H53D(0.157) H54A(0.178) H54B(0.178)
 H54C(0.131) H54D(0.131) H55A(0.179) H55B(0.179) H56A(0.2) H56B(0.2)
 H57A(0.178) H57B(0.178) H58A(0.147) H58B(0.147) H59A(0.134) H59B(0.134)
 H60A(0.153) H60B(0.153) H61A(0.184) H61B(0.184) H62A(0.173) H62B(0.173)
 H59C(0.2) H59D(0.2) H60C(0.166) H60D(0.166) H61C(0.197) H61D(0.197)
 H62C(0.218) H62D(0.218) H63A(0.193) H63B(0.193) H64A(0.162) H64B(0.162)
 H65A(0.199) H65B(0.199) H66A(0.209) H66B(0.209) H63C(0.179) H63D(0.179)
 H64C(0.179) H64D(0.179) H65C(0.189) H65D(0.189) H66C(0.185) H66D(0.185)
 H67A(0.207) H67B(0.207) H68A(0.189) H68B(0.189) H69A(0.208) H69B(0.208)
 H70A(0.276) H70B(0.276) H67C(0.234) H67D(0.234) H68C(0.186) H68D(0.186)
 H69C(0.196) H69D(0.196) H70C(0.228) H70D(0.228)
 Fixed X: H1(0.299995) H1A(0.232039) H1B(0.281802) H1C(0.163958) H2A(0.037884)
 H2B(0.079206) H2C(0.105512) H3A(0.226969) H3B(0.145894) H3C(0.111504)
 H6(0.314052) H8(0.490547) H11A(0.510653) H11B(0.502532) H11C(0.413555)
 H12A(0.416483) H12B(0.3769) H14(0.558471) H16(0.796734) H20A(0.793519)
 H20B(0.750115) H20C(0.673848) H21A(0.828423) H21B(0.862131) H21C(0.875283)
 H22A(0.604807) H22B(0.706447) H22C(0.640455) H23A(0.707582) H23B(0.800952)
 H23C(0.78715) H24A(0.477115) H24B(0.362826) H24C(0.455998) H25A(0.558331)
 H25B(0.534639) H25C(0.579406) H26A(0.287006) H26B(0.358904) H26C(0.378696)
 H29(0.368057) H31(0.308589) H34A(0.341767) H34B(0.327478) H34C(0.232582)
 H35A(0.385521) H35B(0.384954) H37(0.215323) H39(-0.008668) H42A(0.071973)
 H42B(0.008781) H42C(-0.028952) H44A(-0.022417) H44B(-0.045158) H44C(-0.080834)
 H45A(0.005931) H45B(0.029823) H45C(0.120021) H46A(0.213191) H46B(0.124276)
 H46C(0.166994) H47A(0.485212) H47B(0.477635) H47C(0.432456) H47D(0.508337)
 H48A(0.368603) H48B(0.413977) H48C(0.426453) H48D(0.431642) H49A(0.273616)
 H49B(0.220914) H49C(0.27103) H49D(0.265724) H50A(0.287369) H50B(0.215431)
 H50C(0.2717) H50D(0.216337) H51A(0.198181) H51B(0.312163) H51C(0.192782)
 H51D(0.281906) H52A(0.159732) H52B(0.253324) H52C(0.16971) H52D(0.091376)
 H53A(0.133454) H53B(0.054816) H53C(0.027289) H53D(0.043735) H54A(0.179209)
 H54B(0.110201) H54C(0.201489) H54D(0.14405) H55A(0.463143) H55B(0.557331)
 H56A(0.659603) H56B(0.586475) H57A(0.488389) H57B(0.597376) H58A(0.562921)
 H58B(0.45006) H59A(0.058691) H59B(-0.046474) H60A(-0.027123) H60B(0.089509)
 H61A(0.102512) H61B(-0.019872) H62A(0.00143) H62B(0.1199) H59C(0.161717)
 H59D(0.060652) H60C(-0.089175) H60D(-0.014007) H61C(-0.042404) H61D(0.070207)
 H62C(0.111606) H62D(-0.000856) H63A(0.345967) H63B(0.281518) H64A(0.10277)
 H64B(0.181107) H65A(0.106592) H65B(0.224181) H66A(0.238922) H66B(0.147838)
 H63C(0.258967) H63D(0.210922) H64C(0.020697) H64D(0.060971) H65C(0.130497)
 H65D(0.191666) H66C(0.22331) H66D(0.30484) H67A(0.236138) H67B(0.130974)
 H68A(0.176056) H68B(0.060066) H69A(0.059438) H69B(0.179576) H70A(0.226378)
 H70B(0.114159) H67C(0.275186) H67D(0.191478) H68C(0.161048) H68D(0.241665)
 H69C(0.064962) H69D(0.139295) H70C(0.033993) H70D(-0.017634)
 Fixed Y: H1(0.401648) H1A(0.323109) H1B(0.327213) H1C(0.306603) H2A(0.408167)
 H2B(0.49036) H2C(0.418364) H3A(0.433027) H3B(0.494259) H3C(0.408368)
 H6(0.52509) H8(0.594517) H11A(0.592965) H11B(0.658968) H11C(0.647661)
 H12A(0.565119) H12B(0.480049) H14(0.431495) H16(0.430869) H20A(0.612479)
 H20B(0.618909) H20C(0.621316) H21A(0.424417) H21B(0.497995) H21C(0.496073)
 H22A(0.523207) H22B(0.493659) H22C(0.437115) H23A(0.35149) H23B(0.349709)
 H23C(0.42014) H24A(0.3227) H24B(0.347863) H24C(0.398876) H25A(0.469889)
 H25B(0.4688) H25C(0.394776) H26A(0.460472) H26B(0.513207) H26C(0.506093)
 H29(0.265687) H31(0.239101) H34A(0.13995) H34B(0.1273) H34C(0.152171)
 H35A(0.422799) H35B(0.338264) H37(0.277969) H39(0.417917) H42A(0.223575)
 H42B(0.278498) H42C(0.264214) H44A(0.520236) H44B(0.604717) H44C(0.533745)
 H45A(0.573523) H45B(0.650301) H45C(0.60476) H46A(0.601134) H46B(0.639838)
 H46C(0.558248) H47A(0.678715) H47B(0.762245) H47C(0.691639) H47D(0.716665)
 H48A(0.703667) H48B(0.788083) H48C(0.830597) H48D(0.82243) H49A(0.826922)
 H49B(0.749098) H49C(0.778926) H49D(0.84836) H50A(0.785701) H50B(0.715673)
 H50C(0.7703) H50D(0.71357) H51A(0.721104) H51B(0.712475) H51C(0.712632)
 H51D(0.684913) H52A(0.714891) H52B(0.658594) H52C(0.610208) H52D(0.675841)
 H53A(0.564025) H53B(0.616915) H53C(0.601913) H53D(0.538034) H54A(0.513712)
 H54B(0.573184) H54C(0.502204) H54D(0.522229) H55A(0.768473) H55B(0.722413)
 H56A(0.744782) H56B(0.817407) H57A(0.758117) H57B(0.721943) H58A(0.612123)
 H58B(0.633408) H59A(0.455909) H59B(0.413047) H60A(0.278861) H60B(0.252532)
 H61A(0.237078) H61B(0.242518) H62A(0.352415) H62B(0.35633) H59C(0.366893)
 H59D(0.402389) H60C(0.282902) H60D(0.215139) H61C(0.324334) H61D(0.289163)
 H62C(0.412618) H62D(0.430151) H63A(0.724329) H63B(0.656623) H64A(0.788191)
 H64B(0.858303) H65A(0.805017) H65B(0.829813) H66A(0.705955) H66B(0.676515)
 H63C(0.67416) H63D(0.652702) H64C(0.766829) H64D(0.770807) H65C(0.856842)
 H65D(0.841342) H66C(0.771642) H66D(0.782146) H67A(0.150829) H67B(0.193198)
 H68A(0.076837) H68B(0.09161) H69A(-0.015471) H69B(-0.026057) H70A(0.030286)
 H70B(0.00604) H67C(0.107612) H67D(0.104728) H68C(0.003094) H68D(0.005954)
 H69C(-0.032967) H69D(-0.011623) H70C(0.099505) H70D(0.090513)
 Fixed Z: H1(0.136867) H1A(0.053832) H1B(0.004041) H1C(0.006491) H2A(0.027722)
 H2B(0.043176) H2C(0.075897) H3A(-0.05206) H3B(-0.036496) H3C(-0.046294) H6(-
 0.021811) H8(0.089683) H11A(-0.019561) H11B(0.018586) H11C(-0.021595)
 H12A(0.171301) H12B(0.176071) H14(0.111092) H16(0.206439) H20A(0.256177)
 H20B(0.307277) H20C(0.261384) H21A(0.28639) H21B(0.316319) H21C(0.260862)
 H22A(0.320656) H22B(0.348412) H22C(0.314885) H23A(0.098572) H23B(0.137208)
 H23C(0.101965) H24A(0.474847) H24B(0.482998) H24C(0.503197) H25A(0.450616)
 H25B(0.394857) H25C(0.421212) H26A(0.439896) H26B(0.410482) H26C(0.466287)
 H29(0.425482) H31(0.286564) H34A(0.394593) H34B(0.338961) H34C(0.367897)
 H35A(0.254026) H35B(0.234069) H37(0.216941) H39(0.166998) H42A(0.174408)
 H42B(0.138729) H42C(0.190329) H44A(0.130724) H44B(0.147741) H44C(0.177636)
 H45A(0.249628) H45B(0.222444) H45C(0.250034) H46A(0.177787) H46B(0.145332)
 H46C(0.131808) H47A(0.203014) H47B(0.225103) H47C(0.180599) H47D(0.224581)
 H48A(0.144995) H48B(0.152828) H48C(0.232386) H48D(0.176366) H49A(0.186388)
 H49B(0.168445) H49C(0.1684) H49D(0.205426) H50A(0.260561) H50B(0.24373)
 H50C(0.268061) H50D(0.230584) H51A(0.332783) H51B(0.357458) H51C(0.35241)
 H51D(0.389528) H52A(0.411486) H52B(0.424547) H52C(0.431842) H52D(0.413955)
 H53A(0.416975) H53B(0.386244) H53C(0.349643) H53D(0.39019) H54A(0.351853)
 H54B(0.321193) H54C(0.364833) H54D(0.315045) H55A(0.318559) H55B(0.299004)
 H56A(0.366203) H56B(0.370895) H57A(0.420002) H57B(0.43575) H58A(0.396415)
 H58B(0.410862) H59A(0.372601) H59B(0.357594) H60A(0.311374) H60B(0.310659)
 H61A(0.387806) H61B(0.385659) H62A(0.425674) H62B(0.41558) H59C(0.383381)
 H59D(0.402779) H60C(0.357888) H60D(0.34478) H61C(0.286585) H61D(0.294317)
 H62C(0.315043) H62D(0.332064) H63A(0.525631) H63B(0.501186) H64A(0.473642)
 H64B(0.479627) H65A(0.552919) H65B(0.555899) H66A(0.582612) H66B(0.546073)
 H63C(0.510558) H63D(0.559227) H64C(0.525643) H64D(0.47372) H65C(0.543367)
 H65D(0.496898) H66C(0.585863) H66D(0.54633) H67A(0.075513) H67B(0.083062)
 H68A(0.129656) H68B(0.112068) H69A(0.076484) H69B(0.08955) H70A(0.015185)
 H70B(-0.003623) H67C(0.063454) H67D(0.10343) H68C(0.085691) H68D(0.047034)
 H69C(0.037341) H69D(-0.003772) H70C(-0.018606) H70D(0.031891)
;
_shelx_res_checksum              1953
_olex2_submission_special_instructions 'No special instructions were received'