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_7708382
_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 Lu O7, 3(C4 H8 O)'
_chemical_formula_sum            'C70 H109 Lu O10'
_chemical_formula_weight         1285.54
_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             2021-09-19
_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                 93.23(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.210(3)
_cell_length_b                   17.490(4)
_cell_length_c                   28.400(6)
_cell_measurement_reflns_used    11194
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6551(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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'MX1 Beamline Australian Synchrotron'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0408
_diffrn_reflns_Laue_measured_fraction_full 0.965
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_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            70227
_diffrn_reflns_point_group_measured_fraction_full 0.965
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.039
_diffrn_reflns_theta_max         25.039
_diffrn_reflns_theta_min         1.368
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.563
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       block
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.521
_refine_diff_density_min         -2.157
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       0.00106(17)
_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   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         11194
_refine_ls_number_restraints     436
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0803
_refine_ls_R_factor_gt           0.0602
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1047P)^2^+3.8759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8254
_reflns_number_total             11194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           7
_cod_original_cell_volume        6551(2)
_cod_database_code               7708382
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.745
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.101) H1A(0.115) H1B(0.115) H1C(0.115) H2A(0.114) H2B(0.114)
 H2C(0.114) H3A(0.115) H3B(0.115) H3C(0.115) H6(0.082) H8(0.084) H11A(0.124)
 H11B(0.124) H11C(0.124) H12A(0.095) H12B(0.095) H14(0.083) H16(0.082)
 H20A(0.136) H20B(0.136) H20C(0.136) H21A(0.135) H21B(0.135) H21C(0.135)
 H22A(0.113) H22B(0.113) H22C(0.113) H23A(0.127) H23B(0.127) H23C(0.127)
 H24A(0.121) H24B(0.121) H24C(0.121) H25A(0.105) H25B(0.105) H25C(0.105)
 H26A(0.115) H26B(0.115) H26C(0.115) H29(0.077) H31(0.073) H34A(0.107)
 H34B(0.107) H34C(0.107) H35A(0.075) H35B(0.075) H37(0.075) H39(0.077)
 H42A(0.123) H42B(0.123) H42C(0.123) H44A(0.106) H44B(0.106) H44C(0.106)
 H45A(0.107) H45B(0.107) H45C(0.107) H46A(0.102) H46B(0.102) H46C(0.102)
 H47A(0.109) H47B(0.109) H47C(0.109) H47D(0.109) H48A(0.089) H48B(0.089)
 H48C(0.118) H48D(0.118) H49A(0.099) H49B(0.099) H49C(0.099) H49D(0.099)
 H50A(0.102) H50B(0.102) H50C(0.102) H50D(0.102) H51A(0.094) H51B(0.094)
 H51C(0.104) H51D(0.104) H52A(0.11) H52B(0.11) H52C(0.106) H52D(0.106)
 H53A(0.117) H53B(0.117) H53C(0.099) H53D(0.099) H54A(0.095) H54B(0.095)
 H54C(0.082) H54D(0.082) H55A(0.111) H55B(0.111) H56A(0.121) H56B(0.121)
 H57A(0.11) H57B(0.11) H58A(0.09) H58B(0.09) H59A(0.121) H59B(0.121)
 H60A(0.159) H60B(0.159) H61A(0.159) H61B(0.159) H62A(0.139) H62B(0.139)
 H59C(0.123) H59D(0.123) H60C(0.106) H60D(0.106) H61C(0.106) H61D(0.106)
 H62C(0.1) H62D(0.1) H63A(0.159) H63B(0.159) H64A(0.134) H64B(0.134)
 H65A(0.175) H65B(0.175) H66A(0.197) H66B(0.197) H63C(0.148) H63D(0.148)
 H64C(0.138) H64D(0.138) H65C(0.138) H65D(0.138) H66C(0.129) H66D(0.129)
 H67A(0.138) H67B(0.138) H68A(0.102) H68B(0.102) H69A(0.128) H69B(0.128)
 H70A(0.188) H70B(0.188) H67C(0.2) H67D(0.2) H68C(0.156) H68D(0.156)
 H69C(0.176) H69D(0.176) H70C(0.219) H70D(0.219)
 Fixed X: H1(0.235131) H1A(0.281831) H1B(0.164436) H1C(0.231586) H2A(0.104757)
 H2B(0.037736) H2C(0.075704) H3A(0.143259) H3B(0.11311) H3C(0.227333)
 H6(0.314271) H8(0.488196) H11A(0.508312) H11B(0.504699) H11C(0.41373)
 H12A(0.37448) H12B(0.401899) H14(0.557739) H16(0.794124) H20A(0.774963)
 H20B(0.750373) H20C(0.659879) H21A(0.829221) H21B(0.859282) H21C(0.872244)
 H22A(0.594611) H22B(0.698437) H22C(0.661194) H23A(0.793262) H23B(0.709046)
 H23C(0.796132) H24A(0.360607) H24B(0.458649) H24C(0.471491) H25A(0.5796)
 H25B(0.558213) H25C(0.53484) H26A(0.350982) H26B(0.379818) H26C(0.286369)
 H29(0.367733) H31(0.310319) H34A(0.3317) H34B(0.337482) H34C(0.232676)
 H35A(0.385686) H35B(0.392712) H37(0.218247) H39(-0.005309) H42A(-0.024589)
 H42B(0.074361) H42C(0.004964) H44A(-0.016798) H44B(-0.0415) H44C(-0.079072)
 H45A(0.00479) H45B(0.038061) H45C(0.121432) H46A(0.218122) H46B(0.130207)
 H46C(0.160452) H47A(0.483565) H47B(0.473319) H47C(0.431197) H47D(0.505632)
 H48A(0.362813) H48B(0.418066) H48C(0.432164) H48D(0.398277) H49A(0.225178)
 H49B(0.28586) H49C(0.241268) H49D(0.272129) H50A(0.298163) H50B(0.219701)
 H50C(0.219509) H50D(0.288349) H51A(0.192574) H51B(0.305628) H51C(0.199651)
 H51D(0.283149) H52A(0.155351) H52B(0.250716) H52C(0.167179) H52D(0.091296)
 H53A(0.126544) H53B(0.063477) H53C(0.031862) H53D(0.054385) H54A(0.218728)
 H54B(0.137184) H54C(0.134221) H54D(0.19314) H55A(0.458314) H55B(0.551317)
 H56A(0.653627) H56B(0.587371) H57A(0.477385) H57B(0.584553) H58A(0.55614)
 H58B(0.441724) H59A(-0.051733) H59B(0.062013) H60A(0.117788) H60B(-0.001887)
 H61A(0.140362) H61B(0.02232) H62A(-0.016559) H62B(0.10078) H59C(0.163894)
 H59D(0.056591) H60C(-0.087795) H60D(-0.023275) H61C(-0.031296) H61D(0.070316)
 H62C(0.149165) H62D(0.042482) H63A(0.346028) H63B(0.261191) H64A(0.099472)
 H64B(0.179538) H65A(0.122395) H65B(0.236344) H66A(0.169827) H66B(0.273202)
 H63C(0.259826) H63D(0.202182) H64C(0.023233) H64D(0.096097) H65C(0.112708)
 H65D(0.183928) H66C(0.230988) H66D(0.305852) H67A(0.231588) H67B(0.12216)
 H68A(0.066465) H68B(0.18373) H69A(0.061193) H69B(0.180702) H70A(0.116)
 H70B(0.228242) H67C(0.278358) H67D(0.205824) H68C(0.174582) H68D(0.247407)
 H69C(0.057534) H69D(0.1286) H70C(-0.014888) H70D(0.048306)
 Fixed Y: H1(0.424733) H1A(0.327789) H1B(0.305897) H1C(0.318086) H2A(0.415374)
 H2B(0.403861) H2C(0.487513) H3A(0.497766) H3B(0.411313) H3C(0.439781)
 H6(0.526349) H8(0.588464) H11A(0.595436) H11B(0.65838) H11C(0.652427)
 H12A(0.459782) H12B(0.548547) H14(0.423853) H16(0.430145) H20A(0.617364)
 H20B(0.621399) H20C(0.622354) H21A(0.427404) H21B(0.503251) H21C(0.500146)
 H22A(0.510513) H22B(0.510541) H22C(0.434212) H23A(0.416865) H23B(0.351544)
 H23C(0.343554) H24A(0.351169) H24B(0.398312) H24C(0.320326) H25A(0.395055)
 H25B(0.470768) H25C(0.469569) H26A(0.511422) H26B(0.511823) H26C(0.46154)
 H29(0.26632) H31(0.238059) H34A(0.139683) H34B(0.123145) H34C(0.149394)
 H35A(0.332557) H35B(0.419304) H37(0.276126) H39(0.417069) H42A(0.259875)
 H42B(0.22131) H42C(0.276486) H44A(0.522133) H44B(0.606675) H44C(0.5341)
 H45A(0.578468) H45B(0.654316) H45C(0.603628) H46A(0.596239) H46B(0.645937)
 H46C(0.564623) H47A(0.740713) H47B(0.658615) H47C(0.668316) H47D(0.70702)
 H48A(0.698499) H48B(0.779187) H48C(0.817748) H48D(0.787459) H49A(0.747823)
 H49B(0.822194) H49C(0.772192) H49D(0.839079) H50A(0.772914) H50B(0.706594)
 H50C(0.704062) H50D(0.759789) H51A(0.712586) H51B(0.70981) H51C(0.70771)
 H51D(0.676634) H52A(0.704967) H52B(0.649556) H52C(0.608935) H52D(0.673077)
 H53A(0.560042) H53B(0.609982) H53C(0.596357) H53D(0.534386) H54A(0.50648)
 H54B(0.540312) H54C(0.52135) H54D(0.493271) H55A(0.761671) H55B(0.717898)
 H56A(0.73112) H56B(0.808216) H57A(0.751757) H57B(0.716007) H58A(0.603324)
 H58B(0.623711) H59A(0.419537) H59B(0.451606) H60A(0.267458) H60B(0.256662)
 H61A(0.258318) H61B(0.233836) H62A(0.351911) H62B(0.375658) H59C(0.365787)
 H59D(0.40695) H60C(0.291625) H60D(0.214644) H61C(0.315274) H61D(0.266055)
 H62C(0.380405) H62D(0.424071) H63A(0.713145) H63B(0.653134) H64A(0.786643)
 H64B(0.856837) H65A(0.802705) H65B(0.830407) H66A(0.677711) H66B(0.719055)
 H63C(0.674848) H63D(0.65141) H64C(0.762976) H64D(0.772425) H65C(0.841952)
 H65D(0.85346) H66C(0.767551) H66D(0.784578) H67A(0.158095) H67B(0.195322)
 H68A(0.101011) H68B(0.087354) H69A(-0.012788) H69B(-0.025337) H70A(0.00807)
 H70B(0.03164) H67C(0.117762) H67D(0.10647) H68C(-0.003533) H68D(0.006607)
 H69C(-0.024143) H69D(-0.005351) H70C(0.086336) H70D(0.101082)
 Fixed Z: H1(0.133922) H1A(-0.001089) H1B(0.000448) H1C(0.048537)
 H2A(0.074928) H2B(0.026737) H2C(0.042237) H3A(-0.036465) H3B(-0.049279) H3C(-
 0.053644) H6(-0.020695) H8(0.093506) H11A(-0.01849) H11B(0.022279) H11C(-
 0.017213) H12A(0.172995) H12B(0.173886) H14(0.112845) H16(0.209093)
 H20A(0.252632) H20B(0.307112) H20C(0.267208) H21A(0.2878) H21B(0.316847)
 H21C(0.261192) H22A(0.317807) H22B(0.349688) H22C(0.322896) H23A(0.105887)
 H23B(0.098444) H23C(0.139654) H24A(0.485102) H24B(0.503774) H24C(0.475247)
 H25A(0.421699) H25B(0.451181) H25C(0.395279) H26A(0.40884) H26B(0.464331)
 H26C(0.443634) H29(0.425811) H31(0.286969) H34A(0.397863) H34B(0.342658)
 H34C(0.363258) H35A(0.235002) H35B(0.252317) H37(0.216192) H39(0.168678)
 H42A(0.194711) H42B(0.174952) H42C(0.141798) H44A(0.129642) H44B(0.147243)
 H44C(0.175809) H45A(0.250001) H45B(0.2234) H45C(0.252076) H46A(0.17623)
 H46B(0.150019) H46C(0.129125) H47A(0.221066) H47B(0.196279) H47C(0.179599)
 H47D(0.219945) H48A(0.142889) H48B(0.154248) H48C(0.212689) H48D(0.161091)
 H49A(0.169952) H49B(0.189052) H49C(0.178426) H49D(0.215921) H50A(0.267359)
 H50B(0.249557) H50C(0.241011) H50D(0.274122) H51A(0.332667) H51B(0.357698)
 H51C(0.350159) H51D(0.388594) H52A(0.410902) H52B(0.423624) H52C(0.427951)
 H52D(0.405715) H53A(0.414033) H53B(0.374854) H53C(0.348252) H53D(0.389448)
 H54A(0.360467) H54B(0.321645) H54C(0.310908) H54D(0.358803) H55A(0.31624)
 H55B(0.293818) H56A(0.360868) H56B(0.364568) H57A(0.413244) H57B(0.432327)
 H58A(0.392268) H58B(0.40465) H59A(0.361448) H59B(0.365825) H60A(0.318918)
 H60B(0.321237) H61A(0.395231) H61B(0.396112) H62A(0.422698) H62B(0.422811)
 H59C(0.392327) H59D(0.397344) H60C(0.35906) H60D(0.352822) H61C(0.288701)
 H61D(0.299025) H62C(0.314607) H62D(0.319839) H63A(0.518998) H63B(0.502583)
 H64A(0.476635) H64B(0.478689) H65A(0.555021) H65B(0.551642) H66A(0.565296)
 H66B(0.587366) H63C(0.512551) H63D(0.558438) H64C(0.513184) H64D(0.47041)
 H65C(0.554151) H65D(0.51047) H66C(0.591478) H66D(0.549339) H67A(0.079717)
 H67B(0.085886) H68A(0.115158) H68B(0.129689) H69A(0.075932) H69B(0.089186)
 H70A(-0.000556) H70B(0.018917) H67C(0.063817) H67D(0.107941) H68C(0.085845)
 H68D(0.043681) H69C(0.03758) H69D(-0.005074) H70C(0.030506) H70D(-0.016082)
;
_shelx_res_checksum              66393
_olex2_submission_special_instructions 'No special instructions were received'