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_7708377
_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 Dy O7, 3(C4 H8 O)'
_chemical_formula_sum            'C70 H109 Dy O10'
_chemical_formula_weight         1273.07
_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                 93.44(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.212(3)
_cell_length_b                   17.539(4)
_cell_length_c                   28.459(6)
_cell_measurement_reflns_used    2419
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      3
_cell_volume                     6583(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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.961
_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  0.0435
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            113072
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.364
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.191
_exptl_absorpt_correction_T_max  0.88
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.287
_refine_diff_density_min         -2.208
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.00114(16)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         18449
_refine_ls_number_restraints     428
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0911P)^2^+3.1991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1473
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15728
_reflns_number_total             18449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           4
_cod_original_cell_volume        6583(2)
_cod_database_code               7708377
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.797
_olex2_refinement_description
;
1. Shared sites
{H69D, H70B}
2. Others
 Fixed Uiso: H1(0.075) H1A(0.088) H1B(0.088) H1C(0.088) H2A(0.081) H2B(0.081)
 H2C(0.081) H3A(0.086) H3B(0.086) H3C(0.086) H6(0.058) H8(0.067) H11A(0.099)
 H11B(0.099) H11C(0.099) H12A(0.075) H12B(0.075) H14(0.062) H16(0.064)
 H20A(0.111) H20B(0.111) H20C(0.111) H21A(0.109) H21B(0.109) H21C(0.109)
 H22A(0.087) H22B(0.087) H22C(0.087) H23A(0.1) H23B(0.1) H23C(0.1) H24A(0.094)
 H24B(0.094) H24C(0.094) H25A(0.081) H25B(0.081) H25C(0.081) H26A(0.085)
 H26B(0.085) H26C(0.085) H29(0.056) H31(0.053) H34A(0.081) H34B(0.081)
 H34C(0.081) H35A(0.049) H35B(0.049) H37(0.056) H39(0.056) H42A(0.103)
 H42B(0.103) H42C(0.103) H44A(0.078) H44B(0.078) H44C(0.078) H45A(0.076)
 H45B(0.076) H45C(0.076) H46A(0.081) H46B(0.081) H46C(0.081) H47A(0.084)
 H47B(0.084) H47C(0.084) H47D(0.084) H48A(0.083) H48B(0.083) H48C(0.082)
 H48D(0.082) H49A(0.113) H49B(0.113) H49C(0.106) H49D(0.106) H50A(0.087)
 H50B(0.087) H50C(0.087) H50D(0.087) H51A(0.065) H51B(0.065) H51C(0.074)
 H51D(0.074) H52A(0.085) H52B(0.085) H52C(0.081) H52D(0.081) H53A(0.089)
 H53B(0.089) H53C(0.079) H53D(0.079) H54A(0.073) H54B(0.073) H54C(0.074)
 H54D(0.074) H55A(0.093) H55B(0.093) H56A(0.104) H56B(0.104) H57A(0.091)
 H57B(0.091) H58A(0.072) H58B(0.072) H59A(0.077) H59B(0.077) H60A(0.101)
 H60B(0.101) H61A(0.113) H61B(0.113) H62A(0.112) H62B(0.112) H59C(0.129)
 H59D(0.129) H60C(0.101) H60D(0.101) H61C(0.119) H61D(0.119) H62C(0.209)
 H62D(0.209) H63A(0.137) H63B(0.137) H64A(0.101) H64B(0.101) H65A(0.146)
 H65B(0.146) H66A(0.186) H66B(0.186) H63C(0.129) H63D(0.129) H64C(0.108)
 H64D(0.108) H65C(0.144) H65D(0.144) H66C(0.114) H66D(0.114) H67A(0.132)
 H67B(0.132) H68A(0.102) H68B(0.102) H69A(0.126) H69B(0.126) H70A(0.221)
 H70B(0.221) H67C(0.181) H67D(0.181) H68C(0.139) H68D(0.139) H69C(0.127)
 H69D(0.127) H70C(0.141) H70D(0.141)
 Fixed X: H1(0.260784) H1A(0.282957) H1B(0.165662) H1C(0.232174) H2A(0.105403)
 H2B(0.038314) H2C(0.07977) H3A(0.145985) H3B(0.110558) H3C(0.225984)
 H6(0.313678) H8(0.488559) H11A(0.505359) H11B(0.507018) H11C(0.413101)
 H12A(0.374271) H12B(0.407427) H14(0.558488) H16(0.794394) H20A(0.774347)
 H20B(0.762923) H20C(0.664316) H21A(0.828957) H21B(0.863041) H21C(0.871438)
 H22A(0.599069) H22B(0.703661) H22C(0.652839) H23A(0.78877) H23B(0.708768)
 H23C(0.800333) H24A(0.362876) H24B(0.455653) H24C(0.4769) H25A(0.579907)
 H25B(0.559651) H25C(0.535776) H26A(0.354256) H26B(0.380471) H26C(0.287162)
 H29(0.368326) H31(0.310111) H34A(0.333631) H34B(0.33304) H34C(0.231376)
 H35A(0.385056) H35B(0.391016) H37(0.217002) H39(-0.006595) H42A(-0.022551)
 H42B(0.07636) H42C(0.003276) H44A(-0.020274) H44B(-0.044453) H44C(-0.080419)
 H45A(0.005724) H45B(0.034943) H45C(0.121204) H46A(0.217193) H46B(0.128063)
 H46C(0.162128) H47A(0.480249) H47B(0.480273) H47C(0.506438) H47D(0.436164)
 H48A(0.361115) H48B(0.415109) H48C(0.405596) H48D(0.426799) H49A(0.222177)
 H49B(0.285605) H49C(0.260882) H49D(0.241805) H50A(0.294013) H50B(0.218239)
 H50C(0.218687) H50D(0.285799) H51A(0.304289) H51B(0.189546) H51C(0.198753)
 H51D(0.283685) H52A(0.159049) H52B(0.254268) H52C(0.09759) H52D(0.171857)
 H53A(0.130158) H53B(0.059897) H53C(0.035142) H53D(0.047048) H54A(0.200144)
 H54B(0.123228) H54C(0.149374) H54D(0.205843) H55A(0.46294) H55B(0.556682)
 H56A(0.655788) H56B(0.587492) H57A(0.479039) H57B(0.586974) H58A(0.561181)
 H58B(0.446831) H59A(-0.042858) H59B(0.065004) H60A(-0.018408) H60B(0.100854)
 H61A(0.117669) H61B(-0.004181) H62A(-0.011852) H62B(0.108839) H59C(0.164885)
 H59D(0.065701) H60C(-0.087812) H60D(-0.023789) H61C(-0.029366) H61D(0.081291)
 H62C(0.111348) H62D(-0.002104) H63A(0.346617) H63B(0.284208) H64A(0.100972)
 H64B(0.17851) H65A(0.223748) H65B(0.107291) H66A(0.151269) H66B(0.243068)
 H63C(0.262536) H63D(0.209546) H64C(0.024236) H64D(0.078926) H65C(0.125434)
 H65D(0.19526) H66C(0.219808) H66D(0.305019) H67A(0.230147) H67B(0.117783)
 H68A(0.064292) H68B(0.182095) H69A(0.056064) H69B(0.172395) H70A(0.233788)
 H70B(0.123495) H67C(0.254588) H67D(0.166194) H68C(0.247042) H68D(0.173662)
 H69C(0.058673) H69D(0.12893) H70C(-0.022146) H70D(0.02541)
 Fixed Y: H1(0.423035) H1A(0.328545) H1B(0.30634) H1C(0.319888) H2A(0.415)
 H2B(0.407017) H2C(0.488855) H3A(0.496516) H3B(0.410778) H3C(0.435067)
 H6(0.525622) H8(0.592521) H11A(0.594848) H11B(0.657018) H11C(0.653415)
 H12A(0.469195) H12B(0.556538) H14(0.427955) H16(0.430549) H20A(0.61518)
 H20B(0.61991) H20C(0.623154) H21A(0.42722) H21B(0.505343) H21C(0.495834)
 H22A(0.51758) H22B(0.504837) H22C(0.435793) H23A(0.418189) H23B(0.34962)
 H23C(0.347964) H24A(0.347728) H24B(0.399143) H24C(0.322753) H25A(0.39439)
 H25B(0.470925) H25C(0.468207) H26A(0.512222) H26B(0.510692) H26C(0.461948)
 H29(0.265984) H31(0.23805) H34A(0.140182) H34B(0.124551) H34C(0.151283)
 H35A(0.333949) H35B(0.42025) H37(0.276512) H39(0.417398) H42A(0.257817)
 H42B(0.222688) H42C(0.278051) H44A(0.521826) H44B(0.606094) H44C(0.533667)
 H45A(0.577285) H45B(0.653355) H45C(0.605151) H46A(0.59884) H46B(0.645601)
 H46C(0.564535) H47A(0.668566) H47B(0.751467) H47C(0.715816) H47D(0.677168)
 H48A(0.700367) H48B(0.78244) H48C(0.79691) H48D(0.823707) H49A(0.754572)
 H49B(0.826812) H49C(0.842034) H49D(0.77176) H50A(0.77764) H50B(0.710846)
 H50C(0.708095) H50D(0.766487) H51A(0.7149) H51B(0.716313) H51C(0.707778)
 H51D(0.676257) H52A(0.711818) H52B(0.655893) H52C(0.677631) H52D(0.611215)
 H53A(0.564471) H53B(0.615477) H53C(0.601042) H53D(0.539491) H54A(0.508329)
 H54B(0.554332) H54C(0.514304) H54D(0.499134) H55A(0.765267) H55B(0.719988)
 H56A(0.73641) H56B(0.812263) H57A(0.75499) H57B(0.720645) H58A(0.608134)
 H58B(0.626568) H59A(0.418242) H59B(0.456625) H60A(0.276934) H60B(0.25876)
 H61A(0.247461) H61B(0.240204) H62A(0.35592) H62B(0.366021) H59C(0.366236)
 H59D(0.4035) H60C(0.293494) H60D(0.21778) H61C(0.316441) H61D(0.282706)
 H62C(0.415312) H62D(0.428263) H63A(0.727791) H63B(0.657053) H64A(0.785952)
 H64B(0.856967) H65A(0.831652) H65B(0.80515) H66A(0.676783) H66B(0.710048)
 H63C(0.676433) H63D(0.651011) H64C(0.767496) H64D(0.773191) H65C(0.852323)
 H65D(0.84273) H66C(0.771369) H66D(0.78534) H67A(0.159525) H67B(0.193756)
 H68A(0.09852) H68B(0.083668) H69A(-0.006871) H69B(-0.024281) H70A(0.027804)
 H70B(0.003575) H67C(0.127942) H67D(0.113772) H68C(0.011979) H68D(-0.004895)
 H69C(-0.025981) H69D(-0.001106) H70C(0.079148) H70D(0.089558)
 Fixed Z: H1(0.139905) H1A(0.00118) H1B(0.002423) H1C(0.050559) H2A(0.075116)
 H2B(0.026652) H2C(0.043593) H3A(-0.036719) H3B(-0.047737) H3C(-0.053297) H6(-
 0.020813) H8(0.092088) H11A(-0.02088) H11B(0.020319) H11C(-0.017834)
 H12A(0.173956) H12B(0.172281) H14(0.112199) H16(0.208125) H20A(0.250143)
 H20B(0.305732) H20C(0.270277) H21A(0.289987) H21B(0.315318) H21C(0.25976)
 H22A(0.319239) H22B(0.349558) H22C(0.319914) H23A(0.103293) H23B(0.099683)
 H23C(0.139116) H24A(0.483563) H24B(0.50374) H24C(0.475196) H25A(0.421776)
 H25B(0.450353) H25C(0.394581) H26A(0.409114) H26B(0.464741) H26C(0.442397)
 H29(0.425796) H31(0.286908) H34A(0.396904) H34B(0.341487) H34C(0.364565)
 H35A(0.235286) H35B(0.253019) H37(0.216128) H39(0.168043) H42A(0.193778)
 H42B(0.17219) H42C(0.140986) H44A(0.129597) H44B(0.14735) H44C(0.176215)
 H45A(0.24956) H45B(0.222427) H45C(0.250935) H46A(0.176148) H46B(0.148655)
 H46C(0.129184) H47A(0.199328) H47B(0.223126) H47C(0.222859) H47D(0.180946)
 H48A(0.14427) H48B(0.15239) H48C(0.164172) H48D(0.217492) H49A(0.172151)
 H49B(0.192184) H49C(0.211143) H49D(0.174493) H50A(0.265646) H50B(0.24656)
 H50C(0.239633) H50D(0.2714) H51A(0.356038) H51B(0.332507) H51C(0.351833)
 H51D(0.389293) H52A(0.412137) H52B(0.423733) H52C(0.408308) H52D(0.429084)
 H53A(0.416351) H53B(0.380526) H53C(0.346042) H53D(0.388349) H54A(0.356987)
 H54B(0.321255) H54C(0.315114) H54D(0.365908) H55A(0.316851) H55B(0.296387)
 H56A(0.36318) H56B(0.366357) H57A(0.415032) H57B(0.434278) H58A(0.39393)
 H58B(0.407135) H59A(0.3576) H59B(0.371937) H60A(0.312818) H60B(0.31203)
 H61A(0.390067) H61B(0.387773) H62A(0.423023) H62B(0.421386) H59C(0.385553)
 H59D(0.40579) H60C(0.358628) H60D(0.348225) H61C(0.286554) H61D(0.302025)
 H62C(0.317253) H62D(0.33436) H63A(0.523894) H63B(0.501758) H64A(0.47299)
 H64B(0.477444) H65A(0.554139) H65B(0.552395) H66A(0.548807) H66B(0.583591)
 H63C(0.511897) H63D(0.558666) H64C(0.520126) H64D(0.471507) H65C(0.545665)
 H65D(0.501638) H66C(0.589683) H66D(0.551957) H67A(0.078253) H67B(0.079728)
 H68A(0.115696) H68B(0.129647) H69A(0.074159) H69B(0.090784) H70A(0.021609)
 H70B(-0.000464) H67C(0.066177) H67D(0.102216) H68C(0.043088) H68D(0.084805)
 H69C(0.034776) H69D(-0.006389) H70C(0.031835) H70D(-0.018999)
;
_shelx_res_checksum              6631
_olex2_submission_special_instructions 'No special instructions were received'