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_7708375
_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         'C81 H114 Dy2 O9, 2(C7 H8)'
_chemical_formula_sum            'C95 H130 Dy2 O9'
_chemical_formula_weight         1740.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                70.76(3)
_cell_angle_beta                 76.21(3)
_cell_angle_gamma                68.48(3)
_cell_formula_units_Z            2
_cell_length_a                   13.158(3)
_cell_length_b                   16.671(3)
_cell_length_c                   22.238(4)
_cell_measurement_reflns_used    14593
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26
_cell_measurement_theta_min      2
_cell_volume                     4246.0(18)
_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-2014 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.921
_diffrn_measured_fraction_theta_max 0.906
_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  0.0301
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.921
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            51459
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.363
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.802
_exptl_absorpt_correction_T_max  0.8911
_exptl_absorpt_correction_T_min  0.6572
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS(Kabsch, 1993)'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.590
_refine_diff_density_min         -0.875
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1040
_refine_ls_number_reflns         14588
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0639P)^2^+2.6656P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1026
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12252
_reflns_number_total             14588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           complex9
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        4246.1(19)
_cod_database_code               7708375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.813
_shelx_estimated_absorpt_t_min   0.714
_olex2_refinement_description
;
1. Others
 Fixed Sof: C89(0.5) C90(0.5) H90(0.5) C91(0.5) H91(0.5) C92(0.5) H92(0.5)
 C93(0.5) H93(0.5) C94(0.5) H94(0.5) C95(0.5) H95A(0.5) H95B(0.5) H95C(0.5)
 C95A(0.5) H95D(0.5) H95E(0.5) H95F(0.5) C89A(0.5) C90A(0.5) H90A(0.5)
 C91A(0.5) H91A(0.5) C92A(0.5) H92A(0.5) C93A(0.5) H93A(0.5) C94A(0.5) H94A(0.5)
 Fixed Uiso: H1A(0.118) H1B(0.118) H1C(0.118) H2A(0.085) H2B(0.085) H2C(0.085)
 H3A(0.088) H3B(0.088) H3C(0.088) H6(0.057) H8A(0.085) H8B(0.085) H8C(0.085)
 H9(0.051) H12A(0.047) H12B(0.047) H14(0.049) H16A(0.078) H16B(0.078)
 H16C(0.078) H17(0.049) H21A(0.075) H21B(0.075) H21C(0.075) H22A(0.072)
 H22B(0.072) H22C(0.072) H23A(0.071) H23B(0.071) H23C(0.071) H24A(0.069)
 H24B(0.069) H24C(0.069) H25A(0.076) H25B(0.076) H25C(0.076) H26A(0.067)
 H26B(0.067) H26C(0.067) H29(0.049) H31A(0.071) H31B(0.071) H31C(0.071)
 H32(0.047) H35A(0.044) H35B(0.044) H37(0.047) H39A(0.074) H39B(0.074)
 H39C(0.074) H40(0.049) H44A(0.126) H44B(0.126) H44C(0.126) H45A(0.09)
 H45B(0.09) H45C(0.09) H46A(0.117) H46B(0.117) H46C(0.117) H47A(0.065)
 H47B(0.065) H47C(0.065) H48A(0.08) H48B(0.08) H48C(0.08) H50A(0.071)
 H50B(0.071) H50C(0.071) H52(0.056) H54A(0.099) H54B(0.099) H54C(0.099)
 H55(0.056) H58A(0.047) H58B(0.047) H60(0.053) H62A(0.084) H62B(0.084)
 H62C(0.084) H63(0.053) H67A(0.077) H67B(0.077) H67C(0.077) H68A(0.078)
 H68B(0.078) H68C(0.078) H69A(0.073) H69B(0.073) H69C(0.073) H70A(0.067)
 H70B(0.067) H70C(0.067) H70D(0.067) H71A(0.095) H71B(0.095) H71C(0.072)
 H71D(0.072) H72A(0.221) H72B(0.221) H72C(0.084) H72D(0.084) H73A(0.063)
 H73B(0.063) H73C(0.063) H73D(0.063) H74A(0.059) H74B(0.059) H75A(0.078)
 H75B(0.078) H76A(0.073) H76B(0.073) H77A(0.053) H77B(0.053) H78A(0.057)
 H78B(0.057) H79A(0.063) H79B(0.063) H80A(0.057) H80B(0.057) H81A(0.057)
 H81B(0.057) H82(0.077) H83(0.071) H84(0.083) H85(0.084) H86(0.081) H88A(0.157)
 H88B(0.157) H88C(0.157) H90(0.111) H91(0.095) H92(0.098) H93(0.065) H94(0.082)
 H95A(0.219) H95B(0.219) H95C(0.219) H95D(0.119) H95E(0.119) H95F(0.119)
 H90A(0.146) H91A(0.127) H92A(0.098) H93A(0.103) H94A(0.1)
 Fixed X: H1A(-0.185575) H1B(-0.21286) H1C(-0.137662) H2A(0.050996)
 H2B(0.09751) H2C(-0.000524) H3A(-0.069036) H3B(0.05498) H3C(0.004897) H6(-
 0.235803) H8A(-0.321434) H8B(-0.353303) H8C(-0.371933) H9(-0.143404)
 H12A(0.115057) H12B(0.030254) H14(0.0081) H16A(0.10765) H16B(0.112043)
 H16C(0.00827) H17(0.302166) H21A(0.472366) H21B(0.574381) H21C(0.466313)
 H22A(0.460087) H22B(0.565489) H22C(0.454615) H23A(0.469954) H23B(0.571274)
 H23C(0.460861) H24A(0.546302) H24B(0.489213) H24C(0.584043) H25A(0.775745)
 H25B(0.809645) H25C(0.737417) H26A(0.600122) H26B(0.67014) H26C(0.543421)
 H29(0.82159) H31A(0.926182) H31B(0.903101) H31C(0.955805) H32(0.719717)
 H35A(0.458595) H35B(0.543737) H37(0.580483) H39A(0.569121) H39B(0.467174)
 H39C(0.558763) H40(0.303604) H44A(0.160415) H44B(0.055615) H44C(0.175576)
 H45A(0.148774) H45B(0.029916) H45C(0.120097) H46A(0.093828) H46B(0.002122)
 H46C(0.096994) H47A(-0.137215) H47B(-0.034683) H47C(-0.156107) H48A(-0.250953)
 H48B(-0.194421) H48C(-0.232809) H50A(0.02363) H50B(-0.034009) H50C(-0.100646)
 H52(-0.111227) H54A(-0.018787) H54B(0.042819) H54C(-0.081808) H55(0.183425)
 H58A(0.303968) H58B(0.293567) H60(0.379159) H62A(0.469856) H62B(0.559552)
 H62C(0.592464) H63(0.611394) H67A(0.649956) H67B(0.720938) H67C(0.737421)
 H68A(0.696959) H68B(0.697997) H68C(0.595711) H69A(0.463115) H69B(0.562082)
 H69C(0.47979) H70A(0.281574) H70B(0.403215) H70C(0.357849) H70D(0.394867)
 H71A(0.338422) H71B(0.414182) H71C(0.200977) H71D(0.290117) H72A(0.270027)
 H72B(0.18662) H72C(0.240589) H72D(0.124024) H73A(0.212113) H73B(0.132118)
 H73C(0.241462) H73D(0.135941) H74A(0.137999) H74B(0.261793) H75A(0.211337)
 H75B(0.32934) H76A(0.248578) H76B(0.128193) H77A(0.302746) H77B(0.172617)
 H78A(0.315451) H78B(0.189383) H79A(0.266617) H79B(0.196879) H80A(0.362563)
 H80B(0.433354) H81A(0.350661) H81B(0.45153) H82(0.150268) H83(0.331895)
 H84(0.389927) H85(0.261852) H86(0.080966) H88A(-0.058461) H88B(-0.055735)
 H88C(-0.014986) H90(0.826956) H91(0.649169) H92(0.531535) H93(0.591687)
 H94(0.769474) H95A(0.973802) H95B(0.961682) H95C(0.920084) H95D(0.68038)
 H95E(0.593405) H95F(0.714976) H90A(0.855895) H91A(0.92608) H92A(0.819525)
 H93A(0.642784) H94A(0.572597)
 Fixed Y: H1A(1.278085) H1B(1.23958) H1C(1.303908) H2A(1.250578) H2B(1.152654)
 H2C(1.227904) H3A(1.129396) H3B(1.093316) H3C(1.194687) H6(1.161189)
 H8A(1.050099) H8B(1.007077) H8C(1.112386) H9(0.908449) H12A(0.840599)
 H12B(0.807918) H14(0.886724) H16A(0.930095) H16B(0.827674) H16C(0.899038)
 H17(0.825828) H21A(0.83025) H21B(0.747466) H21C(0.730471) H22A(0.64374)
 H22B(0.665218) H22C(0.687808) H23A(0.843459) H23B(0.822839) H23C(0.903492)
 H24A(1.124601) H24B(1.052149) H24C(1.069339) H25A(1.024003) H25B(0.974602)
 H25C(1.078071) H26A(1.047925) H26B(0.943954) H26C(0.973988) H29(0.878791)
 H31A(0.751863) H31B(0.659073) H31C(0.703175) H32(0.668774) H35A(0.752747)
 H35B(0.666828) H37(0.694396) H39A(0.738492) H39B(0.712813) H39C(0.641099)
 H40(0.79416) H44A(0.9778) H44B(0.996946) H44C(0.98169) H45A(0.86952)
 H45B(0.881496) H45C(0.784384) H46A(0.773151) H46B(0.868762) H46C(0.855489)
 H47A(0.789327) H47B(0.784826) H47C(0.809532) H48A(0.698158) H48B(0.597513)
 H48C(0.677197) H50A(0.661168) H50B(0.584432) H50C(0.683344) H52(0.55738)
 H54A(0.400125) H54B(0.429901) H54C(0.486443) H55(0.482248) H58A(0.577265)
 H58B(0.63048) H60(0.412083) H62A(0.250791) H62B(0.205909) H62C(0.256201)
 H63(0.302249) H67A(0.300864) H67B(0.354342) H67C(0.333721) H68A(0.496064)
 H68B(0.507425) H68C(0.567538) H69A(0.519445) H69B(0.460456) H69C(0.415322)
 H70A(1.168587) H70B(1.096784) H70C(1.124222) H70D(1.093332) H71A(1.18647)
 H71B(1.083215) H71C(1.229931) H71D(1.234856) H72A(1.063083) H72B(1.155007)
 H72C(1.138222) H72D(1.177788) H73A(0.990115) H73B(1.082316) H73C(1.004273)
 H73D(1.046237) H74A(0.658891) H74B(0.660639) H75A(0.530051) H75B(0.507591)
 H76A(0.419661) H76B(0.493522) H77A(0.491413) H77B(0.535343) H78A(1.160507)
 H78B(1.161428) H79A(1.224528) H79B(1.157942) H80A(1.083105) H80B(1.113008)
 H81A(0.967623) H81B(0.980263) H82(0.401543) H83(0.356634) H84(0.254301)
 H85(0.1968) H86(0.242192) H88A(0.410881) H88B(0.309194) H88C(0.340648)
 H90(0.414421) H91(0.402353) H92(0.445702) H93(0.501119) H94(0.513188)
 H95A(0.435021) H95B(0.465566) H95C(0.538495) H95D(0.442404) H95E(0.532386)
 H95F(0.531225) H90A(0.492898) H91A(0.435024) H92A(0.378911) H93A(0.38067)
 H94A(0.438544)
 Fixed Z: H1A(0.226903) H1B(0.17764) H1C(0.152364) H2A(0.181124) H2B(0.227477)
 H2C(0.255196) H3A(0.12737) H3B(0.143129) H3C(0.102778) H6(0.279123)
 H8A(0.422042) H8B(0.377451) H8C(0.357233) H9(0.389588) H12A(0.303739)
 H12B(0.363091) H14(0.455883) H16A(0.562997) H16B(0.593346) H16C(0.559286)
 H17(0.51291) H21A(0.479156) H21B(0.463569) H21C(0.509618) H22A(0.440363)
 H22B(0.393728) H22C(0.364998) H23A(0.316143) H23B(0.352884) H23C(0.361636)
 H24A(0.135717) H24B(0.141292) H24C(0.08312) H25A(0.102606) H25B(0.173312)
 H25C(0.155968) H26A(0.247066) H26B(0.265315) H26C(0.255824) H29(0.122099)
 H31A(0.061926) H31B(0.100008) H31C(0.133573) H32(0.149169) H35A(0.227511)
 H35B(0.205949) H37(0.080944) H39A(-0.049792) H39B(-0.056404) H39C(-0.012723)
 H40(-0.001787) H44A(0.098377) H44B(0.065052) H44C(0.024002) H45A(-0.009678)
 H45B(0.032519) H45C(0.040924) H46A(0.159857) H46B(0.141154) H46C(0.180454)
 H47A(0.246353) H47B(0.275611) H47C(0.314412) H48A(0.363217) H48B(0.357657)
 H48C(0.295499) H50A(0.377413) H50B(0.405392) H50C(0.412644) H52(0.269404)
 H54A(0.228153) H54B(0.157225) H54C(0.17666) H55(0.163877) H58A(0.139932)
 H58B(0.19023) H60(0.172413) H62A(0.198569) H62B(0.247427) H62C(0.17441)
 H63(0.289939) H67A(0.378886) H67B(0.389007) H67C(0.321327) H68A(0.262301)
 H68B(0.330838) H68C(0.291867) H69A(0.383954) H69B(0.425728) H69C(0.417301)
 H70A(0.238483) H70B(0.236737) H70C(0.216781) H70D(0.286508) H71A(0.320217)
 H71B(0.340003) H71C(0.244697) H71D(0.282097) H72A(0.413303) H72B(0.37677)
 H72C(0.376078) H72D(0.350066) H73A(0.372148) H73B(0.333493) H73C(0.380237)
 H73D(0.341625) H74A(0.47153) H74B(0.465077) H75A(0.547628) H75B(0.503428)
 H76A(0.481636) H76B(0.484059) H77A(0.381049) H77B(0.376773) H78A(0.112765)
 H78B(0.12476) H79A(0.010465) H79B(0.020705) H80A(-0.030142) H80B(0.003548)
 H81A(0.054394) H81B(0.075347) H82(0.318263) H83(0.334324) H84(0.428923)
 H85(0.508474) H86(0.491782) H88A(0.388548) H88B(0.421463) H88C(0.346245) H90(-
 0.044657) H91(-0.020266) H92(0.068476) H93(0.132828) H94(0.108439) H95A(-
 0.016773) H95B(0.046367) H95C(-0.017921) H95D(0.172191) H95E(0.137213)
 H95F(0.138627) H90A(0.060927) H91A(-0.028519) H92A(-0.064566) H93A(-0.011168)
 H94A(0.078279)
;
_shelx_res_checksum              38654
_olex2_submission_special_instructions 'No special instructions were received'