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_7708381
_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 Gd O7, 3(C4 H8 O)'
_chemical_formula_sum            'C70 H109 Gd O10'
_chemical_formula_weight         1267.82
_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                 94.11(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.228(3)
_cell_length_b                   17.675(4)
_cell_length_c                   28.481(6)
_cell_measurement_reflns_used    15703
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2
_cell_volume                     6642(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.986
_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  0.0341
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            88343
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         1.357
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    1.054
_exptl_absorpt_correction_T_max  0.9
_exptl_absorpt_correction_T_min  0.8
_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    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.0091(3)
_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   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         15703
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0391P)^2^+6.5797P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0858
_refine_ls_wR_factor_ref         0.0888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14027
_reflns_number_total             15703
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02513a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        6642(2)
_cod_database_code               7708381
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Shared sites
{O8, C62A}
2. Others
 Fixed Uiso: H1(0.071) H1A(0.088) H1B(0.088) H1C(0.088) H2A(0.077) H2B(0.077)
 H2C(0.077) H3A(0.082) H3B(0.082) H3C(0.082) H6(0.052) H8(0.064) H11A(0.096)
 H11B(0.096) H11C(0.096) H12A(0.075) H12B(0.075) H14(0.056) H16(0.059)
 H20A(0.115) H20B(0.115) H20C(0.115) H21A(0.11) H21B(0.11) H21C(0.11)
 H22A(0.078) H22B(0.078) H22C(0.078) H23A(0.096) H23B(0.096) H23C(0.096)
 H24A(0.084) H24B(0.084) H24C(0.084) H25A(0.073) H25B(0.073) H25C(0.073)
 H26A(0.077) H26B(0.077) H26C(0.077) H29(0.047) H31(0.044) H34A(0.073)
 H34B(0.073) H34C(0.073) H35A(0.042) H35B(0.042) H37(0.054) H39(0.054)
 H42A(0.124) H42B(0.124) H42C(0.124) H44A(0.075) H44B(0.075) H44C(0.075)
 H45A(0.073) H45B(0.073) H45C(0.073) H46A(0.073) H46B(0.073) H46C(0.073)
 H47A(0.085) H47B(0.085) H47C(0.085) H47D(0.085) H48A(0.074) H48B(0.074)
 H48C(0.098) H48D(0.098) H49A(0.108) H49B(0.108) H49C(0.097) H49D(0.097)
 H50A(0.084) H50B(0.084) H50C(0.084) H50D(0.084) H51A(0.069) H51B(0.069)
 H51C(0.07) H51D(0.07) H52A(0.093) H52B(0.093) H52C(0.078) H52D(0.078)
 H53A(0.095) H53B(0.095) H53C(0.082) H53D(0.082) H54A(0.067) H54B(0.067)
 H54C(0.071) H54D(0.071) H55A(0.122) H55B(0.122) H56A(0.149) H56B(0.149)
 H57A(0.129) H57B(0.129) H58A(0.072) H58B(0.072) H59A(0.056) H59B(0.056)
 H60A(0.078) H60B(0.078) H61A(0.085) H61B(0.085) H62A(0.104) H62B(0.104)
 H59C(0.176) H59D(0.176) H60C(0.136) H60D(0.136) H61C(0.152) H61D(0.152)
 H62C(0.256) H62D(0.256) H63A(0.13) H63B(0.13) H64A(0.1) H64B(0.1) H65A(0.153)
 H65B(0.153) H66A(0.217) H66B(0.217) H63C(0.128) H63D(0.128) H64C(0.118)
 H64D(0.118) H65C(0.142) H65D(0.142) H66C(0.112) H66D(0.112) H67A(0.159)
 H67B(0.159) H68A(0.125) H68B(0.125) H69A(0.143) H69B(0.143) H70A(0.234)
 H70B(0.234) H67C(0.244) H67D(0.244) H68C(0.188) H68D(0.188) H69C(0.233)
 H69D(0.233) H70C(0.394) H70D(0.394)
 Fixed X: H1(0.244487) H1A(0.286102) H1B(0.168756) H1C(0.233537) H2A(0.110089)
 H2B(0.042034) H2C(0.08032) H3A(0.147167) H3B(0.112238) H3C(0.227375)
 H6(0.31482) H8(0.490232) H11A(0.506376) H11B(0.507085) H11C(0.413275)
 H12A(0.37753) H12B(0.412363) H14(0.561298) H16(0.797646) H20A(0.776571)
 H20B(0.761925) H20C(0.665146) H21A(0.833427) H21B(0.865035) H21C(0.876587)
 H22A(0.601881) H22B(0.706675) H22C(0.658781) H23A(0.790839) H23B(0.70929)
 H23C(0.80135) H24A(0.364118) H24B(0.458523) H24C(0.4772) H25A(0.58112)
 H25B(0.563318) H25C(0.53809) H26A(0.359043) H26B(0.386274) H26C(0.291452)
 H29(0.368188) H31(0.309043) H34A(0.330056) H34B(0.333927) H34C(0.230276)
 H35A(0.392272) H35B(0.386365) H37(0.218146) H39(-0.005572) H42A(-0.021106)
 H42B(0.077406) H42C(0.004456) H44A(-0.017667) H44B(-0.044725) H44C(-0.077097)
 H45A(0.010614) H45B(0.036632) H45C(0.125223) H46A(0.220457) H46B(0.132014)
 H46C(0.161382) H47A(0.480026) H47B(0.479105) H47C(0.435511) H47D(0.50577)
 H48A(0.362413) H48B(0.413827) H48C(0.430409) H48D(0.400198) H49A(0.221978)
 H49B(0.280529) H49C(0.269071) H49D(0.24274) H50A(0.296227) H50B(0.219033)
 H50C(0.218983) H50D(0.284604) H51A(0.3017) H51B(0.187686) H51C(0.198828)
 H51D(0.284944) H52A(0.154352) H52B(0.250257) H52C(0.099052) H52D(0.174285)
 H53A(0.125026) H53B(0.057161) H53C(0.036965) H53D(0.050067) H54A(0.200273)
 H54B(0.123444) H54C(0.206895) H54D(0.150479) H55A(0.459912) H55B(0.553735)
 H56A(0.654972) H56B(0.581572) H57A(0.490758) H57B(0.600917) H58A(0.563511)
 H58B(0.451539) H59A(-0.041876) H59B(0.064523) H60A(-0.022526) H60B(0.095952)
 H61A(0.115287) H61B(-0.006597) H62A(-0.001169) H62B(0.118569) H59C(0.156739)
 H59D(0.045779) H60C(-0.088528) H60D(-0.026787) H61C(-0.028552) H61D(0.076748)
 H62C(0.136313) H62D(0.024363) H63A(0.347655) H63B(0.264434) H64A(0.097338)
 H64B(0.173704) H65A(0.210179) H65B(0.104376) H66A(0.2745) H66B(0.178288)
 H63C(0.261566) H63D(0.206318) H64C(0.020404) H64D(0.093618) H65C(0.104827)
 H65D(0.174697) H66C(0.224723) H66D(0.297281) H67A(0.223773) H67B(0.107501)
 H68A(0.070477) H68B(0.189585) H69A(0.059213) H69B(0.178919) H70A(0.227004)
 H70B(0.113193) H67C(0.266654) H67D(0.191094) H68C(0.248635) H68D(0.169231)
 H69C(0.06424) H69D(0.145128) H70C(-0.006246) H70D(0.082466)
 Fixed Y: H1(0.429836) H1A(0.330087) H1B(0.307908) H1C(0.321231) H2A(0.419376)
 H2B(0.405597) H2C(0.489073) H3A(0.496616) H3B(0.411379) H3C(0.435884)
 H6(0.526466) H8(0.593563) H11A(0.595195) H11B(0.657368) H11C(0.652584)
 H12A(0.472975) H12B(0.559153) H14(0.429289) H16(0.431807) H20A(0.617259)
 H20B(0.621027) H20C(0.623238) H21A(0.42939) H21B(0.504159) H21C(0.501176)
 H22A(0.516529) H22B(0.50617) H22C(0.436577) H23A(0.417215) H23B(0.3502)
 H23C(0.348044) H24A(0.34899) H24B(0.39865) H24C(0.322364) H25A(0.39245)
 H25B(0.467788) H25C(0.466988) H26A(0.511247) H26B(0.509822) H26C(0.462579)
 H29(0.267094) H31(0.239521) H34A(0.142854) H34B(0.126685) H34C(0.153449)
 H35A(0.420225) H35B(0.334749) H37(0.2777) H39(0.418283) H42A(0.260368)
 H42B(0.225633) H42C(0.281287) H44A(0.525465) H44B(0.606363) H44C(0.530702)
 H45A(0.575298) H45B(0.651442) H45C(0.604577) H46A(0.595775) H46B(0.645932)
 H46C(0.566245) H47A(0.75304) H47B(0.671396) H47C(0.679809) H47D(0.717886)
 H48A(0.704205) H48B(0.785956) H48C(0.82679) H48D(0.797466) H49A(0.752109)
 H49B(0.826683) H49C(0.84397) H49D(0.778708) H50A(0.77906) H50B(0.712711)
 H50C(0.710119) H50D(0.764931) H51A(0.710983) H51B(0.711894) H51C(0.707271)
 H51D(0.678201) H52A(0.704724) H52B(0.649941) H52C(0.677121) H52D(0.611395)
 H53A(0.55712) H53B(0.607686) H53C(0.602369) H53D(0.540948) H54A(0.50249)
 H54B(0.546659) H54C(0.500565) H54D(0.517861) H55A(0.765776) H55B(0.723375)
 H56A(0.740587) H56B(0.812011) H57A(0.751813) H57B(0.716285) H58A(0.606732)
 H58B(0.628114) H59A(0.415371) H59B(0.456969) H60A(0.276672) H60B(0.255569)
 H61A(0.247677) H61B(0.245544) H62A(0.359875) H62B(0.366803) H59C(0.3728)
 H59D(0.406459) H60C(0.294858) H60D(0.217555) H61C(0.314194) H61D(0.271777)
 H62C(0.389951) H62D(0.423539) H63A(0.72476) H63B(0.662808) H64A(0.787959)
 H64B(0.859386) H65A(0.84284) H65B(0.79909) H66A(0.739071) H66B(0.688211)
 H63C(0.679485) H63D(0.657207) H64C(0.768817) H64D(0.777639) H65C(0.846519)
 H65D(0.859101) H66C(0.775026) H66D(0.792179) H67A(0.164429) H67B(0.189511)
 H68A(0.095077) H68B(0.083143) H69A(-0.013222) H69B(-0.0274) H70A(0.033297)
 H70B(0.014494) H67C(0.118511) H67D(0.106243) H68C(0.008277) H68D(-0.002135)
 H69C(-0.022788) H69D(-0.015178) H70C(0.068797) H70D(0.081963)
 Fixed Z: H1(0.135058) H1A(0.001946) H1B(0.001601) H1C(0.050536) H2A(0.075032)
 H2B(0.027048) H2C(0.040932) H3A(-0.037693) H3B(-0.048721) H3C(-0.053895) H6(-
 0.021152) H8(0.09189) H11A(-0.021137) H11B(0.019733) H11C(-0.018883)
 H12A(0.173619) H12B(0.171013) H14(0.112523) H16(0.209513) H20A(0.252258)
 H20B(0.3075) H20C(0.270436) H21A(0.288813) H21B(0.317969) H21C(0.26245)
 H22A(0.319161) H22B(0.350202) H22C(0.320329) H23A(0.104717) H23B(0.10137)
 H23C(0.140994) H24A(0.482951) H24B(0.503263) H24C(0.474884) H25A(0.421019)
 H25B(0.450482) H25C(0.394684) H26A(0.408142) H26B(0.463796) H26C(0.441454)
 H29(0.425039) H31(0.285842) H34A(0.396346) H34B(0.341217) H34C(0.361762)
 H35A(0.252511) H35B(0.234468) H37(0.214121) H39(0.166448) H42A(0.190628)
 H42B(0.169211) H42C(0.138108) H44A(0.127037) H44B(0.148036) H44C(0.173934)
 H45A(0.248841) H45B(0.221796) H45C(0.249787) H46A(0.175038) H46B(0.149518)
 H46C(0.127547) H47A(0.224549) H47B(0.199908) H47C(0.18193) H47D(0.224203)
 H48A(0.145352) H48B(0.155324) H48C(0.216077) H48D(0.163804) H49A(0.171257)
 H49B(0.190684) H49C(0.216844) H49D(0.178054) H50A(0.266198) H50B(0.24819)
 H50C(0.238297) H50D(0.273243) H51A(0.357622) H51B(0.33255) H51C(0.350188)
 H51D(0.388464) H52A(0.411309) H52B(0.423542) H52C(0.407662) H52D(0.428223)
 H53A(0.413083) H53B(0.376036) H53C(0.345428) H53D(0.387515) H54A(0.356057)
 H54B(0.318902) H54C(0.364699) H54D(0.31394) H55A(0.320711) H55B(0.299145)
 H56A(0.364115) H56B(0.370549) H57A(0.419224) H57B(0.433001) H58A(0.394383)
 H58B(0.408998) H59A(0.356288) H59B(0.369372) H60A(0.313066) H60B(0.312179)
 H61A(0.391272) H61B(0.390008) H62A(0.424605) H62B(0.418845) H59C(0.388653)
 H59D(0.394437) H60C(0.354051) H60D(0.347322) H61C(0.282903) H61D(0.297543)
 H62C(0.312318) H62D(0.318119) H63A(0.518638) H63B(0.503335) H64A(0.471904)
 H64B(0.47573) H65A(0.550958) H65B(0.548953) H66A(0.582711) H66B(0.562804)
 H63C(0.514299) H63D(0.560703) H64C(0.512583) H64D(0.470818) H65C(0.552903)
 H65D(0.509305) H66C(0.589579) H66D(0.54764) H67A(0.077194) H67B(0.078328)
 H68A(0.112433) H68B(0.122976) H69A(0.070709) H69B(0.083769) H70A(0.010455)
 H70B(-0.009246) H67C(0.060792) H67D(0.102593) H68C(0.044027) H68D(0.08287)
 H69C(0.03525) H69D(-0.003707) H70C(0.007767) H70D(-0.027431)
;
_shelx_res_checksum              79219
_olex2_submission_special_instructions 'No special instructions were received'