Modulating the electronic properties of divalent lanthanoid complexes with subtle ligand tuning
Hay, Moya A.; Gable, Robert W.; Boskovic, Colette; Dalton Transactions  (2023) –; doi:10.1039/D2DT03782C

data_7712293
_publ_section_title
;
 Modulating the electronic properties of divalent lanthanoid complexes
 with subtle ligand tuning
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03782C
_journal_year                    2023
_chemical_formula_moiety
'1.56(C26.918 H30.763 Eu0.641 N5.127), 2(C24 H20 B)'
_chemical_formula_sum            'C90 H88 B2 Eu N8'
_chemical_formula_weight         1455.26
_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             2023-02-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-11 deposited with the CCDC.	2023-02-14 downloaded from the CCDC.
;
_cell_angle_alpha                104.24(3)
_cell_angle_beta                 110.37(3)
_cell_angle_gamma                108.29(3)
_cell_formula_units_Z            1
_cell_length_a                   10.940(3)
_cell_length_b                   13.650(3)
_cell_length_c                   14.736(4)
_cell_measurement_reflns_used    66025
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      32.261
_cell_measurement_theta_min      1.223
_cell_volume                     1796.0(12)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'AS QEGUI'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 13.3
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.743
_diffrn_measurement_device_type  'MX1 Beamline Australian Synchrotron'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 0.935
_diffrn_reflns_Laue_measured_fraction_max 0.743
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            32556
_diffrn_reflns_point_group_measured_fraction_full 0.935
_diffrn_reflns_point_group_measured_fraction_max 0.743
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.150
_diffrn_reflns_theta_min         1.608
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2012/1 (Bruker,2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_description       block
_exptl_crystal_F_000             757
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.022
_refine_diff_density_min         -1.774
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     563
_refine_ls_number_reflns         9390
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0576P)^2^+0.9474P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9345
_reflns_number_total             9390
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03782c2.cif
_cod_data_source_block           3-Eu
_cod_original_cell_volume        1795.9(9)
_cod_database_code               7712293
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
;
_diffrn_measurement_detector_type 'Dectris Eiger2 9M'
_olex2_refinement_description
;
1. Shared sites
{Eu1A, Eu1}
2. Others
 Fixed Uiso: H1A(0.034) H1B(0.034) H3(0.035) H4(0.035) H5(0.035) H7A(0.06)
 H7B(0.06) H7C(0.06) H8A(0.034) H8B(0.034) H10(0.053) H11(0.039) H12(0.039)
 H14A(0.078) H14B(0.078) H14C(0.078) H15A(0.036) H15B(0.036) H17(0.057)
 H18(0.052) H19(0.047) H21A(0.07) H21B(0.07) H21C(0.07) H1AA(0.035) H1AB(0.035)
 H3A(0.035) H4A(0.035) H5A(0.035) H7AA(0.06) H7AB(0.06) H7AC(0.06) H8AA(0.036)
 H8AB(0.036) H10A(0.053) H11A(0.039) H12A(0.039) H14D(0.078) H14E(0.078)
 H14F(0.078) H15C(0.036) H15D(0.036) H17A(0.057) H18A(0.052) H19A(0.047)
 H21D(0.07) H21E(0.07) H21F(0.07) H23(0.041) H24(0.047) H25(0.047) H26(0.052)
 H27(0.046) H29(0.039) H30(0.045) H31(0.045) H32(0.043) H33(0.04) H35(0.034)
 H36(0.037) H37(0.037) H38(0.036) H39(0.033) H41(0.038) H42(0.044) H43(0.046)
 H44(0.046) H45(0.041)
 Fixed X: Eu1(0.5) H1A(0.854229) H1B(0.821282) H3(1.011093) H4(1.091275)
 H5(0.996925) H7A(0.738068) H7B(0.708544) H7C(0.860605) H8A(0.662855)
 H8B(0.498784) H10(0.722057) H11(0.687488) H12(0.553585) H14A(0.373312)
 H14B(0.372913) H14C(0.4996) H15A(0.654983) H15B(0.676465) H17(0.467858)
 H18(0.234344) H19(0.09657) H21A(0.116741) H21B(0.071358) H21C(0.21536)
 Eu1A(0.5) H1AA(0.667016) H1AB(0.794146) H3A(0.994977) H4A(1.133765)
 H5A(1.022274) H7AA(0.692902) H7AB(0.768831) H7AC(0.852853) H8AA(0.815553)
 H8AB(0.767417) H10A(0.716559) H11A(0.646417) H12A(0.520766) H14D(0.451967)
 H14E(0.322175) H14F(0.452535) H15C(0.484978) H15D(0.591317) H17A(0.451894)
 H18A(0.261613) H19A(0.117849) H21D(0.185508) H21E(0.05961) H21F(0.188019)
 H23(0.174816) H24(0.33152) H25(0.337569) H26(0.17949) H27(0.027699)
 H29(0.275577) H30(0.436368) H31(0.376313) H32(0.154677) H33(-0.00234) H35(-
 0.033622) H36(-0.1938) H37(-0.382049) H38(-0.404609) H39(-0.237513) H41(-
 0.303856) H42(-0.420623) H43(-0.288642) H44(-0.038986) H45(0.07705)
 Fixed Y: Eu1(0.5) H1A(0.839617) H1B(0.751146) H3(0.825962) H4(0.715366)
 H5(0.522892) H7A(0.379161) H7B(0.352019) H7C(0.370888) H8A(0.865096)
 H8B(0.772221) H10(0.9042) H11(0.847398) H12(0.655589) H14A(0.470528)
 H14B(0.444725) H14C(0.445256) H15A(0.840129) H15B(0.737735) H17(0.847582)
 H18(0.764827) H19(0.570645) H21A(0.407841) H21B(0.398383) H21C(0.388111)
 Eu1A(0.5) H1AA(0.739759) H1AB(0.837401) H3A(0.823581) H4A(0.724077)
 H5A(0.529494) H7AA(0.386437) H7AB(0.361337) H7AC(0.394733) H8AA(0.766759)
 H8AB(0.86629) H10A(0.909467) H11A(0.854552) H12A(0.664177) H14D(0.475168)
 H14E(0.464688) H14F(0.441862) H15C(0.776913) H15D(0.859569) H17A(0.861399)
 H18A(0.759836) H19A(0.570078) H21D(0.404648) H21E(0.405188) H21F(0.382882)
 H23(0.360423) H24(0.549831) H25(0.648703) H26(0.553689) H27(0.362493)
 H29(0.279579) H30(0.199755) H31(0.018027) H32(-0.08179) H33(0.000094)
 H35(0.048706) H36(-0.022004) H37(0.031337) H38(0.158261) H39(0.234896)
 H41(0.113195) H42(0.071972) H43(0.089285) H44(0.142138) H45(0.18477)
 Fixed Z: Eu1(0.5) H1A(0.703067) H1B(0.593456) H3(0.848098) H4(0.934013)
 H5(0.834902) H7A(0.565961) H7B(0.658061) H7C(0.658261) H8A(0.591119)
 H8B(0.538555) H10(0.461193) H11(0.28647) H12(0.175871) H14A(0.147384)
 H14B(0.247527) H14C(0.216693) H15A(0.738409) H15B(0.763857) H17(0.774434)
 H18(0.758304) H19(0.658894) H21A(0.470556) H21B(0.561363) H21C(0.567045)
 Eu1A(0.5) H1AA(0.76452) H1AB(0.764283) H3A(0.875323) H4A(0.912471)
 H5A(0.81067) H7AA(0.569128) H7AB(0.669323) H7AC(0.603689) H8AA(0.596778)
 H8AB(0.612774) H10A(0.463121) H11A(0.282094) H12A(0.173009) H14D(0.156921)
 H14E(0.186513) H14F(0.253829) H15C(0.543844) H15D(0.66528) H17A(0.759916)
 H18A(0.789481) H19A(0.684759) H21D(0.49693) H21E(0.528386) H21F(0.59929)
 H23(0.758603) H24(0.855184) H25(1.011986) H26(1.067971) H27(0.974137)
 H29(0.960002) H30(1.002272) H31(0.892041) H32(0.737955) H33(0.692951)
 H35(0.897773) H36(0.961544) H37(0.944495) H38(0.865368) H39(0.808884)
 H41(0.64776) H42(0.468496) H43(0.372368) H44(0.45929) H45(0.638092)
;
_shelx_res_checksum              42836
_shelx_hkl_checksum              80081
_olex2_submission_special_instructions 'No special instructions were received'