Completely preorganized bis-lactam-1,10-phenanthroline ligands with high stability for efficient separation of Am(III) over Eu(III).
Gao, Fengxin; Xu, Xiaocheng; Yang, Xiaofan; Cao, Hong; Fang, Dong; Xu, Lei; Xu, Chao; Xiao, Chengliang; Dalton transactions (Cambridge, England : 2003) 54 (2025) 2871–2876; doi:10.1039/d4dt02956a

data_7717717
_publ_section_title
;
 Completely preorganized bis-lactam-1,10-phenanthroline ligands with high
 stability for efficient separation of Am(III) over Eu(III).
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2871
_journal_page_last               2876
_journal_paper_doi               10.1039/d4dt02956a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C H Cl3), C42 H46 N4 O2, H2 O'
_chemical_formula_sum            'C44 H50 Cl6 N4 O3'
_chemical_formula_weight         895.58
_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   mixed
_audit_creation_date             2024-12-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-12-19 deposited with the CCDC.	2024-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.77(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.465(10)
_cell_length_b                   14.702(12)
_cell_length_c                   18.759(12)
_cell_measurement_reflns_used    159
_cell_measurement_temperature    302(2)
_cell_measurement_theta_max      54.111
_cell_measurement_theta_min      28.180
_cell_volume                     4536(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      302.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42015
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.655
_diffrn_reflns_theta_min         3.822
_exptl_absorpt_coefficient_mu    3.795
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.0077(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         8331
_refine_ls_number_restraints     348
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1262
_refine_ls_R_factor_gt           0.0836
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1677P)^2^+0.7177P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2380
_refine_ls_wR_factor_ref         0.2824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4826
_reflns_number_total             8331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02956a2.cif
_cod_data_source_block           57693416_file000009_1409876273
_cod_depositor_comments          'Adding full bibliography for 7717717.cif.'
_cod_database_code               7717717
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.659
_shelx_estimated_absorpt_t_min   0.548
_exptl_absorpt_special_details
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 1.54184   16.420   14.722   18.784   89.962   92.712   89.976
;
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.119) H2B(0.119) H00R(0.069) H11A(0.154) H11B(0.154)
 H11C(0.154) H12A(0.138) H12B(0.138) H12C(0.138) H01A(0.078) H01B(0.078)
 H13A(0.126) H13B(0.126) H13C(0.126) H01C(0.103) H01D(0.103) H01E(0.103)
 H01F(0.103) H17(0.079) H16(0.081) H01G(0.133) H01H(0.133) H01I(0.152)
 H23(0.063) H28(0.066) H29(0.067) H30(0.065) H36(0.067) H38(0.079) H39(0.078)
 H42A(0.195) H42B(0.195) H42C(0.195) H43A(0.132) H43B(0.132) H44A(0.16)
 H44B(0.16) H45A(0.217) H45B(0.217) H45C(0.217) H46A(0.108) H46B(0.108)
 H46C(0.108) H46D(0.108) H47A(0.127) H47B(0.127) H48A(0.187) H48B(0.187)
 H48C(0.187) H0AA(0.171) H0AB(0.171) H0AC(0.171) H1AA(0.195) H1AB(0.195)
 H1AC(0.195) H7A(0.173) H7B(0.173) H7C(0.173) H4A(0.139) H4B(0.139) H4C(0.139)
 H6A(0.152) H6B(0.152) H6C(0.152) H9A(0.138) H9B(0.138) H9C(0.138) H8A(0.147)
 H8B(0.147) H2AA(0.2) H2AB(0.2) H2AC(0.2) H1A(0.197) H1B(0.197) H1C(0.197)
 H3A(0.121) H3B(0.121) H3AA(0.183) H3AB(0.183) H3AC(0.183) H4AA(0.149)
 H4AB(0.149) H4AC(0.149) H5AA(0.135) H5AB(0.135) H01J(0.152)
 Fixed X: H2A(0.558922) H2B(0.594634) H00R(0.697777) H11A(0.928895)
 H11B(0.885618) H11C(0.900365) H12A(0.815077) H12B(0.758521) H12C(0.853249)
 H01A(0.81225) H01B(0.769727) H13A(0.737798) H13B(0.688476) H13C(0.750416)
 H01C(0.404622) H01D(0.462111) H01E(0.375177) H01F(0.464713) H17(0.857919)
 H16(0.879001) H01G(0.460626) H01H(0.454699) H01I(0.184121) H23(0.604974)
 H28(0.401833) H29(0.49258) H30(0.339406) H36(0.24155) H38(0.179443)
 H39(0.292433) H42A(0.137551) H42B(0.107446) H42C(0.045371) H43A(0.355989)
 H43B(0.293434) H44A(0.394155) H44B(0.325602) H45A(0.291075) H45B(0.226163)
 H45C(0.287377) H46A(0.871729) H46B(0.919355) H46C(0.86871) H46D(0.904224)
 H47A(0.960959) H47B(0.872797) H48A(0.018225) H48B(0.055317) H48C(0.099492)
 H0AA(0.035501) H0AB(0.059467) H0AC(-0.005095) H1AA(0.097184) H1AB(0.051682)
 H1AC(0.017238) H7A(0.08634) H7B(0.161177) H7C(0.07307) H4A(0.872038)
 H4B(0.781865) H4C(0.847477) H6A(0.902238) H6B(0.886802) H6C(0.932605)
 H9A(0.700286) H9B(0.723075) H9C(0.755721) H8A(0.382308) H8B(0.32353)
 H2AA(0.283148) H2AB(0.222938) H2AC(0.267814) H1A(0.8778) H1B(0.896427)
 H1C(0.965077) H3A(0.947719) H3B(0.994379) H3AA(0.974661) H3AB(0.890953)
 H3AC(0.965619) H4AA(0.177529) H4AB(0.156329) H4AC(0.088583) H5AA(0.441907)
 H5AB(0.375671) H01J(0.189346)
 Fixed Y: H2A(0.261041) H2B(0.189997) H00R(0.173218) H11A(0.102955)
 H11B(0.196981) H11C(0.132909) H12A(-0.004091) H12B(-0.037423) H12C(-0.041286)
 H01A(-0.040822) H01B(-0.00152) H13A(0.203039) H13B(0.111901) H13C(0.136099)
 H01C(0.523661) H01D(0.439066) H01E(0.510315) H01F(0.477145) H17(-0.011109)
 H16(-0.004081) H01G(0.165335) H01H(0.173367) H01I(0.197478) H23(0.250789)
 H28(0.449499) H29(0.363616) H30(0.497733) H36(0.54999) H38(0.638767)
 H39(0.572074) H42A(0.775972) H42B(0.736477) H42C(0.752614) H43A(0.403589)
 H43B(0.432864) H44A(0.290144) H44B(0.317845) H45A(0.193519) H45B(0.271597)
 H45C(0.263615) H46A(0.120737) H46B(0.053247) H46C(0.103044) H46D(0.087463)
 H47A(0.037206) H47B(0.002166) H48A(0.584585) H48B(0.516266) H48C(0.533521)
 H0AA(0.597586) H0AB(0.514754) H0AC(0.585384) H1AA(0.740287) H1AB(0.650669)
 H1AC(0.712144) H7A(0.572166) H7B(0.637203) H7C(0.677569) H4A(0.222601)
 H4B(0.239152) H4C(0.210898) H6A(0.059126) H6B(-0.017836) H6C(0.071198)
 H9A(0.113358) H9B(0.010191) H9C(0.06735) H8A(0.292897) H8B(0.373329)
 H2AA(0.204669) H2AB(0.28701) H2AC(0.25129) H1A(-0.089502) H1B(0.006384) H1C(-
 0.067427) H3A(-0.060317) H3B(0.020864) H3AA(-0.085719) H3AB(-0.123031) H3AC(-
 0.118611) H4AA(0.679706) H4AB(0.76088) H4AC(0.717896) H5AA(0.355875)
 H5AB(0.337191) H01J(0.225044)
 Fixed Z: H2A(0.671841) H2B(0.640899) H00R(0.267746) H11A(0.207358)
 H11B(0.194853) H11C(0.129943) H12A(0.105672) H12B(0.165263) H12C(0.178103)
 H01A(0.510357) H01B(0.576697) H13A(0.157521) H13B(0.15195) H13C(0.093954)
 H01C(0.823599) H01D(0.818307) H01E(0.823532) H01F(0.817946) H17(0.414466)
 H16(0.295743) H01G(0.619761) H01H(0.62627) H01I(0.653126) H23(0.312112)
 H28(0.362846) H29(0.30676) H30(0.476417) H36(0.539398) H38(0.729187)
 H39(0.781738) H42A(0.600007) H42B(0.67173) H42C(0.606948) H43A(0.886967)
 H43B(0.826037) H44A(0.818636) H44B(0.762317) H45A(0.837857) H45B(0.834238)
 H45C(0.900591) H46A(0.573266) H46B(0.525514) H46C(0.597563) H46D(0.522653)
 H47A(0.653442) H47B(0.667178) H48A(0.536685) H48B(0.593572) H48C(0.522639)
 H0AA(0.674311) H0AB(0.627079) H0AC(0.597583) H1AA(0.664458) H1AB(0.683957)
 H1AC(0.621253) H7A(0.504537) H7B(0.498705) H7C(0.499035) H4A(0.207782)
 H4B(0.180163) H4C(0.126515) H6A(0.123049) H6B(0.17863) H6C(0.202986)
 H9A(0.153808) H9B(0.161623) H9C(0.098528) H8A(0.921988) H8B(0.925236)
 H2AA(0.88232) H2AB(0.885503) H2AC(0.955616) H1A(0.658714) H1B(0.692213)
 H1C(0.691227) H3A(0.563382) H3B(0.600975) H3AA(0.572851) H3AB(0.59656)
 H3AC(0.651565) H4AA(0.50634) H4AB(0.556342) H4AC(0.505283) H5AA(0.857501)
 H5AB(0.799433) H01J(0.628425)
;
_shelx_res_checksum              10093
_olex2_submission_special_instructions 'No special instructions were received'