New asymmetric tetradentate phenanthroline chelators with pyrazole and amide groups for complexation and solvent extraction of Ln(III)/Am(III).
Wang, Haolong; Gao, Pengyuan; Cui, Tengfei; Wang, Dongqi; Liu, Jinping; He, Hui; Chen, Zongyuan; Jin, Qiang; Guo, Zhijun; Dalton transactions (Cambridge, England : 2003) 53 (2024) 601–611; doi:10.1039/d3dt03194b

data_7714553
_publ_section_title
;
 New asymmetric tetradentate phenanthroline chelators with pyrazole and
 amide groups for complexation and solvent extraction of Ln(III)/Am(III).
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              601
_journal_page_last               611
_journal_paper_doi               10.1039/d3dt03194b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C22 H22 Eu N8 O10'
_chemical_formula_sum            'C22 H22 Eu N8 O10'
_chemical_formula_weight         710.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-27
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2023-10-27 deposited with the CCDC.	2023-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.093(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1272(3)
_cell_length_b                   14.1154(4)
_cell_length_c                   20.6307(7)
_cell_measurement_reflns_used    12564
_cell_measurement_temperature    301.74(10)
_cell_measurement_theta_max      31.1070
_cell_measurement_theta_min      1.7640
_cell_volume                     2647.44(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.93a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      301.74(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.795
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      4.00  61.00   0.50    1.86    --    3.89  57.00  60.00  114
  2  \w    -13.00  49.00   0.50    1.86    --   -6.24  57.00 150.00  124
  3  \w     10.00  36.00   0.50    1.86    --    3.89 -99.00  30.00   52
  4  \w    -61.00   6.00   0.50    1.86    --   -6.24 -57.00-180.00  134
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0363083000
_diffrn_orient_matrix_UB_12      0.0395193000
_diffrn_orient_matrix_UB_13      0.0153689000
_diffrn_orient_matrix_UB_21      0.0418831000
_diffrn_orient_matrix_UB_22      -0.0309177000
_diffrn_orient_matrix_UB_23      0.0214753000
_diffrn_orient_matrix_UB_31      0.0548717000
_diffrn_orient_matrix_UB_32      -0.0025551000
_diffrn_orient_matrix_UB_33      -0.0222174000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.795
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            19329
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.795
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.937
_diffrn_reflns_theta_min         1.750
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.93a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0283P)^2^+1.9660P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5297
_reflns_number_total             6680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt03194b2.cif
_cod_data_source_block           wanghaol_1025_auto
_cod_depositor_comments          'Adding full bibliography for 7714553.cif.'
_cod_original_cell_volume        2647.44(14)
_cod_database_code               7714553
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C9(H9A,H9B), C17(H17A,H17B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C10(H10), C11(H11), C13(H13), C15(H15), C16(H16)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              97237
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.115
_oxdiff_exptl_absorpt_empirical_full_min 0.935