Hydrophilic 2,9-bis-triazolyl-1,10-phenanthroline ligands enable selective Am(iii) separation: a step further towards sustainable nuclear energy.
Edwards, Alyn C.; Mocilac, Pavle; Geist, Andreas; Harwood, Laurence M.; Sharrad, Clint A.; Burton, Neil A.; Whitehead, Roger C.; Denecke, Melissa A.; Chemical communications (Cambridge, England) 53 (2017) 5001–5004; doi:10.1039/c7cc01855j

data_7119933
_publ_section_title
;
 Hydrophilic 2,9-bis-triazolyl-1,10-phenanthroline ligands enable
 selective Am(iii) separation: a step further towards sustainable nuclear
 energy.
;
_journal_issue                   36
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5001
_journal_page_last               5004
_journal_paper_doi               10.1039/c7cc01855j
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         '2(C F3 O3 S), C40 H38 Eu N16 O5, H2 O'
_chemical_formula_sum            'C42 H40 Eu F6 N16 O12 S2'
_chemical_formula_weight         1290.98
_chemical_melting_point_gt       573
_chemical_name_common            '[Eu(BTrzPhen)2](OTf)3'
_chemical_name_systematic
'aqua-bis(2,9-bis(1-(2-hydroxyethyl)-1H-1,2,3-triazol-4-yl)-1,10-phenanthroline)-europium(III) di(trifluoromethanesulfonate) monohydrat'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2017-02-15 deposited with the CCDC.
2017-04-10 downloaded from the CCDC.
;
_cell_angle_alpha                89.495(2)
_cell_angle_beta                 82.741(2)
_cell_angle_gamma                73.516(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2812(4)
_cell_length_b                   14.0380(5)
_cell_length_c                   18.1066(5)
_cell_measurement_reflns_used    6760
_cell_measurement_temperature    150.02(11)
_cell_measurement_theta_max      27.2870
_cell_measurement_theta_min      3.7170
_cell_volume                     2726.47(16)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
'Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012)'
_diffrn_ambient_temperature      150.02(11)
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.841
_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    -20.00  83.00   1.00   50.80    --   18.86  19.00 -90.00  103
  2  \w      4.00  39.00   1.00   50.80    --   18.86 -57.00-150.00   35
  3  \w     18.00  60.00   1.00   50.80    --   18.86 -99.00-180.00   42
  4  \w    -51.00 -23.00   1.00   50.80    --   18.86 -77.00 -30.00   28
  5  \w     -9.00  83.00   1.00   50.80    --   18.86  77.00  90.00   92
  6  \w    -11.00  81.00   1.00   50.80    --   18.86  77.00 -30.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0942
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22067
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.146
_diffrn_reflns_theta_min         3.203
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.319
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.573
_exptl_crystal_description       block
_exptl_crystal_F_000             1298
_exptl_crystal_preparation       'synthesis, Luminescent'
_exptl_crystal_recrystallization_method acetonitrile
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.454
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     735
_refine_ls_number_reflns         12354
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0574
_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^)+(0.0596P)^2^+0.9185P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1365
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10088
_reflns_number_total             12354
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01855j2.cif
_cod_data_source_block           amad16
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified as 'more
than' ('>') a certain temperature. The value '>573' was changed to
'573' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7119933.cif.
;
_cod_database_code               7119933
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1A_$1-H2A
 2.101 with sigma of 0.02
 C1-O2B1
 1.373 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O2B1) = Uanis(O2B2)
Uanis(C1) = Uanis(C20B)
4. Others
 Sof(O2B2)=Sof(H2B2)=Sof(C20B)=Sof(H20A)=Sof(H20B)=Sof(H19E)=Sof(H19F)=1-FVAR(1)
 Sof(O2B1)=Sof(H2B1)=Sof(H19C)=Sof(H19D)=Sof(C1)=Sof(H1C)=Sof(H1D)=FVAR(1)
5.a Free rotating group:
 O2W(H2WA,H2WB)
5.b Secondary CH2 refined with riding coordinates:
 C20B(H20A,H20B), C15A(H15A,H15B), C15B(H15C,H15D), C16A(H16A,H16B), C16B(H16C,
 H16D), C19A(H19A,H19B), C19B(H19C,H19D), C19B(H19E,H19F), C20A(H20C,H20D),
 C1(H1C,H1D)
5.c Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C7A(H7A), C7B(H7B), C8A(H8A),
 C8B(H8B), C10A(H10A), C10B(H10B), C11A(H11A), C11B(H11B), C14A(H14A),
 C18A(H18A), C18B(H18B)
5.d Idealised tetrahedral OH refined as rotating group:
 O1A(H1A), O1B(H1B), O1W(H1WA), O2A(H2A), O2B1(H2B1), O2B2(H2B2)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'