4,4'-Di-tert-butyl-6-(1H-tetrazol-5-yl)-2,2'-bipyridine: Modification of a Highly Selective N-Donor Ligand for the Separation of Trivalent Actinides from Lanthanides
Maiwald, Martin Maximilian; Wagner, Anna Tessa; Kratsch, Jochen; Skerencak-Frech, Andrej; Trumm, Michael; Geist, Andreas; Roesky, Peter; Panak, Petra J.; Dalton Trans.  (2017) –; doi:10.1039/C7DT01864A

data_7043570
_publ_section_title
;
 4,4'-Di-tert-butyl-6-(1H-tetrazol-5-yl)-2,2'-bipyridine: Modification of
 a Highly Selective N-Donor Ligand for the Separation of Trivalent
 Actinides from Lanthanides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01864A
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'N O3, C19 H25 N6'
_chemical_formula_sum            'C19 H25 N7 O3'
_chemical_formula_weight         399.46
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-05-17 deposited with the CCDC.
2017-07-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.60(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.986(2)
_cell_length_b                   14.179(3)
_cell_length_c                   13.626(3)
_cell_measurement_reflns_used    11173
_cell_measurement_temperature    200.0
_cell_measurement_theta_max      29.15
_cell_measurement_theta_min      2.08
_cell_volume                     2098.7(8)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.0490
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21511
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.010
_diffrn_reflns_theta_min         2.085
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.9826
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       prism
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4121
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0661P)^2^+0.3792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1261
_refine_ls_wR_factor_ref         0.1402
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2780
_reflns_number_total             4121
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01864a2.cif
_cod_data_source_block           HN4tBubipy
_cod_original_cell_volume        2098.7(7)
_cod_database_code               7043570
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C2(H2a), C4(H4), C7(H7), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C17(H17a,H17b,
 H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c)
;
_shelx_res_checksum              80487
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'