Tantalum, Easy as Pi: Understanding Differences in Metal-Imido Bonding Towards Improving Ta/Nb Separations
Weberg, Alexander B.; Schelter, Eric J.; Carroll, Patrick; Gau, Michael; Pandey, Pragati; Lapsheva, Ekaterina; Schatz, George C.; Cheisson, Thibault; Chaudhuri, Subhajyoti; Uruburo, Christian; Chemical Science  (2022) –; doi:10.1039/D2SC01926D

data_1566967
_publ_section_title
;
 Tantalum, Easy as Pi: Understanding Differences in Metal-Imido Bonding
 Towards Improving Ta/Nb Separations
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01926D
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C38 H54 N5 O5 Ta'
_chemical_formula_sum            'C38 H54 N5 O5 Ta'
_chemical_formula_weight         841.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-02-22 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.466(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.8852(4)
_cell_length_b                   15.2484(4)
_cell_length_c                   12.4719(5)
_cell_measurement_reflns_used    18347
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.2200
_cell_measurement_theta_min      2.4350
_cell_volume                     1884.23(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Dectris Pilatus3 R 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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    -67.00  23.00   0.50   60.00    --    6.82 -54.00-165.00  180
  2  \w     -9.00  79.00   0.50   60.00    --    6.82  54.00 -21.00  176
  3  \w     -5.00  22.00   0.50   60.00    --    6.82 -37.00  90.00   54
  4  \w     -8.00  20.00   0.50   60.00    --    6.82  77.00  90.00   56
  5  \w      3.00  30.00   0.50   60.00    --    6.82 -77.00  60.00   54
  6  \w     -1.00  25.00   0.50   60.00    --    6.82  77.00-180.00   52
  7  \w    -22.00  30.00   0.50   60.00    --    6.82 -77.00  90.00  104
  8  \w    -25.00   0.00   0.50   60.00    --   -7.13  77.00-120.00   50
  9  \w    -59.00   9.00   0.50   60.00    --   -7.13 -57.00 150.00  136
 10  \w    -26.00  10.00   0.50   60.00    --   -7.13  77.00 -90.00   72
 11  \w    -25.00  17.00   0.50   60.00    --   -7.13 -77.00   0.00   84
 12  \w    -31.00  25.00   0.50   60.00    --   -7.13  77.00  90.00  112
 13  \w     -5.00  54.00   0.50   60.00    --   -7.13  54.00 -21.00  118
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0407776000
_diffrn_orient_matrix_UB_12      -0.0022110000
_diffrn_orient_matrix_UB_13      0.0319362000
_diffrn_orient_matrix_UB_21      -0.0435969000
_diffrn_orient_matrix_UB_22      -0.0301259000
_diffrn_orient_matrix_UB_23      -0.0418181000
_diffrn_orient_matrix_UB_31      0.0395888000
_diffrn_orient_matrix_UB_32      -0.0353673000
_diffrn_orient_matrix_UB_33      0.0337285000
_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  0.0526
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35379
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.315
_diffrn_reflns_theta_min         2.452
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.965
_exptl_absorpt_correction_T_max  0.09720
_exptl_absorpt_correction_T_min  0.07183
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       needle
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.780
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.052(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         9120
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0231P)^2^+0.4969P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0582
_reflns_Friedel_coverage         0.880
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.944
_reflns_number_gt                7850
_reflns_number_total             9120
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01926d2.cif
_cod_data_source_block           40533
_cod_original_cell_volume        1884.22(14)
_cod_database_code               1566967
_shelx_shelxl_version_number     2018/3