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_1566966
_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_formula_moiety         'C37 H54 N5 O3 Ta'
_chemical_formula_sum            'C37 H54 N5 O3 Ta'
_chemical_formula_weight         797.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-26
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-02-22 deposited with the CCDC.	2022-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                91.362(2)
_cell_angle_beta                 90.315(3)
_cell_angle_gamma                114.430(3)
_cell_formula_units_Z            2
_cell_length_a                   10.1780(3)
_cell_length_b                   12.1307(4)
_cell_length_c                   15.7705(5)
_cell_measurement_reflns_used    22684
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.2780
_cell_measurement_theta_min      2.4790
_cell_volume                     1772.04(11)
_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 1.3 (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 0.999
_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    -21.00  74.00   0.50    8.53    --   -6.82  20.00 144.00  190
  2  \w    -87.00   6.00   0.50    8.53    --   -6.82 -20.00 -22.00  186
  3  \w    -10.00  59.00   0.50    8.53    --    6.51  57.00-120.00  138
  4  \w    -25.00  30.00   0.50    8.53    --    6.51 -77.00 -60.00  110
  5  \w     -8.00  86.00   0.50    8.53    --    6.51  19.00 -90.00  188
  6  \w     -9.00  56.00   0.50    8.53    --    6.51  57.00 150.00  130
  7  \w    -38.00   4.00   0.50    8.53    --   -6.82 -57.00 -60.00   84
  8  \w    -30.00   4.00   0.50    8.53    --   -6.82  77.00 -90.00   68
  9  \w    -23.00  14.00   0.50    8.53    --   -6.82 -77.00 -90.00   74
;
_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      -0.0380452000
_diffrn_orient_matrix_UB_12      -0.0636158000
_diffrn_orient_matrix_UB_13      -0.0058836000
_diffrn_orient_matrix_UB_21      0.0653392000
_diffrn_orient_matrix_UB_22      -0.0044592000
_diffrn_orient_matrix_UB_23      -0.0104940000
_diffrn_orient_matrix_UB_31      0.0119883000
_diffrn_orient_matrix_UB_32      -0.0078051000
_diffrn_orient_matrix_UB_33      0.0433569000
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            35950
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.282
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92599
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.123
_refine_diff_density_min         -2.556
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         8790
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0184P)^2^+16.1343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1068
_refine_ls_wR_factor_ref         0.1090
_reflns_number_gt                7977
_reflns_number_total             8790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01926d2.cif
_cod_data_source_block           40497
_cod_original_cell_volume        1772.04(10)
_cod_database_code               1566966
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22