Ligand Non-Innocence Allows Isolation of a Neutral and Terminal Niobium Nitride
Senthil, Shuruthi; Kwon, Seongyeon; Lim, Hoyoung; Gau, Michael; Baik, Mu-Hyun; Mindiola, Daniel J.; Chemical Communications  (2022) –; doi:10.1039/D2CC04696B

data_7130749
_publ_section_title
;
 Ligand Non-Innocence Allows Isolation of a Neutral and Terminal Niobium
 Nitride
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04696B
_journal_year                    2022
_chemical_formula_moiety         'C38 H58 N3 Nb P2'
_chemical_formula_sum            'C38 H58 N3 Nb P2'
_chemical_formula_weight         711.72
_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             2022-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                101.554(2)
_cell_angle_beta                 111.506(2)
_cell_angle_gamma                99.442(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0304(3)
_cell_length_b                   13.4804(3)
_cell_length_c                   14.1210(3)
_cell_measurement_reflns_used    32800
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5270
_cell_measurement_theta_min      1.9200
_cell_volume                     2182.89(10)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (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, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix 3000HE'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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    -85.00 -58.00   0.50   44.00    --  -14.00 -18.00 111.00   54
  2  \w    -44.00  55.00   0.50   44.00    --  -14.00  18.00 -79.00  198
  3  \w    -59.00   0.00   0.50   44.00    --   14.70 -18.00 111.00  118
  4  \w    -15.00  86.00   0.50   44.00    --   14.70  18.00 -79.00  202
  5  \w    -18.00  13.00   0.50   44.00    --  -14.00 -80.00 178.12   62
  6  \w    -26.00   3.00   0.50   44.00    --  -14.00 -57.00-180.00   58
  7  \w    -14.00  12.00   0.50   44.00    --  -14.00 -80.00 -58.42   52
  8  \w    -25.00  13.00   0.50   44.00    --  -14.00 -77.00-150.00   76
  9  \w    -23.00  10.00   0.50   44.00    --  -14.00 -79.00-103.60   66
 10  \w    -21.00   8.00   0.50   44.00    --  -14.00 -80.00   3.04   58
 11  \w    -59.00   5.00   0.50   44.00    --  -14.00 -57.00 -90.00  128
 12  \w    -23.00   6.00   0.50   44.00    --  -14.00 -77.00  30.00   58
 13  \w    -21.00   5.00   0.50   44.00    --  -14.00 -80.00 -83.59   52
 14  \w    -81.00 -40.00   0.50   44.00    --  -14.00 -37.00 150.00   82
 15  \w    -35.00  47.00   0.50   44.00    --  -14.00  57.00 120.00  164
 16  \w    -21.00   5.00   0.50   44.00    --  -14.00 -80.00-138.26   52
 17  \w    -17.00   9.00   0.50   44.00    --  -14.00 -80.00  83.13   52
 18  \w    -34.00  -1.00   0.50   44.00    --  -14.00 -37.00 150.00   66
 19  \w    -22.00   3.00   0.50   44.00    --  -14.00 -80.00 152.91   50
 20  \w    -21.00   4.00   0.50   44.00    --  -14.00 -18.00 111.00   50
 21  \w    -19.00   6.00   0.50   44.00    --  -14.00 -80.00 165.05   50
 22  \w    -22.00   9.00   0.50   44.00    --  -14.00 -57.00  30.00   62
 23  \w    -57.00 -28.00   0.50   44.00    --  -14.00 -57.00  30.00   58
 24  \w     -5.00  20.00   0.50   44.00    --   14.70  57.00 -30.00   50
 25  \w     -8.00  18.00   0.50   44.00    --   14.70 -37.00 -30.00   52
 26  \w    -53.00 -11.00   0.50   44.00    --   14.70 -37.00 -30.00   84
 27  \w    -51.00   8.00   0.50   44.00    --   14.70 -37.00  90.00  118
 28  \w    -59.00   3.00   0.50   44.00    --   14.70 -19.00-120.00  124
 29  \w     -9.00  39.00   0.50   44.00    --   14.70 -76.00 -11.13   96
 30  \w    -24.00  18.00   0.50   44.00    --   14.70 -77.00  30.00   84
 31  \w    -14.00  11.00   0.50   44.00    --   14.70  80.00 167.43   50
 32  \w    -12.00  20.00   0.50   44.00    --   14.70  77.00-150.00   64
 33  \w    -10.00  25.00   0.50   44.00    --   14.70  77.00 -30.00   70
 34  \w     11.00  61.00   0.50   44.00    --   14.70  37.00 120.00  100
 35  \w    -23.00  35.00   0.50   44.00    --   14.70 -78.00   9.17  116
 36  \w    -18.00  19.00   0.50   44.00    --   14.70 -37.00 -60.00   74
 37  \w    -14.00  11.00   0.50   44.00    --   14.70  80.00 124.88   50
 38  \w    -50.00   1.00   0.50   44.00    --   14.70 -19.00 -90.00  102
 39  \w     -6.00  41.00   0.50   44.00    --   14.70  57.00-150.00   94
 40  \w      9.00  39.00   0.50   44.00    --   14.70 -69.00  38.82   60
 41  \w    -12.00  21.00   0.50   44.00    --   14.70  80.00-175.94   66
 42  \w    -30.00   4.00   0.50   44.00    --   14.70 -69.00  38.82   68
 43  \w    -16.00  38.00   0.50   44.00    --   14.70 -79.00-167.45  108
 44  \w     26.00  52.00   0.50   44.00    --   14.70  57.00 -30.00   52
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-i'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0576614000
_diffrn_orient_matrix_UB_12      0.0125526000
_diffrn_orient_matrix_UB_13      0.0373142000
_diffrn_orient_matrix_UB_21      0.0185673000
_diffrn_orient_matrix_UB_22      0.0034670000
_diffrn_orient_matrix_UB_23      -0.0408619000
_diffrn_orient_matrix_UB_31      0.0016642000
_diffrn_orient_matrix_UB_32      0.0540800000
_diffrn_orient_matrix_UB_33      0.0103914000
_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  0.0768
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            63302
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.923
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.083
_exptl_crystal_description       block
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         9941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0470
_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^)+(0.0674P)^2^+0.0920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                7671
_reflns_number_total             9941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04696b2.cif
_cod_data_source_block           9800_PNP-NbN-NtBuAr
_cod_original_cell_volume        2182.89(9)
_cod_database_code               7130749
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              44333
_shelx_hkl_checksum              46162
_shelx_fab_checksum              47692
_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 2.078
_oxdiff_exptl_absorpt_empirical_full_min 0.418