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_7130748
_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 Cl2 N3 Nb P2, 0.5(C5 H12)'
_chemical_formula_sum            'C40.5 H64 Cl2 N3 Nb P2'
_chemical_formula_weight         818.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.243(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9677(4)
_cell_length_b                   12.7824(4)
_cell_length_c                   21.3828(8)
_cell_measurement_reflns_used    26596
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      2.5060
_cell_volume                     4248.3(2)
_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, 2014)'
_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    -73.00   5.00   0.50   29.73    --    6.51  -8.00  37.00  156
  2  \w    -30.00  73.00   0.50   29.73    --   -6.82   8.00-148.00  206
  3  \w    -86.00   5.00   0.50   29.73    --   -6.82  -8.00  37.00  182
  4  \w    -25.00  30.00   0.50   29.73    --    6.51 -77.00 -60.00  110
  5  \w    -25.00  30.00   0.50   29.73    --    6.51 -77.00-120.00  110
  6  \w    -25.00  30.00   0.50   29.73    --    6.51 -77.00   0.00  110
  7  \w    -10.00  59.00   0.50   29.73    --    6.51  57.00 -90.00  138
  8  \w    -25.00  30.00   0.50   29.73    --    6.51 -77.00  60.00  110
  9  \w    -10.00  59.00   0.50   29.73    --    6.51  57.00   0.00  138
 10  \w    -59.00   9.00   0.50   29.73    --   -6.82 -57.00  60.00  136
 11  \w    -30.00  25.00   0.50   29.73    --   -6.82  77.00-180.00  110
 12  \w    -25.00  17.00   0.50   29.73    --   -6.82 -77.00 -30.00   84
 13  \w    -17.00  25.00   0.50   29.73    --    6.51  77.00-120.00   84
 14  \w    -25.00  30.00   0.50   29.73    --    6.51 -77.00 120.00  110
;
_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      -0.0027887000
_diffrn_orient_matrix_UB_12      -0.0072321000
_diffrn_orient_matrix_UB_13      -0.0333020000
_diffrn_orient_matrix_UB_21      0.0040582000
_diffrn_orient_matrix_UB_22      -0.0548341000
_diffrn_orient_matrix_UB_23      0.0048462000
_diffrn_orient_matrix_UB_31      -0.0453714000
_diffrn_orient_matrix_UB_32      -0.0044603000
_diffrn_orient_matrix_UB_33      -0.0053843000
_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  0.0921
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            123109
_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         2.408
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_description       block
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.069
_refine_diff_density_min         -0.625
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         10530
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1035
_refine_ls_R_factor_gt           0.0669
_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^)+(0.0772P)^2^+11.2345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1812
_reflns_number_gt                7326
_reflns_number_total             10530
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04696b2.cif
_cod_data_source_block           9799_PNPN-NbCl2-NtBuAr
_cod_original_formula_sum        'C40.50 H64 Cl2 N3 Nb P2'
_cod_database_code               7130748
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.904
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_shelx_res_checksum              34888
_shelx_hkl_checksum              31150
_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 1.487
_oxdiff_exptl_absorpt_empirical_full_min 0.776