Synthesis of NPN-Coordinated Tantalum Alkyl Complexes and Their Hydrogenolysis: Isolation of a Terminal Tantalum Hydride Incorporating a Doubly Cyclometalated NPN Scaffold
Batke, Sonja; Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic Chemistry  (2017) –; doi:10.1021/acs.inorgchem.7b00277

data_4345725
_publ_section_title
;
 Synthesis of NPN-Coordinated Tantalum Alkyl Complexes and Their
 Hydrogenolysis: Isolation of a Terminal Tantalum Hydride Incorporating a
 Doubly Cyclometalated NPN Scaffold
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.7b00277
_journal_year                    2017
_chemical_formula_moiety         'C44 H56 N2 P Si2 Ta, C7 H8'
_chemical_formula_sum            'C51 H64 N2 P Si2 Ta'
_chemical_formula_weight         973.14
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
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'Tue Jun 24 13:48:14 2014'
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Olex2 1.2
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'29.06.2016 17:59:10 CEST UTC+02:00  encif 1.46'
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
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_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
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_diffrn_measurement_details
;
  1 omega    4.00   45.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   77.0000   30.0000 82

  2 omega    1.00   86.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000  150.0000 170

  3 omega  -51.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
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  4 omega   -3.00   25.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
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  5 omega   -3.00   54.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -51.00   11.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
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  7 omega  -50.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
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  8 omega  -29.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000 -150.0000 156

  9 omega   -7.00   81.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
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 10 omega   -3.00   86.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000   90.0000 178

 11 omega  -40.00  -11.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -30.0000 58

 12 omega   22.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -30.0000 54

 13 omega   15.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  150.0000 68

 14 omega    6.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000 -120.0000 86

 15 omega  -36.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -90.0000 170

 16 omega    9.00   49.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -60.0000 80

 17 omega   24.00   50.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -80.0000  -49.8631 52

 18 omega   -3.00   87.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000   60.0000 180

 19 omega  -50.00   40.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -57.0000  120.0000 180

 20 omega  -50.00   40.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -57.0000  -90.0000 180

 21 omega   -3.00   28.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000 -180.0000 62

 22 omega  -11.00   89.00   0.5000   12.5000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   77.0000  -90.0000 200

;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_11      -0.0093126000
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_diffrn_orient_matrix_UB_31      -0.0262651000
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_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  0.0549
_diffrn_reflns_av_unetI/netI     0.0454
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_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            66038
_diffrn_reflns_point_group_measured_fraction_full 0.997
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_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         3.320
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    2.483
_exptl_absorpt_correction_T_max  0.871
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_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
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_refine_ls_number_reflns         11469
_refine_ls_number_restraints     0
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0265P)^2^+2.6253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_database_code               4345725
_audit_block_refno               2067
_audit_block_usercomment         'MS370, irregular, yellow'
_chemical_oxdiff_formula         'C51 H64 N2 P1 Si2 Ta1'
_chemical_oxdiff_usercomment     'MS370, irregular, yellow'
_shelx_estimated_absorpt_t_max   0.789
_shelx_estimated_absorpt_t_min   0.789
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_reflns_odcompleteness_theta     26.32
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C37(H37A,H37B), C41(H41A,H41B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C11(H11), C13(H13), C19(H19),
 C20(H20), C21(H21), C22(H22), C24(H24), C26(H26), C28(H28), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56)
2.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C42(H42A,
 H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C57(H57A,H57B,H57C)
;
_shelx_res_checksum              62417
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            13.0048(3)
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_cell_oxdiff_length_c            14.9384(3)
_cell_oxdiff_angle_alpha         94.6661(18)
_cell_oxdiff_angle_beta          115.584(2)
_cell_oxdiff_angle_gamma         108.750(2)
_cell_oxdiff_volume              2327.47(8)
_cell_oxdiff_measurement_reflns_used 24594