Synthesis and reactivity of cyclometalated triamidophosphine complexes of niobium and tantalum.
Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic chemistry 54 (2015) 4094–4103; doi:10.1021/acs.inorgchem.5b00333

data_4343170
_publ_section_title
;
 Synthesis and reactivity of cyclometalated triamidophosphine complexes of
 niobium and tantalum.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4094
_journal_page_last               4103
_journal_paper_doi               10.1021/acs.inorgchem.5b00333
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C46 H44 F3 N3 Nb O3 P S'
_chemical_formula_sum            'C49.5 H48 F3 N3 Nb O3 P S'
_chemical_formula_weight         945.85
_chemical_properties_physical    air-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   geom
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_audit_creation_date
;
'Thu Jul 03 11:50:11 2014'
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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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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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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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;
  1 omega   -8.00   89.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   77.0000  -30.0000 194

  2 omega  -47.00  -17.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega   13.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega   -2.00   83.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  5 omega  -11.00   89.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   17.00   77.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega  -32.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000   30.0000 162

  8 omega  -44.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000 -150.0000 186

  9 omega   17.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000 -120.0000 64

 10 omega   22.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  150.0000 54

 11 omega   22.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000   60.0000 54

 12 omega    2.00   31.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   38.0000  -90.0000 58

 13 omega  -48.00    8.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -30.0000 112

 14 omega   18.00   49.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -30.0000 62

 15 omega  -47.00   50.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -79.0000  117.1702 194

 16 omega   -3.00   87.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000  150.0000 180

 17 omega  -51.00   48.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -75.0000 -145.0000 198

 18 omega  -54.00   44.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -38.0000  -30.0000 196

 19 omega   -3.00   87.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000  -90.0000 180

 20 omega   -3.00   87.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942   57.0000   60.0000 180

 21 omega  -47.00   50.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -79.0000  117.1702 194

 22 omega  -50.00   40.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -57.0000  -90.0000 180

 23 omega  -50.00   40.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -57.0000    0.0000 180

 24 omega  -51.00  -26.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -77.0000  -90.0000 50

 25 omega  -54.00   44.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6942  -38.0000   60.0000 196

;
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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  0.0541
_diffrn_reflns_av_unetI/netI     0.0383
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         3.307
_diffrn_source                   'microfocus X-Ray tube'
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_exptl_absorpt_correction_T_min  0.928
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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            orange
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_exptl_crystal_size_max          0.2511
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_refine_ls_number_reflns         10965
_refine_ls_number_restraints     0
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0357P)^2^+4.4885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_data_source_block           ba_ms16_sq
_cod_original_cell_volume        2208.08(7)
_cod_original_formula_sum        'C49.50 H48 F3 N3 Nb O3 P S'
_cod_database_code               4343170
_audit_block_refno               2089
_audit_block_usercomment         'MS260, plate, orange'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C53 H52 F3 N3 Nb O3 P S'
_chemical_oxdiff_usercomment     'MS260, plate, orange'
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.960
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 Ternary CH refined with riding coordinates:
 C1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C31(H31A,H31B)
2.c 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), C34(H34), C35(H35),
  C36(H36), C37(H37), C39(H39), C41(H41), C43(H43)
2.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              14341
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            12.93050(18)
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_cell_oxdiff_length_c            15.4214(3)
_cell_oxdiff_angle_alpha         106.3805(17)
_cell_oxdiff_angle_beta          107.6771(15)
_cell_oxdiff_angle_gamma         105.6233(15)
_cell_oxdiff_volume              2208.09(6)
_cell_oxdiff_measurement_reflns_used 23309