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_4343174
_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         'C63 H60 N4 Nb P Si, C5 H12'
_chemical_formula_sum            'C68 H72 N4 Nb P Si'
_chemical_formula_weight         1097.26
_chemical_properties_physical    air-sensitive
_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'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
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_audit_block_code                ba_ms12
_audit_creation_date
;
'Tue May 06 14:28:50 2014'
;
_audit_update_record             'Tue May  6 14:32:11 CEST 2014'
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_cell_measurement_reflns_used    151127
_cell_measurement_temperature    110(1)
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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)
;
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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   12.00   50.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  2 omega   -7.00   53.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega   -5.00   89.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  4 omega    8.00   87.00   0.5000    5.0000
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  5 omega   -6.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega   12.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega  -49.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega    8.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  9 omega   -6.00   66.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000   90.0000 144

 10 omega  -10.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 118

 11 omega   12.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -30.0000 74

 12 omega  -12.00   25.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  150.0000 74

 13 omega   34.00   87.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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 14 omega   -2.00   23.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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 15 omega  -49.00  -14.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000    0.0000 70

 16 omega   -1.00   39.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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 17 omega   -2.00   31.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -38.0000  -90.0000 66

 18 omega  -54.00  -12.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -38.0000  150.0000 84

 19 omega   -4.00   74.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000  -30.0000 156

 20 omega  -13.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -150.0000 124

 21 omega   20.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -90.0000 58

 22 omega  -12.00   14.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 52

 23 omega   23.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 52

 24 phi    205.00  231.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.5380   18.5380   20.0000     -     52

 25 omega  -47.00   50.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000   78.4546 194

 26 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000   60.0000 180

 27 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000 -120.0000 180

 28 omega   -7.00   91.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   38.0000 -120.0000 196

 29 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000  -60.0000 180

 30 omega  -50.00   40.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -57.0000  150.0000 180

 31 omega  -12.00   89.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   77.0000   60.0000 202

 32 omega   -3.00   87.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000  -60.0000 180

 33 omega  -47.00   50.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -79.0000   78.4546 194

 34 omega  -52.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -30.0000 202

 35 omega  -52.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000 -180.0000 202

 36 omega  -52.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  -60.0000 202

 37 omega  -52.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000   30.0000 202

 38 omega  -52.00   49.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380  -77.0000  120.0000 202

 39 omega  -54.00   91.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380    0.0000    0.0000 290

 40 omega  -54.00   91.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380    0.0000  120.0000 290

 41 omega  -54.00   91.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380    0.0000  240.0000 290

 42 phi      0.00  120.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   18.5380    0.0000     -     240

 43 phi      0.00   90.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
  18.5380   18.5380  -20.0000     -     180

 44 omega   -3.00   87.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5380   57.0000   30.0000 180

;
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_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_limit_l_min       -26
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_exptl_absorpt_correction_type   gaussian
_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_diff_density_max         0.548
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    constr
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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^)+(0.0261P)^2^+5.3296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0807
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00333_si_001.cif
_cod_data_source_block           ba_ms12
_cod_original_cell_volume        5813.36(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4343174
_audit_block_refno               2033
_audit_block_usercomment         'MS344, block, yellow'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C68 H72 N4 Nb P Si'
_chemical_oxdiff_usercomment     'MS344, block, yellow'
_shelx_estimated_absorpt_t_max   0.971
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_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 Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B), C37(H37A,H37B), C82(H82A,H82B), C83(H83A,H83B),
 C84(H84A,H84B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C13(H13), C17(H17),
 C18(H18), C19(H19), C20(H20), C24(H24), C26(H26), C28(H28), C32(H32), C33(H33),
  C34(H34), C35(H35), C39(H39), C41(H41), C43(H43), C47(H47), C48(H48),
 C49(H49), C50(H50), C51(H51), C53(H53), C54(H54), C55(H55), C56(H56), C57(H57),
  C59(H59), C60(H60), C61(H61), C62(H62), C63(H63)
2.c 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), C81(H81A,H81B,H81C), C85(H85A,
 H85B,H85C)
;
_shelx_res_checksum              71500
_cell_oxdiff_length_a            16.52138(7)
_cell_oxdiff_length_b            17.89020(8)
_cell_oxdiff_length_c            19.80417(11)
_cell_oxdiff_angle_alpha         89.9880(4)
_cell_oxdiff_angle_beta          96.7163(4)
_cell_oxdiff_angle_gamma         90.0116(4)
_cell_oxdiff_volume              5813.36(5)
_cell_oxdiff_measurement_reflns_used 151127