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_4343172
_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         'C48 H52 N3 P2 Ta'
_chemical_formula_sum            'C62 H68 N3 P2 Ta'
_chemical_formula_weight         1098.08
_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   geom
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'Wed Nov 26 11:01:35 2014'
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Olex2 1.2
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;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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;
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;
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omega____ theta____ kappa____ phi______ frames
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  5 omega   -4.00   22.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  6 omega  -24.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  7 omega   -6.00   61.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
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  8 omega   67.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000   60.0000 58

  9 omega   18.00   45.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000  -30.0000 54

 10 omega    1.00   70.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000   30.0000 138

 11 omega  -42.00   57.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000  -30.0000 198

 12 omega   -2.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -120.0000 196

 13 omega    6.00   64.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   60.0000 116

 14 omega   -2.00   53.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000   90.0000 110

 15 omega   62.00   88.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000  -60.0000 52

 16 omega  -42.00  -14.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  -51.4972 56

 17 omega  -35.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  119.4231 188

 18 omega   33.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  -51.4972 52

 19 omega  -40.00   60.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -168.7403 200

 20 omega    6.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000  -90.0000 180

 21 omega   -3.00   74.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -180.0000 154

 22 omega    6.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   60.0000 180

 23 omega  -42.00   48.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -57.0000  120.0000 180

 24 omega  -44.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000   55.0587 206

 25 omega  -42.00   48.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -57.0000  -60.0000 180

 26 omega   -3.00   97.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  -60.0000 200

 27 omega    6.00   96.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   90.0000 180

 28 omega    1.00   99.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000  -90.0000 196

 29 omega   -3.00   97.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  150.0000 200

 30 omega   -3.00   97.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000   30.0000 200

 31 omega  -43.00   57.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000  -30.0000 200

 32 omega  -43.00   60.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -168.7403 206

 33 omega  -42.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000  119.4231 202

;
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_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_11      -0.0035751000
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_diffrn_orient_matrix_UB_31      0.0594723000
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_diffrn_orient_matrix_UB_33      0.0067430000
_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  0.0631
_diffrn_reflns_av_unetI/netI     0.0371
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_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
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_diffrn_reflns_limit_l_min       -25
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
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Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
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;
_exptl_crystal_colour            yellow
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_refine_diff_density_max         1.299
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_refine_diff_density_rms         0.115
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_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         17503
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0331
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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^)+(0.0416P)^2^+1.4338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15315
_reflns_number_total             17503
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00333_si_001.cif
_cod_data_source_block           ba_ms23_sq
_cod_database_code               4343172
_audit_block_refno               2274
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_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.804
_shelxl_version_number           2014/6
_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:
 C7(H7), C22(H22)
2.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), 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), C46(H46A,H46B,H46C), C47(H47A,
 H47B,H47C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              96618
_olex2_submission_special_instructions 'No special instructions were received'
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_cell_oxdiff_angle_beta          88.354(2)
_cell_oxdiff_angle_gamma         69.0792(18)
_cell_oxdiff_volume              2526.17(9)
_cell_oxdiff_measurement_reflns_used 51957
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1
_platon_squeeze_void_probe_radius 1.20