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_4343171
_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         'C49 H55 N3 Nb P Si'
_chemical_formula_sum            'C49 H55 N3 Nb P Si'
_chemical_formula_weight         837.93
_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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;
'Tue Apr 15 16:33:27 2014'
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_cell_angle_alpha                82.8627(15)
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_cell_formula_units_Z            2
_cell_length_a                   10.59319(18)
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_cell_length_c                   16.0085(3)
_cell_measurement_reflns_used    14287
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      28.0860
_cell_measurement_theta_min      3.5890
_cell_volume                     2147.98(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
;
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_computing_publication_material
'encif (Wadepohl, 2009-14); encifer 1.4 (CCDC, 2011)'
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_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD plate'
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_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_details
;
  1 omega   -3.00   24.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   57.0000   60.0000 54

  2 omega  -10.00   89.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   77.0000 -180.0000 198

  3 omega   -8.00   50.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   77.0000  -60.0000 116

  4 omega  -43.00   47.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000   60.0000 180

  5 omega   -1.00   88.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   19.0000    0.0000 178

  6 omega  -54.00   44.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -38.0000  -90.0000 196

  7 omega  -11.00   89.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   77.0000   30.0000 200

  8 omega  -50.00   40.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -57.0000  120.0000 180

  9 omega   -3.00   87.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   57.0000  -90.0000 180

 10 omega  -52.00   49.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000  -30.0000 202

 11 omega   -3.00   87.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161   57.0000  120.0000 180

 12 omega  -52.00   28.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -77.0000 -180.0000 160

 13 omega  -50.00   40.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       18.6161  -57.0000 -150.0000 180

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
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_diffrn_orient_matrix_UB_11      -0.0019412000
_diffrn_orient_matrix_UB_12      -0.0022970000
_diffrn_orient_matrix_UB_13      -0.0439580000
_diffrn_orient_matrix_UB_21      -0.0706493000
_diffrn_orient_matrix_UB_22      0.0147644000
_diffrn_orient_matrix_UB_23      0.0009207000
_diffrn_orient_matrix_UB_31      -0.0046572000
_diffrn_orient_matrix_UB_32      0.0539522000
_diffrn_orient_matrix_UB_33      -0.0078379000
_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  0.0592
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48569
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.972
_diffrn_reflns_theta_min         3.197
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91444
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33c (release 11-04-2014 CrysAlis171 .NET)
(compiled Apr 11 2014,15:12:41)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       irregular
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.2209
_exptl_crystal_size_mid          0.1142
_exptl_crystal_size_min          0.0311
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         10476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0202P)^2^+2.1398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8991
_reflns_number_total             10476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b00333_si_001.cif
_cod_data_source_block           ba_ms10
_cod_database_code               4343171
_audit_block_refno               2018
_audit_block_usercomment         'MS261, irregular, orange'
_shelxl_version_number           2014-3
_chemical_oxdiff_formula         'C49 H55 N3 Nb P Si'
_chemical_oxdiff_usercomment     'MS261, irregular, orange'
_shelx_estimated_absorpt_t_max   0.963
_shelx_estimated_absorpt_t_min   0.963
_reflns_odcompleteness_completeness 99.83
_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:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C37(H37A,H37B), C46(H46A,H46B)
2.c 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)
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), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C)
;
_shelx_res_checksum              75453
_cell_oxdiff_length_a            10.59319(18)
_cell_oxdiff_length_b            13.5033(2)
_cell_oxdiff_length_c            16.0085(3)
_cell_oxdiff_angle_alpha         82.8627(15)
_cell_oxdiff_angle_beta          88.6467(15)
_cell_oxdiff_angle_gamma         70.9964(16)
_cell_oxdiff_volume              2147.98(7)
_cell_oxdiff_measurement_reflns_used 14287