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_4345722
_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         'C36 H38 N4 P Ta'
_chemical_formula_sum            'C36 H38 N4 P Ta'
_chemical_formula_weight         738.62
_chemical_properties_physical    'air-sensitive, moisture-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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb25
_audit_creation_date
;
'Mon Jan 19 17:08:10 2015'
;
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
'30.06.2016 12:48:05 CEST UTC+02:00  encif 1.46'
_cell_angle_alpha                90
_cell_angle_beta                 97.7237(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.75983(15)
_cell_length_b                   18.5817(2)
_cell_length_c                   15.9528(2)
_cell_measurement_reflns_used    27038
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.8510
_cell_measurement_theta_min      3.7210
_cell_volume                     3160.60(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      'perfluoro polyether oil / N~2~'
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_details
;
  1 omega   29.00   55.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000  -30.0000 52

  2 omega   29.00   55.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -77.0000 -180.0000 52

  3 omega   23.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000  -62.9440 72

  4 omega  -44.00   70.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -19.0000 -120.0000 228

  5 omega    4.00   38.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000   90.0000 68

  6 omega    6.00   94.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000  -60.0000 176

  7 omega  -42.00   16.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -57.0000  150.0000 116

  8 omega   -3.00   89.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000    0.0000 184

  9 omega  -43.00  -17.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000  150.3142 52

 10 omega    4.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000  150.3142 110

 11 omega   18.00   44.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -120.0000 52

 12 omega   71.00   97.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -120.0000 52

 13 omega    2.00   79.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   38.0000  150.0000 154

 14 omega  -20.00    6.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000   23.8727 52

 15 omega   32.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662  -80.0000   23.8727 54

 16 omega   -3.00   96.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000 -180.0000 198

 17 omega   38.00   64.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   60.0000 52

 18 omega   -1.00   25.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   77.0000  -90.0000 52

 19 omega   11.00   60.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -119.6173 98

 20 omega  -41.00   59.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -78.0000   70.4575 200

 21 omega  -42.00    5.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000 -119.6173 94

 22 omega    6.00   31.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000   60.0000 50

 23 omega    6.00   96.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       26.8662   57.0000 -180.0000 180

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      0.0392488000
_diffrn_orient_matrix_UB_12      -0.0305332000
_diffrn_orient_matrix_UB_13      -0.0013025000
_diffrn_orient_matrix_UB_21      -0.0267592000
_diffrn_orient_matrix_UB_22      -0.0066428000
_diffrn_orient_matrix_UB_23      -0.0423868000
_diffrn_orient_matrix_UB_31      0.0465800000
_diffrn_orient_matrix_UB_32      0.0219167000
_diffrn_orient_matrix_UB_33      -0.0146602000
_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  0.0633
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            95427
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.868
_diffrn_reflns_theta_min         3.283
_diffrn_source                   'microfocus X-Ray tube'
_exptl_absorpt_coefficient_mu    3.560
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.715
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.097
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.886
_refine_diff_density_min         -1.736
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         11077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^+4.4207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0641
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9756
_reflns_number_total             11077
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic7b00277_si_002.cif
_cod_data_source_block           ba_sb25
_cod_original_cell_volume        3160.61(7)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4345722
_audit_block_refno               2322
_audit_block_usercomment         'sb251, irregualr, yellow'
_chemical_oxdiff_formula         'C36 H38 N4 P Ta'
_chemical_oxdiff_usercomment     'sb251, irregualr, yellow'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.628
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_shelxl_version_number           2014/7
_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:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
2.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C)
;
_shelx_res_checksum              669
_olex2_submission_special_instructions 'No special instructions were received'
_cell_oxdiff_length_a            10.7585(2)
_cell_oxdiff_length_b            18.5840(4)
_cell_oxdiff_length_c            15.9522(2)
_cell_oxdiff_angle_alpha         90.0005(15)
_cell_oxdiff_angle_beta          97.7052(14)
_cell_oxdiff_angle_gamma         90.0054(18)
_cell_oxdiff_volume              3160.61(10)
_cell_oxdiff_measurement_reflns_used 27038