A Tripodal Benzylene-Linked Trisamidophosphine Ligand Scaffold: Synthesis and Coordination Chemistry with Group(IV) Metals.
Batke, Sonja; Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Inorganic chemistry 53 (2014) 4144–4153; doi:10.1021/ic500163c

data_4338075
_publ_section_title
;
 A Tripodal Benzylene-Linked Trisamidophosphine Ligand Scaffold: Synthesis
 and Coordination Chemistry with Group(IV) Metals.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4144
_journal_page_last               4153
_journal_paper_doi               10.1021/ic500163c
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C32 H51 Hf N4 P Si3'
_chemical_formula_sum            'C32 H51 Hf N4 P Si3'
_chemical_formula_weight         785.49
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_jb8
_audit_creation_date
;
'Tue Apr 02 14:57:53 2013'
;
_audit_update_record             'Tue Apr  2 15:01:17 CEST 2013'
_cell_angle_alpha                92.1162(6)
_cell_angle_beta                 109.7773(6)
_cell_angle_gamma                118.7552(9)
_cell_formula_units_Z            2
_cell_length_a                   11.58910(9)
_cell_length_b                   11.99210(11)
_cell_length_c                   15.93941(10)
_cell_measurement_reflns_used    56739
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      31.8920
_cell_measurement_theta_min      3.6480
_cell_volume                     1773.14(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_temperature      110(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_details
;
  1 omega   -5.00   41.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   57.0000  150.0000 92

  2 omega  -59.00  -13.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000  -90.0000 92

  3 omega    2.00   49.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000   60.0000 94

  4 omega   60.00   86.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000  -90.0000 52

  5 omega   32.00   58.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -60.0000 52

  6 omega    3.00   34.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000    0.0000 62

  7 omega  -42.00  -16.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  150.0000 52

  8 omega    4.00   91.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000 -150.0000 174

  9 omega   23.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  150.0000 74

 10 omega  -40.00   19.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -60.0000 118

 11 omega   68.00   99.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000    0.0000 62

 12 omega  -43.00   -4.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   60.0000 78

 13 omega   -4.00   90.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  -90.0000 188

 14 omega  -33.00    9.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000 -150.0000 84

 15 omega    6.00   40.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000  -90.0000 68

 16 omega  -39.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000    0.0000 198

 17 omega    4.00   95.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000   60.0000 182

 18 omega  -26.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   90.0000 172

 19 omega   40.00   66.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000 -150.0000 52

 20 omega   33.00   59.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -90.0000 52

 21 omega   -3.00   50.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  150.0000 106

 22 omega  -50.00   41.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   57.0000  -60.0000 182

 23 omega  -97.00   -6.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026  -57.0000   60.0000 182

 24 omega  -50.00   41.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   57.0000 -150.0000 182

 25 omega    6.00   97.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000  -60.0000 182

 26 omega   -4.00   99.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000 -180.0000 206

 27 omega   -4.00   99.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  -30.0000 206

 28 omega  -43.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   90.0000 206

 29 omega  -43.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   30.0000 206

 30 omega  -46.00   63.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026    0.0000    0.0000 218

 31 omega  -43.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -30.0000 206

 32 omega  -43.00   60.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  150.0000 206

 33 omega   -4.00   99.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000 -150.0000 206

 34 omega   -4.00   99.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000   30.0000 206

 35 omega    6.00   97.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000 -120.0000 182

 36 omega    6.00   97.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000   90.0000 182

 37 omega  -41.00   50.00   0.5000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000   60.0000 182

;
_diffrn_measurement_device       '\k-geometry 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      -0.0411479000
_diffrn_orient_matrix_UB_12      -0.0244099000
_diffrn_orient_matrix_UB_13      -0.0481268000
_diffrn_orient_matrix_UB_21      -0.0298339000
_diffrn_orient_matrix_UB_22      0.0393702000
_diffrn_orient_matrix_UB_23      0.0010463000
_diffrn_orient_matrix_UB_31      0.0570568000
_diffrn_orient_matrix_UB_32      0.0518583000
_diffrn_orient_matrix_UB_33      -0.0076277000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            112371
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.388
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.3126
_exptl_crystal_size_mid          0.2656
_exptl_crystal_size_min          0.1481
_refine_diff_density_max         1.235
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.144
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         12165
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0256
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0120P)^2^+1.6438P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0479
_refine_ls_wR_factor_ref         0.0486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11683
_reflns_number_total             12165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500163c_si_001.cif
_cod_data_source_block           ba_jb8
_cod_depositor_comments
'Adding full bibliography for 4338072--4338082.cif.'
_cod_database_code               4338075
_audit_block_refno               1737
_audit_block_usercomment         'jb100 colourless plate'
_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:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17), C18(H18),
 C24(H24), C25(H25), C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C)
;
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.746
_shelx_hkl_checksum              94730
_cell_oxdiff_length_a            11.58910(9)
_cell_oxdiff_length_b            11.99210(11)
_cell_oxdiff_length_c            15.93941(10)
_cell_oxdiff_angle_alpha         92.1162(6)
_cell_oxdiff_angle_beta          109.7773(6)
_cell_oxdiff_angle_gamma         118.7552(9)
_cell_oxdiff_volume              1773.14(2)
_cell_oxdiff_measurement_reflns_used 56739
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_theta     30.44
_reflns_odcompleteness_iscentric 1