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_4338079
_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         'C30 H45 Cl Hf N3 P Si3'
_chemical_formula_sum            'C30 H45 Cl Hf N3 P Si3'
_chemical_formula_weight         776.87
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb2
_audit_creation_date
;
'Fri Jun 28 17:18:56 2013'
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_audit_update_record             'Mon Aug 12 15:46:11 CEST 2013'
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_cell_angle_gamma                90
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_cell_length_c                   19.14401(10)
_cell_measurement_reflns_used    71999
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      34.1470
_cell_measurement_theta_min      3.4350
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
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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)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
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_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.
;
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'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
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;
  1 omega   12.00   37.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502   57.0000  -60.0000 50

  2 omega -102.00  -76.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
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  3 omega  -25.00    0.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -77.0000  -60.0000 50

  4 omega  -28.00    0.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -80.0000 -179.5650 56

  5 omega  -41.00  -15.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -78.0000 -138.0000 52

  6 omega  -46.00   -3.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -80.0000  -78.9691 86

  7 omega  -41.00    1.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -80.0000   49.8016 84

  8 omega  -44.00  -17.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -43.0000  -55.4527 54

  9 omega  -39.00   64.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -78.0000 -138.0000 206

 10 omega  -39.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -80.0000  167.8946 210

 11 omega  -29.00   66.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -80.0000  -72.4689 190

 12 omega   11.00   40.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000   60.0000 58

 13 omega  -37.00   37.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -57.0000    0.0000 148

 14 omega   39.00   64.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -77.0000  -30.0000 50

 15 omega   21.00   63.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -80.0000   46.8695 84

 16 omega    1.00   57.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   77.0000 -180.0000 112

 17 omega   11.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000  150.0000 180

 18 omega  -26.00   64.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -77.0000   90.0000 180

 19 omega   -5.00   76.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   19.0000  -60.0000 162

 20 omega    5.00  100.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   38.0000   90.0000 190

 21 omega    5.00   96.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   38.0000    0.0000 182

 22 omega  -11.00   16.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   22.0000   55.7983 54

 23 omega -101.00  -10.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -57.0000  150.0000 182

 24 omega   11.00  101.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   57.0000   90.0000 180

 25 omega  -37.00   54.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -57.0000  -60.0000 182

 26 omega    5.00  100.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845   38.0000    0.0000 190

 27 omega  -42.00   82.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       32.2845  -19.0000   30.0000 248

;
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_diffrn_orient_matrix_UB_32      0.0255373000
_diffrn_orient_matrix_UB_33      0.0207815000
_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  0.0401
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.972
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_diffrn_reflns_limit_h_min       -17
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_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            161663
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_max         34.218
_diffrn_reflns_theta_min         3.259
_diffrn_source                   'microfocus X-Ray tube'
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_exptl_absorpt_correction_type   gaussian
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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)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
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_exptl_crystal_colour            colourless
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_refine_diff_density_max         0.919
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0141P)^2^+1.7214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.0391
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_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500163c_si_001.cif
_cod_data_source_block           ba_sb2
_cod_depositor_comments
'Adding full bibliography for 4338072--4338082.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4338079
_audit_block_refno               1794
_audit_block_usercomment         'Sb22, needle, colourless'
_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:
 C5(H5), C6(H6), C7(H7), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C23(H23), C24(H24), C25(H25), C26(H26)
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)
;
_shelx_estimated_absorpt_t_max   0.736
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_shelx_res_checksum              2621
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_cell_oxdiff_length_a            11.39831(13)
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_cell_oxdiff_angle_alpha         90.0028(10)
_cell_oxdiff_angle_beta          106.0071(10)
_cell_oxdiff_angle_gamma         90.0187(10)
_cell_oxdiff_volume              3462.23(7)
_cell_oxdiff_measurement_reflns_used 71999
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_theta     32.50
_reflns_odcompleteness_iscentric 1