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_4338076
_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         'C31 H45 F3 Hf N3 O3 P S Si3'
_chemical_formula_sum            'C31 H45 F3 Hf N3 O3 P S Si3'
_chemical_formula_weight         890.49
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb6
_audit_creation_date
;
'Mon Sep 23 14:46:55 2013'
;
_audit_update_record             'Mon Sep 23 17:20:45 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 105.836(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1196(8)
_cell_length_b                   21.4503(11)
_cell_length_c                   19.9812(11)
_cell_measurement_reflns_used    9505
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      70.6540
_cell_measurement_theta_min      4.4550
_cell_volume                     7471.4(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -24.00   29.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 53

  2 omega   32.00   72.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   38.0000  -60.0000 40

  3 omega  -69.00   17.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       -3.5000  -64.0000  150.0000 86

  4 omega    3.00   42.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       34.0000   80.0000 -177.9534 39

  5 omega   26.00  112.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   77.0000 -134.2085 86

  6 omega   17.00  110.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       42.0000   69.0000  -37.3395 93

  7 omega   23.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000  -79.0000  -28.3701 69

  8 omega   38.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   73.0000   89.2573 80

  9 omega   45.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       62.0000   60.0000 -175.5159 42

 10 omega   72.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   59.0000   10.3973 46

 11 omega   59.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000  -80.0000   69.5744 28

 12 omega   47.00   82.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000 -141.2611 35

 13 omega   58.00   83.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  125.9817 25

 14 omega   14.00   49.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000  -80.0000  125.9817 35

 15 omega   71.00  102.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -158.2912 31

 16 omega   70.00  127.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  134.3336 57

 17 omega   72.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -129.6194 37

 18 omega   38.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  134.3336 30

 19 omega   36.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  -60.0000 48

 20 omega   61.00  101.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -80.7414 40

 21 omega   37.00   69.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000 -129.6194 32

 22 omega   36.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  120.0000 56

 23 omega   38.00  107.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   36.1061 69

 24 omega   74.00  175.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -90.0000 101

 25 omega   36.00   91.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000 -150.0000 55

 26 omega   50.00  105.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -49.8986 55

 27 omega   47.00   94.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000  -30.0000 47

 28 omega   41.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000   30.0000 49

 29 omega   45.00   90.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -25.0000 -120.0000 45

 30 omega   80.00  108.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -21.8854 28

 31 omega   74.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000 -180.0000 104

 32 omega   78.00  117.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000   73.8269 39

 33 omega   -5.00   47.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       26.0000   79.0000   63.4135 52

 34 omega   18.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   57.9676 28

 35 omega   48.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   70.0000  116.4831 95

 36 omega   44.00  144.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       74.0000   77.0000  -50.9907 100

 37 omega   50.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   73.0000 -164.1431 97

 38 omega   52.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   70.0000   32.4101 95

 39 omega   50.00  148.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       78.0000   74.0000 -104.2485 98

 40 omega   53.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   75.0000 -129.8321 99

 41 omega   57.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   75.0000   -6.7485 99

 42 omega   56.00  156.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       86.0000   77.0000  126.7903 100

 43 omega   64.00  164.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       94.0000   77.0000   87.4743 100

 44 omega   68.00  168.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   77.0000  -86.3688 100

 45 omega   79.00  169.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      102.0000   64.0000  -53.2928 90

 46 omega   38.00  104.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000   30.0000 66

 47 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000 -180.0000 100

 48 omega   36.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -38.0000  150.0000 57

 49 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   30.0000 100

 50 omega   36.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   12.0000   90.0000 142

 51 omega  -70.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 100

 52 omega   19.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -130.6001 30

 53 omega   18.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000  -66.7028 28

 54 omega   19.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   79.0000  123.0187 28

 55 omega   18.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   80.0000   11.9346 28

 56 omega   19.00   49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   78.0000 -168.3150 30

 57 omega  -13.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       58.0000  -80.0000 -166.1662 103

 58 omega   53.00  152.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   76.0000   62.7372 99

 59 omega   55.00   80.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       82.0000   71.0000  -25.7709 25

 60 omega   70.00  168.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       98.0000   74.0000 -125.0596 98

 61 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000    0.0000 100

 62 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 100

 63 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  150.0000 100

 64 omega   78.00  178.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -30.0000 100

 65 omega   37.00  140.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -80.0000  -80.7414 103

;
_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      0.0420620000
_diffrn_orient_matrix_UB_12      0.0625495000
_diffrn_orient_matrix_UB_13      0.0199106000
_diffrn_orient_matrix_UB_21      0.0287047000
_diffrn_orient_matrix_UB_22      -0.0032616000
_diffrn_orient_matrix_UB_23      -0.0657537000
_diffrn_orient_matrix_UB_31      -0.0721522000
_diffrn_orient_matrix_UB_32      0.0352269000
_diffrn_orient_matrix_UB_33      -0.0412614000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.180
_diffrn_reflns_av_unetI/netI     0.0760
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            187891
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.070
_diffrn_reflns_theta_min         3.575
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.442
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41325
_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    1.583
_exptl_crystal_description       needle
_exptl_crystal_F_000             3584
_exptl_crystal_size_max          0.2324
_exptl_crystal_size_mid          0.0423
_exptl_crystal_size_min          0.0226
_refine_diff_density_max         3.169
_refine_diff_density_min         -2.248
_refine_diff_density_rms         0.195
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     848
_refine_ls_number_reflns         24733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0783
_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^)+(0.1055P)^2^+8.4490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1783
_refine_ls_wR_factor_ref         0.1907
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18969
_reflns_number_total             24733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500163c_si_001.cif
_cod_data_source_block           ba_sb6_5
_cod_depositor_comments
'Adding full bibliography for 4338072--4338082.cif.'
_cod_original_cell_volume        7471.3(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4338076
_audit_block_refno               1851
_audit_block_usercomment         'SB42, needle, colourless'
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.277
_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:
 C4(H4A,H4B), C8(H8A,H8B), C10(H10A,H10B), C27(H27A,H27B), C32(H32A,H32B),
 C51(H51A,H51B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C9(H9), C11(H11), C19(H19), C23(H23), C24(H24), C25(H25),
 C31(H31), C39(H39), C40(H40), C47(H47), C48(H48), C49(H49), C50(H50), C56(H56),
  C57(H57), C61(H61), C65(H65), C66(H66), C68(H68), C69(H69), C777(H777),
 C888(H888)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C12(H12A,H12B,H12C), C432(H43A,H43B,H43C), C20(H20A,H20B,
 H20C), C22(H22A,H22B,H22C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C36(H36A,
 H36B,H36C), C37(H37A,H37B,H37C), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C63(H63A,H63B,
 H63C), C70(H70A,H70B,H70C), C72(H72A,H72B,H72C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              89803
_cell_oxdiff_length_a            18.1295(9)
_cell_oxdiff_length_b            21.4381(9)
_cell_oxdiff_length_c            19.9782(11)
_cell_oxdiff_angle_alpha         90.077(4)
_cell_oxdiff_angle_beta          105.801(5)
_cell_oxdiff_angle_gamma         89.941(4)
_cell_oxdiff_volume              7471.3(6)
_cell_oxdiff_measurement_reflns_used 9505
_cell_oxdiff_twin_number         2