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_4338081
_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         'C37 H53 Cl N3 P Si3 Ti'
_chemical_formula_sum            'C37 H53 Cl N3 P Si3 Ti'
_chemical_formula_weight         738.41
_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   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_sb1
_audit_creation_date
;
'Fri Jun 28 16:38:13 2013'
;
_audit_update_record             'Fri Jun 28 16:48:48 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 112.201(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.2970(4)
_cell_length_b                   9.31074(14)
_cell_length_c                   22.7693(5)
_cell_measurement_reflns_used    16216
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      27.7270
_cell_measurement_theta_min      3.4530
_cell_volume                     3983.94(16)
_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
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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 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -33.00   -2.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -80.0000 -105.4133 62

  2 omega -100.00  -74.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -38.0000   30.0000 52

  3 omega  -32.00   -5.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -38.0000   30.0000 54

  4 omega  -25.00    1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -80.0000   70.3630 52

  5 omega  -40.00   -6.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -41.0000  -53.9751 68

  6 omega  -88.00  -62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -77.0000  150.0000 52

  7 omega  -38.00    0.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -77.0000  150.0000 76

  8 omega  -55.00  -10.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.0502  -57.0000 -120.0000 90

  9 omega  -27.00    7.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000 -120.0000 68

 10 omega   11.00   48.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000  -60.0000 74

 11 omega   40.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000  -48.4935 50

 12 omega   63.00   89.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000  -60.0000 52

 13 omega   39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000 -120.0000 50

 14 omega  -28.00   15.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000   30.0000 86

 15 omega   20.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000   16.1663 90

 16 omega   -1.00   24.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   79.0000  118.8863 50

 17 omega   39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000  150.0000 50

 18 omega   29.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000  -67.1368 70

 19 omega  -20.00   21.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000  -48.4935 82

 20 omega  -39.00   14.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000  150.0000 106

 21 omega    5.00   66.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   38.0000  120.0000 122

 22 omega    5.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   38.0000 -150.0000 120

 23 omega    8.00   95.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   77.0000  -30.0000 174

 24 omega   24.00   87.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000 -120.0000 126

 25 omega   18.00   57.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   57.0000  150.0000 78

 26 omega  -39.00   -2.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000  -67.1368 74

 27 omega   -1.00   25.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283   79.0000   69.2419 52

 28 omega   38.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000  120.0000 52

 29 omega  -39.00   62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000 -150.0000 202

 30 omega   39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -77.0000   30.0000 50

 31 omega  -39.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -80.0000   96.0946 208

 32 omega  -39.00   -5.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       32.1283  -79.0000   16.1663 68

;
_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      -0.0032790000
_diffrn_orient_matrix_UB_12      0.0138515000
_diffrn_orient_matrix_UB_13      -0.0316213000
_diffrn_orient_matrix_UB_21      -0.0273904000
_diffrn_orient_matrix_UB_22      0.0503736000
_diffrn_orient_matrix_UB_23      -0.0033770000
_diffrn_orient_matrix_UB_31      0.0257420000
_diffrn_orient_matrix_UB_32      0.0554623000
_diffrn_orient_matrix_UB_33      0.0109714000
_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  0.0910
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            101547
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_min         3.171
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93800
_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            red
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.1776
_exptl_crystal_size_mid          0.1332
_exptl_crystal_size_min          0.0847
_refine_diff_density_max         1.004
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     427
_refine_ls_number_reflns         9898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0453P)^2^+2.5447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1122
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7607
_reflns_number_total             9898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500163c_si_001.cif
_cod_data_source_block           ba_sb1
_cod_depositor_comments
'Adding full bibliography for 4338072--4338082.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4338081
_audit_block_refno               1793
_audit_block_usercomment         'sb12, irregular, red'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(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), C31(H31A,H31B)
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), C33(H33), C34(H34), C35(H35), C36(H36),
  C37(H37)
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   0.957
_shelx_estimated_absorpt_t_min   0.957
_shelx_hkl_checksum              2787
_cell_oxdiff_length_a            20.2971(4)
_cell_oxdiff_length_b            9.30921(18)
_cell_oxdiff_length_c            22.7651(7)
_cell_oxdiff_angle_alpha         89.989(2)
_cell_oxdiff_angle_beta          112.152(2)
_cell_oxdiff_angle_gamma         90.0511(16)
_cell_oxdiff_volume              3983.94(17)
_cell_oxdiff_measurement_reflns_used 16216
_reflns_odcompleteness_completeness 68.65
_reflns_odcompleteness_theta     32.50
_reflns_odcompleteness_iscentric 1