A Novel Trisamidophosphine Ligand and Its Group(IV) Metal Complexes
Sietzen, Malte; Wadepohl, Hubert; Ballmann, Joachim; Organometallics 33 (2014) 612–; doi:10.1021/om401018f

data_4082453
_publ_section_title
;
 A Novel Trisamidophosphine Ligand and Its Group(IV) Metal Complexes
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              612
_journal_paper_doi               10.1021/om401018f
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C46 H48 N3 P Zr, 5(C H2 Cl2)'
_chemical_formula_sum            'C51 H58 Cl10 N3 P Zr'
_chemical_formula_weight         1189.69
_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_ms4
_audit_creation_date
;
'Thu May 16 14:40:45 2013'
;
_audit_update_record             'Fri Oct 11 17:25:31 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 98.8698(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.59551(11)
_cell_length_b                   18.37056(14)
_cell_length_c                   20.06023(15)
_cell_measurement_reflns_used    40985
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      27.3000
_cell_measurement_theta_min      3.6540
_cell_volume                     5678.49(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-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 0.9972
_diffrn_measured_fraction_theta_max 0.9483
_diffrn_measurement_details
;
  1 omega  -49.00  -23.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9909   77.0000  150.0000 52

  2 omega  -54.00   49.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000  -16.2348 206

  3 omega  -14.00   66.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909   77.0000  -30.0000 160

  4 omega  -14.00   88.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909   77.0000 -150.0000 204

  5 omega  -52.00   49.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000 -120.0000 202

  6 omega    4.00   30.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909   57.0000  -90.0000 52

  7 omega   13.00   49.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000  150.0000 72

  8 omega   24.00   49.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000  -90.0000 50

  9 omega  -13.00   50.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -80.0000   33.4291 126

 10 omega  -17.00    9.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -38.0000  -30.0000 52

 11 omega   -3.00   23.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909   57.0000  -30.0000 52

 12 omega  -10.00   85.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909   77.0000   90.0000 190

 13 omega  -26.00    0.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000  -60.0000 52

 14 omega   24.00   49.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000  -60.0000 50

 15 phi      8.00  110.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   16.9909    0.0000     -     204

 16 omega  -47.00   50.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -79.0000  100.2012 194

 17 omega  -39.00  -14.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.9909   57.0000   90.0000 50

 18 omega   -5.00   86.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909   57.0000  120.0000 182

 19 omega  -54.00   49.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       16.9909  -77.0000 -180.0000 206

;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_UB_11      -0.0263425000
_diffrn_orient_matrix_UB_12      0.0109172000
_diffrn_orient_matrix_UB_13      -0.0303675000
_diffrn_orient_matrix_UB_21      -0.0079107000
_diffrn_orient_matrix_UB_22      0.0338370000
_diffrn_orient_matrix_UB_23      0.0149728000
_diffrn_orient_matrix_UB_31      0.0369082000
_diffrn_orient_matrix_UB_32      0.0150515000
_diffrn_orient_matrix_UB_33      -0.0115934000
_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  0.0423
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            119970
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.714
_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    0.728
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97046
_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            yellow
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.2348
_exptl_crystal_size_mid          0.1533
_exptl_crystal_size_min          0.1362
_refine_diff_density_max         2.401
_refine_diff_density_min         -1.532
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         12648
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+20.4676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1523
_refine_ls_wR_factor_ref         0.1601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10724
_reflns_number_total             12648
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401018f_si_001.cif
_cod_data_source_block           ba_ms4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4082453
_audit_block_refno               1770
_audit_block_usercomment         'MS176, yellow, irregular'
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C46 H48 N3 P Zr'
_chemical_oxdiff_usercomment     'MS176, yellow, irregular'
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.848
_reflns_odcompleteness_completeness 99.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Restrained distances
 C51-Cl1 \\sim C51-Cl2 \\sim C61-Cl3 \\sim C61-Cl4 \\sim C71A-Cl5A \\sim
C71A-Cl6A \\sim C71B-Cl5B ~
 C71B-Cl6B \\sim C81A-Cl7A \\sim C81B-Cl7B \\sim C81A-Cl8A \\sim C81B-Cl8B
 with sigma of 0.01
 Cl1-Cl2 \\sim Cl3-Cl4 \\sim Cl5A-Cl6A \\sim Cl5B-Cl6B \\sim Cl7A-Cl8A \\sim
Cl7B-Cl8B \\sim Cl9-Cl10
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C51 \\sim C61 \\sim
C71A \\sim C71B \\sim C81A \\sim C81B \\sim C91 \\sim Cl1 \\sim Cl2 \\sim Cl3
\\sim Cl4 \\sim Cl5A \\sim Cl5B \\sim Cl6A \\sim Cl6B \\sim Cl7A \\sim Cl7B
\\sim Cl8A \\sim Cl8B \\sim Cl9 \\sim Cl10: within 0.5A with sigma of 0.02 and
sigma for terminal atoms of 0.04
4. Others
 Sof(Cl5B)=Sof(Cl6B)=Sof(C71B)=Sof(H71C)=Sof(H71D)=1-FVAR(1)
 Sof(Cl5A)=Sof(Cl6A)=Sof(C71A)=Sof(H71A)=Sof(H71B)=FVAR(1)
 Sof(Cl7B)=Sof(Cl8B)=Sof(C81B)=Sof(H81C)=Sof(H81D)=1-FVAR(2)
 Sof(Cl7A)=Sof(Cl8A)=Sof(C81A)=Sof(H81A)=Sof(H81B)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C22(H22A,H22B), C37(H37A,H37B), C51(H51A,H51B), C61(H61A,H61B),
 C71A(H71A,H71B), C71B(H71C,H71D), C81A(H81A,H81B), C81B(H81C,H81D), C91(H91A,
 H91B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C13(H13), C18(H18),
 C19(H19), C20(H20), C21(H21), C24(H24), C26(H26), C28(H28), C33(H33), C34(H34),
  C35(H35), C36(H36), C39(H39), C41(H41), C43(H43)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              49831
_cell_oxdiff_length_a            15.59559(18)
_cell_oxdiff_length_b            18.37122(18)
_cell_oxdiff_length_c            20.0587(2)
_cell_oxdiff_angle_alpha         90.0242(8)
_cell_oxdiff_angle_beta          98.8564(9)
_cell_oxdiff_angle_gamma         90.0047(9)
_cell_oxdiff_volume              5678.49(10)
_cell_oxdiff_measurement_reflns_used 40985