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_4082452
_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 H45 F3 N3 O3 P S Zr, 3(C7 H8)'
_chemical_formula_sum            'C67 H69 F3 N3 O3 P S Zr'
_chemical_formula_weight         1175.50
_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     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_ms5
_audit_creation_date
;
'Tue Oct 01 20:14:07 2013'
;
_audit_update_record             'Tue Oct  1 20:48:31 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 100.743(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2711(6)
_cell_length_b                   12.6818(4)
_cell_length_c                   28.9486(8)
_cell_measurement_reflns_used    11994
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      30.2570
_cell_measurement_theta_min      3.7030
_cell_volume                     5868.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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    'SHELXT (Sheldrick, 2013)'
_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 0.9963
_diffrn_measured_fraction_theta_max 0.8411
_diffrn_measurement_details
;
  1 omega  -99.00  -72.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.9720  -77.0000 -180.0000 54

  2 omega  -34.00   -7.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.9720  -80.0000  158.9077 54

  3 omega  -45.00    1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.9720  -80.0000   -7.5326 92

  4 omega  -36.00   -6.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.9720  -80.0000  -78.3145 60

  5 omega  -31.00    0.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.9720  -77.0000 -180.0000 62

  6 omega  -46.00    1.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -31.9720  -80.0000   92.5153 94

  7 omega   62.00  106.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   19.0000   30.0000 88

  8 omega   35.00   62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -77.0000  120.0000 54

  9 omega   10.00   61.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   57.0000  -60.0000 102

 10 omega   36.00   63.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -78.0000   57.3886 54

 11 omega  -37.00   20.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -77.0000  -30.0000 114

 12 omega  -14.00   46.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   19.0000   30.0000 120

 13 omega   12.00   46.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   41.0000   41.0000 68

 14 omega  -39.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -79.0000 -121.2385 206

 15 omega    6.00   96.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   38.0000 -120.0000 180

 16 omega   32.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -80.0000  -71.8413 66

 17 omega    6.00   96.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   38.0000  120.0000 180

 18 omega   10.00   72.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   57.0000  150.0000 124

 19 omega  -30.00    2.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -80.0000  -71.8413 64

 20 omega   57.00   84.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720   41.0000   41.0000 54

 21 omega  -29.00   62.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -77.0000   30.0000 182

 22 omega  -15.00   12.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -77.0000  120.0000 54

 23 omega  -27.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -79.0000  157.9956 184

 24 omega   39.00   65.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -80.0000   83.9292 52

 25 omega   34.00   64.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -77.0000  -30.0000 60

 26 omega  -36.00   29.00   0.5000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       31.9720  -80.0000   83.9292 130

;
_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      0.0420596000
_diffrn_orient_matrix_UB_12      -0.0109395000
_diffrn_orient_matrix_UB_13      0.0105618000
_diffrn_orient_matrix_UB_21      -0.0054258000
_diffrn_orient_matrix_UB_22      -0.0532412000
_diffrn_orient_matrix_UB_23      -0.0074645000
_diffrn_orient_matrix_UB_31      0.0130513000
_diffrn_orient_matrix_UB_32      0.0131973000
_diffrn_orient_matrix_UB_33      -0.0213227000
_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  0.1558
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            166799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.568
_diffrn_reflns_theta_min         3.205
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_description       needle
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.2813
_exptl_crystal_size_mid          0.0821
_exptl_crystal_size_min          0.0415
_refine_diff_density_max         1.474
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         17954
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0637
_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^)+(0.0307P)^2^+6.9124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1266
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12812
_reflns_number_total             17954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om401018f_si_001.cif
_cod_data_source_block           ba_ms5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4082452
_audit_block_refno               1862
_audit_block_usercomment         'MS175, needle, yellow'
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C67 H69 F3 N3 O3 P1 S1 Zr1'
_chemical_oxdiff_usercomment     'MS175, needle, yellow'
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.970
_reflns_odcompleteness_completeness 84.11
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.50
_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. Same fragment restrains
{C51, C52, C53, C54, C55, C56, C57}
as
{C61, C62, C63, C64, C65, C66, C67}
{C51, C52, C53, C54, C55, C56, C57}
as
{C71, C72, C73, C74, C75, C76, C77}
3.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C15(H15A,H15B), C21(H21A,H21B)
3.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C25(H25), C27(H27), C31(H31),
  C33(H33), C35(H35), C39(H39), C41(H41), C43(H43), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66),
  C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C57(H57A,H57B,H57C), C67(H67A,
 H67B,H67C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              45264
_cell_oxdiff_length_a            16.2713(5)
_cell_oxdiff_length_b            12.6813(3)
_cell_oxdiff_length_c            28.9503(7)
_cell_oxdiff_angle_alpha         90.0156(19)
_cell_oxdiff_angle_beta          100.752(2)
_cell_oxdiff_angle_gamma         90.020(2)
_cell_oxdiff_volume              5868.8(3)
_cell_oxdiff_measurement_reflns_used 11994