Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by Carbazolide-Based PNP Pincer Ligands.
Plundrich, Gudrun T.; Wadepohl, Hubert; Gade, Lutz H.; Inorganic chemistry 55 (2015) 353–; doi:10.1021/acs.inorgchem.5b02498

data_4344789
_publ_section_title
;
 Synthesis and Reactivity of Group 4 Metal Benzyl Complexes Supported by
 Carbazolide-Based PNP Pincer Ligands.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              353
_journal_paper_doi               10.1021/acs.inorgchem.5b02498
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C34 H54 Cl3 N P2 Zr'
_chemical_formula_sum            'C34 H54 Cl3 N P2 Zr'
_chemical_formula_weight         736.29
_chemical_properties_physical    air-sensitive
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
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'Wed Mar 11 11:03:06 2015'
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Olex2 1.2
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
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;
  1 omega   24.00   55.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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  2 omega    0.00   28.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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  3 omega    1.00   91.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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  4 omega    3.00   94.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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  5 omega  -31.00   22.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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  6 omega   34.00   59.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -80.0000   97.5566 50

  7 phi    120.00  168.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
  26.7881   26.7881   20.0000     -     96

  8 omega   -3.00   41.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   77.0000  -90.0000 88

  9 omega    6.00   90.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7881   57.0000 -150.0000 168

 10 omega    4.00   37.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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 11 omega  -33.00   33.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       26.7881  -57.0000 -150.0000 132

 12 omega   -3.00   97.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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 13 omega  -34.00   60.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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 14 omega   26.00   59.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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 15 omega  -42.00  -12.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
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 16 omega  -36.00   60.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000  168.1854 192

 17 omega  -26.00   60.00   0.5000   17.5000
omega____ theta____ kappa____ phi______ frames
    -       28.0000  -80.0000    0.2887 172

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_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_reflns_limit_l_min       -39
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_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.939
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_diffrn_reflns_theta_min         3.265
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35g (release 09-12-2014 CrysAlis171 .NET)
(compiled Dec  9 2014,15:38:47)
Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
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;
_exptl_crystal_colour            red
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_refine_ls_structure_factor_coef Fsqd
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'w=1/[\s^2^(Fo^2^)+(0.0380P)^2^+3.8482P] where P=(Fo^2^+2Fc^2^)/3'
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_cod_database_code               4344789
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_audit_block_usercomment         'gp859, irregular, red'
_chemical_oxdiff_formula         'C34 H54 Cl3 N P2 Zr'
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;
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 Ternary CH refined with riding coordinates:
 C24(H24), C27(H27), C30(H30), C33(H33), C74(H74), C77(H77), C80(H80), C83(H83)
2.b Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C64(H64A,H64B), C65(H65A,H65B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C11(H11), C54(H54), C56(H56), C59(H59), C61(H61)
2.d Idealised Me refined as rotating group:
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;
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