Zirconium Complexes Supported by an N-Perfluoro-Arylated Diamidopyridyl Ligand: Synthesis of Hydrazinediido Complexes
Solveig A. Scholl; Gudrun T. Plundrich; Hubert Wadepohl; Lutz H. Gade; Inorganic Chemistry 52 (2013) 10158–10166; doi:10.1021/ic401603y

data_4335903
_publ_section_title
;
 Zirconium Complexes Supported by an N-Perfluoro-Arylated Diamidopyridyl
 Ligand: Synthesis of Hydrazinediido Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10158
_journal_page_last               10166
_journal_paper_doi               10.1021/ic401603y
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C37 H23 D12 F9 I N5 Zr'
_chemical_formula_weight         950.89
_chemical_properties_physical    air-sensitive
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
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_audit_creation_date
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'Tue Jun 12 16:44:13 2012'
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
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_audit_update_record             'Tue Jun 12 17:08:12 CEST 2012'
_cell_angle_alpha                90.00
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_cell_angle_gamma                90.00
_cell_formula_units_Z            2
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_cell_measurement_temperature    110.00(10)
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
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_diffrn_measurement_details
;
  1 omega  -51.00   35.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -57.0000  150.0000 86

  2 omega   -2.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   57.0000  -60.0000 89

  3 omega   -3.00   87.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   57.0000   60.0000 90

  4 omega   -7.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   77.0000  150.0000 95

  5 omega  -14.00   61.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -99.0000    0.0000 75

  6 omega  -10.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -99.0000 -120.0000 72

  7 omega  -13.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   19.0000  -60.0000 67

  8 omega  -11.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -99.0000   90.0000 73

  9 omega  -12.00   47.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541   77.0000  -90.0000 59

 10 omega   35.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  178.0000  150.0000 61

 11 omega   35.00   96.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  178.0000    0.0000 61

 12 omega   -3.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   57.0000 -150.0000 91

 13 omega    6.00   81.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853 -132.0000 -166.0000 75

 14 omega  -13.00   89.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   77.0000   90.0000 102

 15 omega  -51.00   40.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -57.0000   60.0000 91

 16 omega  -20.00   25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541  -99.0000  -60.0000 45

 17 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000 -180.0000 147

 18 omega   -3.00   88.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853   57.0000    0.0000 91

 19 omega  -20.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -99.0000  -30.0000 82

 20 omega  -20.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -99.0000  -60.0000 82

 21 omega  -20.00   62.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853  -99.0000   30.0000 82

 22 omega  -20.00   25.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541  -99.0000 -150.0000 45

 23 omega  -93.00   31.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541  -19.0000    0.0000 124

 24 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000 -120.0000 147

 25 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000  -90.0000 147

 26 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000  -60.0000 147

 27 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000  -30.0000 147

 28 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000    0.0000 147

 29 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000   30.0000 147

 30 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000 -150.0000 147

 31 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000   60.0000 147

 32 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000  120.0000 147

 33 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000  150.0000 147

 34 omega  -55.00   92.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       18.3853    0.0000   90.0000 147

 35 omega  -92.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541    0.0000 -150.0000 147

 36 omega  -92.00  -67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541    0.0000 -120.0000 25

 37 omega  -92.00   55.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.8541    0.0000 -180.0000 147

;
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_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
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_diffrn_orient_matrix_UB_11      -0.0714744000
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_diffrn_orient_matrix_UB_22      0.0239754000
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_diffrn_reflns_limit_h_min       -11
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
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_exptl_crystal_F_000             932
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_exptl_crystal_size_mid          0.1177
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_refine_diff_density_max         0.503
_refine_diff_density_min         -0.385
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_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         4794
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0140P)^2^+1.5184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_cod_original_cell_volume        1805.68(3)
_cod_original_sg_symbol_H-M      'P 21/m'
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_cell_oxdiff_angle_beta          109.2903(19)
_cell_oxdiff_angle_gamma         90.0300(16)
_cell_oxdiff_volume              1805.69(6)
_cell_oxdiff_measurement_reflns_used 48099
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_theta     26.32
_reflns_odcompleteness_iscentric 1