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_4335905
_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            'C88 H82 F18 K2 N14 Zr2'
_chemical_formula_weight         1938.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ss50
_audit_creation_date
;
'Thu Mar 21 14:54:14 2013'
;
_audit_creation_method           SHELXL-2013
_audit_update_record             'Thu Mar 21 17:07:56 CET 2013'
_cell_angle_alpha                93.1084(8)
_cell_angle_beta                 95.7719(8)
_cell_angle_gamma                111.0070(9)
_cell_formula_units_Z            1
_cell_length_a                   10.21010(10)
_cell_length_b                   13.21438(13)
_cell_length_c                   16.79443(15)
_cell_measurement_reflns_used    31731
_cell_measurement_temperature    110(1)
_cell_measurement_theta_max      32.0740
_cell_measurement_theta_min      3.8690
_cell_volume                     2094.62(4)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 7.9621
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_details
;
  1 omega    1.00   32.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000 -120.0000 62

  2 omega  -60.00  -34.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000  -60.0000 52

  3 omega  -60.00  -17.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000   60.0000 86

  4 omega  -60.00  -20.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000 -120.0000 80

  5 omega   16.00   42.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   77.0000  -60.0000 52

  6 omega  -50.00  -17.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -28.0026   57.0000   60.0000 66

  7 omega   -4.00   43.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000 -150.0000 94

  8 omega   18.00   59.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  150.0000 82

  9 omega   -4.00   98.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000   90.0000 204

 10 omega  -25.00   59.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000   90.0000 168

 11 omega   16.00   53.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000 -180.0000 74

 12 omega  -43.00   -7.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  150.0000 72

 13 omega   -3.00   85.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000    0.0000 176

 14 omega  -23.00   60.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -77.0000  -60.0000 166

 15 omega    7.00   45.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  -90.0000 76

 16 omega    1.00   46.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000    0.0000 90

 17 omega   60.00   86.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000   60.0000 52

 18 omega  -21.00  102.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   19.0000  -90.0000 246

 19 omega  -25.00   72.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -19.0000  120.0000 194

 20 omega  -41.00   50.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000  -90.0000 182

 21 omega    6.00   97.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   57.0000    0.0000 182

 22 omega  -41.00   50.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026  -57.0000  150.0000 182

 23 omega   -4.00   23.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   77.0000  120.0000 54

 24 omega    1.00  101.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0026   38.0000  -90.0000 200

;
_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      0.0232530000
_diffrn_orient_matrix_UB_12      0.0575893000
_diffrn_orient_matrix_UB_13      0.0016595000
_diffrn_orient_matrix_UB_21      0.0556145000
_diffrn_orient_matrix_UB_22      0.0008592000
_diffrn_orient_matrix_UB_23      -0.0224150000
_diffrn_orient_matrix_UB_31      -0.0446930000
_diffrn_orient_matrix_UB_32      -0.0045020000
_diffrn_orient_matrix_UB_33      -0.0362486000
_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  0.0373
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            73620
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.401
_diffrn_reflns_theta_min         3.228
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_type   analytical
_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)
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            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             988
_exptl_crystal_size_max          0.2420
_exptl_crystal_size_mid          0.1575
_exptl_crystal_size_min          0.0488
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.807
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         14155
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0242P)^2^+1.6678P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0812
_refine_ls_wR_factor_ref         0.0831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13179
_reflns_number_total             14155
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401603y_si_002_4.cif
_cod_data_source_block           ga_ss50
_cod_database_code               4335905
_audit_block_refno               1732
_audit_block_usercomment         'SOS701, block, orange'
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.957
_shelxl_version_number           2013-2
_shelx_res_checksum              94035
_cell_oxdiff_length_a            10.21010(10)
_cell_oxdiff_length_b            13.21438(13)
_cell_oxdiff_length_c            16.79443(15)
_cell_oxdiff_angle_alpha         93.1084(8)
_cell_oxdiff_angle_beta          95.7719(8)
_cell_oxdiff_angle_gamma         111.0070(9)
_cell_oxdiff_volume              2094.62(3)
_cell_oxdiff_measurement_reflns_used 31731
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_theta     30.44
_reflns_odcompleteness_iscentric 1