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_4335904
_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            'C25 H23 Cl F9 N5 Zr'
_chemical_formula_weight         691.15
_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
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ss28
_audit_creation_date
;
'Fri Dec 02 10:45:59 2011'
;
_audit_creation_method
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_audit_update_record             'Fri Dec  2 12:30:22 CET 2011'
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9131(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.33527(4)
_cell_length_b                   18.16024(9)
_cell_length_c                   9.30851(5)
_cell_measurement_reflns_used    50898
_cell_measurement_temperature    114.95(18)
_cell_measurement_theta_max      27.9499
_cell_measurement_theta_min      3.2373
_cell_volume                     1316.211(13)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF (Beurskens et al., 1999-2008)'
_diffrn_ambient_temperature      114.95(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9241
_diffrn_detector_type            'Agilent EOS'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_details
;
  1 omega  -12.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334   77.0000 -150.0000 98

  2 omega  -46.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -77.0000   90.0000 92

  3 omega    8.00   82.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334   57.0000  120.0000 74

  4 omega  -42.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -77.0000  -30.0000 88

  5 omega  -13.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334   77.0000    0.0000 99

  6 omega  -45.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -77.0000 -120.0000 91

  7 omega  -67.00  -37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803  -57.0000  -90.0000 30

  8 omega  -48.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803   80.0000  151.0000 71

  9 omega  -54.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -77.0000  120.0000 100

 10 omega   -6.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334   57.0000   30.0000 91

 11 omega  -53.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -57.0000  -90.0000 90

 12 omega  -53.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -57.0000 -180.0000 90

 13 omega  -89.00    9.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803  -38.0000   90.0000 98

 14 omega  -48.00   24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803   80.0000  -22.0000 72

 15 omega   -6.00   85.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334   57.0000  -60.0000 91

 16 omega  -53.00   37.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -57.0000    0.0000 90

 17 omega  -54.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -77.0000 -120.0000 100

 18 omega  -54.00   46.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334  -77.0000  -60.0000 100

 19 omega  -48.00   24.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803   80.0000  151.0000 72

 20 omega  -85.00    5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803  -57.0000   30.0000 90

 21 omega  -57.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334    0.0000  240.0000 146

 22 omega  -57.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334    0.0000    0.0000 146

 23 omega  -57.00   89.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       15.7334    0.0000  120.0000 146

 24 omega  -89.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803    0.0000  240.0000 146

 25 omega  -89.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803    0.0000  120.0000 146

 26 omega  -89.00   57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.2803    0.0000    0.0000 146

 27 phi      0.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
  15.7334   15.7334  -20.0000     -     120

 28 phi      0.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
  15.7334   15.7334   20.0000     -     120

 29 phi      0.00   66.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
  15.7334   15.7334  -40.0000     -     66

 30 phi      0.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
  40.0000   15.7334    0.0000     -     120

;
_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      0.0379917000
_diffrn_orient_matrix_UB_12      0.0015875000
_diffrn_orient_matrix_UB_13      0.0813291000
_diffrn_orient_matrix_UB_21      -0.0760406000
_diffrn_orient_matrix_UB_22      -0.0147550000
_diffrn_orient_matrix_UB_23      0.0062188000
_diffrn_orient_matrix_UB_31      0.0327441000
_diffrn_orient_matrix_UB_32      -0.0361273000
_diffrn_orient_matrix_UB_33      0.0010301000
_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  0.0323
_diffrn_reflns_av_sigmaI/netI    0.0598
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            76245
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         27.9499
_diffrn_reflns_theta_min         3.2373
_diffrn_source                   'Agilent SuperNova (Mo) x-ray Source'
_exptl_absorpt_coefficient_mu    0.610
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.911
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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            colourless
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       box
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.2157
_exptl_crystal_size_mid          0.1459
_exptl_crystal_size_min          0.1087
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         3184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0189
_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^)+(0.0230P)^2^+0.8488P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0507
_refine_ls_wR_factor_ref         0.0517
_reflns_number_gt                3028
_reflns_number_total             3184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401603y_si_002_3.cif
_cod_data_source_block           ga_ss28
_cod_original_cell_volume        1316.210(11)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4335904
_audit_block_refno               1385
_audit_block_usercomment         'sos482_2 block colourless'
_cell_oxdiff_length_a            8.33501(17)
_cell_oxdiff_length_b            18.1609(3)
_cell_oxdiff_length_c            9.30762(18)
_cell_oxdiff_angle_alpha         90.0067(14)
_cell_oxdiff_angle_beta          110.8991(18)
_cell_oxdiff_angle_gamma         89.9875(14)
_cell_oxdiff_volume              1316.21(4)
_cell_oxdiff_measurement_reflns_used 50898
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_theta     25.07
_reflns_odcompleteness_iscentric 1