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_4335902
_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            'C28 H26 F10 N5 Zr'
_chemical_formula_weight         713.76
_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     dual
_atom_sites_solution_secondary   difmap
_audit_block_code                ga_ss19
_audit_creation_method           SHELXL-2013
_audit_update_record             'Thu Jun 20 14:31:11 CEST 2013'
_cell_angle_alpha                90
_cell_angle_beta                 97.987(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9732(18)
_cell_length_b                   14.563(3)
_cell_length_c                   22.387(5)
_cell_measurement_reflns_used    3186
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.24
_cell_measurement_theta_min      2.31
_cell_volume                     2897.1(11)
_computing_cell_refinement
;
SAINT 8.x (Bruker AXS, 1997-2012). Includes estimated systematic errors
 of the unit cell constants from Monte Carlo simulations.
;
_computing_data_collection       'SMART-5.631 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT 8.x (Bruker AXS, 1997-2011)'
_computing_publication_material
'encif (Wadepohl, 2009-13); encifer 1.4 (CCDC, 2011)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR2004 (Giacovazzo et al., 2004)'
_diffrn_ambient_environment      'perfluoro polyether oil'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.19
_diffrn_detector_type            CCD-PXL-KAF2
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS Smart 1000'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1317
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            60392
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.103
_diffrn_reflns_theta_min         2.292
_diffrn_source                   'sealed X-Ray tube (Mo)'
_diffrn_source_type              'fine focus tube'
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  0.963093
_exptl_absorpt_correction_T_min  0.883762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements (Blessing 1995)
SADABS (Sheldrick & Bruker AXS, 2004-2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.130
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
;
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.677
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     375
_refine_ls_number_reflns         5160
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+3.2627P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1187
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3529
_reflns_number_total             5160
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic401603y_si_002_1.cif
_cod_data_source_block           ga_ss19_4_sq
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4335902
_audit_block_refno               1200
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.977
_shelxl_version_number           2013-3
_shelx_res_checksum              27609