Zirconium and Hafnium Complexes Containing N-Alkyl-Substituted Amine Biphenolate Ligands: Unexpected Ligand Degradation and Divergent Complex Constitutions Governed by N-Alkyls
Lan-Chang Liang; Chia-Cheng Chien; Ming-Tsz Chen; Sheng-Ta Lin; Inorganic Chemistry 52 (2013) 7709–7716; doi:10.1021/ic400891b

data_4335387
_publ_section_title
;
 Zirconium and Hafnium Complexes Containing N-Alkyl-Substituted Amine
 Biphenolate Ligands: Unexpected Ligand Degradation and Divergent Complex
 Constitutions Governed by N-Alkyls
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7709
_journal_page_last               7716
_journal_paper_doi               10.1021/ic400891b
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C55 H89 Hf N O4'
_chemical_formula_sum            'C55 H89 Hf N O5'
_chemical_formula_weight         1022.76
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.378(2)
_cell_angle_beta                 82.975(2)
_cell_angle_gamma                84.909(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2961(4)
_cell_length_b                   14.8938(5)
_cell_length_c                   18.2019(7)
_cell_measurement_temperature    200(2)
_cell_volume                     3050.69(19)
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25198
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.48
_exptl_absorpt_coefficient_mu    1.748
_exptl_absorpt_correction_T_max  0.6996
_exptl_absorpt_correction_T_min  0.6132
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       prism
_exptl_crystal_F_000             1076
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.22
_platon_squeeze_details
;
;
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         10707
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+0.3101P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0669
_refine_ls_wR_factor_ref         0.0680
_reflns_number_gt                9924
_reflns_number_total             10707
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400891b_si_002_2.cif
_cod_data_source_block           a13171_5a
_cod_original_cell_volume        3050.69(18)
_cod_database_code               4335387