Synthesis of Zirconium, Hafnium, and Tantalum Complexes with Sterically Demanding Hydrazide Ligands
Jean-Sébastien M. Lehn; Saba Javed; David M. Hoffman; Inorganic Chemistry 46 (2007) 993–1000; doi:10.1021/ic061483w

data_4306997
_publ_contact_author_address
;
Department of Chemistry
Faculty of Science of Technology
Keio University
3-14-1 Hiyoshi, Kohoku-ku
Yokohama 223-8522
Japan
;
_publ_contact_author_email       akitsu@chem.keio.ac.jp
_publ_contact_author_fax         '81 45 566 1697'
_publ_contact_author_name        'Dr. Takashiro AKITSU'
_publ_contact_author_phone       '81 45 566 1790'
_publ_section_title
;
Synthesis of Zirconium, Hafnium, and Tantalum Complexes with Sterically
Demanding Hydrazide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              993
_journal_page_last               1000
_journal_paper_doi               10.1021/ic061483w
_journal_volume                  46
_journal_year                    2007
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C16 H32 Cu N8 Ni O2 '
_chemical_formula_sum            'C16 H32 Cu N8 Ni O2'
_chemical_formula_weight         490.75
_chemical_name_systematic        ?
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'June 12 2005'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 110.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.864(4)
_cell_length_b                   15.393(8)
_cell_length_c                   7.995(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      13.7
_cell_measurement_theta_min      10.3
_cell_volume                     1138.4(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
' MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1991)'
_computing_data_reduction
'teXsan (Molecular Structure Corporation, 2001)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
'teXsan (Molecular Structure Corporation, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'scintillation counter'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC-7R diffractometer'
_diffrn_measurement_method       '\w-2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode generator'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.0640
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            3020
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0.87
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.788
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.591
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, et al., 1968)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.432
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate like'
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details 'Flack (1983), no Friedel pair'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                2232
_reflns_number_total             2714
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic061483wsi20061207_110756_1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4306997