Cationic Zirconium Hydrides Supported by an NNNN-Type Macrocyclic Ligand: Synthesis, Structure, and Reactivity
Heiko Kulinna; Thomas P. Spaniol; Laurent Maron; Jun Okuda; Inorganic Chemistry 51 (2012) 12462–12472; doi:10.1021/ic301880z

data_4331085
_publ_contact_author_address
;
        Institute of Inorganic Chemistry
        RWTH Aachen University
        Landoltweg 1
        D-52056 Aachen
        Germany
;
_publ_contact_author_email       jun.okuda@ac.rwth-aachen.de
_publ_contact_author_fax         0049-241-8092644
_publ_contact_author_name        'Jun Okuda'
_publ_contact_author_phone       0049-241-8094645
_publ_section_title
;
 Cationic Zirconium Hydrides Supported by an NNNN-Type Macrocyclic Ligand:
 Synthesis, Structure, and Reactivity
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12462
_journal_page_last               12472
_journal_paper_doi               10.1021/ic301880z
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C19 H47 N4 Si2 Zr, C24 H12 B Cl8'
_chemical_formula_sum            'C43 H59 B Cl8 N4 Si2 Zr'
_chemical_formula_weight         1073.75
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           110
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4bw -2c'
_symmetry_space_group_name_H-M   'I 41 c d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   24.293(2)
_cell_length_b                   24.293(2)
_cell_length_c                   34.827(3)
_cell_measurement_reflns_used    6125
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.77
_cell_measurement_theta_min      2.37
_cell_volume                     20553(3)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'APEX Area Detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'INCOATEC microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1540
_diffrn_reflns_av_sigmaI/netI    0.1109
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            78510
_diffrn_reflns_theta_full        24.73
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.711
_exptl_absorpt_correction_T_max  0.9586
_exptl_absorpt_correction_T_min  0.7993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Platon Mulabs'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_description       needle
_exptl_crystal_F_000             8864
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.07(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     521
_refine_ls_number_reflns         8772
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      0.921
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0740
_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^)+(0.1006P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1670
_refine_ls_wR_factor_ref         0.1875
_reflns_number_gt                5226
_reflns_number_total             8772
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301880z_si_002_3.cif
_cod_data_source_block           2c
_cod_database_code               4331085