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_4331083
_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
;      
'C26 H62 N8 Si Zr2,2(C32 H12 B1 F24),C6 H12,C6 H4 F2'
;
_chemical_formula_sum            'C102 H102 B2 F50 N8 Si Zr2'
_chemical_formula_weight         2622.07
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.717(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.6582(17)
_cell_length_b                   18.4059(13)
_cell_length_c                   25.2129(18)
_cell_measurement_reflns_used    7046
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.44
_cell_measurement_theta_min      2.21
_cell_volume                     10959.4(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0997
_diffrn_reflns_av_sigmaI/netI    0.1046
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            132363
_diffrn_reflns_theta_full        26.43
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         0.86
_exptl_absorpt_coefficient_mu    0.337
_exptl_absorpt_correction_T_max  0.9512
_exptl_absorpt_correction_T_min  0.8998
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_description       prism
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.356
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1598
_refine_ls_number_reflns         22449
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0730
_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^)+(0.1155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1972
_refine_ls_wR_factor_ref         0.2297
_reflns_number_gt                13335
_reflns_number_total             22449
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301880z_si_002_1.cif
_cod_data_source_block           4b
_cod_database_code               4331083