Synthesis and Structural Analysis of Zr‒Al Heterobimetallic Complexes, [ZrX{(O-2,4-tBu2C6H2-6-CH2)3(μ2-O-2,4-tBu2-C6H2-6-CH2)}N][R2Al(μ2-OiPr)] [X = Cl, Et, iBu; R = Me, Et, iBu]. Unique Reactivity of the iBu Complex
Tewasekson, Udomchai; Tsutsumi, Ken; Nomura, Kotohiro; Organometallics 35 (2016) 866–; doi:10.1021/acs.organomet.5b01027

data_4088340
_publ_section_title
;
 Synthesis and Structural Analysis of Zr--Al Heterobimetallic Complexes,
 [ZrX{(O-2,4-tBu2C6H2-6-CH2)3(\m2-O-2,4-tBu2-C6H2-6-CH2)}N][R2Al(\m2-OiPr)]
 [X = Cl, Et, iBu; R = Me, Et, iBu]. Unique Reactivity of the iBu Complex
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              866
_journal_paper_doi               10.1021/acs.organomet.5b01027
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C57 H88 Al N O4 Zr'
_chemical_formula_sum            'C57 H88 Al N O4 Zr'
_chemical_formula_weight         969.53
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.832(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   13.952(4)
_cell_length_b                   14.190(5)
_cell_length_c                   28.992(9)
_cell_measurement_reflns_used    12406
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.10
_cell_volume                     5739(3)
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r15'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r15'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 6.827
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49465
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2088.00
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.300
_refine_diff_density_max         1.470
_refine_diff_density_min         -1.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     562
_refine_ls_number_reflns         13003
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1253P)^2^+2.3543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2077
_reflns_number_gt                10803
_reflns_number_total             13003
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om5b01027_si_002.cif
_cod_data_source_block           18092015_2Complex5
_cod_original_cell_volume        5739(4)
_cod_database_code               4088340