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_4088339
_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_sum            'C60.5 H79 Al Cl N O4 Zr'
_chemical_formula_weight         1037.95
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_cell_angle_alpha                79.2889(10)
_cell_angle_beta                 81.976(9)
_cell_angle_gamma                89.115(12)
_cell_formula_units_Z            4
_cell_length_a                   14.953(7)
_cell_length_b                   19.122(9)
_cell_length_c                   21.4475(10)
_cell_measurement_reflns_used    15157
_cell_measurement_temperature    93
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     5966(4)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0585
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63541
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2204.00
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.880
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         27226
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0500P)^2^+7.2851P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1561
_reflns_number_gt                20154
_reflns_number_total             27226
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            om5b01027_si_002.cif
_cod_data_source_block           10112014Complex3
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C121 H158 Al2 Cl2 N2 O8 Zr2'
_cod_original_formula_weight         2075.90
_cod_original_formula_moiety         'C121 H158 Al2 Cl2 N2 O8 Zr2'
_cod_original_formula_units_Z            2
_cod_database_code               4088339