Reactivity of B(C6F5)3with Simple Early Transition Metal Alkoxides: Alkoxide-Aryl Exchange, THF Ring-Opening, or Acetonitrile CC Coupling
Lorber, Christian; Choukroun, Robert; Vendier, Laure; Organometallics 27 (2008) 5017–; doi:10.1021/om800234z

data_4071565
_publ_section_title
;
 Reactivity of B(C6F5)3with Simple Early Transition Metal Alkoxides:
 Alkoxide-Aryl Exchange, THF Ring-Opening, or Acetonitrile CC Coupling
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5017
_journal_paper_doi               10.1021/om800234z
_journal_volume                  27
_journal_year                    2008
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H72 O8 Zr2, C2 H3 N'
_chemical_formula_sum            'C34 H75 N O8 Zr2'
_chemical_formula_weight         808.39
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.1407(5)
_cell_length_b                   19.1840(6)
_cell_length_c                   26.3148(8)
_cell_measurement_reflns_used    29000
_cell_measurement_temperature    160
_cell_measurement_theta_max      32.071
_cell_measurement_theta_min      2.5476
_cell_measurement_wavelength     0.71073
_cell_volume                     8653.0(5)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180
_diffrn_detector_area_resol_mean 8.2632
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Oxford-Diffraction XCALIBUR'
_diffrn_measurement_method       \w-\f
_diffrn_orient_matrix_UB_11      -0.0176634161
_diffrn_orient_matrix_UB_12      -0.0216085483
_diffrn_orient_matrix_UB_13      -0.0186238304
_diffrn_orient_matrix_UB_21      -0.0198949955
_diffrn_orient_matrix_UB_22      0.0292597358
_diffrn_orient_matrix_UB_23      -0.0101235077
_diffrn_orient_matrix_UB_31      0.0317387822
_diffrn_orient_matrix_UB_32      0.0063537052
_diffrn_orient_matrix_UB_33      -0.01668125
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            74061
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.523
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
        (compiled Aug 28 2006,13:05:05)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.918
_refine_diff_density_min         -0.63
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.162
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         10703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.1272
_reflns_number_gt                6953
_reflns_number_total             10703
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om800234z_si_002.cif
_cod_data_source_block           (6)
_cod_database_code               4071565