Reaction of five-membered zirconacycloallenoids with the strong Lewis acid B(C6F5)3.
Bender, Georg; Daniliuc, Constantin G.; Wibbeling, Birgit; Kehr, Gerald; Erker, Gerhard; Dalton transactions (Cambridge, England : 2003) 43 (2014) 12210–12213; doi:10.1039/c4dt01137f

data_7031423
_publ_section_title
;
 Reaction of five-membered zirconacycloallenoids with the strong Lewis
 acid B(C6F5)3.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12210
_journal_page_last               12213
_journal_paper_doi               10.1039/c4dt01137f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C37 H24 B F15 Zr'
_chemical_formula_weight         855.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.9730(10)
_cell_angle_beta                 90.0900(10)
_cell_angle_gamma                97.935(2)
_cell_formula_units_Z            2
_cell_length_a                   8.3106(2)
_cell_length_b                   12.2167(3)
_cell_length_c                   17.4089(4)
_cell_measurement_reflns_used    3901
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     1663.31(7)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP (BrukerAXS, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius KappaCCD APEXII'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Montel mirror'
_diffrn_radiation_source         'rotating anode Nonius Fr591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15086
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.10
_exptl_absorpt_coefficient_mu    0.444
_exptl_absorpt_correction_T_max  0.9956
_exptl_absorpt_correction_T_min  0.9570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.708
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         5742
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0000P)^2^+5.7443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1094
_refine_ls_wR_factor_ref         0.1212
_reflns_number_gt                4793
_reflns_number_total             5742
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01137f7.cif
_cod_data_source_block           erk6937
_cod_depositor_comments
'Adding full bibliography for 7031423--7031424.cif.'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031423