Formation of unsaturated vicinal zr(+)/p frustrated lewis pairs by the unique 1,1-carbozirconation reactions.
Xu, Xin; Kehr, Gerald; Daniliuc, Constantin G.; Erker, Gerhard; Journal of the American Chemical Society 136 (2014) 12431–12443; doi:10.1021/ja5068146

data_4122483
_publ_section_title
;
 Formation of unsaturated vicinal zr(+)/p frustrated lewis pairs by the
 unique 1,1-carbozirconation reactions.
;
_journal_issue                   35
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12431
_journal_page_last               12443
_journal_paper_doi               10.1021/ja5068146
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C69.5 H66 B F20 N P Si Zr'
_chemical_formula_weight         1456.32
_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                98.7520(10)
_cell_angle_beta                 93.2670(10)
_cell_angle_gamma                103.8870(10)
_cell_formula_units_Z            4
_cell_length_a                   11.55690(10)
_cell_length_b                   21.2895(4)
_cell_length_c                   29.9729(4)
_cell_measurement_reflns_used    30284
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     7041.96(18)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.052
_diffrn_reflns_av_sigmaI/netI    0.0411
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            100549
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.9885
_exptl_absorpt_correction_T_min  0.8810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.374
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1732
_refine_ls_number_reflns         24596
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0508
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0651P)^2^+6.3070P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1414
_reflns_number_gt                19784
_reflns_number_total             24596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5068146_si_002.cif
_cod_data_source_block           erk7298
_cod_depositor_comments
'Adding full bibliography for 4122478--4122491.cif.'
_cod_original_cell_volume        7041.96(17)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C69.50 H66 B F20 N P Si Zr'
_cod_database_code               4122483