Reactions of (Diphenylphosphinomethyl)zirconocene Chloride with B(C6F5)3: Competition between P/B and P/Zr+Frustrated Lewis Pair Reactions
Xu, Xin; Kehr, Gerald; Daniliuc, Constantin G.; Erker, Gerhard; Organometallics 32 (2013) 7306–; doi:10.1021/om400769y

data_4082084
_publ_section_title
;
 Reactions of (Diphenylphosphinomethyl)zirconocene Chloride with B(C6F5)3:
 Competition between P/B and P/Zr+Frustrated Lewis Pair Reactions
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7306
_journal_paper_doi               10.1021/om400769y
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C49 H29 B Cl3 F15 N O P Zr'
_chemical_formula_weight         1172.08
_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                85.8850(10)
_cell_angle_beta                 83.1480(10)
_cell_angle_gamma                86.2220(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8629(2)
_cell_length_b                   12.9604(3)
_cell_length_c                   14.1655(3)
_cell_measurement_reflns_used    5943
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      4.08
_cell_volume                     2334.67(8)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.041
_diffrn_reflns_av_sigmaI/netI    0.0355
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            22049
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         4.26
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  0.9478
_exptl_absorpt_correction_T_min  0.8414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.760
_refine_diff_density_min         -1.232
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         11220
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+4.9838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1815
_reflns_number_gt                9949
_reflns_number_total             11220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om400769y_si_002.cif
_cod_data_source_block           erk6335
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4082084