Electrophilic fluorination of cationic Pt-aryl complexes
Shubin Zhao; Rui-Yao Wang; Ha Nguyen; Jennifer J. Becker; Michel R. Gagne; Chem.Commun. 48 (2012) 443–; doi:10.1039/c1cc15006e

data_7107157
_publ_section_title
;
 Electrophilic fluorination of cationic Pt-aryl complexes
;
_journal_name_full               Chem.Commun.
_journal_page_first              443
_journal_paper_doi               10.1039/c1cc15006e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C48 H46.75 B F9.5 N O1.38 P3.5 Pt'
_chemical_formula_weight         1154.41
_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                95.002(1)
_cell_angle_beta                 113.180(1)
_cell_angle_gamma                96.172(1)
_cell_formula_units_Z            4
_cell_length_a                   13.666(1)
_cell_length_b                   17.484(2)
_cell_length_c                   22.340(2)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.24
_cell_volume                     4829.3(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            18829
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.096
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2295
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered
BF4-, PF6-, F and lattice water molecules, which were ultimately
modeled through the
use of the SQUEEZE subroutine of the PLATON software suite. PLATON
Reference: P. v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194.
One accessible void per lattice were found, comprising a
total volume of 1249 A3 and contributing a total of 423 electrons.
The void was assigned to four BF4-, two PF6-, ten F- and 5.5 water molecules,
which contribute 4 x 41 + 2 x 52 + 10 x 10 + 5.5 x 10 = 423 electrons,
and occupy about 1000 A3 in space.
The larger volume of the void may be a result of the disorder. The
contributions have been included in all derived crystal quantities.
;
_refine_diff_density_max         1.756
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         18829
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0841
_refine_ls_wR_factor_ref         0.0876
_reflns_number_gt                14551
_reflns_number_total             18829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15006e.txt
_cod_data_source_block           zsnew2c
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C48 H46.75 B F9.50 N O1.38 P3.50 Pt'
_cod_database_code               7107157