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_7107156
_publ_section_title
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 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            'C49 H48 B F5 N O2 P3 Pt'
_chemical_formula_weight         1076.69
_chemical_name_systematic
;

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;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 116.680(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.7695(19)
_cell_length_b                   10.0332(6)
_cell_length_c                   33.988(3)
_cell_measurement_reflns_used    8080
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.22
_cell_measurement_theta_min      2.36
_cell_volume                     9680.2(12)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            18908
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.056
_exptl_absorpt_correction_T_max  0.7921
_exptl_absorpt_correction_T_min  0.5155
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4304
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
Difference electron density maps revealed the presence of disordered
solvate molecules, acetonitrile and water, 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.
Four solvent accessible void per lattice were found. Each comprises a
total volume of 533 A3 and contributing a total of 53 electrons.
The void was thus assigned to one acetonitrile and four water, which
contribute 22 + 4x8 = 54 electrons, and ocuppy about 140 A3 in space.
The larger volume of the void may be a result of the severely disorder
of the water molecules. The contributions have been included in all derived
crystal quantities although the precise composition of the lattice solvate
is somewhat speculative.
;
_refine_diff_density_max         0.915
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9401
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0310P)^2^+15.6600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0707
_reflns_number_gt                8159
_reflns_number_total             9401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc15006e.txt
_cod_data_source_block           zsnew01a
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7107156