Five-coordinate complexes of palladium(ii) and platinum(ii) with α-diimine and 1,5-cyclooctadiene ligands
Bianca, Francesca Di; Bandoli, Giuliano; Dolmella, Alessandro; Antonaroli, Simonetta; Crociani, Bruno; Journal of the Chemical Society, Dalton Transactions  (2002) 212–; doi:10.1039/b106247f

data_7702690
_publ_section_title
;
 Five-coordinate complexes of palladium(ii) and platinum(ii) with
 \a-diimine and 1,5-cyclooctadiene ligands
;
_journal_issue                   2
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              212
_journal_paper_doi               10.1039/b106247f
_journal_year                    2002
_chemical_formula_sum            'C23 H29 B F4 N2 O Pt'
_chemical_formula_weight         631.38
_chemical_name_common            '[PtMe(COD)(2)]BF4'
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'heavy-atom methods'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.61(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.387(9)
_cell_length_b                   7.940(3)
_cell_length_c                   20.650(8)
_cell_measurement_reflns_used    50
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.6
_cell_measurement_theta_min      7.9
_cell_volume                     4799(3)
_computing_cell_refinement       'P3/P4-PC Ver. 4.27 (Nicolet,1991)'
_computing_data_collection       'P3/P4-PC Ver. 4.27 (Nicolet,1991)'
_computing_data_reduction        'P3/P4-PC Ver. 4.27 (Nicolet,1991)'
_computing_molecular_graphics    'SHELXTL NT Version 5.10 (Sheldrick, 1999)'
_computing_publication_material  'SHELXTL NT Version 5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXTL NT Version 5.10 (Sheldrick, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.830
_diffrn_measured_fraction_theta_max 0.830
_diffrn_measurement_device_type  'Nicolet-Siemens R3m/V'
_diffrn_measurement_method       omega-2theta
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0174
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6384
_diffrn_reflns_theta_full        24.05
_diffrn_reflns_theta_max         24.05
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        3%
_diffrn_standards_interval_count 150
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.896
_exptl_absorpt_correction_T_max  0.704
_exptl_absorpt_correction_T_min  0.216
_exptl_absorpt_correction_type   'psi-scan method'
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipeds
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.185
_refine_diff_density_min         -1.963
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       0.00027(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         6224
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0609
_refine_ls_R_factor_gt           0.0505
_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^)+(0.1630P)^2^+22.2574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1304
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                5351
_reflns_number_total             6224
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b106247f.txt
_cod_data_source_block           rom1
_cod_original_cell_volume        4798(3)
_cod_original_sg_symbol_H-M      'P2(1)/c (No. 14)'
_cod_database_code               7702690