Room temperature C-H bond activation on a [PdI-PdI] platform
Henri Doucet; Jitendra K. Bera; Chem.Commun. 49 (2013) 9764–; doi:10.1039/c3cc44493g

data_7109884
_publ_section_title
;
 Room temperature C-H bond activation on a [PdI-PdI] platform
;
_journal_name_full               Chem.Commun.
_journal_page_first              9764
_journal_paper_doi               10.1039/c3cc44493g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C56 H47 N8 O Pd3 S4, 3(BF4), H2O, 2(CH2Cl2)'
_chemical_formula_sum            'C58 H53 B3 Cl4 F12 N8 O2 Pd3 S4'
_chemical_formula_weight         1743.84
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 100.457(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.485(2)
_cell_length_b                   22.628(3)
_cell_length_c                   14.2391(16)
_cell_measurement_reflns_used    6172
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.71
_cell_measurement_theta_min      2.31
_cell_volume                     6173.8(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ortep
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0775
_diffrn_reflns_av_sigmaI/netI    0.0859
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            42227
_diffrn_reflns_theta_full        24.71
_diffrn_reflns_theta_max         24.71
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    1.262
_exptl_absorpt_correction_T_max  0.8046
_exptl_absorpt_correction_T_min  0.7302
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.21
_platon_squeeze_details
;
 PLATON/SQUEEZE estimated the solvent-accessible
 region to contain 395 (198+197) electrons per unit cell. This amounts to 
 nearly 99 electrons per formula unit. The electron densities are 
 tentatively modelled as to two CH2Cl2 and one H2O molecules per formula unit. 
 These solvent and water molecules are included in the formula sum for the 
 calculation of the intensive properties.
;
_refine_diff_density_max         1.992
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     792
_refine_ls_number_reflns         10510
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0952P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1489
_refine_ls_wR_factor_ref         0.1630
_reflns_number_gt                6415
_reflns_number_total             10510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc44493g.txt
_cod_data_source_block           compound_2
_cod_original_cell_volume        6173.7(12)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7109884