Stabilization of an Electron-Unsaturated Pd(I)‒Pd(I) Unit by Double Hemichelation
Werlé, Christophe; Karmazin, Lydia; Bailly, Corinne; Ricard, Louis; Djukic, Jean-Pierre; Organometallics 34 (2015) 3055–; doi:10.1021/acs.organomet.5b00349

data_4087592
_publ_section_title
;
 Stabilization of an Electron-Unsaturated Pd(I)--Pd(I) Unit by Double
 Hemichelation
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              3055
_journal_paper_doi               10.1021/acs.organomet.5b00349
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C24 H18 Cr2 O6 Pd2, 2(C6 D6)'
_chemical_formula_sum            'C36 H18 Cr2 D12 O6 Pd2'
_chemical_formula_weight         887.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.525(1)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.286(1)
_cell_length_b                   11.934(1)
_cell_length_c                   16.148(1)
_cell_measurement_reflns_used    4788
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     1569.9(3)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction        'DENZO & COLLECT'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28039
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         30.057
_diffrn_reflns_theta_min         2.135
_exptl_absorpt_coefficient_mu    1.848
_exptl_absorpt_correction_T_max  1.08437
_exptl_absorpt_correction_T_min  0.951229
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   DENZO/SCALEPACK
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.877
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         4592
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+2.3916P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.0843
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4138
_reflns_number_total             4592
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00349_si_002.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4087592
_shelx_estimated_absorpt_t_min   0.709
_shelx_estimated_absorpt_t_max   0.756
_shelxl_version_number           2013-4
_shelx_res_checksum              33136
_shelx_hkl_checksum              15697