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_4087591
_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         'C29 H30 Cr N2 O3 Pd'
_chemical_formula_sum            'C29 H30 Cr N2 O3 Pd'
_chemical_formula_weight         612.95
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 114.094(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   29.849(3)
_cell_length_b                   12.0939(13)
_cell_length_c                   17.4300(18)
_cell_measurement_reflns_used    4082
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.74
_cell_measurement_theta_min      2.41
_cell_volume                     5743.9(10)
_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-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33204
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.134
_diffrn_reflns_theta_min         1.495
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.035
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6401
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       needle
_exptl_crystal_F_000             2496
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_platon_squeeze_details
;
The residual electron density was assigned to half a molecule of 
the benzene solvent [138/8= 17 e per asymmetric unit; half a
molecule of C6H6 would give 21 e]. 
;
_refine_diff_density_max         1.289
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         6983
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0532P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4036
_reflns_number_total             6983
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00349_si_002.cif
_cod_data_source_block           3c
_cod_original_cell_volume        5743.8(11)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4087591
_shelx_estimated_absorpt_t_min   0.682
_shelx_estimated_absorpt_t_max   0.980
_shelxl_version_number           2013-4
_shelx_res_checksum              33957
_shelx_hkl_checksum              45516