Hemichelation, a Way To Stabilize Electron-Unsaturated Complexes: The Case of T-Shaped Pd and Pt Metallacycles.
Christophe Werlé; Corinne Bailly; Lydia Karmazin-Brelot; Xavier-Frédéric Le Goff; Louis Ricard; Jean-Pierre Djukic; Journal of the American Chemical Society 135 (2013) 17839–17852; doi:10.1021/ja4076327

data_4121195
_publ_contact_author_address
;UMR 7177
Universite de Strasbourg
4 rue Blaise Pascal
67000 Strasbourg
FRANCE
;
_publ_contact_author_email       djukic@unistra.fr
_publ_contact_author_name        'Jean-Pierre DJUKIC'
_publ_contact_author_phone       +33(0)368851523
_publ_section_title
;
 Hemichelation, a Way To Stabilize Electron-Unsaturated Complexes: The
 Case of T-Shaped Pd and Pt Metallacycles.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17839
_journal_page_last               17852
_journal_paper_doi               10.1021/ja4076327
_journal_volume                  135
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C23 H23 Cr N O3 Pd'
_chemical_formula_sum            'C23 H23 Cr N O3 Pd'
_chemical_formula_weight         519.82
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 90.209(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4903(16)
_cell_length_b                   13.664(2)
_cell_length_c                   15.769(3)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.05
_cell_measurement_theta_min      2.50
_cell_volume                     2044.8(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.979
_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  0.0492
_diffrn_reflns_av_sigmaI/netI    0.0681
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19949
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.13
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    1.435
_exptl_absorpt_correction_T_max  0.7822
_exptl_absorpt_correction_T_min  0.7431
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         6.188
_refine_diff_density_min         -4.486
_refine_diff_density_rms         0.304
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.02(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         9381
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0760
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1078P)^2^+27.2880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2075
_refine_ls_wR_factor_ref         0.2118
_reflns_number_gt                8591
_reflns_number_total             9381
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja4076327_si_002_07.cif
_cod_data_source_block           4c_(S)_Strasbourg
_cod_original_cell_volume        2044.9(6)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4121195