Trans-Cis C-Pd-C Rearrangement in Hemichelates
Werlé, C; DOHM, Sebastian; Bailly, Corinne; Karmazin, Lydia; Ricard, Louis; Sieffert, Nicolas; pfeffer, michel; Hansen, Andreas; Grimme, Stefan; Djukic, Jean-Pierre; Dalton Trans.  (2017) –; doi:10.1039/C7DT00872D

data_7042999
_publ_section_title
;
 Trans-Cis C-Pd-C Rearrangement in Hemichelates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00872D
_journal_year                    2017
_chemical_formula_moiety         'C33 H30 Cr N2 O3 Pd, C H2 Cl2'
_chemical_formula_sum            'C34 H32 Cl2 Cr N2 O3 Pd'
_chemical_formula_weight         745.91
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Hygroscopic,Heat-sensitive,Oxygen-sensitive,Light-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-02-14 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                92.884(2)
_cell_angle_beta                 106.314(2)
_cell_angle_gamma                111.707(2)
_cell_formula_units_Z            2
_cell_length_a                   10.4931(3)
_cell_length_b                   11.8295(3)
_cell_length_c                   13.8875(3)
_cell_measurement_reflns_used    2099
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.63
_cell_measurement_theta_min      4.08
_cell_volume                     1513.94(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0729
_diffrn_reflns_Laue_measured_fraction_full 0.941
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10878
_diffrn_reflns_point_group_measured_fraction_full 0.941
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         66.621
_diffrn_reflns_theta_min         3.367
_diffrn_source                   'Cu-ImuS microfocus tube'
_exptl_absorpt_coefficient_mu    9.685
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5638
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.636
_exptl_crystal_description       plate
_exptl_crystal_F_000             756
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.830
_refine_diff_density_min         -1.056
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0460
_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^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3960
_reflns_number_total             5156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00872d2.cif
_cod_data_source_block           trans-3d
_cod_database_code               7042999
_shelx_estimated_absorpt_t_min   0.444
_shelx_estimated_absorpt_t_max   0.830
_shelxl_version_number           2013-4
_shelx_res_checksum              127