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_7043000
_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         'C25 H21 Cr N O3 Pd, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C25.5 H22 Cl Cr N O3 Pd'
_chemical_formula_weight         584.29
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,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
;
2017-03-09 deposited with the CCDC.
2017-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                81.693(3)
_cell_angle_beta                 82.094(3)
_cell_angle_gamma                76.169(3)
_cell_formula_units_Z            4
_cell_length_a                   11.0027(7)
_cell_length_b                   13.4372(7)
_cell_length_c                   16.1063(6)
_cell_measurement_reflns_used    20005
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     2274.8(2)
_computing_cell_refinement       'Denzo (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material
'SHELXL-2013 (Sheldrick, 2013) and PLATON (Spek, 2007)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_unetI/netI     0.1475
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24085
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.443
_diffrn_reflns_theta_min         1.285
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.414
_exptl_absorpt_correction_T_max  0.87667
_exptl_absorpt_correction_T_min  0.65602
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.248
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         10255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.0837
_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^)+(0.0919P)^2^+4.6777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1718
_refine_ls_wR_factor_ref         0.2083
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6358
_reflns_number_total             10255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00872d2.cif
_cod_data_source_block           cis3a_CH2Cl2
_cod_database_code               7043000
_cod_depositor_comments
;

2017-10-27
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C51 H44 Cl2 Cr2 N2 O6 Pd2'
_cod_original_formula_weight         1168.58
_cod_original_formula_moiety         '2(C25 H21 Cr N O3 Pd), C H2 Cl2'
_cod_original_formula_units_Z            2
_shelxl_version_number           2013-4
_shelx_res_checksum              64693