Reactivity of N-heterocyclic carbene‒pyridine palladacyclopentadiene complexes toward halogen addition. The unpredictable course of the reaction
Visentin, Fabiano; Santo, Claudio; Scattolin, Thomas; Demitri, Nicola; Canovese, Luciano; Dalton Trans.  (2017) –; doi:10.1039/C7DT02162C

data_7043837
_publ_section_title
;
 Reactivity of N-heterocyclic carbene--pyridine palladacyclopentadiene
 complexes toward halogen addition. The unpredictable course of the
 reaction
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02162C
_journal_year                    2017
_chemical_formula_moiety         'C30 H31 I2 N3 O8 Pd, 0.75 (C H2 Cl2)'
_chemical_formula_sum            'C30.75 H32.5 Cl1.5 I2 N3 O8 Pd'
_chemical_formula_weight         985.47
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-06-08 deposited with the CCDC.
2017-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.929(2)
_cell_length_b                   15.041(3)
_cell_length_c                   21.431(4)
_cell_measurement_reflns_used    1140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.419
_cell_measurement_theta_min      1.630
_cell_volume                     3514.3(12)
_computing_cell_refinement       XDS
_computing_data_collection       'Elettra XRD1 Data Collection SW'
_computing_data_reduction        'XDS - CCP4'
_computing_molecular_graphics    'Ortep3 for Windows'
_computing_publication_material  enCIFer/publCIF
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    Sir2011
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type
;
'Huber 4-circles Kappa Goniometer, Pilatus 2M detector'
;
_diffrn_measurement_method       'Rotating crystal'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            52503
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         27.419
_diffrn_reflns_theta_min         1.630
_diffrn_source                   'Elettra Synchrotron - XRD1 BL'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.322
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5728
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2012/1 (Bruker, 2012)'
_exptl_crystal_colour            'Dark Yellow'
_exptl_crystal_density_diffrn    1.863
_exptl_crystal_description       'Thin rod'
_exptl_crystal_F_000             1918
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.352
_refine_diff_density_min         -1.955
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         8252
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+34.0717P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1666
_refine_ls_wR_factor_ref         0.1755
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7003
_reflns_number_total             8252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02162c2.cif
_cod_data_source_block           1solv
_cod_original_formula_sum        'C30.75 H32.50 Cl1.50 I2 N3 O8 Pd'
_cod_database_code               7043837
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.955
_exptl_absorpt_special_details
;
SADABS was used to perform the Absorption correction.
Parameters refinement is based on 70889 reflections.
Ratio of minimum to maximum apparent transmission: 1.303
The given Tmin and Tmax were generated using the SHELX SIZE command
;
_shelx_res_checksum              782