Synthesis of (NHC)Pd(salicylaldimine)Cl complexes through template-directed ortho-aromatic metaloxylation of NHC-palladacycles derived from arylimines.
Yang, Jin; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5003–5007; doi:10.1039/c7dt00007c

data_7042493
_publ_section_title
;
 Synthesis of (NHC)Pd(salicylaldimine)Cl complexes through
 template-directed ortho-aromatic metaloxylation of NHC-palladacycles
 derived from arylimines.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5003
_journal_page_last               5007
_journal_paper_doi               10.1039/c7dt00007c
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C40 H46 Cl N3 Pd'
_chemical_formula_sum            'C40 H46 Cl N3 Pd'
_chemical_formula_weight         710.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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-97
_audit_update_record
;
2016-12-30 deposited with the CCDC.
2017-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.854(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.381(10)
_cell_length_b                   14.070(9)
_cell_length_c                   17.588(11)
_cell_measurement_reflns_used    7282
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.9098
_cell_measurement_theta_min      2.1910
_cell_volume                     4045(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART APEX II'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\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  0.0472
_diffrn_reflns_av_unetI/netI     0.0579
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17439
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_T_max  0.9217
_exptl_absorpt_correction_T_min  0.8788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.167
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
During the refinement, the chloroform molecules are
seriously disordered. During the final refinement,
the contribution of the solvent molecules to the crystal
structure is treated by using the Platon/SQUEEZE procedure.
Check using platon shows that there are 699.5\%A^3^ volumes
in the unit cell (approximately 216 electrons,i.e. 
ca. 3.5 chloroform molecules based on the solvents
we have used. In the final cycles of refinement, this 
contribution to the electron density was removed from 
the observed data. The density, the F(000) value, the 
molecular weight and the formula are given without taking 
into account the results obtained with the SQUEEZE option 
PLATON (Spek, 2003). Similar treatments of disordered solvent 
molecules were carried out by St\"ahler et al. (2001).
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
St\"ahler, R., N\"ather, C. & Bensch, W. (2001). Acta Cryst.
C57, 26-27.
;
_refine_diff_density_max         1.270
_refine_diff_density_min         -0.885
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         6878
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1597
_refine_ls_wR_factor_ref         0.1755
_reflns_number_gt                5367
_reflns_number_total             6878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt00007c2.cif
_cod_data_source_block           1b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7042488--7042495.cif.
;
_cod_original_cell_volume        4045(5)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7042493