A new library of arsine, stibine-stabilized N-heterocyclic carbene palladium complexes: synthesis, structures and activities in C-C and C-N coupling reactions.
Yang, Jin; Li, Pinhua; Zhang, Yicheng; Wang, Lei; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14114–14122; doi:10.1039/c4dt01773k

data_7032419
_publ_section_title
;
 A new library of arsine, stibine-stabilized N-heterocyclic carbene
 palladium complexes: synthesis, structures and activities in C-C and C-N
 coupling reactions.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14114
_journal_page_last               14122
_journal_paper_doi               10.1039/c4dt01773k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C45 H53 As Cl2 N2 Pd 0.5(CH2Cl2)'
_chemical_formula_sum            'C45.5 H54 As Cl3 N2 Pd'
_chemical_formula_weight         916.58
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.220(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.684(4)
_cell_length_b                   12.179(5)
_cell_length_c                   35.633(13)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.0524
_cell_measurement_theta_min      2.3971
_cell_volume                     4629(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0300
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            22942
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    1.314
_exptl_absorpt_correction_T_max  0.8074
_exptl_absorpt_correction_T_min  0.7520
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1884
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
During the refinement, the CH2Cl2 molecule is
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 605.5\%A^3^ volumes
in the unit cell (approximately 98 electrons,
i.e. ca. 2 CH2Cl2 molecules based on the solvents
we have used and each host molecule was
distributed 0.5 CH2Cl2 molecule). So the suitable formula
should be C~45~H~53~As~1~Cl~2~N~2~Pd~1~.(CH2Cl2)~0.5~. Some related items
have been corrected in the cif file.
;
_refine_diff_density_max         0.458
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0218P)^2^+4.4483P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0730
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                7035
_reflns_number_total             8110
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7032044
_cod_data_source_file            c4dt01773k2.cif
_cod_data_source_block           2c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_Hall     '-P 2ybn'
_cod_original_sg_symbol_H-M      P21/n
_cod_original_formula_sum        'C45.50 H54 As Cl3 N2 Pd'
_cod_database_code               7032419