Mono- and dinuclear palladium(ii) complexes containing both N-heterocyclic carbenes and tetrazole ligands as catalysts for Hiyama coupling
Yang, Jin; New J. Chem. 40 (2016) 9739–; doi:10.1039/C6NJ02320G

data_7055787
_publ_section_title
;
 Mono- and dinuclear palladium(ii) complexes containing both
 N-heterocyclic carbenes and tetrazole ligands as catalysts for Hiyama
 coupling
;
_journal_issue                   11
_journal_name_full               'New J. Chem.'
_journal_page_first              9739
_journal_paper_doi               10.1039/C6NJ02320G
_journal_volume                  40
_journal_year                    2016
_chemical_formula_moiety         'C61 H77 Cl3 N8 Pd2'
_chemical_formula_sum            'C61 H77 Cl3 N8 Pd2'
_chemical_formula_weight         1241.46
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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-97
_audit_update_record
;
2016-07-21 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                79.27(2)
_cell_angle_beta                 85.87(2)
_cell_angle_gamma                81.40(2)
_cell_formula_units_Z            2
_cell_length_a                   12.632(16)
_cell_length_b                   15.50(2)
_cell_length_c                   19.61(3)
_cell_measurement_reflns_used    3939
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      23.6311
_cell_measurement_theta_min      2.1162
_cell_volume                     3726(9)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0604
_diffrn_reflns_av_unetI/netI     0.1945
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17714
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.9175
_exptl_absorpt_correction_T_min  0.8643
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_platon_squeeze_details
;
During the refinement, there are very large solvent accessible voids 
in the structure. However, no suitable model for any solvent could be 
found in difference Fourier syntheses. Attempts made to model the solvent 
molecule were not successful.The SQUEEZE option in PLATON (Spek, 2003) 
indicated there was a solvent cavity of volume 806.9 \%A^3^ containing 
approximately 268 electrons, ca. 4 CHCl3 molecules based on the solvents 
and each host molecule was distributed 2 CHCl3 molecules. 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). 
References:
Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13
;
_refine_diff_density_max         1.461
_refine_diff_density_min         -1.167
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         12702
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1633
_refine_ls_R_factor_gt           0.0734
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1359
_reflns_number_gt                5814
_reflns_number_total             12702
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6nj02320g2.cif
_cod_data_source_block           5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/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
/usr/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 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7055783--7055788.cif.
;
_cod_original_cell_volume        3725(8)
_cod_original_sg_symbol_Hall     '-P 1 '
_cod_database_code               7055787